CN108084803B - Preparation method of silane modified carbon black color paste - Google Patents
Preparation method of silane modified carbon black color paste Download PDFInfo
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- CN108084803B CN108084803B CN201711423976.XA CN201711423976A CN108084803B CN 108084803 B CN108084803 B CN 108084803B CN 201711423976 A CN201711423976 A CN 201711423976A CN 108084803 B CN108084803 B CN 108084803B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/005—Carbon black
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to a preparation method of silane modified carbon black color paste, belonging to the field of fine chemical engineering. The carbon black color paste is prepared by adopting nonpolar short-chain-length alkyl silane, polar epoxy group or amino silane to react with polar hydroxyl on the surface of the carbon black to obtain the carbon black, and grinding the carbon black. The carbon black color paste produced by the method has good dispersibility and base material adhesion, simple product preparation equipment and mild reaction conditions, and is suitable for industrial production.
Description
Technical Field
The invention relates to a preparation method of silane modified carbon black color paste, belonging to the field of fine chemical engineering.
Background
Carbon black is an amorphous carbon, light, loose and extremely fine black powder, has a very large surface area, and is a product of incomplete combustion or thermal decomposition of carbonaceous materials (e.g., coal, natural gas, heavy oil, fuel oil, etc.) under conditions of insufficient air. The main component of carbon black is carbon, and contains trace amounts of hydrogen, oxygen, sulfur, ash, tar and water. They are classified into carbon black for rubber, coloring carbon black and carbon black for conductivity according to their uses. The silane coupling agent is an industrial additive with wide application, and is a compound with a molecular structure of Y-Si-Xn, wherein Y in the molecule of the silane coupling agent is an organic end group (such as alkyl, amido, vinyl and the like), X is an inorganic end group (such as alkoxy, acyloxy, halogen and the like), and in the using process, X and Y can be respectively combined with inorganic matters and organic matters, so that the surface performance of the material is changed, and the effect of improving the surface modification of the material is achieved.
Carbon black has a strong absorption capacity for various visible wavelengths of light and is expressed as a pure black color, so that it has been developed as a black pigment, and carbon black having such a purpose is called pigment carbon black. Colored carbon blacks are mainly used as colorants for inks, coatings, plastics and rubbers. Compared with rubber carbon black, pigment carbon black has more and more special requirements on quality indexes such as blackness, adhesive force, surface activity, dispersibility, fluidity and the like.
The carbon black is an aggregate with a specific structure formed by aggregating a plurality of carbon black primary particles close to the nanometer level, and the aggregate has rich specific surface and more strong polar groups such as active hydroxyl groups, carboxyl groups and the like. However, in the coating industry, if carbon black is directly used as a pigment, the carbon black particles are easy to self-gather in the preparation and use processes due to the relatively high polarity of the surface of the carbon black, so that the dispersion effect of the carbon black in the coating is insufficient, and the coloring is not uniform. Meanwhile, the carbon black has strong surface and strong polarity, so that the carbon black has poor surface compatibility and insufficient adhesive force to base materials (such as resin, plastic, rubber, wood and the like).
Therefore, researches on how to improve the surface chemical properties of the carbon black structure to obtain carbon black with better compatibility, stronger adhesion and better dispersion performance are continuously carried out on the market.
Disclosure of Invention
The invention aims to: the preparation method of the silane modified carbon black color paste with good compatibility, strong adhesive force and good dispersion performance is provided.
The technical scheme of the invention is as follows:
a preparation method of silane modified carbon black color paste; the method is characterized in that:
the carbon black color paste is a powdery black pigment prepared by carrying out surface treatment on gas carbon black or acetylene carbon black by using a silane coupling agent and then dispersing and grinding; the molecular formula of the silane coupling agent is as follows:
R1-Si(OR2)3
wherein: r1Is any one of alkane with a carbon chain length of 1-8, aminopropyl and glycidol ether oxypropyl;
OR2is methoxy or ethoxy;
the preparation method of the carbon black color paste comprises the following steps:
1) and mixing the silane coupling agent with methanol or ethanol (solvent) according to the ratio of 1: 2-3 to obtain a colorless transparent silanol solution,
2) adding the silanol solution into a metering tank, and putting a certain mass of carbon black into a conical double-spiral mixer with a vacuum and heating device at normal temperature; starting a mixer, controlling the stirring speed at 15-20 revolutions per minute, and controlling the mass ratio of the silanol solution to the carbon black to be 1: 0.8-1.0;
3) slowly adding the silanol solution into a mixer in a spraying mode, stirring and mixing, wherein the feeding time is controlled to be 2.5-3.0 h, and the temperature of a mixing kettle is controlled to be 20-50 ℃; continuously mixing for 0.5-0.6 h after the feeding is finished to obtain a solid mixture of carbon black and silane;
4) pumping the vacuum degree of the mixture to-0.08 to-0.09 MPa under the stirring state, slowly heating to 70-80 ℃ under the vacuum state to react silane with hydroxyl on the surface of carbon black, controlling the heating time to be 3-4 hours, and maintaining the vacuum degree to perform mixing and stirring reaction for 6-8 hours; simultaneously, the low-boiling-point alcohol and the solvent generated by the reaction are recovered by condensation to obtain dry powdery solid;
5) and finally, grinding the solid at a high speed through a three-roll roller mill to obtain the carbon black color paste with the particle size of 0.10-1.25 mu m.
The invention has the beneficial effects that:
1. the invention processes the surface polar group of the carbon black through chemical reaction, reduces the surface polarity of the carbon black, thereby preventing the self-polymerization of the carbon black and improving the dispersion effect of the carbon black.
2. According to the invention, the nonpolar or polar active group is introduced on the surface of the carbon black, so that the compatibility of the carbon black color paste and the base material is ensured, and the adhesive force of the carbon black to the base material is improved.
3. The method has the advantages of simple process, low equipment requirement and mild reaction condition, and is suitable for large-scale industrial production.
Detailed Description
Example 1:
uniformly mixing 100kg of propyl trimethoxy silane and 200kg of methanol to obtain a methanol solution of propyl trimethoxy silane, adding the methanol solution into a metering tank, and putting 300kg of carbon black into a 1000L conical double-spiral mixer at normal temperature; starting a mixer, controlling the stirring speed at 15-20 rpm, slowly adding the methanol solution in the metering tank into the mixer in a spraying mode, stirring and mixing, controlling the feeding time of the methanol solution at 3h, and controlling the temperature of a mixing kettle to be not more than 50 ℃; and continuously mixing for 0.5-0.6 h after the feeding is finished to obtain a solid mixture of the carbon black and the silane.
Pumping the vacuum degree of the solid mixture to-0.08 to-0.09 MPa under the stirring state, slowly heating to 70-75 ℃ for reaction, controlling the heating time to be 3-4 hours, maintaining the vacuum degree, mixing, stirring and reacting for 7-8 hours, recovering methanol through condensation to obtain dry powdery solid, and grinding the powdery solid at high speed by using a three-roll mill to obtain the carbon black color paste with the particle size of 0.10-1.25 mu m.
Example 2
Uniformly mixing 100kg of octyl triethoxysilane and 200kg of ethanol to obtain an ethanol solution of octyl triethoxysilane, adding the ethanol solution into a metering tank, and putting 250kg of carbon black into a 1000L conical double-spiral mixer at normal temperature; starting a mixer, controlling the stirring speed at 15-20 rpm, slowly adding the ethanol solution in the metering tank into the mixer in a spraying mode, stirring and mixing, controlling the feeding time at 3h, and controlling the temperature of a mixing kettle at 20-50 ℃; and continuously mixing for 0.5-0.6 h after the feeding is finished to obtain a solid mixture of the carbon black and the silane.
Pumping the vacuum degree of the solid mixture to-0.08 to-0.09 MPa under the stirring state, slowly heating to 75-80 ℃ for reaction, controlling the heating time to be 3-4 hours, maintaining the vacuum degree, mixing, stirring and reacting for 6-8 hours, recovering ethanol through condensation to obtain dry powdery solid, and grinding the powdery solid at high speed by using a three-roll mill to obtain the carbon black color paste with the particle size of 0.10-1.25 mu m.
Example 3
Mixing 100kg of 3-aminopropyltriethoxysilane with 300kg of ethanol to obtain an ethanol solution of 3-aminopropyltriethoxysilane, adding the ethanol solution into a metering tank, and putting 300kg of carbon black into a 1000L conical double-spiral mixer at normal temperature; starting a mixer, controlling the stirring speed at 15-20 rpm, slowly adding the ethanol solution in the metering tank into the mixer in a spraying mode, stirring and mixing, controlling the feeding time at 4h, and controlling the temperature of a mixing kettle at 20-50 ℃; and after the feeding is finished, continuously mixing for 0.6h to obtain a solid mixture of the carbon black and the amino silane.
Pumping the vacuum degree of the solid mixture to-0.08 to-0.09 MPa under the stirring state, slowly heating to 75-80 ℃ for reaction, controlling the heating time to be 3-4 hours, maintaining the vacuum degree, mixing, stirring and reacting for 6-7 hours, recovering ethanol through condensation to obtain dry powdery solid, and grinding the powdery solid at high speed by using a three-roll mill to obtain the carbon black color paste with the particle size of 0.10-1.25 mu m.
Claims (1)
1. A preparation method of silane modified carbon black color paste; the method is characterized in that:
the carbon black color paste is a powdery black pigment prepared by carrying out surface treatment on gas carbon black or acetylene carbon black by using a silane coupling agent and then dispersing and grinding; the molecular formula of the silane coupling agent is as follows:
R1-Si(OR2)3
wherein: r1Is any one of alkane with a carbon chain length of 1-8, aminopropyl and glycidol ether oxypropyl;
OR2is methoxy or ethoxy;
the preparation method of the carbon black color paste comprises the following steps:
1) and mixing the silane coupling agent and methanol or ethanol according to the ratio of 1: 2-3 to obtain a colorless transparent silanol solution,
2) adding the silanol solution into a metering tank, and putting a certain mass of carbon black into a conical double-spiral mixer with a vacuum and heating device at normal temperature; starting a mixer, controlling the stirring speed at 15-20 revolutions per minute, and controlling the mass ratio of the silanol solution to the carbon black to be 1: 0.8-1.0;
3) slowly adding the silanol solution into a mixer in a spraying mode, stirring and mixing, wherein the feeding time is controlled to be 2.5-3.0 h, and the temperature of a mixing kettle is controlled to be 20-50 ℃; continuously mixing for 0.5-0.6 h after the feeding is finished to obtain a solid mixture of carbon black and silane;
4) pumping the vacuum degree of the mixture to-0.08 to-0.09 MPa under the stirring state, slowly heating to 70-80 ℃ under the vacuum state to react silane with hydroxyl on the surface of carbon black, controlling the heating time to be 3-4 hours, and maintaining the vacuum degree to perform mixing and stirring reaction for 6-8 hours; simultaneously, the low-boiling-point alcohol and the solvent generated by the reaction are recovered by condensation to obtain dry powdery solid;
5) and grinding the powdery solid at a high speed by using a three-roll mill to obtain the carbon black color paste with the particle size of 0.10-1.25 mu m.
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| CN201711423976.XA CN108084803B (en) | 2017-12-25 | 2017-12-25 | Preparation method of silane modified carbon black color paste |
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| CN108084803B true CN108084803B (en) | 2020-11-06 |
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| CN110483861B (en) | 2019-09-26 | 2021-05-25 | 科诺思膜技术(厦门)有限公司 | Nitrile rubber, preparation method thereof and sealing ring |
| CN110982326A (en) * | 2019-12-02 | 2020-04-10 | 武汉疏能新材料有限公司 | Energy-absorbing super-amphiphobic anti-icing coating and preparation method thereof |
| CN112778820A (en) * | 2021-01-27 | 2021-05-11 | 卢建平 | High-filling-amount carbon black printing ink |
| CN113789081B (en) * | 2021-11-03 | 2023-08-01 | 理光感热技术（无锡）有限公司 | Washing-resistant ink |
| CN114316635A (en) * | 2021-12-30 | 2022-04-12 | 宁波德泰化学有限公司 | Amphiphilic carbon black and preparation method thereof |
| CN114686023A (en) * | 2022-05-07 | 2022-07-01 | 山东耐斯特炭黑有限公司 | Production method of high-pigment carbon black for plastic master batch color paste |
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| CN102532975B (en) * | 2011-12-27 | 2014-06-18 | 深圳市乐普泰科技股份有限公司 | Nano aqueous conductive carbon black color paste and preparation method thereof |
| CN107189120A (en) * | 2017-05-19 | 2017-09-22 | 浙江帝恒实业有限公司 | A kind of rubber composite of cracking growth resistance |
| CN107460557A (en) * | 2017-09-22 | 2017-12-12 | 宜宾屏山辉瑞油脂有限公司 | A kind of fibrous raw material coloring agent and preparation method thereof |
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Address after: Luochang Town, Shashi District, Jingzhou City, Hubei Province Patentee after: Hubei Jianghan New Material Co.,Ltd. Address before: Luochang Town, Shashi District, Jingzhou City, Hubei Province Patentee before: JINGZHOU JIANGHAN FINE CHEMICAL Co.,Ltd. |
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