CN116790139A - Preparation method of grinding-free self-dispersing carbon black - Google Patents
Preparation method of grinding-free self-dispersing carbon black Download PDFInfo
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- CN116790139A CN116790139A CN202310772387.1A CN202310772387A CN116790139A CN 116790139 A CN116790139 A CN 116790139A CN 202310772387 A CN202310772387 A CN 202310772387A CN 116790139 A CN116790139 A CN 116790139A
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- 239000006229 carbon black Substances 0.000 title claims abstract description 115
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 238000000227 grinding Methods 0.000 claims abstract description 19
- 239000004342 Benzoyl peroxide Substances 0.000 claims abstract description 16
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000019400 benzoyl peroxide Nutrition 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 16
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004576 sand Substances 0.000 claims abstract description 15
- 239000000178 monomer Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000008247 solid mixture Substances 0.000 claims abstract description 8
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 15
- 230000001877 deodorizing effect Effects 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 239000006185 dispersion Substances 0.000 abstract description 26
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- 238000006116 polymerization reaction Methods 0.000 abstract description 4
- 239000011148 porous material Substances 0.000 abstract description 2
- 238000004332 deodorization Methods 0.000 abstract 1
- 239000011859 microparticle Substances 0.000 abstract 1
- 235000019241 carbon black Nutrition 0.000 description 83
- 241000872198 Serjania polyphylla Species 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 238000002715 modification method Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 229920000578 graft copolymer Polymers 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000011527 polyurethane coating Substances 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Abstract
The invention discloses a preparation method of grinding-free self-dispersing carbon black, which relates to the technical field of carbon black preparation, and comprises the steps of firstly weighing maleic anhydride, benzoyl peroxide and styrene monomer, and mixing to obtain premix A; adding raw material carbon black and the premix A into a stirring kettle, and stirring to obtain a solid mixture B; adding sodium dodecyl benzene sulfonate and deionized water into a reaction kettle to obtain a solution C; adding the solution C and the mixture B into a sand mill, and grinding and dispersing to obtain color paste; adding color paste into a reaction kettle, performing deodorization after reacting under the heating condition of an oil bath to obtain crude carbon black, filtering the crude carbon black by using a suction filter, drying and crushing to obtain dispersed carbon black; adsorbing styrene monomer on the surface of carbon black microparticles by using a carbon black high-pore structure, and treating the carbon black in deionized water to ensure that the monomer adsorbed on the surface of the carbon black prevents the carbon black from self-polymerization; the self-dispersion carbon black is obtained by coating the carbon black after the polymerization reaction of the styrene monomer, so that the required dispersion fineness can be obtained without grinding.
Description
Technical Field
The invention relates to the technical field of carbon black preparation, in particular to a preparation method of grinding-free self-dispersing carbon black.
Background
The carbon black has the main component of carbon, the average particle size of primary particles is between 10 and 100nm, and the carbon black has excellent rubber reinforcement, coloring, electric conduction and ultraviolet absorption functions and has irreplaceable functions in a plurality of fields. Meanwhile, the primary particle size of the carbon black is as small as nano-scale, the surface energy is extremely large, the self-aggregation among particles is strong, and the carbon black is difficult to disperse uniformly in the using process. Accordingly, both the carbon black producer and the user expend much effort to investigate the surface properties of the carbon black in an effort to improve the dispersion properties of the carbon black. Currently, the main modification methods of carbon black mainly include post-treatment oxidation, surfactant treatment, polymer grafting and the like.
Conventional carbon black surface grafting refers to the process of attaching a polymer compound to the surface of carbon black by chemical action. The usability of the carbon black is improved by some special properties of the grafted polymer, such as dispersibility, crosslinking capability, biology, hydrophilicity and lipophilicity, etc.
However, the carbon black prepared by the grafting modification method still needs to be ground and dispersed, and the problems of difficult grinding and difficult dispersion of the carbon black are not fundamentally solved.
Disclosure of Invention
The invention aims to provide a preparation method of grinding-free self-dispersing carbon black; solves the following technical problems:
how to solve the problem that the carbon black is difficult to grind and disperse.
The aim of the invention can be achieved by the following technical scheme:
a preparation method of grinding-free self-dispersing carbon black comprises the following steps:
s1: weighing maleic anhydride, benzoyl peroxide and styrene monomer, and uniformly mixing to obtain a premix solution A;
s2: adding raw material carbon black and the premix A into a stirring kettle, and stirring to obtain a solid mixture B;
s3: adding sodium dodecyl benzene sulfonate and deionized water into a reaction kettle to obtain a solution C;
s4: adding the solution C and the mixture B into a nano sand mill, and grinding and dispersing for 0.5-2 hours to obtain color paste;
s5: adding color paste into a reaction kettle, reacting for 1.5-10h at a rotating speed of 50rpm, simultaneously heating the color paste in an oil bath, controlling the temperature of the oil bath to be 80-95 ℃, deodorizing after the reaction is stopped, obtaining crude carbon black, and recycling styrene monomers in the crude carbon black.
S6: filtering the crude carbon black by using a suction filter, and drying to obtain pre-dispersed grafted carbon black;
s7: and crushing the dried grafted carbon black to obtain the dispersed carbon black.
Wherein, the deionized water is 88 to 94 parts by weight, the raw material carbon black is 5 to 9 parts by weight, the maleic anhydride is 0.02 to 0.1 part by weight, the benzoyl peroxide is 0.02 to 0.1 part by weight, the sodium dodecyl benzene sulfonate is 0.1 to 0.3 part by weight, and the styrene monomer is 0.5 to 1.8 parts by weight.
In a further aspect of the invention: 90-92 parts of deionized water, 6-8 parts of raw material carbon black, 0.04-0.08 part of maleic anhydride, 0.04-0.08 part of benzoyl peroxide, 0.15-0.25 part of sodium dodecyl benzene sulfonate and 0.8-1.5 part of styrene monomer.
In a further aspect of the invention: 91 parts of deionized water, 7 parts of raw material carbon black, 0.06 part of maleic anhydride, 0.06 part of benzoyl peroxide, 0.2 part of sodium dodecyl benzene sulfonate and 1.2 parts of styrene monomer.
In a further aspect of the invention: the particle size of the raw material carbon black is 10nm-100nm.
In a further aspect of the invention: the purity of the styrene monomer, maleic anhydride, benzoyl peroxide and sodium dodecyl benzene sulfonate is not lower than 95%.
In a further aspect of the invention: the stirring kettle in the step S2 is a closed stirring kettle, and the stirring speed is 1000-1500rpm.
In a further aspect of the invention: the nano sand mill in the step S4 is a horizontal sand mill, and the diameter of a grinding medium of the horizontal sand mill is 0.1mm.
The invention has the beneficial effects that:
according to the invention, a high-pore structure of carbon black is utilized to adsorb styrene monomer on the surface of microscopic particles of the carbon black, then grinding and dispersing treatment is carried out on the carbon black in deionized water by utilizing a nano sand mill, and the monomer adsorbed on the surface of the carbon black can prevent the self-polymerization of the carbon black in the process; the styrene monomer is subjected to polymerization reaction on the surface of the dispersed carbon black, the self-dispersion carbon black is obtained by coating the carbon black, the required dispersion fineness can be achieved without grinding in the application process of the carbon black, and meanwhile, the blackness of the carbon black is not influenced by the transparent polystyrene.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
S1: weighing and uniformly mixing 0.08g of maleic anhydride, 0.08g of benzoyl peroxide and 1.6g of styrene monomer with the purity of 97%, thereby obtaining a premix solution A;
s2: adding 8g of raw material carbon black with the particle size of 100nm and the premix solution A into a closed stirring kettle with the stirring speed of 1500rpm, and stirring to obtain a solid mixture B;
s3: adding 0.24 sodium dodecyl benzene sulfonate and 90g deionized water into a reaction kettle to obtain a solution C;
s4: adding the solution C and the mixture B into a horizontal nano sand mill with the grinding medium of 0.1nm, and grinding and dispersing for 1h to obtain color paste;
s5: adding color paste into a reaction kettle, reacting for 3 hours at a rotating speed of 50rpm, simultaneously heating the color paste in an oil bath, controlling the temperature of the oil bath at 95 ℃, deodorizing after stopping the reaction to obtain crude carbon black, and recovering styrene monomers in the crude carbon black;
s6: filtering the crude carbon black by using a suction filter, and drying to obtain pre-dispersed grafted carbon black;
s7: and crushing the dried grafted carbon black to obtain the dispersed carbon black.
Example 2
S1: weighing and uniformly mixing 0.05g of maleic anhydride, 0.05g of benzoyl peroxide and 0.9g of styrene monomer with the purity of 95%, thereby obtaining a premix solution A;
s2: adding 5g of raw material carbon black with the particle size of 10nm and the premix solution A into a closed stirring kettle with the stirring speed of 1000rpm, and stirring to obtain a solid mixture B;
s3: adding 0.28 g of sodium dodecyl benzene sulfonate and 93.72g of deionized water into a reaction kettle to obtain a solution C;
s4: adding the solution C and the mixture B into a horizontal nano sand mill with the grinding medium of 0.1nm, and grinding and dispersing for 1.5 hours to obtain color paste;
s5: adding color paste into a reaction kettle, reacting for 3 hours at a rotating speed of 50rpm, simultaneously heating the color paste in an oil bath, controlling the temperature of the oil bath at 80 ℃, deodorizing after stopping the reaction to obtain crude carbon black, and recovering styrene monomers in the crude carbon black;
s6: filtering the crude carbon black by using a suction filter, and drying to obtain pre-dispersed grafted carbon black;
s7: and crushing the dried grafted carbon black to obtain the dispersed carbon black.
Example 3
S1: weighing and uniformly mixing 0.05g of maleic anhydride, 0.05g of benzoyl peroxide and 0.9g of styrene monomer with the purity of 96%, thereby obtaining a premix solution A;
s2: adding 6g of raw material carbon black with the particle size of 50nm and the premix solution A into a closed stirring kettle with the stirring speed of 1200rpm, and stirring to obtain a solid mixture B;
s3: adding 0.28 g of sodium dodecyl benzene sulfonate and 92.72g of deionized water into a reaction kettle to obtain a solution C;
s4: adding the solution C and the mixture B into a horizontal nano sand mill with the grinding medium of 0.1nm, and grinding and dispersing for 1.5 hours to obtain color paste;
s5: adding color paste into a reaction kettle, reacting for 3 hours at a rotating speed of 50rpm, simultaneously heating the color paste in an oil bath, controlling the temperature of the oil bath at 90 ℃, deodorizing after stopping the reaction to obtain crude carbon black, and recovering styrene monomers in the crude carbon black;
s6: filtering the crude carbon black by using a suction filter, and drying to obtain pre-dispersed grafted carbon black;
s7: and crushing the dried grafted carbon black to obtain the dispersed carbon black.
Example 4
S1: weighing and uniformly mixing 0.03g of maleic anhydride, 0.03g of benzoyl peroxide and 0.6g of styrene monomer with the purity of 95%, thereby obtaining a premix solution A;
s2: adding 5g of raw material carbon black with the particle size of 10nm and the premix solution A into a closed stirring kettle with the stirring speed of 1000rpm, and stirring to obtain a solid mixture B;
s3: adding 0.14 g of sodium dodecyl benzene sulfonate and 94.2g of deionized water into a reaction kettle to obtain a solution C;
s4: adding the solution C and the mixture B into a horizontal nano sand mill with the grinding medium of 0.1nm, and grinding and dispersing for 0.5h to obtain color paste;
s5: adding color paste into a reaction kettle, reacting for 3 hours at a rotating speed of 50rpm, simultaneously heating the color paste in an oil bath, controlling the temperature of the oil bath at 80 ℃, deodorizing after stopping the reaction to obtain crude carbon black, and recovering styrene monomers in the crude carbon black;
s6: filtering the crude carbon black by using a suction filter, and drying to obtain pre-dispersed grafted carbon black;
s7: and crushing the dried grafted carbon black to obtain the dispersed carbon black.
Example 5
S1: weighing 0.035g of maleic anhydride, 0.035g of benzoyl peroxide and 0.63g of styrene monomer with the purity of 96%, and uniformly mixing to obtain a premix solution A;
s2: adding 6.3g of raw material carbon black with the particle size of 60nm and the premix solution A into a closed stirring kettle with the stirring speed of 1300rpm, and stirring to obtain a solid mixture B;
s3: adding 0.16 g of sodium dodecyl benzene sulfonate and 92.84g of deionized water into a reaction kettle to obtain a solution C;
s4: adding the solution C and the mixture B into a horizontal nano sand mill with the grinding medium of 0.1nm, and grinding and dispersing for 0.5h to obtain color paste;
s5: adding color paste into a reaction kettle, reacting for 3 hours at a rotating speed of 50rpm, simultaneously heating the color paste in an oil bath, controlling the temperature of the oil bath at 91 ℃, deodorizing after the reaction is stopped to obtain crude carbon black, and recovering styrene monomers in the crude carbon black;
s6: filtering the crude carbon black by using a suction filter, and drying to obtain pre-dispersed grafted carbon black;
s7: and crushing the dried grafted carbon black to obtain the dispersed carbon black.
Test case
Firstly, the aqueous system evaluation was carried out on the dispersion carbon blacks prepared in examples 1 to 5, respectively, and the evaluation results are as follows:
example 1 the dispersion carbon blacks prepared in examples 1 to 5 were dispersed in an aqueous acrylic coating system by means of a 45mm diameter dispersion disk at 2500rpm for 30min, the fineness of dispersion being less than 10 μm as measured by means of a Markov laser particle sizer.
Example 2 the dispersion carbon blacks prepared in examples 1 to 5 were dispersed in an aqueous polyurethane coating system by means of a 45mm diameter dispersion disk at 2500rpm for 30min, the fineness of dispersion being less than 10 μm as measured by means of a Markov laser particle sizer.
Example 3 the dispersion carbon blacks prepared in examples 1 to 5 were dispersed in an aqueous acrylic ink system by means of a 45mm diameter dispersion disk at 2500rpm for 30min, and the fineness of dispersion was less than 10 μm as measured by means of a Markov laser particle sizer.
Next, the organic solvent system evaluation was carried out on the dispersion carbon blacks prepared in examples 1 to 5, respectively, and the evaluation results were as follows:
example 4: the dispersion carbon blacks prepared in examples 1 to 5 were dispersed in an acrylic coating system by means of a 45mm diameter dispersion disk at 2500rpm for 30min, the fineness of dispersion being less than 10. Mu.m, as measured by means of a Markov laser particle sizer.
Example 5: the dispersion carbon blacks prepared in examples 1 to 5 were dispersed in a nitropolyurethane ink system by means of a 45mm diameter dispersion disk at 2500rpm for 30min, the fineness of dispersion being less than 10. Mu.m, as measured by means of a Markov laser particle sizer.
According to the test result, the dispersion carbon black obtained by the preparation method provided by the invention has smaller dispersion fineness and better dispersion effect.
The foregoing describes one embodiment of the present invention in detail, but the description is only a preferred embodiment of the present invention and should not be construed as limiting the scope of the invention. All equivalent changes and modifications within the scope of the present invention are intended to be covered by the present invention.
Claims (7)
1. The preparation method of the grinding-free self-dispersing carbon black is characterized by comprising the following steps of:
s1: weighing maleic anhydride, benzoyl peroxide and styrene monomer, and uniformly mixing to obtain a premix solution A;
s2: adding raw material carbon black and the premix A into a stirring kettle, and stirring to obtain a solid mixture B;
s3: adding sodium dodecyl benzene sulfonate and deionized water into a reaction kettle to obtain a solution C;
s4: adding the solution C and the mixture B into a nano sand mill, and grinding and dispersing for 0.5-2 hours to obtain color paste;
s5: adding color paste into a reaction kettle, reacting for 1.5-10h at a rotating speed of 50rpm, simultaneously heating the color paste in an oil bath, controlling the temperature of the oil bath to be 80-95 ℃, deodorizing after the reaction is stopped, obtaining crude carbon black, and recycling styrene monomers in the crude carbon black.
S6: filtering the crude carbon black by using a suction filter, and drying to obtain pre-dispersed grafted carbon black;
s7: and crushing the dried grafted carbon black to obtain the dispersed carbon black.
Wherein, the deionized water is 88 to 94 parts by weight, the raw material carbon black is 5 to 9 parts by weight, the maleic anhydride is 0.02 to 0.1 part by weight, the benzoyl peroxide is 0.02 to 0.1 part by weight, the sodium dodecyl benzene sulfonate is 0.1 to 0.3 part by weight, and the styrene monomer is 0.5 to 1.8 parts by weight.
2. The method for producing a milled self-dispersing carbon black according to claim 1, wherein the deionized water is 90 to 92 parts by weight, the raw material carbon black is 6 to 8 parts by weight, the maleic anhydride is 0.04 to 0.08 part by weight, the benzoyl peroxide is 0.04 to 0.08 part by weight, the sodium dodecylbenzenesulfonate is 0.15 to 0.25 part by weight, and the styrene monomer is 0.8 to 1.5 part by weight.
3. The method for producing a milled self-dispersing carbon black according to claim 2, wherein the deionized water is 91 parts, the raw material carbon black is 7 parts, the maleic anhydride is 0.06 parts, the benzoyl peroxide is 0.06 parts, the sodium dodecylbenzenesulfonate is 0.2 parts, and the styrene monomer is 1.2 parts by weight.
4. The method for producing a milled self-dispersing carbon black according to claim 3, wherein the particle diameter of the raw material carbon black is 10nm to 100nm.
5. The method for producing a milled self-dispersing carbon black according to claim 3, wherein the purity of the styrene monomer, maleic anhydride, benzoyl peroxide and sodium dodecylbenzenesulfonate is not lower than 95%.
6. The method for producing a milled self-dispersing carbon black according to claim 1, wherein the stirring vessel in S2 is a closed stirring vessel, and the stirring speed is 1000 to 1500rpm.
7. The method for preparing ground self-dispersing carbon black according to claim 1, wherein the nano sand mill in S4 is a horizontal sand mill, and the grinding medium diameter of the horizontal sand mill is 0.1mm.
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