CN108690377A - A kind of pearlescent pigment and preparation method thereof with thousand pure gold effects - Google Patents
A kind of pearlescent pigment and preparation method thereof with thousand pure gold effects Download PDFInfo
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- CN108690377A CN108690377A CN201810432011.5A CN201810432011A CN108690377A CN 108690377 A CN108690377 A CN 108690377A CN 201810432011 A CN201810432011 A CN 201810432011A CN 108690377 A CN108690377 A CN 108690377A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 65
- 239000000049 pigment Substances 0.000 title claims abstract description 45
- 230000000694 effects Effects 0.000 title claims abstract description 41
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000010931 gold Substances 0.000 title claims abstract description 37
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 168
- 239000002131 composite material Substances 0.000 claims abstract description 94
- 238000002156 mixing Methods 0.000 claims abstract description 84
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 50
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 49
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical group Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 39
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 28
- 238000012805 post-processing Methods 0.000 claims abstract description 28
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000005538 encapsulation Methods 0.000 claims abstract description 26
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 25
- 239000011592 zinc chloride Substances 0.000 claims abstract description 25
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 25
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical group C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 21
- 239000001119 stannous chloride Substances 0.000 claims abstract description 21
- 235000011150 stannous chloride Nutrition 0.000 claims abstract description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 18
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 17
- 235000014121 butter Nutrition 0.000 claims abstract description 17
- 235000011147 magnesium chloride Nutrition 0.000 claims abstract description 17
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 10
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 127
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 118
- 239000007788 liquid Substances 0.000 claims description 88
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 64
- 239000011521 glass Substances 0.000 claims description 50
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 42
- 239000010445 mica Substances 0.000 claims description 40
- 229910052618 mica group Inorganic materials 0.000 claims description 40
- 239000008367 deionised water Substances 0.000 claims description 36
- 229910021641 deionized water Inorganic materials 0.000 claims description 36
- 239000007864 aqueous solution Substances 0.000 claims description 33
- 239000000243 solution Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 20
- 230000015572 biosynthetic process Effects 0.000 claims description 17
- 238000003786 synthesis reaction Methods 0.000 claims description 17
- 239000011259 mixed solution Substances 0.000 claims description 15
- 238000003828 vacuum filtration Methods 0.000 claims description 14
- 238000012423 maintenance Methods 0.000 claims description 11
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 claims description 8
- 239000013049 sediment Substances 0.000 claims description 8
- 238000004062 sedimentation Methods 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- 239000002699 waste material Substances 0.000 claims description 8
- 239000004115 Sodium Silicate Substances 0.000 claims description 7
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 7
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 6
- 235000013399 edible fruits Nutrition 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000006185 dispersion Substances 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
- 238000005660 chlorination reaction Methods 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 238000002242 deionisation method Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- RJDOZRNNYVAULJ-UHFFFAOYSA-L [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] RJDOZRNNYVAULJ-UHFFFAOYSA-L 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Cosmetics (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a kind of pearlescent pigments and preparation method thereof with thousand pure gold effects,It is described that a kind of to have the pearlescent pigment of thousand pure gold effects include base material,The first composite layer is coated successively outside the base material,Second composite layer,Third composite layer,4th composite layer and the 5th composite layer,First composite layer is stannous chloride,Magnesium chloride,Zinc chloride mixing is constituted,Second composite layer is titanium tetrachloride,Nickel chloride and butter of tin mixing are constituted,The third composite layer is that titanium tetrachloride mixes composition with ferric trichloride,4th composite layer is that silica or aluminium oxide are constituted,5th composite layer is that titanium tetrachloride mixes composition with ferric trichloride,The preparation method includes the surface preparation of base material,The Hydrolyze method encapsulation steps and post-processing steps of base material,The product gloss made is bright-coloured,Golden purity is high,Good brightness,Good weatherability,Good dispersion,It is of low cost,Simple production process,It is easy to operate.
Description
Technical field
The present invention relates to a kind of pearlescent pigments, and in particular to a kind of pearlescent pigment with thousand pure gold effects and its preparation side
Method.
Background technology
Pearlescent pigment is made of several metal thin oxide layer cladding mica.Change thin layer of metal oxide, energy
Different pearl effects is generated, publication number CN102127321A discloses a kind of golden yellow pearly-lustre face of high color density and high brightness
The preparation method of material, it is that using the method hydrolyzed, multilayer coating structure iron and titanyl compound are thin successively using synthetic mica as base material
Film, the thickness by accurately controlling sull reaches required different form and aspect, then the good mica base material of coating is passed through
Set temperature calcining makes the crystal form of film be dehydrated conversion, to reach the film interference effect being pre-designed, made from such method
The golden yellow pearlescent pigment of high color density and high brightness also has a certain distance compared with the color of thousand pure golds, and brightness is inadequate,
Cannot meet the needs of making Jewelry product manufacturer;Publication number CN100560658C discloses the golden pearlescent pigment of superpower interference
Production technology, it is using mica as base material, splitting is coated four layers of metal, nonmetal oxide is made with 24K gold effect
The golden pearlescent pigment of fruit, but there is no being pre-processed to mica base material before making, cost of manufacture is higher, produces
For the product come there is also a certain distance compared with the color of thousand pure golds, brightness is poor, cannot meet the need of ornaments manufacturer
It asks, our company goes out a kind of pearlescent pigment and preparation method thereof with thousand pure gold effects for the demand behaviors of ornaments manufacturer.
Invention content
The present invention is directed to the deficiency in background technology, provides that a kind of production method is simple, production cost is low has thousand
The pearlescent pigment and preparation method thereof of pure gold effect, the pearlescent pigment glossiness prepared using this preparation method is good, color
It is beautiful, purity is high.
Technical scheme of the present invention:
A kind of pearlescent pigment with thousand pure gold effects, including base material, it is characterised in that:The base material is natural mica, synthesis
Mica or glass flake, the base material coat the first composite layer, the second composite layer, third composite layer, the 4th composite layer successively outside
With the 5th composite layer, first composite layer is stannous chloride, magnesium chloride, zinc chloride mixing composition, and second composite layer is
Titanium tetrachloride, nickel chloride and butter of tin mixing are constituted, and the third composite layer is that titanium tetrachloride mixes composition with ferric trichloride,
4th composite layer is that silica or aluminium oxide are constituted, and the 5th composite layer is titanium tetrachloride and ferric trichloride mixing structure
At.
The thickness of the base material is 50nm-3000nm, and grain size is 2-1000 μm.
The preferred 60nm-2000nm of thickness of the base material, preferred 5-900 μm of grain size.
A kind of pearlescent pigment preparation method with thousand pure gold effects, it is characterised in that:The preparation method includes base material
Surface preparation, base material Hydrolyze method encapsulation steps and post-processing steps, the surface preparation of the base material includes:First
Step adds deionized water, input natural mica, artificial mica synthesis or glass flake to adjust solid-to-liquid ratio in one liter of glass beaker
1:5~8, later open stirring, then with 20% technical hydrochloric acid tune PH=0.8~1.0, then be put on electric furnace and heat, when warm in beaker
It when degree is raised to 90 DEG C ± 2 DEG C, carries out constant temperature and stirs 40-70 minutes, burning cup temperature is waited to be cooled to 60 DEG C hereinafter, stopping stirring later
It mixes, feeding, is filtered by vacuum, is washed with deionized to neutrality;Material obtained in the first step is put into one liter of glass by second step
In beaker, add deionized water, adjusts solid-to-liquid ratio 1:5~8, later open stirring, then with 20% liquid caustic soda tune PH=9.5~10.0 then
It is put on electric furnace and heats, when burning cup temperature is raised to 90 DEG C ± 2 DEG C, then carry out constant temperature stirring 40~70 minutes, beakers were waited later
Interior temperature is cooled to 60 DEG C hereinafter, stopping stirring, and feeding, vacuum filtration is washed with deionized to neutrality;Third walks, by the
Material obtained is put into two liters of glass beakers in two steps, deionized water is added, and adjust solid-to-liquid ratio 1:15~20, it opens later
Stirring after stirring 60-90 minutes, stops stirring, standing sedimentation 8~12 hours, unprecipitated suspension is then discharged into waste liquid
Pond, the sediment are by surface-treated base material;The Hydrolyze method encapsulation steps of the base material include the first step, one
It rises in glass beaker, 500 milliliters of deionized water is added, choose the base material after surface preparation third step completes, adjust solid
Liquor ratio 1:10~15, it is then turned on stirring, is heated later with water-bath, when temperature rises to 55~60 DEG C, with 20% aqueous hydrochloric acid solution tune
PH=1.3~1.5, after, it is stirred again, mixing time is 5-10 minutes, and second step adds under constant temperature stirring
Enter 3-7 milliliters of 10% potassium chlorate solution, singly flows stannous chloride, magnesium chloride and the zinc chloride mixed solution of dropwise addition 10%, institute again later
It is 30 to state proportions in stannous chloride, magnesium chloride and zinc chloride mixed solution:1:1, after charging, stir 5-10 minutes,
Again with 10% liquid caustic soda solution tune PH=1.8~2.0, and water-bath pot temperature is risen into T=78 DEG C ± 2 DEG C, third step keeps water-bath pot temperature
Degree is under the state of T=78 DEG C ± 2 DEG C, and cocurrent is added dropwise to 60-80 milliliters of 2M titanium tetrachlorides, 10% Nickel dichloride hexahydrate aqueous solution 1-3
The mixed liquor of 3-10 milliliters of milliliter and 10% butter of tin, then with 20% liquid caustic soda maintenance PH=1.8~2.0, charging while, carries out
Stirring, speed of agitator rise with liquid level and are accordingly promoted, and when base material yellow phase slightly biased in silvery white, then stop feeding, stir again later
It mixes 5-10 minutes, the 4th step, steady temperature is T=78 DEG C ± 2 DEG C, and 100-150 milliliters of titanium tetrachloride and ferric trichloride is added dropwise in cocurrent
20-40 milliliters of mixed liquor maintains PH=1.8 with 20% liquid caustic soda~2.0, when the form and aspect of base material are between bluish-green, stop plus
Material, is stirred for 10-20 minutes, the 5th step later, rises 85 DEG C of temperature, and it is 260-380 revs/min to adjust mixing speed later, then is used
20% sodium hydrate aqueous solution tune PH=9.0-9.5, after, it stirs 5-10 minutes, the 6th step, is 85 DEG C of shape keeping temperature
Under state, 10-20 milliliter of 10% 9 sodium silicate aqueous solution or 10% alchlor aqueous solution is added dropwise in cocurrent, with 20% hydrochloric acid maintenance PH=
9.0-9.5 is constant, and then stirring 5-10 minute, and the 7th step adjusts 78-80 DEG C of temperature, adjust mixing speed be 210-310 turn/
Minute, then 20% hydrochloric acid tune PH=1.8-2.2 is used, 5- 10 minutes is stirred later, and the 8th step maintains 78-80 DEG C of temperature, cocurrent to drip
The mixed liquor for adding 10-30 milliliters of 20-70 milliliters of titanium tetrachloride and ferric trichloride, PH=1.8- is maintained with 10% sodium hydrate aqueous solution
2.2, speed of agitator with liquid level rise and accordingly carry rotating speed, when base material form and aspect in golden red stop charging, be stirred for 5- later
10 minutes;The post-processing steps include the first step, and the base material of the 8th step in Hydrolyze method encapsulation steps, taking-up is taken out through vacuum
Then filter is added deionized water and washs pH value to neutrality, second step, the base material that the first step in post-processing steps is handled
Be put into drying machine 3 hours dry, use 720-760 DEG C again later and calcine 20 minutes, after obtain a kind of there is thousand pure golds effect
The pearlescent pigment of fruit.
The weight of natural mica, artificial mica synthesis or glass flake is put into the surface preparation first step of the base material
Amount is 30-100 grams, and stirring is opened in the surface preparation first step of the base material, and mixing speed is 150-200 revs/min.
Stirring, mixing speed 150 are opened in the surface preparation second step of the base material~It is 200 revs/min, described
Stirring is opened in the surface preparation third step of base material, mixing speed is that mixing speed is 260-360 revs/min.
The first step in the Hydrolyze method encapsulation steps of the base material chooses the base material after surface preparation third step completes
Weight is 25-45 grams.
Unlatching stirring in the Hydrolyze method encapsulation steps first step of the base material, mixing speed are 150-240 revs/min.
The temperature of drying machine is 105 DEG C in the post-processing steps second step.
Beneficial effects of the present invention:
The present invention in advance handles the surface of base material, then uses compared with traditional fabrication golden yellow pearlescent pigment method
Hydrolyze method is coated, and carries out post-processing again later, and obtained product gloss is bright-coloured, golden purity height, good brightness, weather-proof
It is the good, good dispersion of property, of low cost, simple production process, easy to operate.
Description of the drawings
Fig. 1 is the structural diagram of the present invention;
Fig. 2 is the flow chart of preparation method of the present invention.
In figure:1, base material, the 2, first composite layer, the 3, second composite layer, 4, third composite layer, the 5, the 4th composite layer, 6,
Five composite layers.
Specific implementation mode
Embodiment 1
The invention discloses a kind of pearlescent pigment with thousand pure gold effects, including base material, the base material is natural mica, synthesis
Mica or glass flake, the base material coat the first composite layer, the second composite layer, third composite layer, the 4th composite layer successively outside
With the 5th composite layer, first composite layer is stannous chloride, magnesium chloride, zinc chloride mixing composition, and second composite layer is
Titanium tetrachloride, nickel chloride and butter of tin mixing are constituted, and the third composite layer is that titanium tetrachloride mixes composition with ferric trichloride,
4th composite layer is that silica or aluminium oxide are constituted, and the 5th composite layer is titanium tetrachloride and ferric trichloride mixing structure
At the thickness of the base material is 50nm-3000nm, and grain size is 2-1000 μm, a kind of pearlescent pigment system with thousand pure gold effects
Preparation Method, the preparation method include the surface preparation of base material, the Hydrolyze method encapsulation steps of base material and post-processing steps, institute
The surface preparation for stating base material includes:The first step adds deionized water in one liter of glass beaker, puts into 10-60 microns of 30-100
Gram natural mica, artificial mica synthesis or glass flake adjust solid-to-liquid ratio 1:5~8, stirring, mixing speed 150- are opened later
200 revs/min, then with 20% technical hydrochloric acid tune PH=0.8~1.0, then be put on electric furnace and heat, it is raised to when burning cup temperature
It at 90 DEG C ± 2 DEG C, carries out constant temperature and stirs 40-70 minutes, burning cup temperature is waited to be cooled to 60 DEG C hereinafter, stopping stirring, takes later
Material, vacuum filtration, is washed with deionized to neutrality;Material obtained in the first step is put into one liter of glass beaker by second step
In, add deionized water, adjusts solid-to-liquid ratio 1:5~8, stirring, mixing speed 150 are opened later~200 revs/min, then with 20%
Liquid caustic soda tune PH=9.5~10.0, then be put on electric furnace and heat, when burning cup temperature is raised to 90 DEG C ± 2 DEG C, then carries out constant temperature and stir
Mix 40~70 minutes, cup temperature of burning equal later was cooled to 60 DEG C hereinafter, stopping stirring, and feeding, vacuum filtration uses deionized water
It washs to neutrality;Third walks, and material obtained in second step is put into two liters of glass beakers, deionized water is added, and adjust
Solid-to-liquid ratio 1:15~20, stirring is opened later, mixing speed is 260-360 revs/min, after stirring 60-90 minutes, stops stirring,
Standing sedimentation 8~12 hours, unprecipitated suspension is then discharged into waste liquid pool, the sediment is by surface-treated
Base material;The Hydrolyze method encapsulation steps of the base material include the first step, and in one liter of glass beaker, 500 milli of deionized water is added
It rises, chooses 25-45 grams of base material after surface preparation third step completes, adjust solid-to-liquid ratio 1:10~15, it is then turned on and stirs
It mixes, mixing speed is 150-240 revs/min, is heated later with water-bath, when temperature rises to 55~It is 60 DEG C, water-soluble with 20% hydrochloric acid
Liquid tune PH=1.3~1.5, after, it is stirred again, mixing time is 5-10 minutes, second step, in constant temperature stirring
Lower 3-7 milliliters of 10% potassium chlorate solution of addition, the stannous chloride, magnesium chloride of single stream dropwise addition 10% and zinc chloride mixing are molten again later
32 milliliters of liquid, proportions are 30 in the stannous chloride, magnesium chloride and zinc chloride mixed solution:1:1, after charging, stir
It mixes 5-10 minutes, then with 10% liquid caustic soda solution tune PH=1.8~2.0, and water-bath pot temperature is risen into T=78 DEG C ± 2 DEG C, third step,
It is under the state of T=78 DEG C ± 2 DEG C to keep water-bath pot temperature, and cocurrent is added dropwise to 60-80 milliliters of 2M titanium tetrachlorides, 10% 6 chloride hydrate
The mixed liquor of 3-10 milliliters of 1-3 milliliters of nickel aqueous solution and 10% butter of tin, then maintain PH=1.8 with 20% liquid caustic soda~2.0, charging
While be stirred, speed of agitator rises with liquid level and is accordingly promoted, when base material yellow phase slightly biased in silvery white, then stop plus
Material, is stirred for 5-10 minutes, the 4th step later, and steady temperature is T=78 DEG C ± 2 DEG C, and titanium tetrachloride 100-150 millis are added dropwise in cocurrent
The mixed liquor with 20-40 milliliters of ferric trichloride is risen, with 20% liquid caustic soda maintenance PH=1.8~2.0, when base material form and aspect to it is bluish-green it
Between when, stop charging, be stirred for later 10-20 minute, the 5th step, rise 85 DEG C of temperature, later adjust mixing speed be 260-380
Rev/min, then with 20% sodium hydrate aqueous solution tune PH=9.0-9.5, after, it stirs 5-10 minute, the 6th step, is keeping warm
In the state that degree is 85 DEG C, 10-20 milliliters of 10% 9 sodium silicate aqueous solution is added dropwise in cocurrent, maintains PH=9.0-9.5 permanent with 20% hydrochloric acid
It is fixed, and then stir 5-10 minutes, the 7th step, 78-80 DEG C of temperature is adjusted, it is 210-310 revs/min to adjust mixing speed, then is used
20% hydrochloric acid tune PH=1.8-2.2, stirs 5- 10 minutes later, and the 8th step maintains 78-80 DEG C of temperature, cocurrent that four chlorinations are added dropwise
The mixed liquor of 10-30 milliliters of 20-70 milliliters of titanium and ferric trichloride, PH=1.8-2.2, stirring are maintained with 10% sodium hydrate aqueous solution
Rotating speed with liquid level rise and accordingly carry rotating speed, when base material form and aspect in golden red stop charging, be stirred for later 5-10 minutes;Institute
It includes the first step to state post-processing steps, and the base material of the 8th step in Hydrolyze method encapsulation steps takes out through vacuum filtration, is then added
Deionized water washs pH value to neutrality, and the base material that the first step in post-processing steps is handled is put into drying machine by second step
Middle drying 3 hours, the temperature of drying machine are 105 DEG C, use 720-760 DEG C again later and calcine 20 minutes, after obtain a kind of tool
There is the pearlescent pigment of thousand pure gold effects.
Embodiment 2
The invention discloses a kind of pearlescent pigment with thousand pure gold effects, including base material, the base material is natural mica, synthesis
Mica or glass flake, the base material coat the first composite layer, the second composite layer, third composite layer, the 4th composite layer successively outside
With the 5th composite layer, first composite layer is stannous chloride, magnesium chloride, zinc chloride mixing composition, and second composite layer is
Titanium tetrachloride, nickel chloride and butter of tin mixing are constituted, and the third composite layer is that titanium tetrachloride mixes composition with ferric trichloride,
4th composite layer is that silica or aluminium oxide are constituted, and the 5th composite layer is titanium tetrachloride and ferric trichloride mixing structure
At the thickness of the base material is 60nm-2000nm, and grain size is 5-900 μm, a kind of pearlescent pigment preparation with thousand pure gold effects
Method, the preparation method include the surface preparation of base material, the Hydrolyze method encapsulation steps of base material and post-processing steps, described
The surface preparation of base material includes:The first step adds deionized water, 30 grams of days of input 40-160 microns in one liter of glass beaker
Right mica, artificial mica synthesis or glass flake, adjust solid-to-liquid ratio 1:5~8, stirring is opened later, and mixing speed is 150 revs/min
Clock, then with 20% technical hydrochloric acid tune PH=0.8~1.0, then be put on electric furnace and heat, it is raised to 90 DEG C ± 2 DEG C when burning cup temperature
When, constant temperature stirring 40 minutes is carried out, cup temperature of burning equal later is cooled to 60 DEG C hereinafter, stopping stirring, and feeding is filtered by vacuum,
It is washed with deionized to neutrality;Material obtained in the first step is put into one liter of glass beaker, adds deionization by second step
Water adjusts solid-to-liquid ratio 1:5~8, later open stirring, mixing speed be 150 revs/min, then with 20% liquid caustic soda tune PH=9.5~
10.0, then be put on electric furnace and heat, when burning cup temperature is raised to 90 DEG C ± 2 DEG C, then constant temperature stirring 40 minutes is carried out, later etc.
It burns cup temperature and is cooled to 60 DEG C hereinafter, stopping stirring, feeding, vacuum filtration is washed with deionized to neutrality;Third walks,
Material obtained in second step is put into two liters of glass beakers, deionized water is added, and adjust solid-to-liquid ratio 1:15, it opens later
Stirring, mixing speed are 260 revs/min, and stirring after sixty minutes, stops stirring, standing sedimentation 8 hours then will be unprecipitated
Suspension is discharged into waste liquid pool, and the sediment is by surface-treated base material;The Hydrolyze method encapsulation steps of the base material
Including the first step, in one liter of glass beaker, 500 milliliters of deionized water is added, chooses surface preparation third step and completes
25 grams of base material afterwards adjusts solid-to-liquid ratio 1:10~15, it is then turned on stirring, mixing speed is 150 revs/min, uses water-bath later
Heating, when temperature rises to 55 DEG C, with 20% aqueous hydrochloric acid solution tune PH=1.3~1.5, after, it is stirred again, mixing time
It it is 5 minutes, 3 milliliters of 10% potassium chlorate solution is added in second step under constant temperature stirring, singly flows the chlorine of dropwise addition 10% again later
Change stannous, magnesium chloride and zinc chloride mixed solution, proportions are in the stannous chloride, magnesium chloride and zinc chloride mixed solution
30:1:1, after charging, stir 5 minutes, then with 10% liquid caustic soda solution tune PH=1.8~2.0, and by water-bath pot temperature rise to T=
78 DEG C ± 2 DEG C, third step keeps water-bath pot temperature under the state of T=78 DEG C ± 2 DEG C, cocurrent is added dropwise to 60 milli of 2M titanium tetrachlorides
Rise, the mixed liquor of 3 milliliters of 1 milliliter of 10% Nickel dichloride hexahydrate aqueous solution and 10% butter of tin, then with 20% liquid caustic soda maintenance PH=
1.8~2.0, charging while, is stirred, and speed of agitator rises with liquid level and accordingly promoted, when base material is in the slightly biased yellow phase of silvery white
When, then stop feeding, it is stirred for later 5 minutes, the 4th step, steady temperature is T=78 DEG C ± 2 DEG C, and titanium tetrachloride 100 is added dropwise in stream
The mixed liquor of 20 milliliters of milliliter and ferric trichloride, with 20% liquid caustic soda maintenance PH=1.8~2.0, when the form and aspect of base material are between bluish-green
When, stop charging, be stirred for later 10 minutes, the 5th step, rises 85 DEG C of temperature, it is 260 revs/min to adjust mixing speed later, then
With 20% sodium hydrate aqueous solution tune PH=9.0-9.5, after, it stirs 5 minutes, the 6th step, is 85 DEG C of shape keeping temperature
Under state, 10 milliliters of 10% 9 sodium silicate aqueous solution is added dropwise in cocurrent, maintains PH=9.0-9.5 constant with 20% hydrochloric acid, and then stirring 5
Minute, the 7th step adjusts 78 DEG C of temperature, and it is 210 revs/min to adjust mixing speed, then with 20% hydrochloric acid tune PH=1.8-2.2, later
Stirring 5 minutes, the 8th step maintain 78 DEG C of temperature, and the mixed liquor of 10 milliliters of 20 milliliters of titanium tetrachloride and ferric trichloride is added dropwise in cocurrent,
PH=1.8-2.2 is maintained with 10% sodium hydrate aqueous solution, speed of agitator rises with liquid level and accordingly carries rotating speed, when the form and aspect of base material
Stop feeding in golden red, be stirred for later 5 minutes;The post-processing steps include the first step, in Hydrolyze method encapsulation steps
The base material of 8th step, takes out through vacuum filtration, and deionized water is then added and washs pH value to neutrality, second step, by post-processing
The base material that the first step is handled in step is put into drying 3 hours in drying machine, and the temperature of drying machine is 105 DEG C, is used again later
720 DEG C calcine 20 minutes, after obtain a kind of pearlescent pigment with thousand pure gold effects.
Embodiment 3
The invention discloses a kind of pearlescent pigment with thousand pure gold effects, including base material, the base material is natural mica, synthesis
Mica or glass flake, the base material coat the first composite layer, the second composite layer, third composite layer, the 4th composite layer successively outside
With the 5th composite layer, first composite layer is stannous chloride, magnesium chloride, zinc chloride mixing composition, and second composite layer is
Titanium tetrachloride, nickel chloride and butter of tin mixing are constituted, and the third composite layer is that titanium tetrachloride mixes composition with ferric trichloride,
4th composite layer is that silica or aluminium oxide are constituted, and the 5th composite layer is titanium tetrachloride and ferric trichloride mixing structure
At the thickness of the base material is 60nm-2000nm, and grain size is 5-900 μm, a kind of pearlescent pigment preparation with thousand pure gold effects
Method, the preparation method include the surface preparation of base material, the Hydrolyze method encapsulation steps of base material and post-processing steps, described
The surface preparation of base material includes:The first step adds deionized water, 100 grams of input 5-25 microns natural in one liter of glass beaker
Mica, artificial mica synthesis or glass flake adjust solid-to-liquid ratio 1:5~8, stirring is opened later, and mixing speed is 200 revs/min
Clock, then with 20% technical hydrochloric acid tune PH=0.8~1.0, then be put on electric furnace and heat, it is raised to 90 DEG C ± 2 DEG C when burning cup temperature
When, constant temperature stirring 70 minutes is carried out, cup temperature of burning equal later is cooled to 60 DEG C hereinafter, stopping stirring, and feeding is filtered by vacuum,
It is washed with deionized to neutrality;Material obtained in the first step is put into one liter of glass beaker, adds deionization by second step
Water adjusts solid-to-liquid ratio 1:5~8, later open stirring, mixing speed be 200 revs/min, then with 20% liquid caustic soda tune PH=9.5~
10.0, then be put on electric furnace and heat, when burning cup temperature is raised to 90 DEG C ± 2 DEG C, then constant temperature stirring 70 minutes is carried out, later etc.
It burns cup temperature and is cooled to 60 DEG C hereinafter, stopping stirring, feeding, vacuum filtration is washed with deionized to neutrality;Third walks,
Material obtained in second step is put into two liters of glass beakers, deionized water is added, and adjust solid-to-liquid ratio 1:15~20, later
Stirring is opened, mixing speed is 360 revs/min, after stirring 90 minutes, stops stirring, then standing sedimentation 12 hours will not sink
The suspension in shallow lake is discharged into waste liquid pool, and the sediment is by surface-treated base material;The Hydrolyze method of the base material coats
Step includes the first step, in one liter of glass beaker, deionized water is added, after selection surface preparation third step completes
45 grams of base material adjusts solid-to-liquid ratio 1:10~15, it is then turned on stirring, mixing speed is 240 revs/min, is added later with water-bath
Heat, when temperature rises to 60 DEG C, with 20% aqueous hydrochloric acid solution tune PH=1.3~1.5, after, it is stirred again, mixing time is
10 minutes, 7 milliliters of 10% potassium chlorate solution was added in second step under constant temperature stirring, singly flowed the chlorine of dropwise addition 10% again later
Change stannous, 32 milliliters of magnesium chloride and zinc chloride mixed solution, three in the stannous chloride, magnesium chloride and zinc chloride mixed solution
Ratio is 30:1:1, after charging, stir 10 minutes, then with 10% liquid caustic soda solution tune PH=1.8~2.0, and by water-bath pot temperature
T=78 DEG C ± 2 DEG C are risen to, third step keeps water-bath pot temperature under the state of T=78 DEG C ± 2 DEG C, cocurrent is added dropwise to 2M titanium tetrachlorides
80 milliliters, the mixed liquor of 10 milliliters of 3 milliliters of 10% Nickel dichloride hexahydrate aqueous solution and 10% butter of tin, then tieed up with 20% liquid caustic soda
Hold PH=1.8~2.0, charging while, is stirred, and speed of agitator rises with liquid level and accordingly promoted, when base material is slightly biased in silvery white
When yellow phase, then stop feeding, be stirred for later 10 minutes, the 4th step, steady temperature is T=78 DEG C ± 2 DEG C, and 2M tetrachloros are added dropwise in stream
The mixed liquor for changing 40 milliliters of 150 milliliters of titanium and 1M ferric trichlorides, with 20% liquid caustic soda maintenance PH=1.8~2.0, when the form and aspect of base material
When between bluish-green, stop charging, be stirred for later 20 minutes, the 5th step, rise 85 DEG C of temperature, it is 380 to adjust mixing speed later
Rev/min, then with 20% sodium hydrate aqueous solution tune PH=9.0-9.5, after, it stirs 10 minutes, the 6th step, is keeping temperature
In the state of 85 DEG C, 20 milliliters of 10% 9 sodium silicate aqueous solution is added dropwise in cocurrent, maintains PH=9.0-9.5 constant with 20% hydrochloric acid, it
Afterwards, be stirred for 10 minutes, the 7th step, adjust 80 DEG C of temperature, adjust mixing speed be 310 revs/min, then with 20% hydrochloric acid tune PH=
1.8-2.2 is stirred 10 minutes, the 8th step later, maintains 80 DEG C of temperature, cocurrent that 70 milliliters of 2M titanium tetrachlorides and 1M tri-chlorinations is added dropwise
The mixed liquor that 30 milliliters of iron maintains PH=1.8-2.2, speed of agitator to rise with liquid level and accordingly carry with 10% sodium hydrate aqueous solution
Rotating speed, when base material form and aspect in golden red stop charging, be stirred for later 10 minutes;The post-processing steps include first
It walks, the base material of the 8th step in Hydrolyze method encapsulation steps takes out through vacuum filtration, and deionized water is then added and washs pH value into
Property, second step, the base material that the first step in post-processing steps is handled is put into drying machine it is 3 hours dry, drying machine
Temperature be 105 DEG C, later again use 760 DEG C calcining 20 minutes, after obtain a kind of pearlescent pigment with thousand pure gold effects.
Embodiment 4
The invention discloses a kind of pearlescent pigment with thousand pure gold effects, including base material, the base material is natural mica, synthesis
Mica or glass flake, the base material coat the first composite layer, the second composite layer, third composite layer, the 4th composite layer successively outside
With the 5th composite layer, first composite layer is stannous chloride, magnesium chloride, zinc chloride mixing composition, and second composite layer is
Titanium tetrachloride, nickel chloride and butter of tin mixing are constituted, and the third composite layer is that titanium tetrachloride mixes composition with ferric trichloride,
4th composite layer is that silica or aluminium oxide are constituted, and the 5th composite layer is titanium tetrachloride and ferric trichloride mixing structure
At the thickness of the base material is 60nm-2000nm, and grain size is 5-900 μm, a kind of pearlescent pigment preparation with thousand pure gold effects
Method, the preparation method include the surface preparation of base material, the Hydrolyze method encapsulation steps of base material and post-processing steps, described
The surface preparation of base material includes:The first step adds deionized water, 60 grams of days of input 10-100 microns in one liter of glass beaker
Right mica, artificial mica synthesis or glass flake, adjust solid-to-liquid ratio 1:5~8, stirring is opened later, and mixing speed is 180 revs/min
Clock, then with 20% technical hydrochloric acid tune PH=0.8~1.0, then be put on electric furnace and heat, it is raised to 90 DEG C ± 2 DEG C when burning cup temperature
When, constant temperature stirring 55 minutes is carried out, cup temperature of burning equal later is cooled to 60 DEG C hereinafter, stopping stirring, and feeding is filtered by vacuum,
It is washed with deionized to neutrality;Material obtained in the first step is put into one liter of glass beaker, adds deionization by second step
Water adjusts solid-to-liquid ratio 1:5~8, later open stirring, mixing speed be 180 revs/min, then with 20% liquid caustic soda tune PH=9.5~
10.0, then be put on electric furnace and heat, when burning cup temperature is raised to 90 DEG C ± 2 DEG C, then constant temperature stirring 55 minutes is carried out, later etc.
It burns cup temperature and is cooled to 60 DEG C hereinafter, stopping stirring, feeding, vacuum filtration is washed with deionized to neutrality;Third walks,
Material obtained in second step is put into two liters of glass beakers, deionized water is added, and adjust solid-to-liquid ratio 1:15~20, later
Stirring is opened, mixing speed is 310 revs/min, after stirring 75 minutes, stops stirring, then standing sedimentation 10 hours will not sink
The suspension in shallow lake is discharged into waste liquid pool, and the sediment is by surface-treated base material;The Hydrolyze method of the base material coats
Step includes the first step, in one liter of glass beaker, deionized water is added, after selection surface preparation third step completes
32 grams of base material adjusts solid-to-liquid ratio 1:10~15, it is then turned on stirring, mixing speed is 230 revs/min, is added later with water-bath
Heat, when temperature rises to 58 DEG C, with 20% aqueous hydrochloric acid solution tune PH=1.3~1.5, after, it is stirred again, mixing time 8
Minute, 5 milliliters of 10% potassium chlorate solution is added in second step under constant temperature stirring, later the chlorination of single stream dropwise addition 10% again
32 milliliters of stannous, magnesium chloride and zinc chloride mixed solution, three's ratio in the stannous chloride, magnesium chloride and zinc chloride mixed solution
Example is 30:1:1, after charging, stir 7 minutes, then with 10% liquid caustic soda solution tune PH=1.8~2.0, and by water-bath pot temperature liter
To T=78 DEG C ± 2 DEG C, third step keeps water-bath pot temperature under the state of T=78 DEG C ± 2 DEG C, cocurrent is added dropwise to 2M titanium tetrachlorides 70
The mixed liquor of milliliter, 7 milliliters of 2 milliliters of 10% Nickel dichloride hexahydrate aqueous solution and 10% butter of tin, then with 20% liquid caustic soda maintenance PH
=1.8~2.0, charging while, is stirred, and speed of agitator rises with liquid level and accordingly promoted, when base material is in the slightly biased yellow phase of silvery white
When, then stop feeding, it is stirred for later 8 minutes, the 4th step, steady temperature is T=78 DEG C ± 2 DEG C, and 2M titanium tetrachlorides 35 are added dropwise in stream
The mixed liquor of 20 milliliters of milliliter and 1M ferric trichlorides, with 20% liquid caustic soda maintenance PH=1.8~2.0, when base material form and aspect to it is bluish-green it
Between when, stop charging, be stirred for later 10-20 minute, the 5th step, rise 85 DEG C of temperature, later adjust mixing speed be 270 revs/min
Clock, then with 20% sodium hydrate aqueous solution tune PH=9.0-9.5, after, it stirs 8 minutes, the 6th step, is 85 DEG C keeping temperature
In the state of, 15 milliliters of 10% alchlor aqueous solution is added dropwise in cocurrent, maintains PH=9.0-9.5 constant with 20% hydrochloric acid, and then
Stirring 8 minutes, the 7th step adjust 79 DEG C of temperature, and it is 180 revs/min to adjust mixing speed, then with 20% hydrochloric acid tune PH=1.8-
2.2, it stirs 8 minutes later, the 8th step, maintains 79 DEG C of temperature, cocurrent that 12 milli of 35 milliliters of 1M titanium tetrachlorides and ferric trichloride is added dropwise
The mixed liquor risen maintains PH=1.8-2.2, speed of agitator to rise with liquid level and accordingly carry rotating speed with 10% sodium hydrate aqueous solution,
When base material form and aspect in golden red stop charging, be stirred for later 8 minutes;The post-processing steps include the first step, hydrolysis
The base material of 8th step in method encapsulation steps takes out through being filtered by vacuum, then addition deionized water washing pH value to neutrality, and second
Step, the base material that the first step in post-processing steps is handled, which is put into drying 3 hours, the temperature of drying machine in drying machine, is
105 DEG C, later again with 740 DEG C calcine 20 minutes, after obtain a kind of pearlescent pigment with thousand pure gold effects.
Embodiment 5
The invention discloses a kind of pearlescent pigment with thousand pure gold effects, including base material, the base material is natural mica, synthesis
Mica or glass flake, the base material coat the first composite layer, the second composite layer, third composite layer, the 4th composite layer successively outside
With the 5th composite layer, first composite layer is stannous chloride, magnesium chloride, zinc chloride mixing composition, and second composite layer is
Titanium tetrachloride, nickel chloride and butter of tin mixing are constituted, and the third composite layer is that titanium tetrachloride mixes composition with ferric trichloride,
4th composite layer is that silica or aluminium oxide are constituted, and the 5th composite layer is titanium tetrachloride and ferric trichloride mixing structure
At the thickness of the base material is 60nm-2000nm, and grain size is 5-900 μm, a kind of pearlescent pigment preparation with thousand pure gold effects
Method, the preparation method include the surface preparation of base material, the Hydrolyze method encapsulation steps of base material and post-processing steps, described
The surface preparation of base material includes:The first step adds deionized water, 30 grams of input 20-80 microns natural in one liter of glass beaker
Mica, artificial mica synthesis or glass flake adjust solid-to-liquid ratio 1:5~8, stirring is opened later, and mixing speed is 150 revs/min
Clock, then with 20% technical hydrochloric acid tune PH=0.8~1.0, then be put on electric furnace and heat, it is raised to 90 DEG C ± 2 DEG C when burning cup temperature
When, constant temperature stirring 40 minutes is carried out, cup temperature of burning equal later is cooled to 60 DEG C hereinafter, stopping stirring, and feeding is filtered by vacuum,
It is washed with deionized to neutrality;Material obtained in the first step is put into one liter of glass beaker, adds deionization by second step
Water adjusts solid-to-liquid ratio 1:5~8, later open stirring, mixing speed be 150 revs/min, then with 20% liquid caustic soda tune PH=9.5~
10.0, then be put on electric furnace and heat, when burning cup temperature is raised to 90 DEG C ± 2 DEG C, then constant temperature stirring 40 minutes is carried out, later etc.
It burns cup temperature and is cooled to 60 DEG C hereinafter, stopping stirring, feeding, vacuum filtration is washed with deionized to neutrality;Third walks,
Material obtained in second step is put into two liters of glass beakers, deionized water is added, and adjust solid-to-liquid ratio 1:15, it opens later
Stirring, mixing speed are 260 revs/min, and stirring after sixty minutes, stops stirring, standing sedimentation 8 hours then will be unprecipitated
Suspension is discharged into waste liquid pool, and the sediment is by surface-treated base material;The Hydrolyze method encapsulation steps of the base material
Including the first step, in one liter of glass beaker, deionized water is added, chooses the base material after surface preparation third step completes
25 grams, adjust solid-to-liquid ratio 1:10~15, it is then turned on stirring, mixing speed is 220 revs/min, is heated later with water-bath, when
Temperature rises to 55 DEG C, with 20% aqueous hydrochloric acid solution tune PH=1.3~1.5, after, it being stirred again, mixing time is 5 minutes,
3 milliliters of 10% potassium chlorate solution is added in second step under constant temperature stirring, and list flows the stannous chloride of dropwise addition 10%, chlorine again later
Change magnesium and zinc chloride mixed solution, proportions are 30 in the stannous chloride, magnesium chloride and zinc chloride mixed solution:1:1, add
After material, stir 5 minutes, then with 10% liquid caustic soda solution tune PH=1.8~2.0, and water-bath pot temperature is risen into T=78 DEG C ± 2 DEG C,
Third step keeps water-bath pot temperature under the state of T=78 DEG C ± 2 DEG C, cocurrent is added dropwise to 60 milliliters of 2M titanium tetrachlorides, 10% 6 hydration
The mixed liquor of 3 milliliters of 1 milliliter of nickel chloride aqueous solution and 10% butter of tin, then maintain PH=1.8 with 20% liquid caustic soda~2.0, charging
While be stirred, speed of agitator rises with liquid level and is accordingly promoted, when base material yellow phase slightly biased in silvery white, then stop plus
Material, is stirred for 5 minutes, the 4th step later, and steady temperature is T=78 DEG C ± 2 DEG C, and 100 milliliters of titanium tetrachloride and three oxidations are added dropwise in stream
The mixed liquor that 20 milliliters of iron maintains PH=1.8 with 20% liquid caustic soda~2.0, when the form and aspect of base material are between bluish-green, stop charging,
It is stirred for later 10 minutes, the 5th step, rises 85 DEG C of temperature, it is 350 revs/min to adjust mixing speed later, then with 20% sodium hydroxide
Aqueous solution tune PH=9.0-9.5, after, it stirs 5 minutes, the 6th step, in the state that it is 85 DEG C to keep temperature, cocurrent is added dropwise
10% 9 10 milliliters of sodium silicate aqueous solution maintains PH=9.0-9.5 constant, and then stirs 5 minutes, the 7th step with 20% hydrochloric acid,
78 DEG C of temperature is adjusted, it is 260 revs/min to adjust mixing speed, then uses 20% hydrochloric acid tune PH=1.8-2.2, later stirring 5 minutes, the
Eight steps, maintain 78 DEG C of temperature, and the mixed liquor of 10 milliliters of 20 milliliters of titanium tetrachloride and ferric trichloride is added dropwise in cocurrent, with 10% hydroxide
Sodium water solution maintains PH=1.8-2.2, and speed of agitator rises with liquid level and accordingly carries rotating speed, when the form and aspect of base material are stopped in golden red
It only feeds, is stirred for later 5 minutes;The post-processing steps include the first step, the base of the 8th step in Hydrolyze method encapsulation steps
Material, takes out through vacuum filtration, and deionized water is then added and washs pH value to neutrality, second step, by post-processing steps first
The base material that step is handled is put into drying 3 hours in drying machine, and the temperature of drying machine is 105 DEG C, later again with 720 DEG C of calcinings 20
Minute, after obtain a kind of pearlescent pigment with thousand pure gold effects.
Embodiment 6
The invention discloses a kind of pearlescent pigment with thousand pure gold effects, including base material, the base material is natural mica, synthesis
Mica or glass flake, the base material coat the first composite layer, the second composite layer, third composite layer, the 4th composite layer successively outside
With the 5th composite layer, first composite layer is stannous chloride, magnesium chloride, zinc chloride mixing composition, and second composite layer is
Titanium tetrachloride, nickel chloride and butter of tin mixing are constituted, and the third composite layer is that titanium tetrachloride mixes composition with ferric trichloride,
4th composite layer is that silica or aluminium oxide are constituted, and the 5th composite layer is titanium tetrachloride and ferric trichloride mixing structure
At the thickness of the base material is 60nm-2000nm, and grain size is 5-900 μm, a kind of pearlescent pigment preparation with thousand pure gold effects
Method, the preparation method include the surface preparation of base material, the Hydrolyze method encapsulation steps of base material and post-processing steps, described
The surface preparation of base material includes:The first step adds deionized water, 100 grams of input 100-400 microns in one liter of glass beaker
Natural mica, artificial mica synthesis or glass flake adjust solid-to-liquid ratio 1:5~8, later open stirring, mixing speed be 200 turns/
Minute, then with 20% technical hydrochloric acid tune PH=0.8~1.0, then be put on electric furnace and heat, it is raised to 90 DEG C ± 2 when burning cup temperature
DEG C when, carry out constant temperature and stir 70 minutes, cup temperature of burning equal later is cooled to 60 DEG C hereinafter, stopping stirring, and feeding, vacuum is taken out
Filter, is washed with deionized to neutrality;Material obtained in the first step is put into one liter of glass beaker by second step, add from
Sub- water adjusts solid-to-liquid ratio 1:5~8, later open stirring, mixing speed be 200 revs/min, then with 20% liquid caustic soda tune PH=
9.5~10.0, then be put on electric furnace and heat, when burning cup temperature is raised to 90 DEG C ± 2 DEG C, then carries out constant temperature and stir 70 minutes, it
Equal cup temperature of burning is cooled to 60 DEG C hereinafter, stopping stirring afterwards, and feeding, vacuum filtration is washed with deionized to neutrality;Third
Step, material obtained in second step is put into two liters of glass beakers, deionized water is added, and adjust solid-to-liquid ratio 1:15~20, it
Stirring is opened afterwards, and mixing speed is 360 revs/min, after stirring 90 minutes, stops stirring, standing sedimentation 12 hours then will not
The suspension of precipitation is discharged into waste liquid pool, and the sediment is by surface-treated base material;The Hydrolyze method packet of the base material
It includes the first step to cover step, in one liter of glass beaker, deionized water is added, after selection surface preparation third step completes
45 grams of base material, adjust solid-to-liquid ratio 1:10~15, it is then turned on stirring, mixing speed is 210 revs/min, is added later with water-bath
Heat, when temperature rises to 60 DEG C, with 20% aqueous hydrochloric acid solution tune PH=1.3~1.5, after, it is stirred again, mixing time is
10 minutes, 7 milliliters of 10% potassium chlorate solution was added in second step under constant temperature stirring, singly flowed the chlorine of dropwise addition 10% again later
Change stannous, 32 milliliters of magnesium chloride and zinc chloride mixed solution, three in the stannous chloride, magnesium chloride and zinc chloride mixed solution
Ratio is 30:1:1, after charging, stir 10 minutes, then with 10% liquid caustic soda solution tune PH=1.8~2.0, and by water-bath pot temperature
T=78 DEG C ± 2 DEG C are risen to, third step keeps water-bath pot temperature under the state of T=78 DEG C ± 2 DEG C, cocurrent is added dropwise to 2M titanium tetrachlorides
80 milliliters, the mixed liquor of 10 milliliters of 3 milliliters of 10% Nickel dichloride hexahydrate aqueous solution and 10% butter of tin, then tieed up with 20% liquid caustic soda
Hold PH=1.8~2.0, charging while, is stirred, and speed of agitator rises with liquid level and accordingly promoted, when base material is slightly biased in silvery white
When yellow phase, then stop feeding, be stirred for later 10 minutes, the 4th step, steady temperature is T=78 DEG C ± 2 DEG C, and 2M tetrachloros are added dropwise in stream
The mixed liquor for changing 30 milliliters of 100 milliliters of titanium and 1M ferric trichlorides, with 20% liquid caustic soda maintenance PH=1.8~2.0, when the form and aspect of base material
When between bluish-green, stop charging, be stirred for later 20 minutes, the 5th step, rise 85 DEG C of temperature, it is 380 to adjust mixing speed later
Rev/min, then with 20% sodium hydrate aqueous solution tune PH=9.0-9.5, after, it stirs 10 minutes, the 6th step, is keeping temperature
In the state of 85 DEG C, 20 milliliters of 10% 9 sodium silicate aqueous solution is added dropwise in cocurrent, maintains PH=9.0-9.5 constant with 20% hydrochloric acid, it
Afterwards, be stirred for 10 minutes, the 7th step, adjust 80 DEG C of temperature, adjust mixing speed be 310 revs/min, then with 20% hydrochloric acid tune PH=
1.8-2.2 is stirred 10 minutes, the 8th step later, maintains 80 DEG C of temperature, cocurrent that 40 milliliters of 2M titanium tetrachlorides and 1M tri-chlorinations is added dropwise
The mixed liquor that 20 milliliters of iron maintains PH=1.8-2.2, speed of agitator to rise with liquid level and accordingly carry with 10% sodium hydrate aqueous solution
Rotating speed, when base material form and aspect in golden red stop charging, be stirred for later 10 minutes;The post-processing steps include first
It walks, the base material of the 8th step in Hydrolyze method encapsulation steps takes out through vacuum filtration, and deionized water is then added and washs pH value into
Property, second step, the base material that the first step in post-processing steps is handled is put into drying machine it is 3 hours dry, drying machine
Temperature be 105 DEG C, later again use 760 DEG C calcining 20 minutes, after obtain a kind of pearlescent pigment with thousand pure gold effects.
Claims (9)
1. a kind of pearlescent pigment with thousand pure gold effects, including base material, it is characterised in that:The base material is natural mica, closes
Coat the first composite layer, the second composite layer, third composite layer, the 4th compound successively at mica or glass flake, outside the base material
Layer and the 5th composite layer, first composite layer are stannous chloride, magnesium chloride, zinc chloride mixing composition, second composite layer
It mixes and constitutes for titanium tetrachloride, nickel chloride and butter of tin, the third composite layer is titanium tetrachloride and ferric trichloride mixing structure
At the 4th composite layer is that silica or aluminium oxide are constituted, and the 5th composite layer is that titanium tetrachloride and ferric trichloride are mixed
It closes and constitutes.
2. a kind of pearlescent pigment with thousand pure gold effects according to claim 1, it is characterised in that:The thickness of the base material
Degree is 50nm-3000nm, and grain size is 2-1000 μm.
3. a kind of pearlescent pigment with thousand pure gold effects according to claim 2, it is characterised in that:The thickness of the base material
Spend preferred 60nm-2000nm, preferred 5-900 μm of grain size.
4. a kind of pearlescent pigment preparation method with thousand pure gold effects, it is characterised in that:The preparation method includes base material
Surface preparation, the Hydrolyze method encapsulation steps of base material and post-processing steps, the surface preparation of the base material include:First
Step adds deionized water, input natural mica, artificial mica synthesis or glass flake to adjust solid-to-liquid ratio in one liter of glass beaker
1:5~8, later open stirring, then with 20% technical hydrochloric acid tune PH=0.8~1.0, then be put on electric furnace and heat, when warm in beaker
It when degree is raised to 90 DEG C ± 2 DEG C, carries out constant temperature and stirs 40-70 minutes, burning cup temperature is waited to be cooled to 60 DEG C hereinafter, stopping stirring later
It mixes, feeding, is filtered by vacuum, is washed with deionized to neutrality;Material obtained in the first step is put into one liter of glass by second step
In beaker, add deionized water, adjusts solid-to-liquid ratio 1:5~8, later open stirring, then with 20% liquid caustic soda tune PH=9.5~10.0 then
It is put on electric furnace and heats, when burning cup temperature is raised to 90 DEG C ± 2 DEG C, then carry out constant temperature stirring 40~70 minutes, beakers were waited later
Interior temperature is cooled to 60 DEG C hereinafter, stopping stirring, and feeding, vacuum filtration is washed with deionized to neutrality;Third walks, by the
Material obtained is put into two liters of glass beakers in two steps, deionized water is added, and adjust solid-to-liquid ratio 1:15~20, it opens later
Stirring after stirring 60-90 minutes, stops stirring, standing sedimentation 8~12 hours, unprecipitated suspension is then discharged into waste liquid
Pond, the sediment are by surface-treated base material;The Hydrolyze method encapsulation steps of the base material include the first step, one
It rises in glass beaker, 500 milliliters of deionized water is added, choose the base material after surface preparation third step completes, adjust solid
Liquor ratio 1:10~15, it is then turned on stirring, is heated later with water-bath, when temperature rises to 55~60 DEG C, with 20% aqueous hydrochloric acid solution tune
PH=1.3~1.5, after, it is stirred again, mixing time is 5-10 minutes, and second step adds under constant temperature stirring
Enter 3-7 milliliters of 10% potassium chlorate solution, singly flows stannous chloride, magnesium chloride and the zinc chloride mixed solution of dropwise addition 10%, institute again later
It is 30 to state proportions in stannous chloride, magnesium chloride and zinc chloride mixed solution:1:1, after charging, stir 5-10 minutes,
Again with 10% liquid caustic soda solution tune PH=1.8~2.0, and water-bath pot temperature is risen into T=78 DEG C ± 2 DEG C, third step keeps water-bath pot temperature
Degree is under the state of T=78 DEG C ± 2 DEG C, and cocurrent is added dropwise to 60-80 milliliters of 2M titanium tetrachlorides, 10% Nickel dichloride hexahydrate aqueous solution 1-3
The mixed liquor of 3-10 milliliters of milliliter and 10% butter of tin, then with 20% liquid caustic soda maintenance PH=1.8~2.0, charging while, carries out
Stirring, speed of agitator rise with liquid level and are accordingly promoted, and when base material yellow phase slightly biased in silvery white, then stop feeding, stir again later
It mixes 5-10 minutes, the 4th step, steady temperature is T=78 DEG C ± 2 DEG C, and 100-150 milliliters of titanium tetrachloride and ferric trichloride is added dropwise in cocurrent
20-40 milliliters of mixed liquor maintains PH=1.8 with 20% liquid caustic soda~2.0, when the form and aspect of base material are between bluish-green, stop plus
Material, is stirred for 10-20 minutes, the 5th step later, rises 85 DEG C of temperature, and it is 260-380 revs/min to adjust mixing speed later, then is used
20% sodium hydrate aqueous solution tune PH=9.0-9.5, after, it stirs 5-10 minutes, the 6th step, is 85 DEG C of shape keeping temperature
Under state, 10-20 milliliter of 10% 9 sodium silicate aqueous solution or 10% alchlor aqueous solution is added dropwise in cocurrent, with 20% hydrochloric acid maintenance PH=
9.0-9.5 is constant, and then stirring 5-10 minute, and the 7th step adjusts 78-80 DEG C of temperature, adjust mixing speed be 210-310 turn/
Minute, then 20% hydrochloric acid tune PH=1.8-2.2 is used, 5- 10 minutes is stirred later, and the 8th step maintains 78-80 DEG C of temperature, cocurrent to drip
The mixed liquor for adding 10-30 milliliters of 20-70 milliliters of titanium tetrachloride and ferric trichloride, PH=1.8- is maintained with 10% sodium hydrate aqueous solution
2.2, speed of agitator with liquid level rise and accordingly carry rotating speed, when base material form and aspect in golden red stop charging, be stirred for 5- later
10 minutes;The post-processing steps include the first step, and the base material of the 8th step in Hydrolyze method encapsulation steps, taking-up is taken out through vacuum
Then filter is added deionized water and washs pH value to neutrality, second step, the base material that the first step in post-processing steps is handled
Be put into drying machine 3 hours dry, use 720-760 DEG C again later and calcine 20 minutes, after obtain a kind of there is thousand pure golds effect
The pearlescent pigment of fruit.
5. a kind of pearlescent pigment preparation method with thousand pure gold effects according to claim 4, it is characterised in that:It is described
The weight that natural mica, artificial mica synthesis or glass flake are put into the surface preparation first step of base material is 30-100
Gram, stirring is opened in the surface preparation first step of the base material, mixing speed is 150-200 revs/min.
6. a kind of pearlescent pigment preparation method with thousand pure gold effects according to claim 5, it is characterised in that:It is described
Stirring, mixing speed 150 are opened in the surface preparation second step of base material~200 revs/min, the surface of the base material is pre-
It handles and opens stirring in third step, mixing speed is that mixing speed is 260-360 revs/min.
7. a kind of pearlescent pigment preparation method with thousand pure gold effects according to claim 6, it is characterised in that:It is described
The first step in the Hydrolyze method encapsulation steps of base material, it is 25-45 to choose the substrate weight after surface preparation third step completes
Gram.
8. wanting a kind of pearlescent pigment preparation method with thousand pure gold effects described in 7 according to right, it is characterised in that:The base
Unlatching stirring in the Hydrolyze method encapsulation steps first step of material, mixing speed are 150-240 revs/min.
9. a kind of pearlescent pigment preparation method with thousand pure gold effects according to claim 8, it is characterised in that:It is described
The temperature of drying machine is 105 DEG C in post-processing steps second step.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112143263A (en) * | 2020-10-15 | 2020-12-29 | 深圳市宝瑞莱珠宝首饰有限公司 | Processing technology of 18K gold titanium crystal pearlescent pigment |
| CN115895293A (en) * | 2022-11-16 | 2023-04-04 | 福建坤彩材料科技股份有限公司 | Pearlescent pigment suitable for powder coating and preparation method and application thereof |
| CN116875082A (en) * | 2023-07-10 | 2023-10-13 | 江苏贝丽得新材料有限公司 | A kind of preparation method of high flash and high whiteness pearlescent pigment |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031850A (en) * | 1987-09-11 | 1989-03-22 | 默克专利股份有限公司 | Golden colour lustre pigments |
| CN1622981A (en) * | 2001-07-12 | 2005-06-01 | 默克专利股份有限公司 | Multilayer pigments based on glass flakes |
| US20080011198A1 (en) * | 2004-04-19 | 2008-01-17 | Jiansheng Fu | Pigment Having Angle Dependence of the Interference Colors and Its Production Process |
| CN101353488A (en) * | 2008-09-25 | 2009-01-28 | 河北欧克精细化工股份有限公司 | High saturation degree multilayer nacreous pigment and preparation thereof |
| CN101434759A (en) * | 2007-11-12 | 2009-05-20 | 温州大学 | Preparation of high glaze glass-based pearlescent pigment |
| CN104870571A (en) * | 2012-12-20 | 2015-08-26 | 默克专利股份有限公司 | pigment |
| CN107325589A (en) * | 2017-07-05 | 2017-11-07 | 江苏贝丽得新材料有限公司 | A kind of glittering Gold production effect pearlescent pigment of high-purity titanium ferroalloy and preparation method thereof |
-
2018
- 2018-05-08 CN CN201810432011.5A patent/CN108690377A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031850A (en) * | 1987-09-11 | 1989-03-22 | 默克专利股份有限公司 | Golden colour lustre pigments |
| US5009711A (en) * | 1987-09-11 | 1991-04-23 | Merck Patent Gesellschaft Mit Beschrankter Haftung | Golden color luster pigments |
| CN1622981A (en) * | 2001-07-12 | 2005-06-01 | 默克专利股份有限公司 | Multilayer pigments based on glass flakes |
| US20080011198A1 (en) * | 2004-04-19 | 2008-01-17 | Jiansheng Fu | Pigment Having Angle Dependence of the Interference Colors and Its Production Process |
| CN101434759A (en) * | 2007-11-12 | 2009-05-20 | 温州大学 | Preparation of high glaze glass-based pearlescent pigment |
| CN101353488A (en) * | 2008-09-25 | 2009-01-28 | 河北欧克精细化工股份有限公司 | High saturation degree multilayer nacreous pigment and preparation thereof |
| CN104870571A (en) * | 2012-12-20 | 2015-08-26 | 默克专利股份有限公司 | pigment |
| CN107325589A (en) * | 2017-07-05 | 2017-11-07 | 江苏贝丽得新材料有限公司 | A kind of glittering Gold production effect pearlescent pigment of high-purity titanium ferroalloy and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112143263A (en) * | 2020-10-15 | 2020-12-29 | 深圳市宝瑞莱珠宝首饰有限公司 | Processing technology of 18K gold titanium crystal pearlescent pigment |
| CN112143263B (en) * | 2020-10-15 | 2021-12-10 | 深圳市宝瑞莱珠宝首饰有限公司 | Processing technology of 18K gold titanium crystal pearlescent pigment |
| CN115895293A (en) * | 2022-11-16 | 2023-04-04 | 福建坤彩材料科技股份有限公司 | Pearlescent pigment suitable for powder coating and preparation method and application thereof |
| CN116875082A (en) * | 2023-07-10 | 2023-10-13 | 江苏贝丽得新材料有限公司 | A kind of preparation method of high flash and high whiteness pearlescent pigment |
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