CN108296137B - Super-amphiphobic coating material for catalyst and preparation method and application thereof - Google Patents
Super-amphiphobic coating material for catalyst and preparation method and application thereof Download PDFInfo
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- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0406—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases the gas being air
- B05D3/0426—Cooling with air
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/10—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by other chemical means
- B05D3/107—Post-treatment of applied coatings
- B05D3/108—Curing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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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
- C09D125/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
- C09D125/02—Homopolymers or copolymers of hydrocarbons
- C09D125/04—Homopolymers or copolymers of styrene
- C09D125/06—Polystyrene
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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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/16—Homopolymers or copolymers of vinylidene fluoride
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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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/18—Homopolymers or copolymers of tetrafluoroethene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2401/00—Form of the coating product, e.g. solution, water dispersion, powders or the like
- B05D2401/30—Form of the coating product, e.g. solution, water dispersion, powders or the like the coating being applied in other forms than involving eliminable solvent, diluent or dispersant
- B05D2401/32—Form of the coating product, e.g. solution, water dispersion, powders or the like the coating being applied in other forms than involving eliminable solvent, diluent or dispersant applied as powders
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention relates to the technical field of preparation of super-amphiphobic materials, and particularly provides a super-amphiphobic coating for a catalyst, and a preparation method and application thereof. The invention also provides a preparation method of the super-amphiphobic coating, and all the nano particles are in a good dispersion state when being sprayed on the coating body by spraying the low-concentration particles for multiple times. Through heating to the glutinous fluidization temperature of coating body to the nanoparticle for it is "inlaying" promptly when contacting the coating body, on being fixed in the coating body, then through cooling off earlier and heat and ultrasonic treatment to the coating is whole again, makes the nanoparticle get into the coating body under the relative position that keeps dispersed state, thereby has avoided the condition that the nanoparticle reunites to appear.
Description
Technical Field
The invention belongs to the technical field of super-amphiphobic materials, and particularly relates to a super-amphiphobic coating material for a catalyst, and a preparation method and application thereof.
Background
Super-amphiphobic (also called as omniphobic) materials have the advantages of antifouling, antifogging, low adhesiveness, self-cleaning and the like, so that a great deal of demand exists in numerous fields of daily life and industrial production. However, the super-amphiphobic material is still in the research and development stage at present, the actual industrial product is rare, and even the coating product which is claimed to be capable of being subjected to 'omniphobic' on the market at present is difficult to popularize due to the problems of unstable super-amphiphobic performance and short service life. In view of this, more and more research is being devoted to the development of super-amphiphobic materials.
If the mechanical property of the super-amphiphobic coating coated on the surface of the catalyst is insufficient or unstable, the pollution on the surface of the catalyst and the inactivation of the catalyst cannot be avoided, and the inactivation of the catalyst can be accelerated; even when the coating comes off, the reaction system is mixed, which brings about more adverse effects.
Studies have shown that two essential factors in the construction of solid surfaces with super-amphiphobic properties are low surface energy and a rough microstructure, especially a rough microstructure that plays a key role in the oleophobic properties. Inorganic fine particles such as nano silica, nano titania, and carbon nanotubes have been favored by researchers because of their microscopic size, which is suitable for constructing a surface roughness structure. However, the nanoparticles have fatal defects, namely easy agglomeration, which causes the distribution quantity of the nanoparticles in the organic amphiphobic material to be limited, and once the concentration of the nanoparticles is too high, self-agglomeration is formed and the nanoparticles cannot be uniformly distributed in the organic material; moreover, the agglomerated nanoparticles are easy to be compatible with organic materials, so that the inner part of the super-amphiphobic material is layered, and the mechanical property and the stability of the coating material are seriously influenced.
Therefore, chinese patent document CN105820605A discloses a method for preparing a super-amphiphobic nano coating based on flower-like titanium dioxide nano particles, which comprises preparing flower-like titanium dioxide nano particles, modifying the flower-like titanium dioxide nano particles with low surface energy to obtain super-amphiphobic powder, and then directly coating the super-amphiphobic powder on a solid surface needing to obtain super-amphiphobic performance by gluing. Although the technology stated that the inorganic powder can be distributed on the surface of the coating in a concentration of almost one hundred percent, in the actual use process of the coating, the flower-like nano titanium dioxide is extremely easy to be lost, and the super-amphiphobic performance of the coating can be maintained only by continuously supplementing the powder, namely, the super-amphiphobic coating prepared by the technology still has the problems of poor stability and short service life. Therefore, how to overcome the defect that the content of inorganic particles in the existing super-amphiphobic nano coating is too small or is extremely easy to lose is a problem which needs to be solved in the field.
In the field of catalysts, it is known that hydrogenation catalysts are prone to generate carbon deposits (also called coking) during operation, and when the carbon deposits cover the active centers of the catalysts, the catalysts are deactivated, and then the catalysts must be regenerated to recover the activity, which inevitably reduces the catalytic efficiency and increases the energy consumption of production. If the catalyst has a super-amphiphobic surface, the carbon deposition rate can be slowed down, and the service life of the catalyst is prolonged. However, reports about super-amphiphobic catalysts do not appear at present.
Disclosure of Invention
The invention aims to overcome the defect that the service life is too short due to too little inorganic particle content or extremely easy loss in the existing super-amphiphobic nano coating, and further provides a preparation method and application of a super-amphiphobic coating which has uniform inorganic particle distribution, high content and durable performance and can be used for the surface of a catalyst.
Therefore, the technical scheme adopted by the invention for realizing the purpose is as follows:
a preparation method of a super-amphiphobic coating material comprises the following steps:
s1, providing a substrate, coating the substrate with the coating body material, and curing to obtain a coating body;
s2, heating the inorganic nano-particles to T1Dispersing the inorganic nano particles on the surface of the coating body, heating the coating body until the temperature of the inorganic nano particles is consistent with that of the coating body, keeping the temperature for 5-10 min until the coating body reaches a viscous state, cooling and curing to obtain a coating precursor;
the volume ratio of the inorganic nano particles to the coating body is 0.02-0.05: 1;
the T is1The temperature is 0.5-2 ℃ higher than the viscosity fluidization temperature of the coating body material;
s3, repeating the operation of the step S2 for 20-100 times on the coating precursor to obtain the super-amphiphobic coating material.
The thickness of the coating body is 60-500 μm.
And mixing the coating body material and a fluorosilane coupling agent according to a mass ratio of 1: 0.1-0.15, and coating the mixture on the substrate.
The coating body is made of one or more of silica gel, polytetrafluoroethylene, polyvinylidene fluoride, fluorinated polyurethane and fluorine modified polystyrene.
The coating body is made of a mixture of polytetrafluoroethylene and polyvinylidene fluoride in a mass ratio of 1: 1; or the coating body material is fluorine modified polystyrene.
The inorganic nano particles are one or more of nano aluminum oxide, nano silicon dioxide and nano titanium dioxide.
In step S2, ultrasonic treatment is also applied while the coating body is in a viscous state.
The super-amphiphobic coating material prepared by the preparation method.
The application of the super-amphiphobic coating material in the preparation of a catalyst.
One of the applications is to wrap a layer of the super-amphiphobic coating material in a viscous flow state on the surface of the catalyst, and then cool the catalyst under ultrasonic operation to obtain the super-amphiphobic catalyst.
The technical scheme provided by the invention has the following advantages:
1. the super-amphiphobic coating provided by the invention contains uniformly distributed inorganic nanoparticles accounting for 0.5-0.83 of the volume of the coating, and the higher content of the inorganic nanoparticles enables the surface of the coating to have stronger roughness; meanwhile, the fluorosilane coupling agent contained in the coating body can reduce the surface energy of the inorganic nano particles; the prepared coating shows good super-amphiphobic performance due to the lower surface energy and the stronger roughness, the inorganic nanoparticles and the coating body are uniformly distributed, the structure is stable, the loss is not easy to occur, and the super-amphiphobic coating is coated on the surface of the catalyst, so that the inactivation and the surface pollution of the catalyst can be effectively avoided.
2. According to the preparation method of the super-amphiphobic coating, the low-concentration particle spraying is carried out for multiple times, so that the agglomeration phenomenon of inorganic nano particles in the spraying process is ensured, and all nano particles are in a good dispersion state when being sprayed onto the coating body. Through heating to the glutinous fluidization temperature of coating body to the nanoparticle for it is "inlaying" promptly when contacting the coating body, on being fixed in the coating body, then through cooling off earlier and heat and ultrasonic treatment to the coating is whole again, makes the nanoparticle get into the coating body under the relative position that keeps dispersed state, the phenomenon of reunion does not appear. Similarly, the steps are repeated for a plurality of times, so that the relative position of the nano particles can not be changed when the nano particles contact the coating body, and the nano particles only push downwards layer by layer, thereby avoiding the agglomeration of the nano particles. When the catalyst surface is coated, the operation of cooling while ultrasound is carried out enables air in catalyst pores to escape from the catalyst pores through the surface of the coating in the curing process, so that pore channels are formed on the surface, and the contact between the catalyst and reactants is facilitated.
Detailed Description
Example 1
The super-amphiphobic coating material provided by the embodiment is prepared by the following steps:
s1, coating 20g of polytetrafluoroethylene and 3g of fluorosilane coupling agent into a substrate coating with the thickness of 60 mu m in a spraying manner;
s2, heating 1g of nano silicon dioxide to 330 ℃, and then spraying the nano silicon dioxide on the surface of the polytetrafluoroethylene base layer; after cooling the polytetrafluoroethylene, integrally heating the obtained composite coating to 328 ℃, preserving the heat, simultaneously starting ultrasonic treatment for 10min, turning off the ultrasonic treatment, and cooling to room temperature;
s3, continuously repeating the step S2 on the coating obtained in the step S2 for 50 times to obtain the super-amphiphobic coating material.
Example 2
The super-amphiphobic coating material provided by the embodiment is prepared by the following steps:
s1, coating 20g of fluorine modified polystyrene and 2.5g of silane coupling agent into a substrate coating with the thickness of 100 mu m by adopting a spraying mode;
s2, heating 1g of nano titanium dioxide to 170 ℃, and then spraying the nano titanium dioxide on the surface of the fluorine modified polystyrene substrate; after the obtained coating is cooled, the whole composite coating is heated to 170 ℃, the temperature is preserved, meanwhile, the ultrasonic treatment is started for 10min, the ultrasonic treatment is stopped, and the composite coating is cooled to room temperature;
s3, continuously repeating the step S2 on the coating obtained in the step S2 for 50 times to obtain the super-amphiphobic coating material.
Example 3
The super-amphiphobic coating material provided by the embodiment is prepared by the following steps:
s1, coating 10g of polytetrafluoroethylene, 10g of polyvinylidene fluoride and 2.8g of silane coupling agent into a substrate coating with the thickness of 30 mu m in a spraying mode;
s2, heating 1g of nano-alumina to 330 ℃, and then spraying the nano-alumina on the surfaces of polytetrafluoroethylene and polyvinylidene fluoride base layers; after the obtained coating is cooled, the whole composite coating is heated to 330 ℃, the temperature is preserved, meanwhile, the ultrasonic treatment is started for 10min, the ultrasonic treatment is stopped, and the composite coating is cooled to room temperature;
s3, continuously repeating the step S2 on the coating obtained in the step S2 for 50 times to obtain the super-amphiphobic coating material.
The super-amphiphobic coatings obtained in examples 1-3 were subjected to static contact angle measurements using pure water and glycerol, respectively, and the results are shown in the following table.
TABLE 1 contact Angle test results for the super-amphiphobic coatings obtained in the examples
Examples of the experiments
A, B, C, D parts of suspension bed hydrogenation catalyst is taken, a layer of super-amphiphobic coating material obtained in examples 1, 2 and 3 is wrapped outside A, B, C parts of the catalyst respectively, the catalyst is cooled under ultrasonic operation to obtain super-amphiphobic catalysts A ', B' and C ', the super-amphiphobic catalysts A', B 'and C' and the catalyst D are used in the suspension bed hydrogenation process under the same condition, carbon deposition is measured after 3 periods of continuous operation, and the measurement results are shown in the following table:
TABLE 2 carbon deposition test results
In the table, wt% means the carbon deposit amount in the used catalyst calculated based on the mass of the clean catalyst, and it can be seen from the experimental results that the carbon deposit amount of the super-amphiphobic catalyst prepared by the invention is obviously less than that of the catalyst without the super-amphiphobic coating under the same operation condition, which shows that the super-amphiphobic coating material for the catalyst provided by the invention can effectively prolong the service life of the catalyst.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are intended to be within the scope of the invention.
Claims (9)
1. The preparation method of the super-amphiphobic coating material is characterized by comprising the following steps of:
s1, providing a substrate, coating the substrate with the coating body material and a fluorosilane coupling agent after mixing according to the mass ratio of 1: 0.1-0.15, and curing to obtain a coating body;
s2, heating the inorganic nano-particles to T1Dispersing the inorganic nano particles on the surface of the coating body, heating the coating body until the temperature of the inorganic nano particles is consistent with that of the coating body, keeping the temperature for 5-10 min until the coating body reaches a viscous state, cooling and curing to obtain a coating precursor;
the volume ratio of the inorganic nano particles to the coating body is 0.02-0.05: 1;
the T is1The temperature is 0.5-2 ℃ higher than the viscosity fluidization temperature of the coating body material;
s3, repeating the operation of the step S2 for 20-100 times on the coating precursor to obtain the super-amphiphobic coating material.
2. The method of preparing a super-amphiphobic coating material of claim 1, wherein the thickness of the coating body is 60-500 μm.
3. The preparation method of the super-amphiphobic coating material according to claim 1 or 2, wherein the coating body material is one or more of silica gel, polytetrafluoroethylene, polyvinylidene fluoride, fluorinated polyurethane and fluorine modified polystyrene.
4. The preparation method of the super-amphiphobic coating material according to claim 3, wherein the coating body material is a mixture of polytetrafluoroethylene and polyvinylidene fluoride in a mass ratio of 1: 1; or the coating body material is fluorine modified polystyrene.
5. The preparation method of the super-amphiphobic coating material according to claim 3, wherein the inorganic nanoparticles are one or more of nano-alumina, nano-silica and nano-titania.
6. The method of preparing a super-amphiphobic coating material according to any one of claim 3, wherein in step S2, an ultrasonic treatment is further applied while the coating body is in a viscous state.
7. A super-amphiphobic coating material prepared by the preparation method of any one of claims 1 to 6.
8. Use of the superamphiphobic coating material according to claim 7 in the preparation of a catalyst.
9. Use according to claim 8, characterized in that the catalyst is coated with a layer of said super-amphiphobic coating material in viscous state and then cooled under ultrasonic operation to obtain the super-amphiphobic catalyst.
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CN101910263A (en) * | 2007-05-29 | 2010-12-08 | 伊诺瓦材料有限责任公司 | Surfaces having particles and related methods |
CN103923540A (en) * | 2014-04-22 | 2014-07-16 | 吴俊� | Super-amphiphobic coating |
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