CN111138891A - Pre-dispersed carbon black and preparation method and application thereof - Google Patents
Pre-dispersed carbon black and preparation method and application thereof Download PDFInfo
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- 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
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
Abstract
The invention relates to the technical field of carbon black preparation, in particular to pre-dispersed carbon black and a preparation method and application thereof. The preparation method of the pre-dispersed carbon black comprises the following steps: (1) adding carbon black into the mixed acid solution, heating and refluxing to obtain acid-treated carbon black; (2) dispersing the carbon black treated by acid in a solvent, then adding diphenylmethane bismaleimide, dioctadecyl amine and a catalyst, and carrying out heating reflux reaction to obtain the pre-dispersed carbon black. According to the method, diphenylmethane bismaleimide and dioctadecyl amine are grafted onto carbon black, so that the carbon black has excellent dispersing performance.
Description
Technical Field
The invention relates to the technical field of carbon black preparation, in particular to pre-dispersed carbon black and a preparation method and application thereof.
Background
Carbon black is a light, loose, fine black powder with a large specific surface area, and can be classified into conductive carbon black, reinforcing carbon black, wear-resistant carbon black, and the like, according to the properties of carbon black. Carbon black is very prone to agglomeration due to its low density and large specific surface area. In particular, in the application of plastics processing, carbon black is not well dispersed in the plastic, thus limiting the performance of its properties. In the prior art, although a dispersing agent is added to disperse carbon black in the preparation process of plastics, the dispersing agent needs to be metered and added again in the actual production process, so that the operation steps are increased; most importantly, the dispersants added in the existing plastic preparation process are conventional dispersants, and cannot disperse carbon black in the plastic to the maximum extent, so that more carbon black needs to be added to achieve the required effect, and the cost of the plastic product is correspondingly increased.
In conclusion, the development of the pre-dispersed carbon black which has a good dispersion effect in the plastic preparation process and does not need to add a dispersant additionally has important values for fully exerting the effect of the carbon black, saving the cost and simplifying the production steps.
Disclosure of Invention
The invention provides a predispersed carbon black and a preparation method thereof in order to solve the technical problems. The pre-dispersed carbon black prepared by the method has excellent dispersing performance.
The technical problem to be solved by the invention is realized by the following technical scheme:
a preparation method of pre-dispersed carbon black comprises the following steps:
(1) adding carbon black into the mixed acid solution, heating and refluxing to obtain acid-treated carbon black;
(2) dispersing the carbon black treated by acid in a solvent, then adding diphenylmethane bismaleimide, dioctadecyl amine and a catalyst, and carrying out heating reflux reaction to obtain the pre-dispersed carbon black.
Preferably, the mixed acid solution in the step (1) is a mixed acid solution composed of concentrated sulfuric acid and concentrated nitric acid.
Further preferably, the volume usage ratio of the concentrated sulfuric acid to the concentrated nitric acid is 1-3: 1-3.
Preferably, in the step (1), the carbon black is added into a 5-15 times of mixed acid solution, heated and refluxed for 5-10 hours, washed to be neutral by water, and dried to obtain the acid-treated carbon black.
Preferably, the solvent in step (2) is toluene.
Preferably, the use amount ratio of the carbon black subjected to acid treatment in the step (2), the diphenylmethane bismaleimide and the dioctadecyl amine is 1: 2-4: 1-2.
Most preferably, the acid treated carbon black, diphenylmethane bismaleimide, dioctadecyl amine are used in step (2) in a ratio of 1:2: 1.
Preferably, the catalyst is 4-dimethylaminopyridine; the dosage ratio of the 4-dimethylaminopyridine to the carbon black is 0.5-1: 1.
Preferably, in the step (2), the carbon black subjected to acid treatment is dispersed in a solvent in an amount which is 20-40 times that of the carbon black, then diphenylmethane bismaleimide, dioctadecylamine and a catalyst are added, heating reflux reaction is carried out for 3-6 hours, and precipitates are taken out, washed by toluene and dried to obtain the pre-dispersed carbon black.
The invention also provides the pre-dispersed carbon black prepared by the preparation method.
The invention also provides an application of the carbon black as a conductive agent in high polymer plastics.
Preferably, the polymer plastic is ABS plastic.
Has the advantages that: the invention provides a brand-new preparation method of pre-dispersed carbon black, which grafts diphenylmethane bismaleimide and dioctadecyl amine on the carbon black to ensure that the carbon black has excellent dispersing performance. Particularly, the pre-dispersed carbon black prepared by the method can be fully dispersed in ABS plastics without adding a dispersing agent, so that the use amount of the carbon black can be reduced, the cost is saved, the weighing and adding steps of the dispersing agent are reduced, the production steps are saved, and the optimization of the production process is facilitated.
Detailed Description
The present invention will be further explained with reference to specific examples, which are not intended to limit the present invention in any way.
EXAMPLE 1 preparation of Pre-dispersed carbon Black
(1) 100g of carbon black (U.S. Kabot VULCANXC68 carbon black) was added to 1L of a carbon black mixture prepared by mixing 3:1, heating and refluxing for 8 hours in a mixed acid solution consisting of concentrated nitric acid (the mass fraction is 60%) and concentrated sulfuric acid (the mass fraction is 90%), then washing with water to be neutral, and drying to obtain acid-treated carbon black;
(2) dispersing the carbon black treated by the acid in 3L of toluene, then adding 200g of diphenylmethane bismaleimide, 100g of dioctadecyl amine and 50g of 4-dimethylaminopyridine, carrying out heating reflux reaction for 5h, taking a precipitate, washing with toluene, and drying to obtain the pre-dispersed carbon black.
EXAMPLE 2 preparation of Pre-dispersed carbon Black
(1) 100g of carbon black (U.S. Kabot VULCANXC68 carbon black) was added to 1.5L of a carbon black mixture prepared by mixing together carbon black (carbon black) in a volume ratio of 1: 3, heating and refluxing for 5 hours in a mixed acid solution consisting of concentrated nitric acid (the mass fraction is 60%) and concentrated sulfuric acid (the mass fraction is 90%), then washing with water to be neutral, and drying to obtain acid-treated carbon black;
(2) dispersing the carbon black treated by the acid in 4L of toluene, then adding 300g of diphenylmethane bismaleimide, 200g of dioctadecyl amine and 100g of 4-dimethylaminopyridine, carrying out heating reflux reaction for 5h, taking a precipitate, washing with toluene, and drying to obtain the pre-dispersed carbon black.
Comparative example 1 preparation of Pre-dispersed carbon Black
(1) 100g of carbon black (U.S. Kabot VULCANXC68 carbon black) was added to 1L of a carbon black mixture prepared by mixing 3:1, heating and refluxing for 8 hours in a mixed acid solution consisting of concentrated nitric acid (the mass fraction is 60%) and concentrated sulfuric acid (the mass fraction is 90%), then washing with water to be neutral, and drying to obtain acid-treated carbon black;
(2) dispersing the carbon black treated by the acid in 3L of toluene, then adding 300g of diphenylmethane bismaleimide and 50g of 4-dimethylaminopyridine, carrying out heating reflux reaction for 5h, taking a precipitate, washing with toluene, and drying to obtain the pre-dispersed carbon black.
Comparative example 1 differs from example 1 in that comparative example 1 only grafts the carbon black with diphenylmethane bismaleimide; while example 1 uses diphenylmethane bismaleimide and dioctadecyl amine to graft carbon black.
Comparative example 2 preparation of Pre-dispersed carbon Black
(1) 100g of carbon black (U.S. Kabot VULCANXC68 carbon black) was added to 1L of a carbon black mixture prepared by mixing 3:1, heating and refluxing for 8 hours in a mixed acid solution consisting of concentrated nitric acid (the mass fraction is 60%) and concentrated sulfuric acid (the mass fraction is 90%), then washing with water to be neutral, and drying to obtain acid-treated carbon black;
(2) dispersing the carbon black treated by the acid in 3L of toluene, then adding 300g of dioctadecyl amine and 50g of 4-dimethylaminopyridine, carrying out heating reflux reaction for 5h, taking a precipitate, washing with toluene, and drying to obtain the pre-dispersed carbon black.
Comparative example 2 differs from example 1 in that comparative example 2 only uses dioctadecyl amine to graft the carbon black; while example 1 uses diphenylmethane bismaleimide and dioctadecyl amine to graft carbon black.
Comparative example 3 preparation of Pre-dispersed carbon Black
(1) 100g of carbon black (U.S. Kabot VULCANXC68 carbon black) was added to 1L of a carbon black mixture prepared by mixing 3:1, heating and refluxing for 8 hours in a mixed acid solution consisting of concentrated nitric acid (the mass fraction is 60%) and concentrated sulfuric acid (the mass fraction is 90%), then washing with water to be neutral, and drying to obtain acid-treated carbon black;
(2) dispersing the carbon black treated by the acid in 3L of toluene, then adding 200g of diphenylmethane bismaleimide, 100g of octadecylamine and 50g of 4-dimethylaminopyridine, carrying out heating reflux reaction for 5h, taking a precipitate, washing with toluene, and drying to obtain the pre-dispersed carbon black.
Comparative example 3 differs from example 1 in that comparative example 3 employs diphenylmethane bismaleimide and octadecylamine to graft carbon black; while example 1 uses diphenylmethane bismaleimide and dioctadecyl amine to graft carbon black.
Comparative example 4 preparation of Pre-dispersed carbon Black
(1) 100g of carbon black (U.S. Kabot VULCANXC68 carbon black) was added to 1L of a carbon black mixture prepared by mixing 3:1, heating and refluxing for 8 hours in a mixed acid solution consisting of concentrated nitric acid (the mass fraction is 60%) and concentrated sulfuric acid (the mass fraction is 90%), then washing with water to be neutral, and drying to obtain acid-treated carbon black;
(2) dispersing the carbon black treated by the acid in 3L of toluene, then adding 200g of coco primary alkylamine, 100g of dioctadecyl amine and 50g of 4-dimethylaminopyridine, carrying out heating reflux reaction for 5h, taking out precipitate, washing with toluene, and drying to obtain the pre-dispersed carbon black.
Comparative example 4 differs from example 1 in that comparative example 4 employs cocoalkyl primary amine and dioctadecyl amine to graft carbon black; while example 1 uses diphenylmethane bismaleimide and dioctadecyl amine to graft carbon black.
Comparative example 5 preparation of Pre-dispersed carbon Black
(1) 100g of carbon black (U.S. Kabot VULCANXC68 carbon black) was added to 1L of a carbon black mixture prepared by mixing 3:1, heating and refluxing for 8 hours in a mixed acid solution consisting of concentrated nitric acid (the mass fraction is 60%) and concentrated sulfuric acid (the mass fraction is 90%), then washing with water to be neutral, and drying to obtain acid-treated carbon black;
(2) dispersing the carbon black treated by the acid in 3L of toluene, then adding 200g of coco primary alkylamine, 100g of octadecylamine and 50g of 4-dimethylaminopyridine, carrying out heating reflux reaction for 5h, taking out precipitate, washing with toluene, and drying to obtain the pre-dispersed carbon black.
Comparative example 5 differs from example 1 in that comparative example 5 employs cocoalkyl primary amine and octadecyl amine to graft carbon black; while example 1 uses diphenylmethane bismaleimide and dioctadecyl amine to graft carbon black.
Experimental example ABS sample strip conductive surface resistivity test
Mixing the pre-dispersed carbon black prepared in the examples 1 and 2 and the comparative examples 1 to 5 with ABS plastic (the ABS plastic with the brand number of TR558A of Korean LG company), wherein the mass ratio of the pre-dispersed carbon black is 5%, and the mass ratio of the ABS plastic is 95%; and then extruding the mixture by a double-screw extruder to prepare ABS test sample strips 1-7, and testing the surface resistivity of the ABS test sample strips according to the IEC60093 standard, wherein the test results are shown in Table 1.
TABLE 1 surface resistivity test
| Sample strip | Predispersed carbon black type | Surface resistivity (omega/m)2) |
| ABS test specimen 1 | Example 1 Pre-dispersed carbon Black | 1.4x104 |
| ABS test specimen 2 | Example 2 Pre-dispersed carbon Black | 3.7x104 |
| ABS test specimen No. 3 | Comparative example 1 Pre-dispersed carbon Black | 4.4x106 |
| ABS test specimen No. 4 | Comparative example 2 Pre-dispersed carbon Black | 6.2x106 |
| ABS test specimen No. 5 | Comparative example 3 Pre-dispersed carbon Black | 5.6x105 |
| ABS test specimen No. 6 | Comparative example 4 Pre-dispersed carbon Black | 8.3x105 |
| ABS test specimen 7 | Comparative example 5 Pre-dispersed carbon Black | 4.9x106 |
As can be seen from the results of ABS tests 1 and 2 in Table 1, they gave a surface resistivity of 10 with the addition of 5% of predispersed carbon black4The grade shows that the predispersed carbon black provided by the invention has excellent conductive effect when being added into ABS plastic without adding a dispersant, and can effectively prevent the ABS plastic from generating static electricity.
As can be seen from the test results of ABS test bars 3 and 4, the surface resistivity thereof was 106The grade is 2 orders of magnitude larger than that of the ABS test sample strip 1; this shows that the carbon black has to be grafted simultaneously with diphenylmethane bismaleimide and dioctadecyl amine to obtain carbon black with excellent conductive effect on ABS plastic; only one of diphenylmethane bismaleimide and dioctadecyl amine is adopted to graft the carbon black, and the carbon black with excellent conductive effect on ABS plastic can not be obtained.
As can be seen from the test results of ABS test bars 5 and 6, the surface resistivity thereof was 105～6Compared with an ABS test sample strip 1, the grade is 1-2 orders of magnitude larger; this shows that the carbon black has to be grafted by two amine substances, i.e. diphenylmethane bismaleimide and dioctadecyl amine, to obtain the carbon black with excellent conductive effect on ABS plastic; the carbon black is grafted by other combined amine substances, and the carbon black with excellent conductive effect on ABS plastics cannot be obtained.
Claims (10)
1. A preparation method of pre-dispersed carbon black is characterized by comprising the following steps:
(1) adding carbon black into the mixed acid solution, heating and refluxing to obtain acid-treated carbon black;
(2) dispersing the carbon black treated by acid in a solvent, then adding diphenylmethane bismaleimide, dioctadecyl amine and a catalyst, and carrying out heating reflux reaction to obtain the pre-dispersed carbon black.
2. The method for preparing predispersed carbon black as claimed in claim 1, wherein the mixed acid solution in step (1) is a mixed acid solution of concentrated sulfuric acid and concentrated nitric acid.
3. The method for preparing pre-dispersed carbon black according to claim 2, wherein the volume ratio of concentrated sulfuric acid to concentrated nitric acid is 1-3: 1-3.
4. The method for preparing the pre-dispersed carbon black according to claim 1, wherein the carbon black obtained in the step (1) is added into a 5-15 times amount of the mixed acid solution, heated and refluxed for 5-10 hours, washed with water to be neutral, and dried to obtain the acid-treated carbon black.
5. The method of claim 1, wherein the solvent used in step (2) is toluene.
6. The method for preparing pre-dispersed carbon black according to claim 1, wherein the amount ratio of the carbon black subjected to acid treatment in the step (2), the diphenylmethane bismaleimide and the dioctadecyl amine is 1: 2-4: 1-2; preferably, the amount ratio of the acid-treated carbon black, diphenylmethane bismaleimide, dioctadecyl amine in step (2) is 1:2: 1.
7. The method of claim 1, wherein the catalyst is 4-dimethylaminopyridine; the dosage ratio of the 4-dimethylaminopyridine to the carbon black is 0.5-1: 1.
8. The method for preparing the pre-dispersed carbon black according to claim 1, wherein the acid-treated carbon black is dispersed in a solvent in an amount of 20 to 40 times that of the acid-treated carbon black in the step (2), then diphenylmethane bismaleimide, dioctadecylamine and a catalyst are added to carry out heating reflux reaction for 3 to 6 hours, and the precipitate is taken out, washed with toluene and dried to obtain the pre-dispersed carbon black.
9. The pre-dispersed carbon black prepared by the preparation method according to any one of claims 1 to 8.
10. Use of the carbon black according to claim 9 as a conductive agent in high molecular plastics.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115863676A (en) * | 2022-12-16 | 2023-03-28 | 中汽创智科技有限公司 | Preparation method of carbon-supported platinum electrocatalyst, carbon-supported platinum electrocatalyst and application |
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| CN115863676A (en) * | 2022-12-16 | 2023-03-28 | 中汽创智科技有限公司 | Preparation method of carbon-supported platinum electrocatalyst, carbon-supported platinum electrocatalyst and application |
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