CN116254018A - Modified carbon black color paste applied to pigment inkjet ink and preparation method thereof - Google Patents
Modified carbon black color paste applied to pigment inkjet ink and preparation method thereof Download PDFInfo
- Publication number
- CN116254018A CN116254018A CN202111505050.1A CN202111505050A CN116254018A CN 116254018 A CN116254018 A CN 116254018A CN 202111505050 A CN202111505050 A CN 202111505050A CN 116254018 A CN116254018 A CN 116254018A
- Authority
- CN
- China
- Prior art keywords
- carbon black
- modified carbon
- solution
- color paste
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000006229 carbon black Substances 0.000 title claims abstract description 81
- 150000001721 carbon Chemical class 0.000 title claims abstract description 40
- 239000000049 pigment Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims description 12
- 239000000976 ink Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims description 25
- 239000003607 modifier Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 15
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 235000010288 sodium nitrite Nutrition 0.000 claims description 6
- 238000006193 diazotization reaction Methods 0.000 claims description 5
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- 239000012954 diazonium Substances 0.000 claims description 2
- 150000001989 diazonium salts Chemical class 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 7
- 238000004519 manufacturing process Methods 0.000 claims 2
- APRRQJCCBSJQOQ-UHFFFAOYSA-N 4-amino-5-hydroxynaphthalene-2,7-disulfonic acid Chemical compound OS(=O)(=O)C1=CC(O)=C2C(N)=CC(S(O)(=O)=O)=CC2=C1 APRRQJCCBSJQOQ-UHFFFAOYSA-N 0.000 claims 1
- 239000012670 alkaline solution Substances 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 9
- 238000007641 inkjet printing Methods 0.000 abstract description 5
- 239000004922 lacquer Substances 0.000 abstract 1
- 239000003973 paint Substances 0.000 abstract 1
- 239000002023 wood Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 22
- QPILZZVXGUNELN-UHFFFAOYSA-M sodium;4-amino-5-hydroxynaphthalene-2,7-disulfonate;hydron Chemical compound [Na+].OS(=O)(=O)C1=CC(O)=C2C(N)=CC(S([O-])(=O)=O)=CC2=C1 QPILZZVXGUNELN-UHFFFAOYSA-M 0.000 description 8
- 230000008859 change Effects 0.000 description 7
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- 238000009826 distribution Methods 0.000 description 5
- 238000007639 printing Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 238000012544 monitoring process Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 3
- 239000011324 bead Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 102220042174 rs141655687 Human genes 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000000123 paper Substances 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical class OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 description 1
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- YWXCBLUCVBSYNJ-UHFFFAOYSA-N 2-(2-sulfanylethylsulfonyl)ethanethiol Chemical group SCCS(=O)(=O)CCS YWXCBLUCVBSYNJ-UHFFFAOYSA-N 0.000 description 1
- 241000872198 Serjania polyphylla Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229950000244 sulfanilic acid Drugs 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- NJRXVEJTAYWCQJ-UHFFFAOYSA-N thiomalic acid Chemical compound OC(=O)CC(S)C(O)=O NJRXVEJTAYWCQJ-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
- 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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/005—Carbon black
-
- 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
- C09D11/324—Inkjet printing inks characterised by colouring agents containing carbon black
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention is used in the field of high-grade ink-jet printing ink, in particular to modified carbon black color paste applied to pigment ink-jet ink. The modified carbon black is shown in the following structural formula; the invention also prepares the carbon black color paste by using the modified carbon black through a certain process condition. The carbon black color paste can meet the application field requirements of digital ink, paint, wood lacquer and the like.
Description
Technical Field
The invention is used in the field of high-grade ink-jet printing ink, in particular to modified carbon black color paste applied to pigment ink-jet ink.
Background
The ink jet printing technology has been rising in the last 80 th century, and early dye inks were prepared by directly dissolving pigments in the ink, which had poor durability and water resistance. The black azo dye is replaced by carbon black later, so that the stability of the ink is improved, but the ink has insufficient performance in high-end printing occasions such as office and outdoor advertising.
The pigment inkjet ink required in the current high-end printing occasion needs to have the characteristics of superfine pigment particle size, higher storage stability, pure and stable color and the like, and has higher technical threshold and high added value. In general, it is necessary to grind pigment particles, and when the pigment is ground into nano-sized particles of about 100nm, the pigment particles are more likely to reagglomerate due to interactions between the particles, resulting in a re-increase in particle size and an increase in viscosity of the system. In addition, in the process of ink-jet printing, the aggregation of pigment particles can cause the blockage of a printer nozzle, can also affect the printing quality, and cannot meet the high-end application requirements.
In order to solve these problems, it is now possible to enhance the dispersibility of pigments by modifying the surface of the pigments in addition to the addition of dispersants. The pigment surface modification is to select proper surface modifier to cover the surface of pigment to change the polarity of pigment and to raise the matching performance with dispersing medium.
One patent reported by the de-solid company in 2009 (CN 101597441) mentions a method of surface modification of pigments (carbon black): a pigment (carbon black) to be modified is bonded to a substituted or unsubstituted 1, 2-benzenedicarboxylic acid having an amine group or a salt thereof by diazotization coupling reaction, and the modified pigment is useful for improving the inter-color bleed control of an inkjet ink. Inkjet inks are used to print fabrics, foils, films, sheets and papers. The modification process is shown as the following formula:
the use of mercaptosuccinic acid to modify carbon black containing a mercaptoethyl sulfone group is reported by the cabot corporation in 2003 (CN 1665896 a), and after a certain post-treatment, the particle size distribution of the modified carbon black paste is about 112nm, but the storage time of the modified carbon black is not preferred to exceed 3 months.
The color company of sen describes a method of preparing a self-dispersing pigment in one of 2008 (CN 101855302). The pigment surface is modified by covalent bonding and the end use can be used for paper, textile, fiber, metal ornaments and plastic, wood coloration, writing instruments and filter printing inks. The modification process involves linking the organic groups and charged end groups by an intermediate in the reactive molecule to produce a surface stable modified pigment. The stabilization is achieved by a homogeneous distribution of similarly charged groups that are covalently bound to the submicron pigment particles by repulsive forces. In a specific example, the modified carbon black can be prepared by chloridizing carbon black with chlorosulfonic acid and then reacting with sulfanilic acid.
In order to smooth the printing process, the spray nozzle is not blocked and stained in the long-term use process, and the printed image is kept to be high in stability, so that the pigment color paste is required to be nanocrystallized. Meanwhile, the nano pigment color paste needs to have higher dispersion stability, so that the particle size of the color paste is ensured not to change in the high-temperature and low-temperature environment in the transportation and storage processes. However, the stability of the modified carbon black in the above patent is still to be solved, so that the technical problem that the normal carbon black is easy to agglomerate when stored in an aqueous system for a long time needs to be solved, and the modified carbon black can be modified and is connected with a high-polarity group with stronger hydrophilicity. Meanwhile, the common carbon black color paste in the market usually emits red phase, and the blue light carbon black is more suitable for aesthetic sense of people, and is more high-grade and is mostly used in high-grade ink-jet printing.
Disclosure of Invention
The invention relates to a modified carbon black color paste applied to pigment inkjet ink and a preparation method thereof.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
modified carbon black color paste applied to pigment inkjet ink, wherein the modified carbon black is shown in the following structural formula:
wherein ∈is carbon black, R 4 、R 5 Can be identical or different and are selected from-CH 3 Or H; r is R 1 、R 2 R is R 3 Are selected from polar groups which may be the same or different.
R in the structural formula of the modified carbon black 1 、R 2 R is R 3 Can be identical or different and are selected from-SO 3 H. Carboxyl or-OH; r is R 4 、R 5 Can be identical or different and are selected from-CH 3 Or H.
The preparation method of the modified carbon black color paste applied to pigment inkjet ink comprises the steps of adding diazonium salt and a modifier into carbon black serving as a raw material to carry out diazotization reaction, adjusting the pH value of a reaction system to be alkaline, and filtering and discharging to obtain the modified carbon black.
The reaction formula is as follows:
the diazotization reaction in the preparation method of the modified carbon black color paste is to take carbon black as a raw material, add deionized water in the range of normal temperature to 50 ℃, and fully stir, wherein the mass ratio of water to carbon black is 20:1-5:1; then adding a modifier, continuously stirring for half an hour, adding hydrochloric acid equivalent to the modifier sample and sodium nitrite solution with mass fraction of 5% -25%, reacting for 12-24 hours, and detecting the end point of the reaction by using a newly prepared H acid solution; wherein the mass ratio of the modifier to the carbon black is 1:10-3:1, and the molar ratio of the modifier to the sodium nitrite is 1:1-1.5:1.
And after the reaction is detected to be carried out to an end point, adding an alkali solution into the reaction system to adjust the pH to 7-9.
The alkali liquor is selected from one or more of sodium carbonate solution, sodium bicarbonate solution, potassium carbonate solution, potassium bicarbonate solution, sodium hydroxide solution and potassium hydroxide solution.
The application of the modified carbon black color paste in pigment inkjet ink.
The invention has the advantages that:
according to the invention, the high-polarity hydrophilic and easy-to-disperse groups such as sulfonic groups are introduced into the surface of the carbon black, so that the polarity of the carbon black is changed, the water solubility of the carbon black is increased, the carbon black is easier to disperse in water, and the amino groups in the modifier molecules can also enable each pigment molecule to generate intermolecular hydrogen bond interaction and the like, so that the stability of carbon black particles can be improved. After the carbon black color paste is stored and tested, various values such as particle size, conductivity and viscosity are not obviously changed. Meanwhile, as the molecular skeleton of the acid blue 52 is adopted in the molecular structure of the modifier, the color of the modified carbon black color paste can be changed into blue light black, so that the product has higher quality and better appearance.
Detailed Description
The following description of the embodiments of the present invention is further provided in connection with the accompanying examples, and it should be noted that the embodiments described herein are for the purpose of illustration and explanation only, and are not limiting of the invention.
The raw materials in the examples described below are all commercially available.
Preparation example
Example 1
(1) Carbon black modification
The reaction formula is:
200g of carbon black powder was added to a 3000mL four-necked flask, 2000mL of distilled water was added thereto, and after sufficient stirring, 20g of modifier 1 and 5g of hydrochloric acid (mass fraction: 36%) were added thereto, and after stirring at room temperature for 30 minutes, 15.9g of 20% by mass sodium nitrite solution was added dropwise. And after the sodium nitrite solution is completely dripped, heating to 40 ℃, and keeping the reaction temperature until the reaction is finished. And (3) adding 30mL of deionized water and a small amount of sodium carbonate into 0.2g H acid until the solution is completely dissolved to obtain a new H acid solution, monitoring the reaction process by using the H acid solution, observing the joint position of a permeation ring of the reaction solution and the H acid solution, taking out the joint position after 18 hours of reaction, and taking out the reaction, wherein the pH of the material is adjusted to 8-9, filtering, washing with 1000mL of deionized water, and obtaining a filter cake with a wet weight of 500g and a solid content of 42% for the next processing without drying.
(2) Preparation of color paste
Adding 500g of the wet filter cake obtained in the last step into a 3000mL beaker, adding 900g of deionized water, stirring for 60min at 3000r/min by using a stirrer, adding the obtained black paste into a horizontal sand mill, adding 0.6-0.8 mm zirconium beads accounting for 20% of the mass of the material, circularly sanding for 4h, monitoring the particle size change in the sanding process by using a nano-particle size zeta potential analyzer, and finally obtaining the color paste with the particle size D90=130 nm.
Example 2
(1) Carbon black modification
The reaction formula is:
taking 100g of carbon black powder, adding 1000mL of deionized water, stirring until dispersion, adding 10g of modifier 2 while stirring, dispersing for 5min, adding 3g of hydrochloric acid with the mass fraction of 36%, stirring for 30min at normal temperature, and dripping NaNO 2 7.5g (mass fraction 20%) of the solution was added dropwise over 20min, followed by heating to 40 ℃. The reaction was incubated at this temperature and the extent of progress of the reaction was monitored using a fresh H acid solution. After 21H of reaction, no obvious purple appears at the junction of the permeation ring and the H acid solution, which indicates that the reaction is basically completed, the pH is adjusted to 8-9, and 270g of wet cake with 37% of solid content is obtained after filtration and washing and is used in the subsequent color paste preparation process.
(2) Preparation of color paste
The resulting 270g wet cake of modified carbon black was mixed with 400mL deionized water in a 2000mL beaker and stirred using a stirrer for 1h to thoroughly disperse, with a stirrer revolution of 3000r/min. And placing the obtained feed liquid into a horizontal sand mill, adding 0.6-0.8 mm zirconium beads accounting for 20% of the mass of the feed liquid, circularly sanding, monitoring the particle size change in the sanding process through a nano-particle size zeta potential analyzer, and sanding for 6 hours to obtain the color paste with the particle size D90=128 nm.
Example 3
(1) Carbon black modification
The reaction formula is:
1500mL of deionized water, 150g of carbon black and 15g of modifier 3 are added into a four-mouth bottle, after the mixture is fully stirred for 30min at normal temperature, 3g of concentrated hydrochloric acid is added, and NaNO with the mass fraction of 20% is slowly added dropwise 2 9.7g of the solution was heated to 35-40℃and reacted at this temperature to the end point. The end point of the reaction was detected by fresh H acid solution. After the reaction is finished, regulating the pH of the system to 8-9 by using a potassium carbonate solution with the mass fraction of 5%, discharging and filtering to obtain 360g of wet cake with the solid content of 41.6%, and using the wet cake for the next processing without drying.
(2) Preparation of color paste
360g of the wet cake with a solids content of 41.6% were added to a 2000mL beaker and 650mL of deionized water were added and dispersed by means of a stirrer with a revolution of 3000r/min for 1h. Then the feed liquid is added into a horizontal sand mill, and zirconium beads with the diameter of 0.6-0.8 mm are added, wherein the dosage is 20% of the mass of the material. And (3) after 3.5 hours of circulating sanding, monitoring the particle size change by a nano-particle size zeta potential analyzer to obtain the color paste particle size D90=117 nm.
Application examples
The following examples illustrate in detail the performance and effect of the modified carbon black paste obtained by the preparation of the above examples, taking the samples obtained by the above examples as examples, and the other compounds defined by the present invention also have the corresponding effect characteristics.
1) Filterability test of modified carbon black ink
The filterability of the modified carbon black paste was tested according to the technical conditions of the water-based dye for QBT 4974-2016 inkjet inks. Respectively taking 1000mL of modified color paste, pouring a sample into a liquid storage device provided with a membrane with a filtering precision of 0.45 mu m and a diameter of 47mm, filtering 100mL and 1000mL under 0.2MPa by using an air pump, and recording the time for filtering 100mL of color paste as T 1 The time for filtering 1000mL of color paste is T 2 . Calculate the filterability as T 1 /T 2 . The carbon black paste samples of examples 1 to 3 and cabot were compared as follows:
in the filtration performance test, generally speaking, the faster the filtration speed, the fewer the blocked voids in the filter membrane, and a filtration performance approaching 0.1 indicates that the blocked filter membrane has fewer voids as the filtration proceeds. As can be seen from the above table, the modified carbon black pastes prepared with 3 different modifiers each had a filtration property similar to or even slightly better than that of the Cabot sample, wherein the filtration time T in example 3 2 Is superior to carbon black color paste samples of cabot corporation.
2) Stability test of modified carbon black ink
The stability of the modified carbon black paste was tested according to the method of testing the storage stability of inkjet inks QB/T5489-2020. 30mL of the color paste of examples 1-3 and the sample of cabot corporation were respectively taken and kept at 60 ℃ for 168 hours, and then the viscosity, the particle size distribution, the surface tension value, the conductivity value and the pH value were tested, and the results of calculating the rate of change of each value are shown in the following table:
the color paste samples of examples 1-3 and the carbon black color paste sample of cabot company show little change in viscosity, particle size distribution, surface tension value, conductivity value and pH value in stability test. Wherein the stability of the sample of example 3 was due to the carbon black of cabot corporation.
Comprehensive test data can be seen: the particle size of the carbon black color paste prepared from the modified carbon black can be below 130nm after grinding and other treatments, and meanwhile, the carbon black color paste has good filterability, and the viscosity, the particle size distribution, the surface tension value, the conductivity value and the pH value of the carbon black color paste after stability test are not greatly changed, so that the carbon black color paste prepared from the modified carbon black provided by the invention has excellent dispersibility and stability.
Claims (7)
1. The modified carbon black color paste applied to pigment inkjet ink is characterized in that: the modified carbon black is shown in the following structural formula:
wherein ∈is carbon black, R 4 、R 5 Can be identical or different and are selected from-CH 3 Or H; r is R 1 、R 2 R is R 3 Are selected from polar groups which may be the same or different.
2. The modified carbon black paste of claim 1 wherein R in the modified carbon black formula 1 、R 2 R is R 3 Can be identical or different and are selected from-SO 3 H. Carboxyl or-OH; r is R 4 、R 5 Can be identical or different and are selected from-CH 3 Or H.
3. A process for preparing the modified carbon black paste used for pigment ink-jet ink, which is characterized in that the carbon black is taken as raw material, diazonium salt and modifier are added for diazotization reaction, then the pH value of the reaction system is regulated to be alkaline, and then the carbon black is obtained after filtering and discharging.
4. A process for preparing modified carbon black paste for pigment inkjet inks according to claim 3 wherein,
the reaction formula is as follows:
the diazotization reaction in the preparation method of the modified carbon black color paste is to take carbon black as a raw material, add deionized water in the range of normal temperature to 50 ℃, and fully stir, wherein the mass ratio of water to carbon black is 20:1-5:1; then adding a modifier, continuously stirring for half an hour, adding hydrochloric acid equivalent to the modifier sample and sodium nitrite solution with mass fraction of 5% -25%, reacting for 12-24 hours, and detecting the end point of the reaction by using a newly prepared H acid solution; wherein the mass ratio of the modifier to the carbon black is 1:10-3:1, and the molar ratio of the modifier to the sodium nitrite is 1:1-1.5:1.
5. The method for preparing a modified carbon black paste for pigment inkjet ink according to claim 4 wherein an alkaline solution is added to the reaction system to adjust the pH to 7 to 9 after the reaction is detected to be finished.
6. The method for preparing modified carbon black paste applied to pigment inkjet ink according to claim 4 wherein the alkali solution is selected from one or more of sodium carbonate solution, sodium bicarbonate solution, potassium carbonate solution, potassium bicarbonate solution, sodium hydroxide solution, potassium hydroxide solution.
7. Use of the modified carbon black paste of claim 1, wherein: the modified carbon black color paste is applied to pigment inkjet ink.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111505050.1A CN116254018B (en) | 2021-12-10 | 2021-12-10 | Modified carbon black color paste applied to pigment inkjet ink and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111505050.1A CN116254018B (en) | 2021-12-10 | 2021-12-10 | Modified carbon black color paste applied to pigment inkjet ink and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116254018A true CN116254018A (en) | 2023-06-13 |
| CN116254018B CN116254018B (en) | 2023-10-31 |
Family
ID=86681192
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111505050.1A Active CN116254018B (en) | 2021-12-10 | 2021-12-10 | Modified carbon black color paste applied to pigment inkjet ink and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116254018B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09183224A (en) * | 1996-01-04 | 1997-07-15 | Canon Inc | Black pigment ink, ink set, and ink-jet recording method and ink-jet equipment |
| EP1085060A2 (en) * | 1999-09-17 | 2001-03-21 | Canon Kabushiki Kaisha | Aqueous ink for ink-jet recording, ink set, ink-jet recording process and bleeding reducing method |
| US20040018140A1 (en) * | 2001-07-25 | 2004-01-29 | Degussa Ag | Process for the production of modified carbon black |
| CN101056953A (en) * | 2004-11-04 | 2007-10-17 | 惠普开发有限公司 | Inkjet compositions |
| CN109972425A (en) * | 2017-12-28 | 2019-07-05 | 沈阳化工研究院有限公司 | A kind of carbon black color paste and preparation method thereof |
-
2021
- 2021-12-10 CN CN202111505050.1A patent/CN116254018B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09183224A (en) * | 1996-01-04 | 1997-07-15 | Canon Inc | Black pigment ink, ink set, and ink-jet recording method and ink-jet equipment |
| EP1085060A2 (en) * | 1999-09-17 | 2001-03-21 | Canon Kabushiki Kaisha | Aqueous ink for ink-jet recording, ink set, ink-jet recording process and bleeding reducing method |
| US20040018140A1 (en) * | 2001-07-25 | 2004-01-29 | Degussa Ag | Process for the production of modified carbon black |
| CN101056953A (en) * | 2004-11-04 | 2007-10-17 | 惠普开发有限公司 | Inkjet compositions |
| CN109972425A (en) * | 2017-12-28 | 2019-07-05 | 沈阳化工研究院有限公司 | A kind of carbon black color paste and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116254018B (en) | 2023-10-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109890908B (en) | Process for producing quinacridone solid solution pigment, pigment dispersion liquid, and ink-jet ink | |
| US20040171738A1 (en) | Pigments dispersions based on water and acrylate | |
| BRPI0409672B1 (en) | "PREPARATION OF WATER COLORING, PROCESS FOR PRODUCTION, AND SET OF PRINT INKS UNDERSTANDING THE SAME". | |
| CN102816456B (en) | Method for preparing core pigment red 170 by inorganic nano material modification | |
| CN101942217B (en) | Preparation method for special pigment for aqueous printing ink | |
| CN102847497A (en) | Preparation method and application of nanometer pigment microcapsule | |
| CN102146245B (en) | Lanxiang ultra black automobile refinishing coating and preparation method thereof | |
| CN116254018B (en) | Modified carbon black color paste applied to pigment inkjet ink and preparation method thereof | |
| CN102532938A (en) | Preparation method of pigment preparations containing superfine phthalocyanine pigment particles | |
| CN111902490A (en) | Process for producing quinacridone solid solution pigment, pigment dispersion liquid, and ink-jet ink | |
| CN116751463A (en) | Composite pigment coated with nano aluminum hydroxide and preparation method thereof | |
| US9068093B2 (en) | Surface modification of carbon black | |
| CN105524484A (en) | Preparation method for C.I. pigment red 176 | |
| CN109763353A (en) | A kind of preparation method of UV-curable waterborne printing inks | |
| CN114657799A (en) | Environment-friendly ink-jet printing dye ink for artificial cotton and preparation method thereof | |
| CN110499041B (en) | Preparation method of easy-to-filter EVA wax-based composite spherical pigment yellow 14 | |
| CN106833005A (en) | A kind of method for preparing permeability azo organic pigment high | |
| CN114591514B (en) | Environment-friendly lignin-based dispersing agent for azo pigment and preparation method thereof | |
| EP1762597B1 (en) | Pigment dispersant, and pigment composition, pigment dispersion and printing ink using the same | |
| JP4369115B2 (en) | Process for producing benzimidazolone monoazo pigment composition for ink jet recording | |
| CN103421340A (en) | Preparation method of brilliant orange pigment | |
| JP2005206797A (en) | Alkoxylated polyalkylene imine having anionic group,pigment containing the polyalkylene imine, method for producing the pigment and application of the pigment | |
| CN111423744B (en) | Quinacridone pigment composition and preparation method and application thereof | |
| CN108504190A (en) | A kind of coating heat-transferring printing paper ink and preparation method thereof | |
| CN117024990B (en) | Application of polyether amine-crown ether compound in azo pigment modification |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |