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CN114561109A - High-purity carbon black nano material based on powder pretreatment and preparation method thereof - Google Patents

High-purity carbon black nano material based on powder pretreatment and preparation method thereof Download PDF

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CN114561109A
CN114561109A CN202210111247.5A CN202210111247A CN114561109A CN 114561109 A CN114561109 A CN 114561109A CN 202210111247 A CN202210111247 A CN 202210111247A CN 114561109 A CN114561109 A CN 114561109A
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carbon black
purity carbon
purity
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temperature
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卢建平
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Xingjiang Texong Fine Chemical Co ltd
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Xingjiang Texong Fine Chemical Co ltd
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    • C09C1/56Treatment of carbon black ; Purification
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44Carbon
    • C09C1/48Carbon black
    • C09C1/56Treatment of carbon black ; Purification
    • C09C1/565Treatment 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
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    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract

The invention relates to the technical field of carbon black materials, in particular to a high-purity carbon black nano material based on powder pretreatment and a preparation method thereof. The feed comprises the following raw materials in parts by weight: high-purity carbon black, a titanate coupling agent, octadecanol, a dispersant, a grafting agent and an oxidation treatment agent, and the balance being water; in the high-purity carbon black nano material based on powder pretreatment and the preparation method thereof, the particle size of the carbon black prepared by the invention is smaller than that of the carbon black prepared by the traditional process, the specific surface area is large, meanwhile, the conversion rate of carbon is close to 100%, no pollutant is generated in the preparation process, the carbon black is relatively more environment-friendly, the number of groups on the surface of the carbon black can be increased through the added oxidation treating agent, the volatility and local polarity of the groups are improved, the aggregation possibility among carbon black particles is reduced, the dispersibility of the carbon black in a matrix is improved, meanwhile, the purity of the carbon black cannot be influenced, and the oxidation effect is better.

Description

High-purity carbon black nano material based on powder pretreatment and preparation method thereof
Technical Field
The invention relates to the technical field of carbon black materials, in particular to a high-purity carbon black nano material based on powder pretreatment and a preparation method thereof.
Background
The compounding method of the nano carbon black and the rubber solves the problems of dispersion of the nano material and strengthening the interface effect between the nano material and the matrix to a certain extent, but the carbon black has poor dispersibility and unobvious reinforcing effect when being applied to the matrix, and meanwhile, the reinforcing effect is further reduced on the basis of poor dispersibility due to the fact that the purity of the carbon black prepared by the traditional process is poor, so that the defects of the prior art are overcome.
Disclosure of Invention
The invention aims to provide a high-purity carbon black nano material based on powder pretreatment and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the above objects, in one aspect, the present invention provides a high purity carbon black nanomaterial pretreated based on powder, comprising the following raw materials in parts by weight: 20-30 parts of high-purity carbon black, 1-3 parts of titanate coupling agent, 1-3 parts of octadecanol, 1-5 parts of dispersant, 5-10 parts of grafting agent, 300 parts of oxidation treatment agent and 400 parts of water in balance.
As a further improvement of the technical scheme, the preparation method of the high-purity carbon black comprises the following steps:
s1.1, introducing hydrocarbon into plasma generated in advance at high temperature, and rapidly passing through the plasma at high temperature;
And S1.2, then entering another high-temperature environment again, and finally cooling and separating to obtain the high-purity carbon black.
The carbon black prepared by the method has smaller particle size and larger specific surface area compared with the carbon black prepared by the traditional process, and meanwhile, the carbon conversion rate is close to 100 percent, no pollutant is generated in the preparation process, and the method is relatively more environment-friendly.
As a further improvement of the technical scheme, in the S1.1, the plasma temperature is 3200-.
As a further improvement of the technical scheme, the dispersing agent is at least one selected from maleic anhydride, methacrylic acid, acrylic acid, styrene sulfonic acid and polyoxyethylene ether, so that carbon black particles are uniformly distributed in a water washing system and are better modified.
As a further improvement of the technical scheme, the grafting agent is selected from at least one of anionic polyacrylamide and polystyrene, so that the polymer branch chain on the surface of the carbon black can greatly reduce the aggregation of the carbon black, and the dispersibility of the carbon black in a polymer matrix can be improved.
In a further improvement of this aspect, the oxidation treatment agent is at least one selected from a nitric acid solution and a hydrogen peroxide solution, and the oxidation treatment agent oxidizes the carbon black to increase the number of groups on the surface of the carbon black, increase the volatility and local polarity of the groups, reduce the possibility of aggregation between carbon black particles, and increase the dispersibility of the carbon black in the matrix.
In another aspect, the present invention provides a method for preparing a high purity carbon black nanomaterial based on powder pretreatment according to any one of claims 1 to 6, comprising the steps of;
s2.1, keeping the oxidation treatment agent at a low temperature through a water bath, adding high-purity carbon black, and stirring after heating;
s2.2, adding the mixture into the low-temperature water bath again, washing and filtering the mixture, and then adding water again;
s2.3, adding a titanate coupling agent, octadecanol, a dispersing agent and a grafting agent, and heating and stirring;
and S2.4, cooling to room temperature after stirring, then filtering, washing, and finally drying to obtain the high-purity nano carbon black.
Preferably, in S2.1, the low-temperature water bath is 0-10 ℃, and after high-purity carbon black is added for 10-15min, the temperature is raised to 80-100 ℃.
Preferably, in S2.2, the low-temperature water bath is 0-10 ℃, and the washing and the filtering are repeated for 3-5 times.
Preferably, in S2.3, the temperature is raised to 70-90 ℃ and the stirring time is 1-1.5 h.
Compared with the prior art, the invention has the beneficial effects that:
1. in the high-purity carbon black nano material based on powder pretreatment and the preparation method thereof, the particle size of the carbon black prepared by the invention is smaller than that of the carbon black prepared by the traditional process, the specific surface area is large, the carbon conversion rate is close to 100%, no pollutant is generated in the preparation process, and the preparation method is relatively more environment-friendly.
2. According to the high-purity carbon black nano material based on powder pretreatment and the preparation method thereof, the oxidation treatment agent is added, so that the number of groups on the surface of carbon black can be increased, the volatility and local polarity of the groups are improved, the possibility of aggregation among carbon black particles is reduced, the dispersibility of the carbon black in a matrix is improved, meanwhile, the purity of the carbon black cannot be influenced, and the oxidation effect is good.
Drawings
Fig. 1 is a schematic view of the entire structure of embodiment 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1 high purity carbon black nanomaterial based on powder pretreatment and method of preparation thereof comprising:
preparation of high-purity carbon black
1. Introducing hydrocarbon into plasma generated in advance at high temperature, and rapidly passing through the plasma at the high temperature, wherein the temperature is 3200-3500 ℃;
2. Then the carbon black enters another high-temperature environment again, wherein the temperature is 600-1000 ℃, and finally the high-purity carbon black can be prepared through cooling separation.
Preparation of high-purity nano carbon black
1. Keeping 300 parts of oxidation treatment agent in a water bath at 10 ℃ for 15min, adding 20 parts of high-purity carbon black, heating to 100 ℃, and stirring;
2. adding into 10 deg.C low temperature water bath, repeatedly washing and filtering for 3-5 times, and adding water again;
3. adding 1 part of titanate coupling agent, 1 part of octadecanol, 1 part of dispersant and 5 parts of grafting agent, heating to 70 ℃, and stirring for 1-1.5 h;
4. and cooling to room temperature after stirring, then filtering, washing, and finally drying to obtain the high-purity nano carbon black.
Example 2 high purity carbon black nanomaterial based on powder pretreatment and method of preparation thereof comprising:
preparation of high-purity carbon black
1. Introducing hydrocarbon into plasma generated in advance at high temperature, and rapidly passing through the plasma at the high temperature, wherein the temperature is 3200-3500 ℃;
2. then entering another high temperature environment again, wherein the temperature is 600-1000 ℃, and finally cooling and separating to prepare the high-purity carbon black.
Preparation of high-purity nano carbon black
1. Keeping 330 parts of oxidation treatment agent in a water bath at 7 ℃ for 10-15min, adding 23 parts of high-purity carbon black, heating to 100 ℃, and stirring;
2. adding into low temperature water bath at 7 deg.C, repeatedly washing and filtering for 3-5 times, and adding water again;
3. adding 1 part of titanate coupling agent, 1 part of octadecanol, 2 parts of dispersant and 7 parts of grafting agent, heating to 70 ℃, and stirring for 1-1.5 h;
4. and cooling to room temperature after stirring, then filtering, washing, and finally drying to obtain the high-purity nano carbon black.
Example 3 high purity carbon black nanomaterials based on powder pretreatment and methods of making the same, comprising:
preparation of high-purity carbon black
1. Introducing hydrocarbon into plasma generated in advance at high temperature, and rapidly passing through the plasma at the high temperature, wherein the temperature is 3200-3500 ℃;
2. then entering another high temperature environment again, wherein the temperature is 600-1000 ℃, and finally cooling and separating to prepare the high-purity carbon black.
Preparation of high-purity nano carbon black
1. Keeping 350 parts of oxidation treatment agent in a water bath at 5 ℃ for 10-15min, adding 25 parts of high-purity carbon black, heating to 90 ℃, and stirring;
2. adding into 5 deg.C low temperature water bath again, repeatedly washing and filtering for 3-5 times, and adding water again;
3. Adding 2 parts of titanate coupling agent, 2 parts of octadecanol, 3 parts of dispersant and 8 parts of grafting agent, heating to 80 ℃, and stirring for 1-1.5 h;
4. and cooling to room temperature after stirring, then filtering, washing, and finally drying to obtain the high-purity nano carbon black.
Example 4 high purity carbon black nanomaterials based on powder pretreatment and methods of making the same, comprising:
preparation of high-purity carbon black
1. Introducing hydrocarbon into plasma generated in advance at high temperature, and rapidly passing through the plasma at the high temperature, wherein the temperature is 3200-3500 ℃;
2. then entering another high temperature environment again, wherein the temperature is 600-1000 ℃, and finally cooling and separating to prepare the high-purity carbon black.
Preparation of high-purity nano carbon black
1. Keeping 380 parts of oxidation treatment agent in a water bath at 3 ℃ for 10-15min, adding 28 parts of high-purity carbon black, heating to 80 ℃, and stirring;
2. adding into 3 deg.C low temperature water bath again, repeatedly washing and filtering for 3-5 times, and adding water again;
3. adding 3 parts of titanate coupling agent, 3 parts of octadecanol, 4 parts of dispersant and 9 parts of grafting agent, heating to 90 ℃, and stirring for 1-1.5 h;
4. and cooling to room temperature after stirring, then filtering, washing, and finally drying to obtain the high-purity nano carbon black.
Example 5 high purity carbon black nanomaterial based on powder pretreatment and method of preparation thereof comprising:
preparation of high purity carbon black
1. Introducing hydrocarbon into plasma generated in advance at high temperature, and rapidly passing through the plasma at high temperature, wherein the temperature is 3200-3500 ℃;
2. then the carbon black enters another high-temperature environment again, wherein the temperature is 600-1000 ℃, and finally the high-purity carbon black can be prepared through cooling separation.
Preparation of high-purity nano carbon black
1. Keeping 400 parts of oxidation treatment agent in a water bath at 0 ℃ for 10-15min, adding 30 parts of high-purity carbon black, heating to 80 ℃, and stirring;
2. adding into low temperature water bath at 0 deg.C again, repeatedly washing and filtering for 3-5 times, and adding water again;
3. adding 3 parts of titanate coupling agent, 3 parts of octadecanol, 5 parts of dispersant and 10 parts of grafting agent, heating to 90 ℃, and stirring for 1-1.5 h;
4. and cooling to room temperature after stirring, then filtering, washing, and finally drying to obtain the high-purity nano carbon black.
In the above examples 1 to 5, the particle size of the carbon black prepared by the present invention is smaller than that of the carbon black prepared by the conventional process, the specific surface area is large, the carbon conversion rate is close to 100%, no pollutant is generated during the preparation process, and the carbon black is relatively more environment-friendly;
The dispersing agent is selected from at least one of maleic anhydride, methacrylic acid, acrylic acid, styrene sulfonic acid and polyoxyethylene ether, so that carbon black particles are uniformly distributed in a water washing system and are better modified;
the grafting agent is selected from at least one of anionic polyacrylamide and polystyrene, so that the polymer branched chain on the surface of the carbon black can greatly reduce the aggregation of the carbon black, and the dispersibility of the carbon black in a polymer matrix can be improved;
the oxidation treatment agent is at least one selected from a nitric acid solution and a hydrogen peroxide solution, the number of groups on the surface of the carbon black can be increased, the volatility and the local polarity of the groups are improved, the possibility of aggregation among carbon black particles is reduced, and the dispersibility of the carbon black in a matrix is improved by oxidizing the carbon black, and other impurities cannot be remained in the carbon black by performing liquid phase oxidation by using the nitric acid solution or the hydrogen peroxide solution, so that the purity of the carbon black cannot be influenced, and the oxidation effect is good.
The relevant indexes of the high-purity carbon black nano material prepared by the invention based on powder pretreatment are shown in the following table 1:
TABLE 1
Example 1 Example 2 Example 3 Example 4 Example 5
Particle size (nm) 23 21 18 19 20
Density (g.cm) -3 1.093 1.091 1.085 1.088 1.091
Shore Hardness (HA) 62 59 65 57 61
Dispersibility in water Is better Is better Is preferably used Is preferably used Is preferably used
Purity (%) 99.7 99.7 99.8 99.8 99.7
As shown in Table 1, in examples 1 to 3, the carbon black materials had small particle diameters, low densities, and good dispersibility, and the hardness was maintained between 57 and 65, and the purity was maintained at 99.7% or higher.
Comparative example 1
1. Keeping 350 parts of oxidation treatment agent in a water bath at 5 ℃ for 10-15min, adding 25 parts of carbon black, heating to 90 ℃, and stirring;
2. adding into 5 deg.C low temperature water bath again, repeatedly washing and filtering for 3-5 times, and adding water again;
3. adding 2 parts of titanate coupling agent, 2 parts of octadecanol, 3 parts of dispersant and 8 parts of grafting agent, heating to 80 ℃, and stirring for 1-1.5 h;
4. and cooling to room temperature after stirring, then filtering, washing, and finally drying to obtain the high-purity nano carbon black.
Comparative example 2
Preparation of high-purity carbon black
1. Introducing hydrocarbon into plasma generated in advance at high temperature, and rapidly passing through the plasma at the high temperature, wherein the temperature is 3200-3500 ℃;
2. then entering another high temperature environment again, wherein the temperature is 600-1000 ℃, and finally cooling and separating to prepare the high-purity carbon black.
Preparation of high-purity nano carbon black
1. Adding 25 parts of high-purity carbon black into 2 parts of titanate coupling agent, 2 parts of octadecanol, 3 parts of dispersant and 8 parts of grafting agent, heating to 80 ℃, and stirring for 1-1.5 hours;
4. and cooling to room temperature after stirring, then filtering, washing, and finally drying to obtain the high-purity nano carbon black.
The high-purity carbon black nano material prepared by the invention has higher purity, dispersibility and smaller particle size, has a larger relationship with the prepared high-purity carbon black and an oxidation treatment agent, and in order to verify the related technical scheme, the applicant performs the following tests:
comparative examples 1 to 2: by using the method of example 3, the prepared carbon black material was examined for relevant indicators with the removal of high purity carbon black and oxidation treatment agent, as shown in table 2:
TABLE 2
Comparative example 1 Comparative example 2 Example 3 Conventional example
Particle size (nm) 40 24 18 57
Density (g.cm)-3 1.133 1.108 1.085 1.136
Shore Hardness (HA) 65 63 65 63
Dispersibility In general Difference (D) Is preferably used Difference (D)
Purity (%) 80.9 88.7 99.8 82.1
As shown in table 2, in comparative example 1, in comparison with example 3, in the case of removing the high purity carbon black alone, the particle size of the carbon black is increased, the density is increased, the dispersibility is affected, and the purity is greatly reduced; comparative example 2 in comparison with example 3, in the case of removing the oxidation treatment agent alone, the density and particle diameter of the carbon black were increased slightly, but the dispersibility was poor and the purity was also affected; the conventional example is a common carbon black material, compared with example 3, the particle size and density of the carbon black are greatly increased, and the dispersibility and purity are obviously inferior to those of example 3, so that the raw material formula in the invention can be shown to be an important factor influencing the high purity and dispersibility of the carbon black.
As shown in Table 2, in comparative example 1, when the step of preparing modified carbon black was separately removed, the filtration accuracy of the carbon black nanomaterial was significantly reduced compared to example 3, and in comparative example 2, when the nano white carbon black was separately removed, the hardness of the carbon black nanomaterial was significantly reduced compared to example 3, so that it can be shown that the carbon black nanomaterial prepared according to the present invention has characteristics of high filtration accuracy and high hardness
The foregoing shows and describes the general principles, principal features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. The high-purity carbon black nano material based on powder pretreatment is characterized by comprising the following raw materials in parts by weight: 20-30 parts of high-purity carbon black, 1-3 parts of titanate coupling agent, 1-3 parts of octadecanol, 1-5 parts of dispersant, 5-10 parts of grafting agent, 300 parts of oxidation treatment agent and 400 parts of water in balance.
2. The powder pretreatment based high purity carbon black nanomaterial of claim 1, wherein: the preparation method of the high-purity carbon black comprises the following steps:
s1.1, introducing hydrocarbon into plasma generated in advance at high temperature, and rapidly passing through the plasma at high temperature;
s1.2, then entering another high-temperature environment again, and finally cooling and separating to prepare the high-purity carbon black.
3. The high purity carbon black nanomaterial based on powder pretreatment of claim 2, characterized in that: in the S1.1, the plasma temperature is 3200-.
4. The high purity carbon black nanomaterial based on powder pretreatment of claim 1, characterized in that: the dispersing agent is selected from at least one of maleic anhydride, methacrylic acid, acrylic acid, styrene sulfonic acid and polyoxyethylene ether.
5. The high purity carbon black nanomaterial based on powder pretreatment of claim 1, characterized in that: the grafting agent is selected from at least one of anionic polyacrylamide and polystyrene.
6. The high purity carbon black nanomaterial based on powder pretreatment of claim 1, characterized in that: the oxidation treatment agent is at least one selected from a nitric acid solution and a hydrogen peroxide solution.
7. A method for preparing the high-purity carbon black nanomaterial based on powder pretreatment according to any one of claims 1 to 6, characterized by comprising the steps of;
s2.1, keeping the oxidation treatment agent at a low temperature through a water bath, adding high-purity carbon black, and stirring after heating;
s2.2, adding the mixture into the low-temperature water bath again, washing and filtering the mixture, and then adding water again;
s2.3, adding a titanate coupling agent, octadecanol, a dispersing agent and a grafting agent, and heating and stirring;
and S2.4, stirring, cooling to room temperature, filtering, washing, and drying to obtain the high-purity nano carbon black.
8. The method for preparing high-purity carbon black nano-material based on powder pretreatment as claimed in claim 7, wherein the method comprises the following steps: and in the S2.1, the low-temperature water bath is 0-10 ℃, and the high-purity carbon black is added for 10-15min and then heated to 80-100 ℃.
9. The method for preparing high-purity carbon black nano-material based on powder pretreatment as claimed in claim 7, wherein the method comprises the following steps: and in the S2.2, the low-temperature water bath is 0-10 ℃, and the washing and the filtering are repeated for 3-5 times.
10. The method for preparing high-purity carbon black nano-material based on powder pretreatment as claimed in claim 7, wherein the method comprises the following steps: in the step S2.3, the temperature is raised to 70-90 ℃, and the stirring time is 1-1.5 h.
CN202210111247.5A 2022-01-29 2022-01-29 High-purity carbon black nano material based on powder pretreatment and preparation method thereof Pending CN114561109A (en)

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CN101336267A (en) * 2005-11-30 2008-12-31 阿克马法国公司 Pulverulent composition based on carbon nanotubes, methods of obtaining them and its uses, especially in polymeric materials
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CN107033632A (en) * 2017-04-20 2017-08-11 安徽春辉仪表线缆集团有限公司 A kind of hyper-branched polyester functional graft carbon black conductive filler and preparation method thereof
CN108084744A (en) * 2017-12-22 2018-05-29 江南大学 A kind of method that self-dispersing nano carbon black is prepared based on sulfydryl-alkene click-reaction
CN108864774A (en) * 2018-07-20 2018-11-23 江南大学 A kind of preparation method of the reactive self-dispersing nano carbon black of cotton fabric dyeing process
CN113861511A (en) * 2021-11-11 2021-12-31 青岛伊克斯达智能装备有限公司 Modified pyrolysis carbon black, preparation method thereof and aging-resistant rubber compound

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* Cited by examiner, † Cited by third party
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US5952429A (en) * 1995-06-14 1999-09-14 Nippon Shokubai Co., Ltd. Carbon black graft polymer, method for production thereof, and use thereof
JP2005120284A (en) * 2003-10-17 2005-05-12 Toda Kogyo Corp Black complex particle powder and coating and resin composition each containing the black complex particle powder
JP2005255705A (en) * 2004-03-09 2005-09-22 Tokai Carbon Co Ltd Water-dispersible carbon black pigment
CN101336267A (en) * 2005-11-30 2008-12-31 阿克马法国公司 Pulverulent composition based on carbon nanotubes, methods of obtaining them and its uses, especially in polymeric materials
JP2008285632A (en) * 2007-05-21 2008-11-27 Mikuni Color Ltd High jetness carbon black dispersion, process for producing the same, and coating material composition using the high jetness carbon black dispersion
CN102036650A (en) * 2008-05-21 2011-04-27 三好化成株式会社 Surface-treated powder and cosmetic comprising the same
CN103642281A (en) * 2013-12-19 2014-03-19 宁波佛来斯通新材料有限公司 Modified carbon black, and preparation method and application thereof in preparation of black chemical powdered ink
CN107033632A (en) * 2017-04-20 2017-08-11 安徽春辉仪表线缆集团有限公司 A kind of hyper-branched polyester functional graft carbon black conductive filler and preparation method thereof
CN108084744A (en) * 2017-12-22 2018-05-29 江南大学 A kind of method that self-dispersing nano carbon black is prepared based on sulfydryl-alkene click-reaction
CN108864774A (en) * 2018-07-20 2018-11-23 江南大学 A kind of preparation method of the reactive self-dispersing nano carbon black of cotton fabric dyeing process
CN113861511A (en) * 2021-11-11 2021-12-31 青岛伊克斯达智能装备有限公司 Modified pyrolysis carbon black, preparation method thereof and aging-resistant rubber compound

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