CN116041987A - Preparation method of self-dispersing water-based carbon black - Google Patents
Preparation method of self-dispersing water-based carbon black Download PDFInfo
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- CN116041987A CN116041987A CN202211589704.8A CN202211589704A CN116041987A CN 116041987 A CN116041987 A CN 116041987A CN 202211589704 A CN202211589704 A CN 202211589704A CN 116041987 A CN116041987 A CN 116041987A
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- 239000006229 carbon black Substances 0.000 title claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 30
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 28
- 239000007800 oxidant agent Substances 0.000 claims abstract description 22
- 230000003647 oxidation Effects 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 238000000227 grinding Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 230000001590 oxidative effect Effects 0.000 claims abstract description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 241000872198 Serjania polyphylla Species 0.000 claims abstract description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 7
- 239000001257 hydrogen Substances 0.000 claims abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 7
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 7
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 5
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 claims description 20
- 238000004519 manufacturing process Methods 0.000 claims description 9
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 7
- 239000000460 chlorine Substances 0.000 claims description 7
- 229910052801 chlorine Inorganic materials 0.000 claims description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- 239000011324 bead Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000003801 milling Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 13
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000007529 inorganic bases Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 150000007530 organic bases Chemical class 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- OTJFQRMIRKXXRS-UHFFFAOYSA-N (hydroxymethylamino)methanol Chemical compound OCNCO OTJFQRMIRKXXRS-UHFFFAOYSA-N 0.000 description 1
- ITBPIKUGMIZTJR-UHFFFAOYSA-N [bis(hydroxymethyl)amino]methanol Chemical compound OCN(CO)CO ITBPIKUGMIZTJR-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
-
- 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
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
- C09C1/565—Treatment of carbon black ; Purification comprising an oxidative treatment with oxygen, ozone or oxygenated compounds, e.g. when such treatment occurs in a region of the furnace next to the carbon black generating reaction zone
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to the field of chemical industry. A method for preparing self-dispersing aqueous carbon black, comprising the steps of: step 1), primary oxidation: oxidizing carbon black with a strong oxidizing agent to obtain a first mixture; step 2), primary centrifugal separation: centrifuging the first mixture obtained in step 1) to obtain a first precipitate; step 3), grinding: grinding the first precipitate obtained in step 2) into powder with particle size not more than 200 nm; step 4), secondary oxidation: oxidizing the powder obtained in the step 3) with a strong oxidizing agent to obtain a second mixture; step 5), secondary centrifugal separation: centrifuging the second mixture obtained in step 4) to obtain a second precipitate; step 6), neutralization treatment: neutralizing the hydrogen on the carboxyl group of the second precipitate obtained in step 5). The self-dispersing water-based carbon black obtained by the method has good dispersibility and stability in water.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a pigment.
Background
Carbon black is a natural black pigment that has excellent water resistance and weather resistance, and is generally used as a black pigment ink. However, carbon black is a water-insoluble particle, and is temporarily very fine after stirring and grinding, but is not stable in water.
Disclosure of Invention
The invention aims to provide a preparation method of self-dispersing water-based carbon black, which aims to solve the technical problems.
The technical problems solved by the invention can be realized by adopting the following technical scheme:
a method for preparing self-dispersing aqueous carbon black, comprising the steps of:
step 1), primary oxidation: oxidizing carbon black with a strong oxidizing agent to obtain a first mixture;
step 2), primary centrifugal separation: centrifuging the first mixture obtained in step 1) to obtain a first precipitate;
step 3), grinding: grinding the first precipitate obtained in step 2) into powder with particle size not more than 200 nm;
step 4), secondary oxidation: oxidizing the powder obtained in the step 3) with a strong oxidizing agent to obtain a second mixture;
step 5), secondary centrifugal separation: centrifuging the second mixture obtained in step 4) to obtain a second precipitate;
step 6), neutralization treatment: neutralizing the hydrogen on the carboxyl group of the second precipitate obtained in step 5).
Preferably, the specific surface area of the carbon black in step 1) is 300m 2 /g-500m 2 /g。
Preferably, the strong oxidizing agent in step 1) and step 3) is hypochlorite.
The effective effects are as follows: the self-dispersing water-based carbon black obtained by the method has good dispersibility and stability in water.
Detailed Description
The invention is further described below in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the implementation of the invention easy to understand.
A method for preparing self-dispersing aqueous carbon black, comprising the steps of: step 1), primary oxidation: the carbon black is oxidized with a strong oxidizing agent to obtain a first mixture. Step 2), primary centrifugal separation: centrifuging the first mixture obtained in step 1) to obtain a first precipitate. Step 3), grinding: grinding the first precipitate obtained in step 2) into a powder having a particle size of not more than 200 nm. Step 4), secondary oxidation: oxidizing the powder obtained in step 3) with a strong oxidizing agent to obtain a second mixture. Step 5), secondary centrifugal separation: centrifuging the second mixture obtained in step 4) to obtain a second precipitate. Step 6), neutralization treatment: adding the second precipitate obtained in the step 5) into alkali for neutralization.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Step 1), primary oxidation: the carbon black is oxidized with a strong oxidizing agent to obtain a first mixture. The carbon black with different surface areas is oxidized by hypochlorite, the effective chlorine content of the hypochlorite is 12 percent, and the molar ratio of the carbon black to the strong oxidant is 1:0.4-0.8. The oxidation reaction temperature was about 40 ℃, and the time required for oxidation was recorded as follows:
according to the above table, when the specific surface area of the carbon black is 300m 2 /g-500m 2 The oxidation time per gram is preferably, the specific surface area of the carbon black is preferably 300m 2 /g-500m 2 And/g. Meanwhile, it has been found that as the specific surface area of carbon black decreases, carbon black particles become larger and the time required for oxidation increases. However, when the specific surface area is increased to a certain extent, the aggregation phenomenon of carbon black becomes serious, and instead, the time required for oxidation is not reduced and increased.
Further adopts the surface area of 400m 2 The carbon black per gram is selected from different effective chlorine contents, the oxidation efficiency is tested at different reaction temperatures, the test shows that the effective chlorine of hypochlorite is 10% -15%, the temperature is 40-60 ℃ during the oxidation reaction, and the reaction time is within the range of 0.5-1.8 hours along with the rise of the temperature.
Therefore, it is further preferable that the specific surface area of the carbon black of the present invention is 300m 2 /g-500m 2 The effective chlorine of hypochlorite is 10% -15%, the temperature is 40-60 ℃ during oxidation reaction, and the reaction time is 1.5-2 hours, thereby being convenient for mechanized control during industrial batch production.
The oxidation is to an oxygen content of 6-12% and can be measured by a thermal Fisher's FlashSmart elemental analyzer.
The chemical reaction formula of the chemical reaction mainly occurring in the oxidation process is as follows:
C-H+M(ClO) x C-COOM, wherein M is a metal ion.
Step 2), primary centrifugal separation: centrifuging the first mixture obtained in step 1) to obtain a first precipitate.
Step 3), grinding: grinding the first precipitate obtained in step 2) into a powder having a particle size of not more than 200 nm. Grinding may be performed by a grinder. Preferably, the speed of the mill is 3000-4000rpm and the milling time is 2-6 hours. Preferably, 0.2-0.4mm zirconium beads are added to the milling chamber of the mill. The invention selects the grinding material. The zirconium is selected as the material, the zirconium beads are firm and wear-resistant, the service life is long, and the powder cannot fall into the ground object, so that the purity of the ground object is ensured. The size is selected to be 0.2-0.4mm, so that gaps among zirconium beads meet the requirement of grinding the ground objects to the grain size of 90-120nm.
After the centrifugal separation in the step 2), the surface of the carbon black is provided with water, and the carbon black with water can be directly taken as a first precipitate and directly put into a grinding machine. The carbon black with water may be first subjected to a drying treatment, and the dried carbon black may be fed into a grinder as a first precipitate. In the present invention, preferably, the carbon black with water is directly fed as a first precipitate into the mill. In the initial stage of grinding, the water on the first precipitate plays a role of a refrigerant, and can cool down the grinding machine and the zirconium beads. In the grinding process, water on the first precipitate evaporates to play a role in driving carbon black powder to move, so that the grinding efficiency can be improved.
Step 4), secondary oxidation: oxidizing the powder obtained in step 3) with a strong oxidizing agent to obtain a second mixture. The invention can effectively reduce the particle size of the carbon black through twice oxidation, and solves the problem that the carbon black can not meet the requirement of the particle size by only one-time oxidation (the particle size after one-time oxidation is about 150-200nm and is larger).
The oxidation is to an oxygen content of 10-16% and can be measured by a thermal Fisher's FlashSmart elemental analyzer.
In step 3), the obtained powder has smaller particle size, nitrogen can be introduced into the mixture of the powder and the strong oxidant to ensure the oxidation efficiency, and the carbon black particles are dispersed by using the nitrogen, so that the aggregation of the carbon black particles is reduced. The strong oxidizing agent of step 4) is preferably hypochlorite. The effective chlorine of hypochlorite is 10% -15%. The temperature of the oxidation reaction is 40-60 ℃ and the reaction time is 0.5-2.0 hours. The molar ratio of powder to strong oxidizer is preferably 1:0.3-0.6.
The method is consistent with the strong oxidants used in the step 1), compared with the method adopting different strong oxidants, the method can effectively reduce the storage cost and the use cost of the strong oxidants, avoid the interaction of partial substances between the two strong oxidants, and is favorable for improving the production safety.
Step 5), secondary centrifugal separation: centrifuging the second mixture obtained in step 4) to obtain a second precipitate. The invention can effectively remove inorganic salt and other impurities generated in the reaction process in the solution through twice centrifugal separation.
Step 6), neutralization treatment: neutralizing the hydrogen on the carboxyl group of the second precipitate obtained in step 5). Preferably, the hydrogen on the carboxyl group of the second precipitate is neutralized with a base. The base may be an inorganic base or an organic base, wherein the inorganic base is: sodium hydroxide, lithium hydroxide, potassium hydroxide, calcium hydroxide, magnesium hydroxide, sodium carbonate, potassium carbonate, lithium carbonate, magnesium carbonate, calcium carbonate, and the like; the organic bases include: methylamine, dimethylamine, trimethylamine, monoethylamine, diethylamine, monomethylamine, dimethanolamine, trimethanolamine, monoethanolamine, diethanolamine, triethanolamine, and the like. Preferably, the base is sodium hydroxide, lithium hydroxide, monoethanolamine, diethanolamine, triethanolamine
It is further preferred that the second precipitate obtained in step 5) is diluted with water and then added with a base to neutralize the hydrogen on the carboxyl group. The problems that the second precipitate is in a solid state, alkali is directly added and stirring is not uniform can be effectively avoided by diluting and then neutralizing.
After step 6), water is added to a dispersion having a carbon black concentration of 12-15%. Water can be added directly in step 6) quantitatively until the carbon black concentration is 12-15%. Alternatively, a portion of the carbon black may be added in step 6) and water may be added until the carbon black concentration is 12 to 15%. Preferably, water is added directly, so that the reaction rate in step 6) is increased. And when water is added, nitrogen is added, and can impact the carbon black, so that the mixing degree of the carbon black and alkali is improved, the neutralization process is accelerated, and the dispersion uniformity and stability of the carbon black in water are improved. The nitrogen may be recovered after the use of step 4). The nitrogen is also beneficial to reducing oxygen in the production environment and improving the safety of the production environment. The amount of water added can be calculated on the basis of the mass of the original carbon black, i.e. the mass ratio of carbon black in step 1) to water in step 6) is preferably 15:65-75, more preferably 15:70. For example: the raw carbon black had a mass of 15g, and 70g of water was added thereto.
Step 4) and step 6) do not suggest stirring with a stirring device to increase efficiency, thereby avoiding mixing of powder on the stirring device into the carbon black and thus increasing purity of the carbon black. The stirring device was replaced with nitrogen.
The dispersion of carbon black is reflected in the change in particle diameter, so that the dispersibility and stability of carbon black can be judged by measuring the average particle diameter. The obtained samples were prepared separately according to the methods in the tables.
The change in average particle diameter of the above 4 samples was measured by using an SZ-100 particle diameter meter using HORIBA as follows:
from the table above, it can be seen that:
1. the performance of 4 samples obtained by the method is relatively stable.
2. The dispersion of the carbon black can be improved by introducing nitrogen in the steps 4) and 6).
3. Sample 1 is the optimal sample.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A method for preparing self-dispersing aqueous carbon black, comprising the steps of:
step 1), primary oxidation: oxidizing carbon black with a strong oxidizing agent to obtain a first mixture;
step 2), primary centrifugal separation: centrifuging the first mixture obtained in step 1) to obtain a first precipitate;
step 3), grinding: grinding the first precipitate obtained in step 2) into powder with particle size not more than 200 nm;
step 4), secondary oxidation: oxidizing the powder obtained in the step 3) with a strong oxidizing agent to obtain a second mixture;
step 5), secondary centrifugal separation: centrifuging the second mixture obtained in step 4) to obtain a second precipitate;
step 6), neutralization treatment: neutralizing the hydrogen on the carboxyl group of the second precipitate obtained in step 5).
2. The method for producing a self-dispersing aqueous carbon black according to claim 1, wherein the specific surface area of the carbon black in step 1) is 300m 2 /g-500m 2 /g。
3. The method for producing a self-dispersing aqueous carbon black according to claim 1, wherein the strong oxidizing agent in step 1) and step 3) is hypochlorite.
4. The method for producing a self-dispersing aqueous carbon black according to claim 3, wherein the hypochlorite in step 1) has an effective chlorine content of 10% to 15%, the molar ratio of carbon black to strong oxidizer is 1:0.4 to 0.8, the oxidation reaction temperature is 40 ℃ to 60 ℃ and the reaction time is 1.5 to 2 hours.
5. The method for producing a self-dispersing aqueous carbon black according to claim 3, wherein the hypochlorite in the step 4) has an available chlorine of 10 to 15%, a molar ratio of the powder to the strong oxidizing agent of 1:0.3 to 0.6, and the oxidation reaction temperature is 40 to 60 ℃ and the reaction time is 0.5 to 2.0 hours.
6. The process for producing a self-dispersing aqueous carbon black according to claim 1, wherein the grinding is carried out in step 3) by a grinder having a rotation speed of 3000 to 4000rpm for 2 to 6 hours.
7. The method for producing a self-dispersing aqueous carbon black according to claim 6, wherein 0.2 to 0.4mm of zirconium beads are added to the milling chamber of the mill.
8. The method for producing a self-dispersing aqueous carbon black according to claim 1, wherein the surface of the carbon black is water-bearing after the centrifugal separation in step 2), and the water-bearing carbon black is directly fed into a mill as the first precipitate.
9. The process for producing a self-dispersing aqueous carbon black according to claim 1, wherein the second precipitate obtained in step 5) is diluted with water and then a base is added to neutralize hydrogen on the carboxyl group.
10. The process for the preparation of a self-dispersing aqueous carbon black according to claim 1, wherein the mass ratio of carbon black in step 1) to water in step 6) is preferably 15:65-75.
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