CN106752108B - A kind of yellow cadmium system occlusion pigment, ceramic ink and preparation method thereof - Google Patents
A kind of yellow cadmium system occlusion pigment, ceramic ink and preparation method thereof Download PDFInfo
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- CN106752108B CN106752108B CN201611096171.4A CN201611096171A CN106752108B CN 106752108 B CN106752108 B CN 106752108B CN 201611096171 A CN201611096171 A CN 201611096171A CN 106752108 B CN106752108 B CN 106752108B
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- cadmium
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- 239000000049 pigment Substances 0.000 title claims abstract description 42
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 36
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000000919 ceramic Substances 0.000 title claims description 39
- 238000002360 preparation method Methods 0.000 title claims description 25
- 239000003086 colorant Substances 0.000 claims abstract description 50
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920005646 polycarboxylate Polymers 0.000 claims abstract description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 12
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000331 cadmium sulfate Inorganic materials 0.000 claims abstract description 10
- 238000010304 firing Methods 0.000 claims abstract description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000007641 inkjet printing Methods 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 10
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 4
- 238000005554 pickling Methods 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 3
- 239000006210 lotion Substances 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 229910002012 Aerosil® Inorganic materials 0.000 claims 1
- 125000001033 ether group Chemical group 0.000 claims 1
- 238000005516 engineering process Methods 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 238000007639 printing Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 8
- 235000019353 potassium silicate Nutrition 0.000 description 8
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- IVORCBKUUYGUOL-UHFFFAOYSA-N 1-ethynyl-2,4-dimethoxybenzene Chemical compound COC1=CC=C(C#C)C(OC)=C1 IVORCBKUUYGUOL-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- -1 cadmium salt Chemical class 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- 239000000908 ammonium hydroxide Substances 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000002932 luster Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 229910003130 ZrOCl2·8H2O Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 2
- 229910000369 cadmium(II) sulfate Inorganic materials 0.000 description 2
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910003243 Na2SiO3·9H2O Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910006213 ZrOCl2 Inorganic materials 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 description 1
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000004814 ceramic processing Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 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
- C09C1/0009—Pigments for ceramics
- C09C1/0012—Pigments for ceramics containing zirconium and silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M1/00—Inking and printing with a printer's forme
- B41M1/26—Printing on other surfaces than ordinary paper
- B41M1/34—Printing on other surfaces than ordinary paper on glass or ceramic surfaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
-
- 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
- C09C1/0081—Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a kind of yellow cadmium system occlusion pigment, the colorant powder fineness is 0.5-3 μm.The present invention also provides a kind of methods of yellow cadmium system occlusion pigment：Using cadmium sulfate, zirconium oxychloride, thiocarbamide, urea, white carbon, polycarboxylate, polyvinylpyrrolidone as raw material, stirring is extremely dissolved after raw material is placed in water mixing, solution is placed in reaction kettle, 5-24h is reacted under the conditions of 60-200 DEG C of temperature, rotating speed 100-300r/min, natural cooling obtains colorant presoma after completion of the reaction, and yellow cadmium system occlusion pigment finished product is obtained after washing, firing, baking step；Cadmium sulfate in raw material, zirconium oxychloride, thiocarbamide, urea, white carbon, polycarboxylate, polyvinylpyrrolidone molar ratio be（6-15）：（25-40）：（5-35）：（60-250）：（10-50）：（0.02-8.0）：（0.01-4.0）.
Description
Technical field
The invention belongs to inorganic color fields and ceramic material field, and in particular to a kind of cadmium system occlusion pigment of yellow with
And preparation method thereof, further relate to the ceramic ink and preparation method thereof using the colorant.
Background technology
Ceramic pigment belongs to inorganic color class, famous high-temperature stability is presented in ceramic idiosome and glaze, makes it
It is different from widely used inorganic pigment in other industry, such as coating, printing pigment.In traditional ceramic industry, color
The various aspects of performance of glaze is always to influence the key index of ceramic quality, including colour stability, chemical stability, color
The controllability and variation range of degree, at present to the research of ceramic pigment also mainly around promoted above-mentioned Key Performance Indicator into
Row.Inorganic color is different from organic toner, and being largely because it has good color and luster and quality power, but these are excellent
Good characteristic is only limited in the application environment of low temperature, once encountering hot conditions, inorganic color can occur to volatilize or aoxidized,
To influence colour generation color and luster, keep its application limited.In this regard, occlusion pigment comes into being.Package, is exactly by colour generation as its name suggests
Particle is wrapped in translucency number, the package phase of high-temperature stable, its high temperature is improved under the premise of not influencing colorant color generation property
Stability, chemical stability and environmental-protecting performance.Occlusion pigment is mainly used in the necks such as meat ceramics, sanitary ceramics, the art pottery
Domain, application range are very extensive.
In traditional ceramics industry, requirement of the ceramic printing technique to colorant granularity is that can all be sieved by 325 mesh（I.e.
Colorant fineness is less than 45 μm）, therefore the more rough preparation sides such as solid sintering technology, clincker process are mainly used in traditional handicraft
Method prepares colorant powder.It is many more first also simultaneously with the improvement of ceramic processing technique with the promotion of ceramic grade
Into volume technology be applied in ceramic printing technique, such as ink-jet printing technology.Ink-jet printing technology is a kind of non-contact
The digital printing technologies of formula, by by ceramic ink using nozzle be ejected into ceramic frit surface realize it is non-contact, at high speed, it is low
The printing of the word or image of noise.In ink jet printing metal, ceramic pigment powder by deep processing be prepared into ceramic ink into
Row application.Since in ink-jet printing process, ceramic ink need to be ejected by nozzle, so this requires be scattered in ceramic ink
Colorant diameter of particle in water is small as far as possible, size distribution ceramic pigment that is narrow as far as possible, and being prepared in traditional technology
Material is difficult to be caused to be easy plug nozzle and is dfficult to apply in ink-jet printing technology since grain size is excessive, particle diameter distribution is wide.
Invention content
To solve the above problems, the cadmium system silicon that the present invention provides a kind of colorant powder fineness is small, particle size distribution range is narrow
Sour zirconium occlusion pigment.
Cadmium system colorant is because its coloration ability is widely used by force, however the problem of its heat resistance and feature of environmental protection in the same time limit
Its application is made.Often heat resistance is insufficient during heat treatment for cadmium system colorant, in the temperature environment of ceramic glaze sintering
In（800 DEG C or more）It can almost be aoxidized completely, generate cadmium oxide, become greyish black color substance, it is original beautiful to lose
Colour generation.When prepared by cadmium system colorant become occlusion pigment, the shortcomings that not tolerating high temperature can not only be overcome, while also solving cadmium
Be colorant not environmentally the problem of.
The cadmium system occlusion pigment provided in the present invention wraps up carrier using zirconium silicate as it, and colour generation is yellow, colorant
Powder fineness is 0.5-3 μm.
The method for preparing occlusion pigment in the prior art include solid sintering technology, clincker process, double-contracting method, sol-gel method,
Microemulsion method etc., and the ripe technical solution for being applied to large-scale industrial production is to prepare package color using chemical coprecipitation
Material, preparation process are：Using zirconium oxychloride（ZrOCl2·8H2O）And cadmium salt（CdSO4·8H2O）It is dissolved in water as raw material
Afterwards, then with vulcanized sodium（Na2S）And highly basic（Such as NaOH）And waterglass（Na2SiO3·9H2O）Mixing, adjustment pH value is in 5.5-
10.5 or so, after forming co-precipitation, then the presoma is washed, is dried, mineralizer firing（Firing condition is 900-
1200 DEG C, firing time 10-90min）, last pickling, grinding, drying can be obtained final product.Using chemical coprecipitation legal system
The disadvantage of standby cadmium system occlusion pigment maximum is manufactured colorant grain size between 3-20 μm, and colorant powder fineness is average at 10 μm
More than, when in applied to high-end printing technology or fine printing technology, colorant powder is excessive, is unable to meet demand.Such as answer
For the colorant fineness requirement in ink jet printing at least below 3 μm, colorant powder is also required to when preparing high-end fine ceramics surface
More thinner, better, above-mentioned requirements all cannot be satisfied using the colorant that prior art preparation goes out.And occlusion pigment prepare after due to
Its special physical arrangement can not be refined further, if can destroy its package structure by the strength fragmentation colorant causes
Internal structure is exposed, to cause pigment color to ruin color under the high temperature conditions, loses the practicality.
A kind of a kind of cadmium system occlusion pigment of yellow is prepared to solve the above problems, being proposed in the present invention using hydro-thermal method
Method, and provide the colorant prepared by this method, further, also provide a kind of ceramic ink made of the colorant and
The preparation method of the ink.The technical problem to be solved in the present invention is solved by following scheme：
The method provided by the invention for preparing above-mentioned yellow cadmium system occlusion pigment, it is characterised in that：
Using cadmium sulfate, zirconium oxychloride, thiocarbamide, urea, white carbon, polycarboxylic acids ammonium salt, polyvinylpyrrolidone as raw material,
Stirring is added in reaction kettle, to dissolving in 60-200 DEG C of temperature, rotating speed 100-300r/min items after raw material is placed in water mixing
5-24h is reacted under part, natural cooling obtains colorant presoma after completion of the reaction, and yellow is obtained after washing, firing, baking step
Cadmium system occlusion pigment finished product；
Mole of cadmium sulfate, zirconium oxychloride, thiocarbamide, urea, white carbon, polycarboxylate, polyvinylpyrrolidone in raw material
Than for（6-15）：（25-40）：（5-35）：（60-250）：（10-50）：（0.02-8.0）：（0.01-4.0）.
In the present invention, using thiocarbamide（CH4N2S）Instead of vulcanized sodium in the prior art（Na2S）, thiocarbamide is by hydrolyzing instead
S should be released2-, greatly reduce the generating rate of cadmium sulfide so that the cadmium sulfide grain size smaller that is prepared in reaction, grain size
It more uniformly spreads.Meanwhile using urea（CO（NH2）2）Replace highly basic in the prior art（Such as NaOH）, urea passes through hydrolysis
Reaction generates ammonia, and ammonia is dissolved in water and forms ammonium hydroxide, and ammonium hydroxide is reacted with zirconium oxychloride generates zirconium hydroxide, due to ammonium hydroxide alkalinity
It is weak, greatly reduce the generating rate of zirconium hydroxide so that the grain size smaller of the zirconium hydroxide colloid obtained in reaction.Further
Scheme in the present invention is improved, the waterglass in raw material is replaced using white carbon.White carbon is powdered water
Being commonly called as amorphous silica or silicic acid is closed, the most basic unit for constituting particle is silica primary partical
（Primary particle）, which is spherical shape, and surface energy is very big, and grain size is minimum, only 10nm or so.This hair
Bright inventor has found in practice process, uses waterglass more preferably using white carbon ratio in preparation process, is primarily due to
White carbon compares waterglass, and the silicate solution of formation is easier to wash, on the other hand, after adding waterglass, reaction system
PH value will produce promotion by a relatively large margin, and the adjusting that strong acid carries out pH value need to be added dropwise, but use white carbon to reaction system
PH value influence is smaller, can adjust pH value to desirable value without the use of strong acid.By the improvement to reactant, in preparation process
The mix precursor grain size of generation substantially reduces.Further, in raw material white carbon also can be used with same effect two
Silica aerogel powder replaces.
Polycarboxylate and PVP are also used in the present invention（Polyvinylpyrrolidone）As dispersant.PVP is a kind of nonionic
Type high-molecular compound, is incorporated herein, and can play good dispersion effect to the reaction system, prevent the reunion of particle.
Further preferably, cadmium sulfate, zirconium oxychloride, thiocarbamide, urea, white carbon, polycarboxylate, polyvinyl pyrrole in raw material
The molar ratio of alkanone is（10-12）：（28-32）：（18-21）：（160-180）：（20-25）：（0.1-6.0）：（0.15-4.0）.
The firing step used in the present invention refers to：By lithium fluoride and colorant presoma obtained with mass ratio 0.05-
0.10：1 is mixed, and after being ground up, sieved, mixture is calcined 10-60min under the conditions of 900-1200 DEG C.
Its product is carried out pickling with mixed acid, is then washed to again by further preferably processing after completing to be burnt into step
Washing lotion is neutrality, is then dried again, and colorant finished product is made.
It is also provided in the present invention a kind of using above-mentioned yellow cadmium system's occlusion pigment as the ceramic ink of colorant additive, institute
The preparation method for stating ceramic ink is to mix colorant with solvent, is ground to grain graininess D100 less than 1 μm, wherein colorant with it is molten
The mass percentage of agent is respectively 30-50%, 50-70%.The solvent that the ink uses is ether solvent.
A kind of application process of above-mentioned ceramic ink is also provided in the present invention：The ceramic ink silk-screen or ink-jet are printed
It brushes in ceramic glaze version, is calcined under the conditions of 800-1300 DEG C.
The present invention has the advantages that：
1, the present invention provides the yellow cadmium system occlusion pigment that a kind of powder fineness is only 0.5-3 μm, the colorant color and luster is gorgeous
It is beautiful it is full, coloration is high, using ceramic ink made of yellow cadmium system colorant in the present invention be suitable for all kinds of fine-structure mesh version silk-screens, ink-jet
Printing, high-end printing technology or fine printing technology, fine and smooth color effects can be presented and meanwhile avoid blocking halftone hole and
Jet orifice.
2, replaced using thiocarbamide, urea, white carbon in the preparation method of yellow cadmium system occlusion pigment in the present invention existing
Vulcanized sodium, highly basic in technology and waterglass raw material, further reduced the fineness of colorant.
3, the yellow cadmium system occlusion pigment in the present invention is prepared using hydrothermal synthesis method, and it is bent can effectively to control heating
Line, the progress for controlling the process in reaction system, sufficiently promoting reaction.
4, use polycarboxylate and PVP as dispersant in the yellow cadmium system occlusion pigment preparation process in the present invention, it can
Effectively achieve the effect that dispersion.
Specific implementation mode
Colorant, colorant preparation method and the applying for the colorant in the present invention are carried out further with reference to embodiment
Explanation.
There is provided in the present embodiment it is a kind of develop the color, the yellow cadmium system occlusion pigment that fineness is small, the powder fineness of the colorant is
0.5-3μm。
The molar ratio in table carries out the preparation of yellow cadmium system occlusion pigment according to the following recipe：
Specific preparation method following steps：
1. step weighs cadmium sulfate according to formula table（CdSO4•8H2O）And zirconium oxychloride（ZrOCl2•8H2O）, add water-soluble
Solution；The addition quality of water is 3-5 times of solids weight.
2. weighing urea, thiocarbamide according to formula table, it is dissolved in water；The addition quality of water is 5-10 times of solids weight.
3. weighing dispersant polycarboxylate and PVP according to formula table, it is dissolved in 2000-2500ml water.
4. by step 1. -3. in solution mix, add silicon source, be uniformly mixed；It in this step can be auxiliary by ultrasonic wave
Help dispersion.
5. by step 4. in mixed reaction solution pour into reaction kettle, adjustment temperature be 60-200 DEG C, rotating speed 100-
300r/min reacts 5-24h.
6. by step 5. in obtain precursors take out, washing, filter, drying.
7. by step 6. treated presoma with mineralizer lithium fluoride with mass ratio 1:0.05-0.1 is mixed, grinding
10min is mixed, 325 mesh sieve is crossed, 10-60min is then kept the temperature under the conditions of 900-1200 DEG C, being taken out after heat preservation makes its chilling
Cooling.
8. by step 7. in colorant powder nitric acid acidwashing obtained, be washed to after pickling washing lotion be neutrality, after drying i.e.
Occlusion pigment needed for obtaining.
The preferred polycarboxylic acids ammonium salt of polycarboxylate used in the present invention, the polycarboxylate used in the present embodiment are DAD
6227 polycarboxylic acids ammonium salts of DISPERSANT.
Comparative example 4：The cadmium system occlusion pigment prepared using traditional technology
Preparation method is as follows：
Step is 1.：CdSO in mass ratio4·8H2O 11%、ZrOCl2·8H2O 36.8%, vulcanized sodium 5.6%, sodium hydroxide
12%, waterglass 32.2%, the concentrated sulfuric acid 2.4% takes raw material.
2. cadmium sulfate is configured to No. 1 solution with zirconium hydroxide, vulcanized sodium is configured to No. 2 solution with sodium hydroxide,
3. above-mentioned 1, No. 2 solution is dripped to respectively in 2000-2500ml aqueous mediums, stirred in drop, pH is maintained at 7.5-
9.5, stir 30min after dripping off.
4. waterglass is configured to No. 3 solution, the concentrated sulfuric acid is configured to No. 4 solution, in first dripping to No. 3 solution 3., after dripping off
No. 4 solution are dripped again, and 30min is stirred after dripping off.
5. washing, filtering to conductivity to be less than at 500,80-110 DEG C and dry, by Qian Qu Ti ︰ mineralizer lithium fluoride mass ratioes
For the ratio weighing ball milling 10min of 1 ︰ 0.05-0.1, sieving is packed into crucible, and 20min or so is kept the temperature at 1100 DEG C, is quickly taken
Go out chilling, take nitric acid dousing 1h, add water wet-milling 30s, crosses 325 mesh sieve, be washed to pH and be in neutrality, drying.
Colorant obtained above is tested to the fineness of colorant using Malvern Particle Size Analyzer.
The preparation method of ceramic ink is：By colorant obtained and solvent with mass percent 30%:70%--50%：50% into
Row mixing is ground to grain graininess D100 and is less than 1 μm, and the solvent used in preparation process is commercially available ethers ceramic ink solvent.
By in the ceramic ink ink jet printing prepared and clear frit version, after fixed colour developing is calcined under the conditions of 800-1300 DEG C, utilize
Color difference meter tests brightness value L*With yellow value degree b*。
Test result is as follows：
The colorant fineness that the embodiment of the present invention is prepared it can be seen from test result is significantly less than traditional handicraft preparation
The colorant fineness gone out, and the colorant particle size distribution that embodiment is prepared in the present invention is narrow.And in the embodiment of the present invention
Colorant be added in ink in application, the high colouring effect of yellowing is good, wherein being best with embodiment 6,7,8,9,10.It is using
It has also been found that, comparative example 1,3,4 easily blocks jet orifice in ink jet printing in the process, and especially comparative example 4 can not almost answer
For in the screen painting of ink jet printing and small-bore.
It finally needs to illustrate, the technical solution being only to illustrate in above-described embodiment in the present invention makes ability
Domain those of ordinary skill further understands the central principle of technical solution in the present invention in depth, and not to the present invention
Technical solution limited.Although the embodiment of the present invention is described in detail with reference to preferred embodiment, this field
Those of ordinary skill should understand that still be modified or replaced equivalently technical scheme of the present invention, and these are changed
Or equivalent replacement can not make the range of modified technical solution disengaging technical solution of the present invention.
Claims (7)
1. a kind of yellow cadmium system occlusion pigment, it is characterised in that：The colorant powder fineness is 0.5-3 μm；
The preparation method of yellow cadmium system occlusion pigment is：
Using cadmium sulfate, zirconium oxychloride, thiocarbamide, urea, white carbon, polycarboxylate, polyvinylpyrrolidone as raw material, by raw material
Solution is placed in reaction kettle, in 60-200 DEG C of temperature, rotating speed 100-300r/min conditions by stirring to dissolving after being placed in water mixing
Lower reaction 5-24h, after completion of the reaction natural cooling obtain colorant presoma, yellow cadmium is obtained after washing, firing, baking step
It is occlusion pigment finished product；
Cadmium sulfate in raw material, zirconium oxychloride, thiocarbamide, urea, white carbon, polycarboxylate, polyvinylpyrrolidone molar ratio be
（6-15）：（25-40）：（5-35）：（60-250）：（10-50）：（0.02-8.0）：（0.01-4.0）；
The firing step is by lithium fluoride and colorant presoma obtained with mass ratio 0.05-0.1：1 is mixed, ground
After sieve, mixture is calcined into 10-60min under the conditions of 900-1200 DEG C.
2. yellow cadmium as described in claim 1 system occlusion pigment, it is characterised in that：The preparation side of yellow cadmium system occlusion pigment
In method, white carbon is replaced using aerosil powder in raw material.
3. yellow cadmium as described in claim 1 system occlusion pigment, it is characterised in that：The preparation side of yellow cadmium system occlusion pigment
In method, cadmium sulfate in raw material, zirconium oxychloride, thiocarbamide, urea, white carbon, polycarboxylate, polyvinylpyrrolidone molar ratio be
（10-12）：（28-32）：（18-21）：（160-180）：（20-25）：（0.1-6.0）：（0.15-4.0）.
4. yellow cadmium as described in claim 1 system occlusion pigment, it is characterised in that：The preparation side of yellow cadmium system occlusion pigment
In method, after being burnt into step, by the mixed acid pickling of its product, it is neutrality to be then washed to washing lotion again, is then dried again.
5. a kind of using yellow cadmium as described in claim 1 system's occlusion pigment as the ceramic ink of colorant additive, feature
It is：The preparation method of the ceramic ink is to mix colorant with solvent, is ground to grain graininess D100 and is less than 1 μm, wherein
The mass percentage of colorant and solvent is respectively 30-50%, 50-70%.
6. ceramic ink as claimed in claim 5, it is characterised in that：The solvent is ether solvent.
7. a kind of application process of the ceramic ink as described in claim 5-6, it is characterised in that：By the ceramic ink silk-screen or
Person's ink jet printing is calcined in ceramic glaze version under the conditions of 800-1300 DEG C.
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| CN108047810B (en) * | 2017-12-15 | 2020-12-29 | 佛山市扬子颜料有限公司 | Grain size control agent for wrapping red ink and yellow ink, and preparation method and application method thereof |
| IT201800005984A1 (en) * | 2018-06-04 | 2019-12-04 | CERAMIC INK FOR DIGITAL PRINTING AND PROCESS OF PREPARATION OF THE SAME. | |
| CN113429831B (en) * | 2021-07-31 | 2023-03-14 | 石河子大学 | Method for preparing water-based zirconia ceramic ink for ink-jet printing by using microreactor |
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