CN114316635A - Amphiphilic carbon black and preparation method thereof - Google Patents

Amphiphilic carbon black and preparation method thereof Download PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
carbon black
silane
sodium chloride
amphiphilic
hydrophobic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202111681652.2A
Other languages
Chinese (zh)
Inventor
黄锡甫
卜庆朋
纪益彪
周迎春
朱社教
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ningbo Detai Chemical Co ltd
Original Assignee
Ningbo Detai Chemical Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ningbo Detai Chemical Co ltd filed Critical Ningbo Detai Chemical Co ltd
Priority to CN202111681652.2A priority Critical patent/CN114316635A/en
Publication of CN114316635A publication Critical patent/CN114316635A/en
Pending legal-status Critical Current

Links

Images

Landscapes

  • 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

Amphiphilic carbon black and preparation method thereof
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.
Figure BDA0003445899530000111
Table 2: examples first to fifth and comparative examples first to fourth
Figure BDA0003445899530000112
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.
CN202111681652.2A 2021-12-30 2021-12-30 Amphiphilic carbon black and preparation method thereof Pending CN114316635A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111681652.2A CN114316635A (en) 2021-12-30 2021-12-30 Amphiphilic carbon black and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111681652.2A CN114316635A (en) 2021-12-30 2021-12-30 Amphiphilic carbon black and preparation method thereof

Publications (1)

Publication Number Publication Date
CN114316635A true CN114316635A (en) 2022-04-12

Family

ID=81023248

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111681652.2A Pending CN114316635A (en) 2021-12-30 2021-12-30 Amphiphilic carbon black and preparation method thereof

Country Status (1)

Country Link
CN (1) CN114316635A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116041986A (en) * 2022-12-22 2023-05-02 山西盛达威科技有限公司 Preparation method of water-soluble carbon black

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1064042A (en) * 1963-04-26 1967-04-05 Phillips Petroleum Co Partial oxidation of carbon black
WO2012158610A1 (en) * 2011-05-13 2012-11-22 William Marsh Rice University Temperature-assisted migration of amphiphilic nanoparticles through liquid interfaces
CN103642198A (en) * 2013-12-02 2014-03-19 厦门凯纳石墨烯技术有限公司 Graphene/carbon black thermoplastic resin master batch with high dispersibility and preparation method thereof
CN103897225A (en) * 2014-01-23 2014-07-02 怡维怡橡胶研究院有限公司 Rubber composition containing organic silane coupling agent and carbon black and preparation method of rubber composition
CN107416844A (en) * 2017-08-09 2017-12-01 中国石油天然气股份有限公司 Nano silicon dioxide dispersion and preparation method with parents characteristic and double grains minor structure
CN107474313A (en) * 2017-09-19 2017-12-15 荆州市江汉精细化工有限公司 A kind of rubber chemicals of modification and preparation method thereof
CN108084803A (en) * 2017-12-25 2018-05-29 荆州市江汉精细化工有限公司 A kind of preparation method of silane-modified carbon black color paste
CN108298558A (en) * 2018-01-03 2018-07-20 中国石油天然气股份有限公司 Contain parents' molecular sieve and preparation method thereof containing lipophilic group on the inside of hydrophilic radical in outside
CN111117301A (en) * 2020-01-08 2020-05-08 郑州久源化工有限公司 Preparation method and application of modified carbon black
CN111302357A (en) * 2020-02-24 2020-06-19 吉林大学 Porous amphiphilic molecular sieve containing hydrophilic groups outside pores and containing oleophilic groups inside pores, preparation method and application thereof
CN112960675A (en) * 2019-12-12 2021-06-15 臻鼎科技股份有限公司 Porous silica, method for producing same and use thereof

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1064042A (en) * 1963-04-26 1967-04-05 Phillips Petroleum Co Partial oxidation of carbon black
WO2012158610A1 (en) * 2011-05-13 2012-11-22 William Marsh Rice University Temperature-assisted migration of amphiphilic nanoparticles through liquid interfaces
CN103642198A (en) * 2013-12-02 2014-03-19 厦门凯纳石墨烯技术有限公司 Graphene/carbon black thermoplastic resin master batch with high dispersibility and preparation method thereof
CN103897225A (en) * 2014-01-23 2014-07-02 怡维怡橡胶研究院有限公司 Rubber composition containing organic silane coupling agent and carbon black and preparation method of rubber composition
CN107416844A (en) * 2017-08-09 2017-12-01 中国石油天然气股份有限公司 Nano silicon dioxide dispersion and preparation method with parents characteristic and double grains minor structure
CN107474313A (en) * 2017-09-19 2017-12-15 荆州市江汉精细化工有限公司 A kind of rubber chemicals of modification and preparation method thereof
CN108084803A (en) * 2017-12-25 2018-05-29 荆州市江汉精细化工有限公司 A kind of preparation method of silane-modified carbon black color paste
CN108298558A (en) * 2018-01-03 2018-07-20 中国石油天然气股份有限公司 Contain parents' molecular sieve and preparation method thereof containing lipophilic group on the inside of hydrophilic radical in outside
CN112960675A (en) * 2019-12-12 2021-06-15 臻鼎科技股份有限公司 Porous silica, method for producing same and use thereof
CN111117301A (en) * 2020-01-08 2020-05-08 郑州久源化工有限公司 Preparation method and application of modified carbon black
CN111302357A (en) * 2020-02-24 2020-06-19 吉林大学 Porous amphiphilic molecular sieve containing hydrophilic groups outside pores and containing oleophilic groups inside pores, preparation method and application thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
MONGKOL TIPPLOOK,ET AL.: "Facile In Situ Synthesis of Amphiphilic Carbon-Supported Pt:Innovative Catalyst Preparation for Proton Exchange Membrane Fuel Cells", 《ACS APPL. ENERGY MATER.》 *
岑兰等: "炭黑改性及其在橡胶中的应用研究进展", 《中国橡胶》 *
王芹等: "Janus颗粒表面活性剂的研究进展", 《应用化学》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116041986A (en) * 2022-12-22 2023-05-02 山西盛达威科技有限公司 Preparation method of water-soluble carbon black

Similar Documents

Publication Publication Date Title
CN102408757B (en) Solvent-based nano silicon oxide concentrated pulp and preparation method thereof
US7544418B2 (en) Polymer-encapsulated pigments and associated methods
CN110494505B (en) Coated pigments
JP6031175B2 (en) Titanium dioxide pigment, method for producing the same, and printing ink composition
CN110028862A (en) A kind of compound super hydrophobic coating of modified Nano and preparation method thereof
CN108841042B (en) Inorganic nano material and high-polymerization-degree ammonium polyphosphate compound flame retardant and preparation method thereof
CN113150634A (en) High-wear-resistance weather-resistant coating for automobiles and preparation method thereof
CN114395276A (en) Janus structure carbon black and preparation method thereof
JP6322474B2 (en) Hydrophobic silica powder, rubber molding composition containing the same, and method for producing the same
CN114316635A (en) Amphiphilic carbon black and preparation method thereof
CN111808550B (en) Wollastonite for ethylene-vinyl acetate resin hot melt adhesive and preparation method thereof
CN109401435B (en) Wear-resistant water-based ink and preparation process thereof
CN108585890A (en) a kind of ceramic dispersants
WO2007020855A1 (en) Process for producing spherical inorganic particle
CN115725209B (en) Nano composite coating and preparation method thereof
CN102850828A (en) Active nano silica composition and preparation method thereof
JP6283580B2 (en) Hydrophobic silica-based powder, rubber molding composition containing the same, and method for producing the same
CN113461338A (en) Nano glass powder for PERC back silver and preparation method thereof
CN111925670B (en) Preparation method of ultraviolet-proof polymer-coated nano aluminum oxide pigment
JP3472982B2 (en) Method for producing silica / carbon black composite particles and method for producing coating solution containing the composite particles
CN101225248A (en) Colour development material and preparation method thereof
CN113321221A (en) Method for preparing white carbon black by using iron tailings
CN110528301A (en) A kind of aqueous heat sublimation ink-jet ink preparation of the high rate of transform
CN110760239A (en) Composite nano material reinforced water-based epoxy primer and preparation method thereof
CN107083099A (en) A kind of powdery paints flowing anti-caking auxiliary agent and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20220412

RJ01 Rejection of invention patent application after publication