CN114316635A - Amphiphilic carbon black and preparation method thereof - Google Patents
Amphiphilic carbon black and preparation method thereof Download PDFInfo
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- CN114316635A CN114316635A CN202111681652.2A CN202111681652A CN114316635A CN 114316635 A CN114316635 A CN 114316635A CN 202111681652 A CN202111681652 A CN 202111681652A CN 114316635 A CN114316635 A CN 114316635A
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- carbon black
- silane
- sodium chloride
- amphiphilic
- hydrophobic
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- 239000006229 carbon black Substances 0.000 title claims abstract description 249
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 182
- 229910000077 silane Inorganic materials 0.000 claims abstract description 99
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 96
- 239000011780 sodium chloride Substances 0.000 claims abstract description 91
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 62
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 55
- 238000003756 stirring Methods 0.000 claims abstract description 53
- 238000010791 quenching Methods 0.000 claims abstract description 49
- 230000000171 quenching effect Effects 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 230000008569 process Effects 0.000 claims abstract description 26
- 238000000227 grinding Methods 0.000 claims abstract description 24
- 150000001721 carbon Chemical class 0.000 claims abstract description 23
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 21
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 238000002791 soaking Methods 0.000 claims abstract description 11
- -1 silane modified carbon Chemical class 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 18
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 230000002378 acidificating effect Effects 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims description 2
- 125000003342 alkenyl group Chemical group 0.000 claims description 2
- 239000007822 coupling agent Substances 0.000 claims description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 229910021385 hard carbon Inorganic materials 0.000 claims description 2
- 239000005055 methyl trichlorosilane Substances 0.000 claims description 2
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 2
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 2
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 claims description 2
- UMXXGDJOCQSQBV-UHFFFAOYSA-N n-ethyl-n-(triethoxysilylmethyl)ethanamine Chemical compound CCO[Si](OCC)(OCC)CN(CC)CC UMXXGDJOCQSQBV-UHFFFAOYSA-N 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 229910021384 soft carbon Inorganic materials 0.000 claims description 2
- GBXOGFTVYQSOID-UHFFFAOYSA-N trichloro(2-methylpropyl)silane Chemical compound CC(C)C[Si](Cl)(Cl)Cl GBXOGFTVYQSOID-UHFFFAOYSA-N 0.000 claims description 2
- RYPYGDUZKOPBEL-UHFFFAOYSA-N trichloro(hexadecyl)silane Chemical compound CCCCCCCCCCCCCCCC[Si](Cl)(Cl)Cl RYPYGDUZKOPBEL-UHFFFAOYSA-N 0.000 claims description 2
- PYJJCSYBSYXGQQ-UHFFFAOYSA-N trichloro(octadecyl)silane Chemical compound CCCCCCCCCCCCCCCCCC[Si](Cl)(Cl)Cl PYJJCSYBSYXGQQ-UHFFFAOYSA-N 0.000 claims description 2
- RCHUVCPBWWSUMC-UHFFFAOYSA-N trichloro(octyl)silane Chemical compound CCCCCCCC[Si](Cl)(Cl)Cl RCHUVCPBWWSUMC-UHFFFAOYSA-N 0.000 claims description 2
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- JAUUQAGOKRRGIR-UHFFFAOYSA-N butan-2-yl-chloro-diethylsilane Chemical compound CCC(C)[Si](Cl)(CC)CC JAUUQAGOKRRGIR-UHFFFAOYSA-N 0.000 claims 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical class CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims 1
- 230000001804 emulsifying effect Effects 0.000 abstract 1
- 235000019241 carbon black Nutrition 0.000 description 208
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical group CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 16
- 229960003493 octyltriethoxysilane Drugs 0.000 description 16
- 239000006185 dispersion Substances 0.000 description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 description 10
- 239000002270 dispersing agent Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 10
- PKDCQJMRWCHQOH-UHFFFAOYSA-N triethoxysilicon Chemical compound CCO[Si](OCC)OCC PKDCQJMRWCHQOH-UHFFFAOYSA-N 0.000 description 10
- 238000005507 spraying Methods 0.000 description 9
- 238000003801 milling Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 3
- 230000002159 abnormal effect Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000000080 wetting agent Substances 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- JAJWGJBVLPIOOH-IZYKLYLVSA-M sodium taurocholate Chemical compound [Na+].C([C@H]1C[C@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC(=O)NCCS([O-])(=O)=O)C)[C@@]2(C)[C@@H](O)C1 JAJWGJBVLPIOOH-IZYKLYLVSA-M 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- QAUWMTWMFXYNMQ-UHFFFAOYSA-N C(C)O.C(CCCCCCC)[Si](OCC)(OCC)OCC Chemical compound C(C)O.C(CCCCCCC)[Si](OCC)(OCC)OCC QAUWMTWMFXYNMQ-UHFFFAOYSA-N 0.000 description 1
- GZVUUPZCHCULFW-UHFFFAOYSA-N CCO.CCO[SiH](OCC)OCC Chemical compound CCO.CCO[SiH](OCC)OCC GZVUUPZCHCULFW-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- INJVFBCDVXYHGQ-UHFFFAOYSA-N n'-(3-triethoxysilylpropyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CCCNCCN INJVFBCDVXYHGQ-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003335 steric effect Effects 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
- ZOYFEXPFPVDYIS-UHFFFAOYSA-N trichloro(ethyl)silane Chemical compound CC[Si](Cl)(Cl)Cl ZOYFEXPFPVDYIS-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses an amphiphilic carbon black and a preparation method thereof, wherein the amphiphilic carbon black comprises carbon black: 96-99 parts; hydrophobic silane coupling agent: 0.2-2 parts of a solvent; hydrophilic silane coupling agent: 0.2-2 parts. The preparation method of the amphiphilic carbon black comprises the following steps: sodium chloride is crushed and sieved and then is added into a tank with stirring; conveying the heated sodium chloride to a quenching section of a carbon black reaction furnace through compressed air, and quenching the carbon black in the carbon black reaction furnace; grinding carbon black containing sodium chloride by a grinding mill, cooling, and adding a silane solution in the process of secondary grinding; soaking the hydrophobic modified carbon black in water to remove sodium chloride; dispersing the hydrophobically modified carbon black in a stirring kettle containing ethanol, then adding a catalyst, uniformly stirring, and adding hydrophilic silane; distilling the hydrophilic silane modified carbon black at low temperature under negative pressure, and drying until the heating loss is lower than 1 wt.%; the amphiphilic carbon black has the advantages of excellent dispersibility in an oily system and an aqueous system and certain emulsifying property.
Description
Technical Field
The invention relates to amphiphilic carbon black and a preparation method thereof.
Background
The carbon black has the characteristics of small particle size, very large surface area, less surface groups and difficult dispersion in an aqueous system or an oily system, the dispersion process of the carbon black is a physical process, and a plurality of separate sub-processes are also included in the total process. Mechanical dispersion of carbon black in aqueous or oily systems is the breaking up of the carbon black from agglomerates into smaller aggregates and simultaneous wetting by the medium. The carbon black dispersion process is also accompanied by a random uniform distribution process of carbon black particles, and if the viscosity of the solution system is low or a surfactant is added, secondary agglomeration of the dispersed carbon black particles occurs. This effect reduces the color strength and hiding power of the carbon black, and in order to prevent secondary agglomeration, a dispersant and a wetting agent must be added during the dispersion of the carbon black.
Chinese patent CN101481108A discloses a method for producing easily dispersible carbon black, wherein the production steps of the method are almost the same as those of the traditional furnace carbon black, but a certain amount of potassium carbonate is added into raw oil, a silane coupling agent is added before the carbon black enters a filter bag, and the silane coupling agent reacts with the carbon black to improve the dispersibility of the carbon black in the material.
Chinese patent CN 101910325B discloses a surface-treated carbon black aqueous dispersion and a method for producing the same, which carbon black is suitable as an aqueous carbon black for inkjet printers. The preparation method comprises the steps of oxidizing carbon black to form a large number of oxygen-containing groups, greatly improving the hydrophilicity of the carbon black, then adding an amino-containing compound and a triazine series condensing agent at normal temperature, carrying out condensation reaction on hydrophilic functional groups on the surface of the carbon black and the amino compound, removing large particles and unreacted organic matters after the reaction is finished, purifying the carbon black, concentrating and discharging, wherein the application direction of the carbon black is narrow.
Chinese patent CN103965664B discloses a carbon black particle dispersant, its preparation method and application, the dispersant of the carbon black comprises sodium taurocholate or the mixture of sodium dodecyl benzene sulfonate and sodium taurocholate, glycol and organic solvent, the dispersant can make the carbon black aggregate disperse smaller, the direction of the invention is high performance polyethylene pipe.
Chinese patent CN111423748A discloses a production process of a high-temperature resistant dispersant for dispersing carbon black color paste to a nanometer level, wherein the dispersant produced by the production process is coated on the surface of carbon black to form a barrier layer with a certain thickness by utilizing the adsorption effect of a polar section in the dispersant and the surface of the carbon black and the compatibility of a flexible section to a base material, so that the agglomeration effect among carbon black particles is reduced, and the carbon black obtains better dispersion stability.
In summary, there are two types of methods for improving the dispersibility of carbon black: firstly, the surface of carbon black is modified in a hydrophilic or hydrophobic way, so that the dispersibility of the carbon black in water or oil is improved; secondly, in the process of reuse, a dispersant is added into the system while the carbon black is crushed by mechanical force, so that the agglomeration effect of the carbon black is reduced, and the dispersibility of the carbon black is improved.
Disclosure of Invention
The invention aims to solve the technical problem that conventional carbon black is prepared into amphiphilic carbon black which can be dispersed in an oily or aqueous system, so that the grinding time is shortened, the use amount of a dispersing agent and a wetting agent is reduced, and the energy conservation and the consumption reduction can be realized.
In order to solve the technical problems, the technical scheme of the invention is as follows: an amphiphilic carbon black comprises the following components in parts by weight:
a carbon black component:
carbon black: 96-99 parts;
hydrophobic silane coupling agent: 0.2-2 parts of a solvent;
hydrophilic silane coupling agent: 0.2-2 parts.
Further, the carbon black is soft or hard carbon black; and/or the hydrophobic silane coupling agent is at least one of octadecyl trichlorosilane, hexadecyl trichlorosilane, octyl trichlorosilane, ethyl trichlorosilane, methyl trichlorosilane, isobutyl trichlorosilane, corresponding triethoxy silicon or trimethoxy silane thereof, or various silane coupling agents containing alkenyl and fluorine;
and/or the hydrophilic siloxane coupling agent is at least one of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltriethoxysilane, N- (beta-aminoethyl) -gamma-aminopropylmethyldimethoxysilane and diethylaminomethyltriethoxysilane.
Further, the preparation method of the amphiphilic carbon black is characterized by comprising the following steps:
(1a) crushing and sieving sodium chloride, and adding sodium chloride powder into a tank with a stirrer for later use;
(2a) sending preheated sodium chloride to a quenching section of a carbon black reaction furnace through compressed air, and then adding quenching water into the quenching section of the carbon black reaction furnace to quench the carbon black in the quenching section of the carbon black reaction furnace;
(3a) grinding carbon black containing sodium chloride by a grinding mill, cooling, and adding an ethanol solution containing a hydrophobic silane coupling agent in the process of secondary grinding;
(4a) soaking the hydrophobic modified carbon black in water to remove sodium chloride;
(5a) dispersing the hydrophobically modified carbon black in a stirring kettle containing ethanol, then adding a catalyst, uniformly stirring, and adding hydrophilic silane;
(6a) and (3) distilling the hydrophilic silane modified carbon black at low temperature under negative pressure, and drying until the heating loss is lower than 1 wt.%.
Further, the preparation method of the amphiphilic carbon black is characterized in that the sodium chloride is crushed and sieved with a mesh number of 100-300 meshes, and the preheating temperature of the sodium chloride is 200-500 ℃.
Further, after sodium chloride is added into a quenching section of the carbon black reaction furnace, the temperature of the carbon black is ensured to be more than or equal to 820 ℃, and then quenching water is added to reduce the temperature of the carbon black to be below 800 ℃.
The mass ratio of the sodium chloride to the carbon black is 2-10.
Further, the milled carbon black is cooled to 20 ℃ to 50 ℃.
Further, the preparation steps of the silane solution are as follows: dissolving silane in ethanol, uniformly stirring at a high speed until the silane content is 5-50 wt%, adding a catalyst accounting for 0.2-1 wt% of the mass of the silane, uniformly stirring, standing for 5-30 min, and using the silane, wherein the silane accounts for 0.2-3 wt% of the amount of carbon black.
Further, the catalyst is a weakly acidic catalyst or a weakly basic catalyst.
Further, the weakly acidic catalyst is acetic acid.
Further, the weak alkaline catalyst is ammonia water, a water solution of triethanolamine and a water solution of ethylenediamine.
After the technical scheme is adopted, the amphiphilic carbon black has excellent dispersibility in an oily system and an aqueous system, and is 2-15 orders of magnitude of the carbon black without adopting the technology, sodium chloride is adopted as a covering agent, the melting point of the sodium chloride is 801 ℃, when the sodium chloride is added into a quenching section of a carbon black reaction furnace, the temperature of the sodium chloride is lower, the carbon black is cooled, but the temperature of the carbon black is ensured to be more than or equal to 820 ℃, the sodium chloride is in a molten state, the carbon black is adhered to the surface of the molten sodium chloride, after quenching water is added, the temperature of the carbon black is reduced to be less than or equal to 800 ℃, the sodium chloride is changed into a solid, and the carbon black is embedded in the sodium chloride solid, so that the collective carbon black is covered.
Drawings
FIG. 1 is a schematic illustration of the preparation of an amphiphilic carbon black of the present invention;
FIG. 2 is an SEM image of an amphiphilic carbon black aggregate of the present invention.
Detailed Description
In order that the present invention may be more readily and clearly understood, a more particular description of the invention briefly described above will be rendered by reference to specific embodiments that are illustrated in the appended drawings.
Example one
An amphiphilic carbon black comprises the following components in parts by weight:
a carbon black component:
carbon black: 98.6 parts of a mixture;
hydrophobic type silane: 0.3 part;
hydrophilic silane: 1.1 parts;
the carbon black is N110;
the hydrophobic silane is octyl triethoxysilane;
the hydrophilic silane is gamma-glycidyl ether oxypropyl triethoxysilane;
preparing a hydrophobic silane solution, namely dissolving silane in ethanol, uniformly stirring at a high speed until the content of the silane is 10 wt%, adding acetic acid accounting for 0.5 wt% of the mass of the silane as a catalyst, uniformly stirring, and standing for 10min to obtain the hydrophobic silane solution.
The preparation method of the amphiphilic carbon black comprises the following steps:
(1a) sodium chloride is crushed and sieved by a 300-mesh sieve, and sodium chloride powder is added into a tank with a stirrer and preheated to 300 ℃;
(2a) conveying preheated sodium chloride powder to a quenching section of a carbon black reaction furnace by compressed air, wherein the mass ratio of sodium chloride to carbon black is 4, the temperature of the carbon black is higher than 820 ℃, then adding quenching water into the quenching section of the carbon black reaction furnace, and reducing the temperature of the carbon black in the quenching section to 680-720 ℃;
(3a) milling carbon black containing sodium chloride by a mill, cooling to 40-50 ℃, and spraying an ethanol solution of octyl triethoxysilane into the system by using compressed air in the secondary grinding process;
(4a) soaking the hydrophobic modified carbon black in hot water to remove sodium chloride;
(5a) dispersing the hydrophobically modified carbon black in a stirring kettle containing ethanol, adding gamma-glycidyl ether oxypropyltriethoxysilane into the system, uniformly stirring, slowly dropwise adding ammonia water, reacting for 1h, and drying at low temperature under negative pressure until the heating decrement is lower than 1 wt.%.
Example two
An amphiphilic carbon black comprises the following components in parts by weight:
a carbon black component:
carbon black: 98.6 parts of a mixture;
hydrophobic type silane: 0.3 part;
hydrophilic silane: 1.1 parts;
the carbon black is N220;
the hydrophobic silane is octyl triethoxysilane;
the hydrophilic silane is gamma-glycidyl ether oxypropyl triethoxysilane;
preparing a hydrophobic silane solution, namely dissolving silane in ethanol, uniformly stirring at a high speed until the content of the silane is 10 wt%, adding acetic acid accounting for 0.5 wt% of the mass of the silane as a catalyst, uniformly stirring, and standing for 10min to obtain the hydrophobic silane solution.
The preparation method of the amphiphilic carbon black comprises the following steps:
(1a) sodium chloride is crushed and sieved by a 260-mesh sieve, and sodium chloride powder is added into a tank with a stirrer and preheated to 300 ℃;
(2a) conveying preheated sodium chloride powder to a quenching section of a carbon black reaction furnace by compressed air, wherein the mass ratio of sodium chloride to carbon black is 4, the temperature of the carbon black is higher than 820 ℃, then adding quenching water into the quenching section of the carbon black reaction furnace, and reducing the temperature of the carbon black in the quenching section to 680-720 ℃;
(3a) milling carbon black containing sodium chloride by a mill, cooling to 40-50 ℃, and spraying an octyltriethoxysilane ethanol solution into a system by using compressed air in a secondary grinding process;
(4a) soaking the hydrophobic modified carbon black in hot water to remove sodium chloride;
(5a) dispersing the hydrophobically modified carbon black in a stirring kettle containing ethanol, adding gamma-glycidoxypropyltriethoxysilane into the stirring kettle, uniformly stirring, slowly dropwise adding ammonia water, reacting for 1h, drying at low temperature under negative pressure, and drying until the heating decrement is lower than 1 wt.%.
EXAMPLE III
An amphiphilic carbon black comprises the following components in parts by weight:
a carbon black component:
carbon black: 98.6 parts of a mixture;
hydrophobic type silane: 0.3 part;
hydrophilic silane: 1.1 parts;
the carbon black is N330;
the hydrophobic silane is octyl triethoxysilane;
the hydrophilic silane is gamma-glycidyl ether oxypropyl triethoxysilane;
preparing a hydrophobic silane solution, namely dissolving silane in ethanol, uniformly stirring at a high speed until the content of the silane is 10 wt%, adding acetic acid accounting for 0.5 wt% of the mass of the silane as a catalyst, uniformly stirring, and standing for 10min to obtain the hydrophobic silane solution.
The preparation method of the amphiphilic carbon black comprises the following steps:
(1a) sodium chloride is crushed and sieved by a 200-mesh sieve, and sodium chloride powder is added into a tank with a stirrer and preheated to 300 ℃;
(2a) conveying preheated sodium chloride powder to a quenching section of a carbon black reaction furnace by compressed air, wherein the mass ratio of sodium chloride to carbon black is 4, the temperature of the carbon black is higher than 820 ℃, then adding quenching water into the quenching section of the carbon black reaction furnace, and reducing the temperature of the carbon black in the quenching section to 680-720 ℃;
(3a) milling carbon black containing sodium chloride by a mill, cooling to 40-50 ℃, and spraying an octyltriethoxysilane ethanol solution into a system by using compressed air in a secondary grinding process;
(4a) soaking the hydrophobic modified carbon black in hot water to remove sodium chloride;
(5a) dispersing the hydrophobically modified carbon black in a stirring kettle containing ethanol, adding gamma-glycidoxypropyltriethoxysilane into the stirring kettle, uniformly stirring, slowly dropwise adding ammonia water, reacting for 1h, drying at low temperature under negative pressure, and drying until the heating decrement is lower than 1 wt.%.
Example four
An amphiphilic carbon black comprises the following components in parts by weight:
a carbon black component:
carbon black: 98.6 parts of a mixture;
hydrophobic type silane: 0.3 part;
hydrophilic silane: 1.1 parts;
the carbon black is N550;
the hydrophobic silane is octyl triethoxysilane;
the hydrophilic silane is gamma-glycidyl ether oxypropyl triethoxysilane;
preparing a hydrophobic silane solution, namely dissolving silane in ethanol, uniformly stirring at a high speed until the content of the silane is 10 wt%, adding acetic acid with the mass of 0.5 wt% of the silane as a catalyst, uniformly stirring, and standing for 10min to obtain the hydrophobic silane solution.
The preparation method of the amphiphilic carbon black comprises the following steps:
(1a) sodium chloride is crushed and sieved by a 160-mesh sieve, and sodium chloride powder is added into a tank with a stirrer and preheated to 300 ℃;
(2a) conveying preheated sodium chloride powder to a quenching section of a carbon black reaction furnace by compressed air, wherein the mass ratio of sodium chloride to carbon black is 4, the temperature of the carbon black is higher than 820 ℃, then adding quenching water into the quenching section of the carbon black reaction furnace, and reducing the temperature of the carbon black in the quenching section to 680-720 ℃;
(3a) milling carbon black containing sodium chloride by a mill, cooling to 40-50 ℃, and spraying an octyltriethoxysilane ethanol solution into a system by using compressed air in a secondary grinding process;
(4a) soaking the hydrophobic modified carbon black in hot water to remove sodium chloride;
(5a) dispersing the hydrophobically modified carbon black in a stirring kettle containing ethanol, adding gamma-glycidoxypropyltriethoxysilane into the stirring kettle, uniformly stirring, slowly dropwise adding ammonia water, reacting for 1h, drying at low temperature under negative pressure, and drying until the heating decrement is lower than 1 wt.%.
EXAMPLE five
An amphiphilic carbon black comprises the following components in parts by weight:
a carbon black component:
carbon black: 98.6 parts of a mixture;
hydrophobic type silane: 0.3 part;
hydrophilic silane: 1.1 parts;
the carbon black is N660;
the hydrophobic silane is octyl triethoxysilane;
the hydrophilic silane is gamma-glycidyl ether oxypropyl triethoxysilane;
preparing a hydrophobic silane solution, namely dissolving silane in ethanol, uniformly stirring at a high speed until the content of the silane is 10 wt%, adding acetic acid accounting for 0.5 wt% of the mass of the silane as a catalyst, uniformly stirring, and standing for 10min to obtain the hydrophobic silane solution.
The preparation method of the amphiphilic carbon black comprises the following steps:
(1a) sodium chloride is crushed and sieved by a 160-mesh sieve, and sodium chloride powder is added into a tank with a stirrer and preheated to 300 ℃;
(2a) conveying preheated sodium chloride powder to a quenching section of a carbon black reaction furnace by compressed air, wherein the mass ratio of sodium chloride to carbon black is 4, the temperature of the carbon black is higher than 820 ℃, then adding quenching water into the quenching section of the carbon black reaction furnace, and reducing the temperature of the carbon black in the quenching section to 680-720 ℃;
(3a) milling carbon black containing sodium chloride by a mill, cooling to 40-50 ℃, and spraying an octyltriethoxysilane ethanol solution into a system by using compressed air in a secondary grinding process;
(4a) soaking the hydrophobic modified carbon black in hot water to remove sodium chloride;
(5a) dispersing the hydrophobically modified carbon black in a stirring kettle containing ethanol, adding gamma-glycidoxypropyltriethoxysilane into the stirring kettle, uniformly stirring, slowly dropwise adding ammonia water, reacting for 1h, drying at low temperature under negative pressure, and drying until the heating decrement is lower than 1 wt.%.
Comparative example 1
An amphiphilic carbon black comprises the following components in parts by weight:
a carbon black component:
carbon black: 98.6 parts of a mixture;
hydrophobic type silane: 0.3 part;
hydrophilic silane: 1.1 parts;
the carbon black is N660;
the hydrophobic silane is octyl triethoxysilane;
the hydrophilic silane is gamma-glycidyl ether oxypropyl triethoxysilane;
preparing a hydrophobic silane solution, namely dissolving silane in ethanol, uniformly stirring at a high speed until the content of the silane is 10 wt%, adding acetic acid accounting for 0.5 wt% of the mass of the silane as a catalyst, uniformly stirring, and standing for 10min to obtain the hydrophobic silane solution.
The preparation method of the amphiphilic carbon black comprises the following steps:
(1a) grinding carbon black by a grinding mill, cooling to 40-50 ℃, and spraying an octyl triethoxysilane ethanol solution into a system by using compressed air in a secondary grinding process;
(2a) dispersing the hydrophobically modified carbon black in a stirring kettle containing ethanol, adding gamma-glycidoxypropyltriethoxysilane into the stirring kettle, uniformly stirring, slowly dropwise adding ammonia water, reacting for 1h, drying at low temperature under negative pressure, and drying until the heating decrement is lower than 1 wt.%.
Comparative example No. two
An amphiphilic carbon black comprises the following components in parts by weight:
a carbon black component:
carbon black: 98.6 parts of a mixture;
hydrophobic type silane: 0.3 part;
hydrophilic silane: 1.1 parts;
the carbon black is N660;
the hydrophobic silane is octyl triethoxysilane;
the hydrophilic silane is gamma-glycidyl ether oxypropyl triethoxysilane;
preparing a hydrophobic silane solution, namely dissolving silane in ethanol, uniformly stirring at a high speed until the content of the silane is 10 wt%, adding acetic acid accounting for 0.5 wt% of the mass of the silane as a catalyst, uniformly stirring, and standing for 10min to obtain the hydrophobic silane solution.
The preparation method of the amphiphilic carbon black comprises the following steps:
(1a) sodium chloride is crushed and sieved by a 160-mesh sieve, and sodium chloride powder is added into a tank with a stirrer and preheated to 300 ℃;
(2a) conveying preheated sodium chloride powder to a quenching section of a carbon black reaction furnace by compressed air, wherein the mass ratio of sodium chloride to carbon black is 4, the temperature of the carbon black is higher than 820 ℃, then adding quenching water into the quenching section of the carbon black reaction furnace, and reducing the temperature of the carbon black in the quenching section to 680-720 ℃;
(3a) milling carbon black containing sodium chloride by a mill, cooling to 40-50 ℃, and spraying an octyltriethoxysilane ethanol solution into a system by using compressed air in a secondary grinding process;
(4a) soaking the hydrophobic modified carbon black in hot water to remove sodium chloride;
(5a) dispersing the hydrophobically modified carbon black in a stirring kettle containing ethanol, adding gamma-glycidoxypropyltriethoxysilane into the stirring kettle, uniformly stirring, slowly dropwise adding ammonia water, reacting for 1h, drying at low temperature under negative pressure, and drying until the heating decrement is lower than 1 wt.%.
Comparative example three
An amphiphilic carbon black comprises the following components in parts by weight:
a carbon black component:
carbon black: 98.6 parts of a mixture;
hydrophobic type silane: 1.4 parts;
the carbon black is N660;
the hydrophobic silane is octyl triethoxysilane;
preparing a hydrophobic silane solution, namely dissolving silane in ethanol, uniformly stirring at a high speed until the content of the silane is 10 wt%, adding acetic acid accounting for 0.5 wt% of the mass of the silane as a catalyst, uniformly stirring, and standing for 10min to obtain the hydrophobic silane solution.
The preparation method of the amphiphilic carbon black comprises the following steps:
(1a) sodium chloride is crushed and sieved by a 160-mesh sieve, and sodium chloride powder is added into a tank with a stirrer and preheated to 300 ℃;
(2a) conveying preheated sodium chloride powder to a quenching section of a carbon black reaction furnace by compressed air, wherein the mass ratio of sodium chloride to carbon black is 4, the temperature of the carbon black is higher than 820 ℃, then adding quenching water into the quenching section of the carbon black reaction furnace, and reducing the temperature of the carbon black in the quenching section to 680-720 ℃;
(3a) milling carbon black containing sodium chloride by a mill, cooling to 40-50 ℃, and spraying an octyltriethoxysilane ethanol solution into a system by using compressed air in a secondary grinding process;
(4a) soaking the hydrophobic modified carbon black in hot water to remove sodium chloride
(5a) Dispersing carbon black in a stirring kettle containing ethanol, adding octyl triethoxysilane into the stirring kettle, stirring uniformly, slowly dropwise adding ammonia water, reacting for 1h, drying at low temperature under negative pressure, and drying until the heating decrement is less than 1 wt.%.
Drying the carbon black until the heating loss is less than 1 wt.%.
Comparative example No. four
Carbon black: 98.6 parts of a mixture;
hydrophilic silane: 1.4 parts;
the carbon black is N660;
the hydrophilic silane is gamma-glycidyl ether oxypropyl triethoxysilane;
the preparation method of the amphiphilic carbon black comprises the following steps:
(1a) sodium chloride is crushed and sieved by a 160-mesh sieve, and sodium chloride powder is added into a tank with a stirrer and preheated to 300 ℃;
(2a) conveying preheated sodium chloride powder to a quenching section of a carbon black reaction furnace by compressed air, wherein the mass ratio of sodium chloride to carbon black is 4, the temperature of the carbon black is higher than 820 ℃, then adding quenching water into the quenching section of the carbon black reaction furnace, and reducing the temperature of the carbon black in the quenching section to 680-720 ℃;
(3a) milling carbon black containing sodium chloride by a mill, cooling to 40-50 ℃, and spraying a gamma-glycidyl ether oxypropyl triethoxysilane ethanol solution into a system by using compressed air in a secondary grinding process;
(4a) soaking the hydrophobic modified carbon black in hot water to remove sodium chloride;
(5a) dispersing carbon black in a stirring kettle containing ethanol, adding gamma-glycidyl ether oxypropyl triethoxysilane into the stirring kettle, stirring uniformly, slowly dropwise adding ammonia water, reacting for 1h, drying at low temperature under negative pressure, and drying until the heating decrement is less than 1 wt.%.
Table 1: the amphiphilic carbon blacks in examples one to five and comparative examples one to four have dispersion stability in water. The method for testing the dispersibility stability of the amphiphilic carbon black in water comprises the steps of grinding 15 wt.% of carbon black and 85 wt.% of water for 30min by a horizontal sand mill, standing, stopping the experiment when obvious layering occurs, and recording the time.
Table 2: examples first to fifth and comparative examples first to fourth
Among them, the components and the parts by mass of the components of the amphiphilic carbon black in examples one to five and comparative examples one to four differ only in the inconsistency of the carbon black and the inconsistency of the mesh number of sodium chloride due to the inconsistency of the carbon black.
As shown in Table 1, the dispersion stability of the amphiphilic carbon black of the invention in water is 3-12 orders of magnitude of that of the modified carbon black in an abnormal process; and the stability does not vary much when different carbon blacks are used, because the non-uniform particle size of the carbon black results in non-uniform aggregates that are matched by different amounts of sodium chloride.
As shown in Table 2, the dispersion stability of the amphiphilic carbon black in xylene is close to 2-15 orders of magnitude of that of modified carbon black in an abnormal process; and when different carbon blacks are used, the dispersion stability in xylene does not change much because the dispersion of the amphiphilic carbon black in xylene does not change much because the particle size of the carbon black is not uniform, resulting in non-uniform aggregates and different numbers of sodium chloride are adopted to match the aggregates.
The working principle of the invention is as follows:
the amphiphilic carbon black has good dispersibility in oil and water and is 2-15 orders of magnitude of carbon black modified in an abnormal process, sodium chloride is used as a covering material (the melting point of the sodium chloride is 801 ℃), the covering material is added into a system at a temperature higher than the melting point of the sodium chloride, the sodium chloride is in a molten state, carbon black aggregates are adhered to the surface of the molten sodium chloride in the molten state, after chilled water is introduced, the temperature of the carbon black containing the sodium chloride is reduced to be below 800 ℃, the sodium chloride is changed into solid crystals from the molten state, the carbon black aggregates are embedded in sodium chloride crystals, then hydrophobic silane is added into the system in the grinding process to modify the surface of the exposed carbon black, the sodium chloride is dissolved and removed, the carbon black aggregates embedded in the sodium chloride are exposed, and then hydrophilic silane is used for modification (the surface of the carbon black modified by the hydrophobic silane can generate steric effect and has no active group, so that the hydrophilic silane can only modify the part which is not modified by the hydrophobic silane), a part of hydrophilic and the other part of hydrophobic are formed on a carbon black aggregate, and the dispersibility of the carbon black in an oily or aqueous system is improved similar to a surfactant. The amphiphilic carbon black disclosed by the invention has excellent dispersibility in an oily system and a water-based system, reduces the grinding time and the use of a dispersing agent and a wetting agent, and can save energy and reduce consumption.
The above embodiments are provided to further explain the technical problems, technical solutions and advantages of the present invention in detail, it should be understood that the above embodiments are only examples of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection of the present invention.
Claims (10)
1. The amphiphilic carbon black is characterized by comprising the following components in parts by mass and preparation steps:
amphiphilic carbon black component:
carbon black: 96-99 parts;
hydrophobic silane coupling agent: 0.2-2 parts of a solvent;
hydrophilic silane coupling agent: 0.2-2 parts.
2. The amphiphilic carbon black of claim 1, wherein:
the carbon black is soft or hard carbon black;
and/or the hydrophobic silane coupling agent is at least one of octadecyltrichlorosilane, hexadecyl trichlorosilane, octyl trichlorosilane, ethyltriethylchlorosilane, methyl trichlorosilane, isobutyl trichlorosilane, corresponding triethoxysilanes or trimethoxys thereof, or various silane coupling agents containing alkenyl and fluorine;
and/or the hydrophilic siloxane coupling agent is at least one of gamma-aminopropyltriethoxysilane, gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, N- (beta-aminoethyl) -gamma-aminopropylmethyldimethoxysilane and diethylaminomethyltriethoxysilane.
3. The process for the preparation of amphiphilic carbon black according to claim 1, characterized in that it comprises the following steps:
(1a) crushing and sieving sodium chloride, and adding sodium chloride powder into a tank with a stirrer for later use;
(2a) conveying the heated sodium chloride to a quenching section of a carbon black reaction furnace through compressed air, and then adding quenching water into the quenching section of the carbon black reaction furnace to quench the carbon black in the carbon black reaction furnace;
(3a) grinding carbon black containing sodium chloride by a grinding mill, cooling, and adding a silane solution in a secondary grinding process, wherein the silane solution is an ethanol solution containing hydrophobic silane;
(4a) soaking the hydrophobic modified carbon black in water to remove sodium chloride;
(5a) dispersing the hydrophobically modified carbon black in a stirring kettle containing ethanol, then adding a catalyst, uniformly stirring, and adding hydrophilic silane;
(6a) and (3) distilling the hydrophilic silane modified carbon black at low temperature under negative pressure, and drying until the heating loss is lower than 1 wt.%.
4. The method for preparing amphiphilic carbon black according to claim 3, wherein the sodium chloride is crushed and sieved, the mesh number of the screen is 100-300 meshes, and the preheating temperature of the sodium chloride is 200-500 ℃.
5. The preparation method of amphiphilic carbon black according to claim 3, wherein after the sodium chloride is added into a quenching section of a carbon black reaction furnace, the temperature of the carbon black is more than or equal to 820 ℃, then quenching water is added to reduce the temperature of the carbon black to be below 800 ℃, and the mass ratio of the sodium chloride to the carbon black is 2-10.
6. A process for the preparation of the amphiphilic carbon black of claim 3, wherein the milled carbon black is cooled to a temperature of from 20 ℃ to 50 ℃.
7. A method of preparing the amphiphilic carbon black of claim 3, wherein the silane solution is prepared by the steps of: dissolving silane in ethanol, uniformly stirring at a high speed until the silane content is 5-50 wt%, adding a catalyst accounting for 0.2-1 wt% of the mass of the silane, uniformly stirring, standing for 5-30 min, and using the silane, wherein the silane accounts for 0.2-3 wt% of the amount of carbon black.
8. A process for producing an amphiphilic carbon black according to any one of claims 2 or 7, characterized in that the catalyst is a weakly acidic catalyst or a weakly basic catalyst.
9. A process for preparing an amphiphilic carbon black according to claim 8 wherein the weakly acidic catalyst is acetic acid.
10. The process for producing an amphiphilic carbon black according to claim 8, wherein the weakly basic catalyst is ammonia, triethanolamine or ethylenediamine.
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