CN104151943A - Grafting self-dispersive carbon black dispersion liquid and preparation method thereof - Google Patents
Grafting self-dispersive carbon black dispersion liquid and preparation method thereof Download PDFInfo
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- CN104151943A CN104151943A CN201410348975.3A CN201410348975A CN104151943A CN 104151943 A CN104151943 A CN 104151943A CN 201410348975 A CN201410348975 A CN 201410348975A CN 104151943 A CN104151943 A CN 104151943A
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- 239000006185 dispersion Substances 0.000 title claims abstract description 91
- 239000007788 liquid Substances 0.000 title claims abstract description 73
- 239000006229 carbon black Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000049 pigment Substances 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 8
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical group [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 32
- 239000003738 black carbon Substances 0.000 claims description 29
- 235000019241 carbon black Nutrition 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 20
- 235000010288 sodium nitrite Nutrition 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 14
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000000047 product Substances 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- 150000008065 acid anhydrides Chemical class 0.000 claims description 3
- 239000012675 alcoholic extract Substances 0.000 claims description 3
- 125000002843 carboxylic acid group Chemical group 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims description 3
- 125000002490 anilino group Chemical class [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 claims 5
- 239000002245 particle Substances 0.000 abstract description 12
- 238000007639 printing Methods 0.000 abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 3
- -1 aniline compound Chemical class 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N N-phenyl amine Natural products NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 abstract 1
- 241000872198 Serjania polyphylla Species 0.000 abstract 1
- 230000001476 alcoholic effect Effects 0.000 abstract 1
- 239000000976 ink Substances 0.000 description 19
- ALYNCZNDIQEVRV-UHFFFAOYSA-N 4-aminobenzoic acid Chemical compound NC1=CC=C(C(O)=O)C=C1 ALYNCZNDIQEVRV-UHFFFAOYSA-N 0.000 description 14
- 239000003610 charcoal Substances 0.000 description 13
- 150000001448 anilines Chemical class 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 239000004743 Polypropylene Substances 0.000 description 8
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 description 7
- 229950000244 sulfanilic acid Drugs 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000007795 chemical reaction product Substances 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 6
- 239000008187 granular material Substances 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000032683 aging Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 239000003125 aqueous solvent Substances 0.000 description 2
- DMSMPAJRVJJAGA-UHFFFAOYSA-N benzo[d]isothiazol-3-one Chemical compound C1=CC=C2C(=O)NSC2=C1 DMSMPAJRVJJAGA-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 description 1
- 229940005991 chloric acid Drugs 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000006193 diazotization reaction Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
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- Inks, Pencil-Leads, Or Crayons (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a grafting self-dispersive carbon black dispersion liquid and a preparation method thereof. The dispersion liquid which is stably stored under the conditions of high temperature and normal temperature is obtained by removing unsatisfactory carbon black particles through centrifugal filtration after carbon black with a surface with polar reaction groups, namely phenolic hydroxyl group, alcoholic hydroxyl group, carboxyl group and the like, and an aniline compound capable of reacting with the groups on the surface of the carbon black are selected to react under a catalyst and certain condition. The grafting self-dispersive carbon black dispersion liquid disclosed by the invention has the characteristic of grafting self-dispersion; water-based ink-jet ink processed through the grafting self-dispersive carbon black dispersion liquid has very good printing property, is smooth without plugging a head, is sharp in printing letter on common carbon paper and resistant in erasure, meet the requirement of thermally foamed type printing ink and can serve as a water-based carbon black pigment dispersion liquid of a thermally foamed type ink-jet printer.
Description
Technical field
The present invention relates to a kind of grafting from disperse black carbon dispersion liquid and preparation method thereof.
Background technology
At present, the preparation of carbon black color paste mainly contains that dispersion agent (or resin) disperses and to two kinds of methods of carbon black graft modification.
Dispersion agent dispersion technology is exactly the effect (normally disperseing to combine with grinding) by mechanical external force, make the pigment pulverizing of flocculating and the primary particle that is dispersed into mutual isolation, dispersant adsorption makes it charged in surface of pigments simultaneously, and form electric double layer around at pigment particles, produce mutual repulsive force, thereby reach the effect of stable dispersion within the shelf lives.
By grafting, carbon blacksurface being carried out to modification, is the new technology in carbon black dispersion field thereby reach stable dispersion.Charcoal blacks surface comprises multiple different functional group, has developed the surface that some methods are carried out modified pigment both at home and abroad, and some is to carry out modification by polymkeric substance, and some is polymer-modified by diazotization; By being prepared by the technology of carbon blacksurface modification to carbon black color paste, be applied to spray ink Printing field at home also in more blank.
Dispersion agent disperse black carbon mill base is only applicable in ink-jet field, in piezoelectric ink jet technique class ink, conventionally show blackness not high in the ink of thermal ink-jetting process type conventionally, the high defect of modulation ink difficulty, and application is restricted.
Summary of the invention
In order to solve above-mentioned existing problems, the present invention has prepared from disperse black carbon dispersion liquid from dispersion technology by connecing skill, is a kind of ink-jet nano-water dispersible pigment dispersion, and in the ink applicable to piezo type and thermal type, its application is more extensive.
The object of the present invention is to provide a kind of grafting from disperse black carbon dispersion liquid.
Another object of the present invention is to provide the preparation method of a kind of grafting from disperse black carbon dispersion liquid.
The technical solution used in the present invention is:
Grafting, from a disperse black carbon dispersion liquid, is made by the raw material of following mass fraction: 10～15 parts of carbon blacks, 1～3 part of amino benzenes compounds, 0.5～3 part of catalyzer, 0～0.5 part, sterilant, 79 ~ 87 parts of solvents.
Further, above-mentioned carbon black is that surface is with the carbon black of polar reaction group.
Further, above-mentioned polar reaction group is at least one in phenolic hydroxyl group, alcoholic extract hydroxyl group, carboxyl.
Further, above-mentioned amino benzenes compounds is amino benzenes compounds or its salt with acidic-group.
Further, above-mentioned acidic-group is selected from least one in carboxylic acid group, sulfonic group, acid anhydrides.
Further, above-mentioned catalyzer is Sodium Nitrite, or is the composition of Sodium Nitrite and acid additive.
Further, above-mentioned solvent is water, or is the mixture of water and following at least one material: Diethylene Glycol, triethylene glycol, glycerine, 1,3-PD.
Further, in said mixture, the mass percent of water is not less than 95%.
Grafting, from a preparation method for disperse black carbon dispersion liquid, comprises the following steps:
1) by following quality proportioning, take each raw material: 10～15 parts of carbon blacks, 1～3 part of amino benzenes compounds, 0.5～3 part of catalyzer, 0～0.5 part, sterilant, 79 ~ 87 parts of solvents;
2) amino benzenes compounds and sterilant are added in solvent, stir it is fully dissolved;
3) under the rotating speed of 800～1000 rpm, will in above-mentioned amino benzenes compounds solution, add carbon black, obtain the pigment composition mixing, then toward wherein adding catalyzer, the conditions of 50～90 ℃, continue stirring reaction 10～20h;
4) reacted product is transferred in tubular-bowl centrifuge and carries out centrifugal treating, centrifugal rotational speed is 8000～15000rpm, and centrifugal flow is 0.5～5kg/min, obtains the dispersion liquid after centrifugal treating;
5) above-mentioned dispersion liquid is filtered, get filtrate and be grafting from disperse black carbon dispersion liquid.
Further, step 2) rotating speed of described stirring is 300～500rpm, and churning time is 10～30min.
The invention has the beneficial effects as follows:
1) the granularity D of dispersion liquid of the present invention
99all be less than 300nm, in the time of 30 ℃, viscosity is less than 2.5cP, and surface tension is all greater than 70mN/m, has grafting from the feature of dispersion liquid; Stable performance under high temperature, normal temperature condition, can be used for the aqueous carbon black pigment dispersion liquid of Thermal Bubble Ink-jet Printer printer.
2) the preparation-obtained ink-jet of the inventive method, with nano aqueous carbon black from dispersion liquid, possesses from disperseing the high surface tension of mill base, low viscous feature, and aging rear viscosity, change of granularity is little, meets the requirement of stability; The ink for ink-jet print that the ink-jet that method of the present invention prepares is processed into from dispersion liquid with nano aqueous Pigment black, test printing smoothness plug not on ink-jet printer, on common transfer paper, printing character is sharp keen, and resistance to wiping meets the requirement of heat foamable formula marking ink.Dispersion liquid of the present invention can be used as the aqueous carbon black pigment dispersion liquid of Thermal Bubble Ink-jet Printer printer.
Embodiment
Grafting, from a preparation method for disperse black carbon dispersion liquid, comprises the following steps:
1) take the raw material of following quality proportioning: 10～15 parts of carbon blacks, 1～3 part of amino benzenes compounds, 0.5～3 part of catalyzer, 0～0.5 part, sterilant, 79 ~ 87 parts of solvents;
2) amino benzenes compounds and sterilant are added in solvent, stir it is fully dissolved;
3) under the rotating speed of 800～1000 rpm, will in above-mentioned amino benzenes compounds solution, add carbon black, obtain the pigment composition mixing, then toward wherein adding catalyzer, the conditions of 50～90 ℃, continue stirring reaction 10～20h;
4) reacted product is transferred in tubular-bowl centrifuge and carries out centrifugal treating, centrifugal rotational speed is 8000～15000rpm, and centrifugal flow is 0.5～5kg/min, obtains the dispersion liquid after centrifugal treating;
5) above-mentioned dispersion liquid is filtered, get filtrate and be grafting from disperse black carbon dispersion liquid.
Preferably, above-mentioned carbon black is that surface is with the carbon black of polar reaction group.
Preferably, above-mentioned polar reaction group is at least one in phenolic hydroxyl group, alcoholic extract hydroxyl group, carboxyl.
Preferably, above-mentioned amino benzenes compounds is amino benzenes compounds or its salt with acidic-group.。
Preferably, above-mentioned acidic-group is selected from least one in carboxylic acid group, sulfonic group, acid anhydrides.
Further preferred, above-mentioned amino benzenes compounds is para-amino benzoic acid or Sulphanilic Acid.
Preferably, above-mentioned catalyzer is Sodium Nitrite, or is the composition of Sodium Nitrite and acid additive.
Preferably, above-mentioned acid additive is selected from hydrochloric acid, sulfuric acid, crosses at least one in chloric acid, acetic acid.
Preferably, above-mentioned solvent is water, or is the mixture of water and following at least one material: Diethylene Glycol, triethylene glycol, glycerine, 1,3-PD.
Preferably, in said mixture, the mass percent of water is not less than 95%.
Preferably, above-mentioned steps 2) rotating speed of described stirring is 300～500rpm, and churning time is 10～30min.
Further preferred, above-mentioned steps 2) rotating speed of described stirring is 500rpm, and churning time is 20min.
Preferably, above-mentioned steps 2) temperature of described stirring is 50 ~ 100 ℃.
Preferably, above-mentioned steps 3) temperature of described reaction is 80 ℃.
Preferably, above-mentioned steps 3) rotating speed of described stirring is 800rpm.
Preferably, above-mentioned steps 5) in filter to adopt aperture precision be the filtration unit of 0.22～0.5 μ m.
Below in conjunction with specific embodiment, the present invention is further illustrated, but be not limited to this.
embodiment 1
1) take the raw material of following quality hundred umbers: 15 parts of the C.I.PBK7 carbon blacks of U.S. Cabot Cabot company, 1 part of para-amino benzoic acid, 1 part of catalyzer Sodium Nitrite, 83 parts of solvent deionized water;
2) 77 parts of deionized waters are heated to 80 ℃ and constant temperature, add 1 part of graft compound para-amino benzoic acid, in container, be stirred to completely and be uniformly dissolved, mixing speed is 500rpm, and the time is 20min;
3) under the speed conditions of 1000 rpm, 15 parts of Cabot charcoal blacks will be added in above-mentioned mixed solution, the charcoal blacks mixture that obtains being mixed, 1 part of catalyzer Sodium Nitrite is dissolved in deionized water in the deionized water of 6 parts, after dissolving well, slowly add in pigment composition, under 80 ℃ of conditions of constant temperature, the stirring velocity reaction 12h with 800rpm, is cooled to room temperature;
4) reacted product is transferred to and in whizzer, carries out centrifugal treating, centrifugal rotational speed is 8000rpm, centrifugal flow is 4.5kg/min, obtain the dispersion liquid after centrifugal treating, centrifugal treating is for by reaction product part unreacted or react completely, and a small amount of particle diameter larger granules of pigments is got rid of;
5) dispersion liquid after centrifugal treating processing being filtered with PP filter membrane or 0.5 μ m foldable filter element that precision is 0.22 μ m, get filtrate and be grafting from disperse black carbon dispersion liquid, is a kind of ink-jet nano-water dispersible pigment dispersion.
embodiment 2
1) take the raw material of following quality hundred umbers: 15 parts of the C.I.PBK7 carbon blacks of U.S. Cabot Cabot company, 2 parts of para-amino benzoic acid, 2 parts of catalyzer Sodium Nitrites, 81 parts of solvent deionized water;
2) 75 parts of deionized waters are heated to 80 ℃ and constant temperature, add 2 parts of graft compound para-amino benzoic acid, in container, be stirred to completely and be uniformly dissolved, mixing speed is 500rpm, and the time is 20min;
3) under the speed conditions of 1000 rpm, 15 parts of Cabot charcoal blacks will be added in above-mentioned mixed solution, the charcoal blacks mixture that obtains being mixed, 2 parts of catalyzer Sodium Nitrites are dissolved in deionized water in the deionized water of 6 parts, after dissolving well, slowly add in pigment composition, under 80 ℃ of conditions of constant temperature, the stirring velocity reaction 12h with 800rpm, is cooled to room temperature;
4) reacted product is transferred to and in whizzer, carries out centrifugal treating, centrifugal rotational speed is 8000rpm, centrifugal flow is 4.5kg/min, obtain the dispersion liquid after centrifugal treating, centrifugal treating is for by reaction product part unreacted or react completely, and a small amount of particle diameter larger granules of pigments is got rid of;
5) dispersion liquid after centrifugal treating processing being filtered with PP filter membrane or 0.5 μ m foldable filter element that precision is 0.22 μ m, get filtrate and be grafting from disperse black carbon dispersion liquid, is a kind of ink-jet nano-water dispersible pigment dispersion.
embodiment 3
1) take the raw material of following quality hundred umbers: 15 parts of the C.I.PBK7 carbon blacks of U.S. Cabot Cabot company, 3 parts of para-amino benzoic acid, 3 parts of catalyzer Sodium Nitrites, 79 parts of solvent deionized water;
2) 69 parts of deionized waters are heated to 80 ℃ and constant temperature, add 3 parts of graft compound para-amino benzoic acid, in container, be stirred to completely and be uniformly dissolved, mixing speed is 500rpm, and the time is 20min;
3) under the speed conditions of 1000 rpm, 15 parts of Cabot charcoal blacks will be added in above-mentioned mixed solution, the charcoal blacks mixture that obtains being mixed, 3 parts of catalyzer Sodium Nitrites are dissolved in deionized water in the deionized water of 10 parts, after dissolving well, slowly add in pigment composition, under 80 ℃ of conditions of constant temperature, the stirring velocity reaction 12h with 800rpm, is cooled to room temperature;
4) reacted product is transferred to and in whizzer, carries out centrifugal treating, centrifugal rotational speed is 8000rpm, centrifugal flow is 4.5kg/min, obtain the dispersion liquid after centrifugal treating, centrifugal treating is for by reaction product part unreacted or react completely, and a small amount of particle diameter larger granules of pigments is got rid of;
5) dispersion liquid after centrifugal treating processing being filtered with PP filter membrane or 0.5 μ m foldable filter element that precision is 0.22 μ m, get filtrate and be grafting from disperse black carbon dispersion liquid, is a kind of ink-jet nano-water dispersible pigment dispersion.
embodiment 4
1) take the raw material of following quality hundred umbers: 15 parts of the C.I. PBK7 carbon blacks of Degussa, 2 parts of Sulphanilic Acid, 1 part of 1 part of catalyzer hydrochloric acid and Sodium Nitrite, 77 parts of deionized waters and 4 parts of Diethylene Glycol solvents;
2) 77 parts of deionized waters and 4 parts of Diethylene Glycols are stirred and be heated to 90 ℃ and constant temperature, add 2 parts of graft compound Sulphanilic Acid, in container, be stirred to completely and be uniformly dissolved, mixing speed is 500rpm, and the time is 10min;
3) under the speed conditions of 800 rpm, 15 parts of Degussa charcoal blacks will be added in above-mentioned mixed solution, the charcoal blacks mixture that obtains being mixed, 1 part of catalyzer hydrochloric acid and 1 part of Sodium Nitrite add in pigment composition, under 90 ℃ of conditions of constant temperature, stirring velocity reaction 10h with 1000rpm, is cooled to room temperature;
4) reacted product is transferred to and in whizzer, carries out centrifugal treating, centrifugal rotational speed is 15000rpm, centrifugal flow is 5kg/min, obtain the dispersion liquid after centrifugal treating, centrifugal treating is for by reaction product part unreacted or react completely, and a small amount of particle diameter larger granules of pigments is got rid of;
5) dispersion liquid after centrifugal treating processing being filtered with PP filter membrane or 0.5 μ m foldable filter element that aperture precision is 0.2 μ m, get filtrate and be grafting from disperse black carbon dispersion liquid, is a kind of ink-jet nano-water dispersible pigment dispersion.
embodiment 5
1) take the raw material of following quality hundred umbers: 10 parts of the C.I. PBK7 carbon blacks of Degussa, 2 parts of Sulphanilic Acid, 1 part of catalyst sulfuric acid of catalyzer and 1 part of Sodium Nitrite, 0.2 part of sterilant BIT-20,81.8 parts of water and 4 parts of 1,3-PDs;
2) 81.8 parts of water and 4 parts of 1,3-PDs are heated to 90 ℃ and constant temperature, add 2 parts of graft compound Sulphanilic Acid, 0.2 part of sterilant BIT-20 is stirred to completely and is uniformly dissolved in container, and mixing speed is 300rpm, and the time is 30min;
3) under the speed conditions of 1000 rpm, 10 parts of Degussa charcoal blacks will be added in above-mentioned mixed solution, the charcoal blacks mixture that obtains being mixed, 1 part of catalyst sulfuric acid and 1 part of Sodium Nitrite add in pigment composition, under 90 ℃ of conditions of constant temperature, stirring velocity reaction 20h with 800rpm, is cooled to room temperature;
4) reacted product is transferred to and in whizzer, carries out centrifugal treating, centrifugal rotational speed is 8000rpm, centrifugal flow is 0.5kg/min, obtain the dispersion liquid after centrifugal treating, centrifugal treating is for by reaction product part unreacted or react completely, and a small amount of particle diameter larger granules of pigments is got rid of;
5) dispersion liquid after centrifugal treating processing being filtered with PP filter membrane or 0.5 μ m foldable filter element that aperture precision is 0.22 μ m, get filtrate and be grafting from disperse black carbon dispersion liquid, is a kind of ink-jet nano-water dispersible pigment dispersion.
embodiment 6
1) take the raw material of following quality hundred umbers: 10 parts of the C.I. PBK7 carbon blacks of Degussa, 2 parts of Sulphanilic Acid, 0.5 part of Sodium Nitrite of catalyzer, 0.5 part of sterilant BIT-20,87 parts of aqueous solvent;
2) 87 parts of aqueous solvent are heated to 90 ℃ and constant temperature, add 0.5 part of 2 parts of graft compound Sulphanilic Acid and sterilant BIT-20 to be stirred to completely and to be uniformly dissolved in container, mixing speed is 300rpm, and the time is 30min;
3), under the speed conditions of 1000 rpm, will in above-mentioned mixed solution, add 10 parts of Degussa charcoal blacks, the charcoal blacks mixture that obtains being mixed, 0.5 part of Sodium Nitrite is added in pigment composition, under 90 ℃ of conditions of constant temperature, the stirring velocity reaction 20h with 800rpm, is cooled to room temperature;
4) reacted product is transferred to and in whizzer, carries out centrifugal treating, centrifugal rotational speed is 8000rpm, centrifugal flow is 0.5kg/min, obtain the dispersion liquid after centrifugal treating, centrifugal treating is for by reaction product part unreacted or react completely, and a small amount of particle diameter larger granules of pigments is got rid of;
5) dispersion liquid after centrifugal treating processing being filtered with PP filter membrane or 0.5 μ m foldable filter element that aperture precision is 0.22 μ m, get filtrate and be grafting from disperse black carbon dispersion liquid, is a kind of ink-jet nano-water dispersible pigment dispersion.
The grafting of preparing in embodiment is made to further effect detection from disperse black carbon dispersion liquid below.
The carbon black dispersion liquid of preparation in the present embodiment 1 ~ 3 is tested to its stability and print performance with the following methods.
one, whether the physicochemical characteristics of test dispersion liquid meets from the feature and the stability test thereof that disperse mill base
According to existing, to the analysis from disperse black carbon dispersion liquid, from the dispersion liquid of dispersal pattern, there is low viscosity, high capillary feature, common viscosity <3.0 cP in the time of 30 ℃, the features such as surface tension >70mN/m.
By the ink-jet nano-water dispersible pigment dispersion preparing in embodiment 1 ~ 3, be contained in the round vase of 1kg, be directly placed in the constant temperature oven of 60 ℃ 7 days, the D of contrast before and after placing
99the variation of particle diameter, viscosity (30 ℃), compares.D
99corresponding particle diameter when the number cumulative particle size distribution percentage ratio that refers to sample particle reaches 99%.
Table 1 embodiment 1 ~ 3 stability test result
The physicochemical property that the dispersion liquid making in embodiment 1-3 is carried out is tested as shown in table 1, therefrom the granularity D of known dispersion liquid
99all be less than 300nm, in the time of 30 ℃, viscosity is less than 2.5cP, and surface tension is all greater than 70mN/m, has grafting from the feature of dispersion liquid; The dispersion liquid of preparation is carried out to test in aging 1 week, and with aging front contrast, change of granularity is very little, aging rear D
99still, in 300nm, viscosity variation is less than 1cP; As can be seen from Table 1 optimum dispersion liquid formula is embodiment 2.
two, be mixed with ink and print performance test
The ink-jet nano-water dispersible pigment dispersion that embodiment 1 ~ 3 is prepared, the formulated providing according to table 2 becomes water-based jet ink, concrete operations are for adding successively deionized water, wetting Agent for Printing Inks, auxiliary agent, sterilant according to the ratio of formula, the dispersion liquid that adds again this experiment to make after stirring, under the condition of rotating speed 300-500 rpm, stir 30min, by aperture precision, be finally the polypropylene PP membrane filtration of 0.22 μ m, be made into ink for ink-jet print.
In table 2 embodiment 1 ~ 3, the dispersion liquid of preparation is processed into the formula of water-based jet ink
The water-based jet ink being processed in table 2 is printed to test, on Canon IP 4980 printers, be set to common paper/gray level printing, the monochromatic color lump of black and document that printing fraction of coverage is 90%.Water-based jet ink on Canon IP4980, print continuously monochromatic color lump that fraction of coverage is 90% more than 15 pages smoothness do not stop up printhead,, on common transfer paper, typewrite clear sharp keen meanwhile, be judged as " good ".Test result is as shown in table 3, therefrom can find out that the water-based jet ink that dispersion liquid of the present invention is processed into has good print performance.
Table 3 dispersion liquid of the present invention is processed into the print performance test result of water-based jet ink
In sum, the preparation-obtained ink-jet of the inventive method, possesses from disperseing the high surface tension of mill base from dispersion liquid with nano aqueous carbon black, low viscous feature, and aging rear viscosity, change of granularity is little, meets the requirement of stability; The ink for ink-jet print that the ink-jet that method of the present invention prepares is processed into from dispersion liquid with nano aqueous Pigment black, test printing smoothness plug not on ink-jet printer, on common transfer paper, printing character is sharp keen, and resistance to wiping meets the requirement of heat foamable formula marking ink.
Claims (10)
1. grafting, from a disperse black carbon dispersion liquid, is characterized in that: the raw material by following mass fraction is made: 10～15 parts of carbon blacks, 1～3 part of amino benzenes compounds, 0.5～3 part of catalyzer, 0～0.5 part, sterilant, 79 ~ 87 parts of solvents.
2. a kind of grafting according to claim 1, from disperse black carbon dispersion liquid, is characterized in that: described carbon black is the carbon black of surface with polar reaction group.
3. a kind of grafting according to claim 2, from disperse black carbon dispersion liquid, is characterized in that: described polar reaction group is at least one in phenolic hydroxyl group, alcoholic extract hydroxyl group, carboxyl.
4. a kind of grafting according to claim 1, from disperse black carbon dispersion liquid, is characterized in that: described amino benzenes compounds is amino benzenes compounds or its salt with acidic-group.
5. a kind of grafting according to claim 4, from disperse black carbon dispersion liquid, is characterized in that: described acidic-group is selected from least one in carboxylic acid group, sulfonic group, acid anhydrides.
6. a kind of grafting according to claim 1, from disperse black carbon dispersion liquid, is characterized in that: described catalyzer is Sodium Nitrite, or is the composition of Sodium Nitrite and acid additive.
7. a kind of grafting according to claim 1, from disperse black carbon dispersion liquid, is characterized in that: described solvent is water, or is the mixture of water and following at least one material: Diethylene Glycol, triethylene glycol, glycerine, 1,3-PD.
8. a kind of grafting according to claim 7, from disperse black carbon dispersion liquid, is characterized in that: in described mixture, the mass percent of water is not less than 95%.
9. described in claim 1, a kind of grafting, from the preparation method of disperse black carbon dispersion liquid, is characterized in that: comprise the following steps:
1) by proportioning raw materials claimed in claim 1, take each raw material;
2) amino benzenes compounds and sterilant are added in solvent, stir it is fully dissolved;
3) under the rotating speed of 800～1000 rpm, will in above-mentioned amino benzenes compounds solution, add carbon black, obtain the pigment composition mixing, then toward wherein adding catalyzer, the conditions of 50～90 ℃, continue stirring reaction 10～20h;
4) reacted product is transferred in tubular-bowl centrifuge and carries out centrifugal treating, centrifugal rotational speed is 8000～15000rpm, and centrifugal flow is 0.5～5kg/min, obtains the dispersion liquid after centrifugal treating;
5) above-mentioned dispersion liquid is filtered, get filtrate and be grafting from disperse black carbon dispersion liquid.
10. preparation method according to claim 9, is characterized in that: step 2) rotating speed of described stirring is 300～500rpm, churning time is 10～30min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112456467A (en) * | 2020-11-19 | 2021-03-09 | 沈阳化工研究院有限公司 | Modified carbon black applied to spinning resin coloring and preparation method thereof |
| CN114437570A (en) * | 2020-11-05 | 2022-05-06 | 中国石油化工股份有限公司 | Preparation method of nano cross-linking agent for guanidine gum fracturing fluid and prepared cross-linking agent |
| CN117025026A (en) * | 2023-09-11 | 2023-11-10 | 青岛亚坦文具有限公司 | Preparation method of inkjet ink |
| CN117186688A (en) * | 2023-08-31 | 2023-12-08 | 广东超邦科技有限公司 | Water-based self-dispersion pigment ink and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1160415A (en) * | 1994-12-15 | 1997-09-24 | 卡伯特公司 | Ink jet ink formulations contg. modified carbon products |
| WO1997038053A2 (en) * | 1996-04-05 | 1997-10-16 | Cabot Corporation | Ink compositions and method for generating images produced therefrom |
| CN1227584A (en) * | 1996-06-14 | 1999-09-01 | 卡伯特公司 | Modified carbon products for inks and coatings |
| US6069190A (en) * | 1996-06-14 | 2000-05-30 | Cabot Corporation | Ink compositions having improved latency |
| US6328894B1 (en) * | 1998-01-29 | 2001-12-11 | Cabot Corporation | Processes of purifying a dispersion and making inkjet inks |
-
2014
- 2014-07-21 CN CN201410348975.3A patent/CN104151943A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1160415A (en) * | 1994-12-15 | 1997-09-24 | 卡伯特公司 | Ink jet ink formulations contg. modified carbon products |
| WO1997038053A2 (en) * | 1996-04-05 | 1997-10-16 | Cabot Corporation | Ink compositions and method for generating images produced therefrom |
| CN1227584A (en) * | 1996-06-14 | 1999-09-01 | 卡伯特公司 | Modified carbon products for inks and coatings |
| US6069190A (en) * | 1996-06-14 | 2000-05-30 | Cabot Corporation | Ink compositions having improved latency |
| US6328894B1 (en) * | 1998-01-29 | 2001-12-11 | Cabot Corporation | Processes of purifying a dispersion and making inkjet inks |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114437570A (en) * | 2020-11-05 | 2022-05-06 | 中国石油化工股份有限公司 | Preparation method of nano cross-linking agent for guanidine gum fracturing fluid and prepared cross-linking agent |
| CN114437570B (en) * | 2020-11-05 | 2023-06-27 | 中国石油化工股份有限公司 | Preparation method of nano cross-linking agent for guanidine gum fracturing fluid and prepared cross-linking agent |
| CN112456467A (en) * | 2020-11-19 | 2021-03-09 | 沈阳化工研究院有限公司 | Modified carbon black applied to spinning resin coloring and preparation method thereof |
| CN117186688A (en) * | 2023-08-31 | 2023-12-08 | 广东超邦科技有限公司 | Water-based self-dispersion pigment ink and preparation method thereof |
| CN117025026A (en) * | 2023-09-11 | 2023-11-10 | 青岛亚坦文具有限公司 | Preparation method of inkjet ink |
| CN117025026B (en) * | 2023-09-11 | 2024-04-02 | 青岛亚坦文具有限公司 | A kind of preparation method of inkjet ink |
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