Preparation method of high-activity nano-catalyst material

Abstract

The invention belongs to the technical field of nano-catalysts, and particularly relates to a preparation method of a high-activity nano-catalyst material, which comprises the following specific steps: weighing raw materials according to the weight of each component, and mixing the raw materials in a reaction kettle to obtain a platinum mixed solution; placing the platinum mixed solution in an ultrasonic dispersion machine, and adding the titanium nitride mesoporous carrier, so that the platinum mixed solution can be uniformly diffused in pores of the titanium nitride mesoporous carrier by utilizing ultrasonic oscillation to obtain a platinum impregnated load; and placing the platinum impregnated load in a vacuum roller press for rolling. According to the preparation method, a layer of anti-corrosion protective film is formed on the surface of the platinum nanowire catalyst, so that the problem that an existing high-activity nano catalyst material is corroded can be solved, and the influence on the use performance of the high-activity nano catalyst material can be avoided to a certain extent.

Description

Technical Field

[0001] The invention relates to the technical field of nano catalysts, and in particular to a method for preparing a high-activity nano catalyst material. Background Art

[0002] Highly active nanocatalyst materials refer to catalyst materials with high specific surface area, high activity and high selectivity, and their particle size is usually between 1-100 nanometers. These materials show excellent catalytic performance in chemical reactions and are widely used in many fields.

[0003] However, the existing high-activity nanocatalyst materials may come into contact with various chemical substances during the application process, and the chemical substances may corrode the high-activity nanocatalyst materials, thereby affecting the performance of the high-activity nanocatalyst materials. Therefore, a method for preparing a high-activity nanocatalyst material is invented. Summary of the invention

[0004] To solve the above technical problems, according to one aspect of the present invention, the present invention provides the following technical solutions:

[0005] A method for preparing a highly active nanocatalyst material comprises the following specific steps:

[0006] Step 1, taking materials: weighing the raw materials according to the amount of each component, the raw materials include: platinum acetylacetonate, solvent, anhydrous phloroglucinol, hexadecyltrimethylammonium chloride, titanium nitride mesoporous carrier, temperature resistant agent, volatile solvent;

[0007] Step 2, stirring: placing platinum acetylacetonate, a solvent, anhydrous phloroglucinol, hexadecyltrimethylammonium chloride, a temperature-resistant agent and a volatile solvent in a reaction kettle and mixing them to obtain a platinum mixed solution;

[0008] Step 3, dispersion: placing the platinum mixed solution in an ultrasonic disperser and adding the titanium nitride mesoporous carrier, so that the platinum mixed solution can be evenly diffused in the pores of the titanium nitride mesoporous carrier by ultrasonic oscillation to obtain platinum impregnation loading;

[0009] Step 4, rolling: placing the platinum impregnation load in a vacuum roller press for rolling, during which a vacuum operation is performed to remove excess gas in the platinum impregnation load and the platinum residual solution, until the platinum residual solution is completely filled in the pores of the platinum impregnation load, thereby obtaining a platinum roller-pressed load;

[0010] Step 5, drying: drying the platinum support to obtain a platinum nanowire catalyst, and during this process, a plurality of pores are formed in the platinum nanowire catalyst due to the volatilization of the volatile solvent;

[0011] Step 6, soaking: soaking the platinum nanowire catalyst in an anti-corrosion solution to form a protective layer on the outer surface of the platinum nanowire catalyst;

[0012] Step seven, centrifugal drying: centrifugal drying the immersed platinum nanowire catalyst to form a protective film on the surface of the platinum nanowire catalyst.

[0013] As a preferred embodiment of the method for preparing a highly active nanocatalyst material described in the present invention, the raw materials in step 1 include, by weight: 4-12 parts of platinum acetylacetonate, 2-4 parts of solvent, 3-6 parts of anhydrous phloroglucinol, 2-6 parts of hexadecyltrimethylammonium chloride, 4-8 parts of titanium nitride mesoporous carrier, 2-8 parts of temperature-resistant agent, and 4-6 parts of volatile solvent.

[0014] As a preferred embodiment of the method for preparing a highly active nanocatalyst material according to the present invention, the solvent is a mixture of one or more of oleamide and 1-octadecene.

[0015] As a preferred embodiment of the method for preparing a highly active nanocatalyst material according to the present invention, the temperature-resistant agent is a mixture of one or more of copper aluminum oxide, zirconium oxide, vanadium titanium, tungsten titanium, platinum and palladium.

[0016] As a preferred embodiment of the method for preparing a highly active nanocatalyst material according to the present invention, the volatile solvent is a mixture of one or more of methanol, ethanol, acetone, ethyl acetate, benzene and toluene.

[0017] As a preferred embodiment of the method for preparing a highly active nanocatalyst material according to the present invention, the stirring speed in step 2 is 60 to 100 r / min, and the stirring time is 6 to 12 min.

[0018] As a preferred embodiment of the method for preparing a highly active nanocatalyst material according to the present invention, the working frequency of the ultrasonic disperser in step 3 is 7 to 12 kHz, and the dispersion time is 4 to 6 minutes.

[0019] As a preferred embodiment of the method for preparing a highly active nanocatalyst material according to the present invention, the vacuum pressure of the vacuum roller press in step 4 is 0.004-0.008 Pa, and the roller pressing pressure is 2-3 MPa.

[0020] As a preferred embodiment of the method for preparing a highly active nanocatalyst material according to the present invention, the raw materials of the anti-corrosion solution include, by weight, 10-16 parts of phenolic fluororesin, 10-16 parts of unsaturated polyester resin, 10-16 parts of epoxy resin, and 2-6 parts of adhesive.

[0021] As a preferred embodiment of the method for preparing a highly active nanocatalyst material according to the present invention, the preparation process of the anti-corrosion solution is as follows:

[0022] Process 1: mixing phenol fluorine resin, unsaturated polyester resin and epoxy resin to obtain mixture A;

[0023] Process 2: Mixing and heating the mixture A and the adhesive to obtain an antiseptic solution.

[0024] Compared with existing technologies:

[0025] By forming an anti-corrosion protective film on the surface of the platinum nanowire catalyst, the problem of corrosion of existing high-activity nanocatalyst materials can be solved, thereby avoiding the impact on the performance of the high-activity nanocatalyst materials to a certain extent; in addition, by adding a temperature-resistant agent to the raw material, the platinum nanowire catalyst can still maintain catalytic activity in a high or low temperature environment; in addition, by using a volatile solvent to form a plurality of holes in the high-activity nanocatalyst material, its specific surface area can be increased, thereby providing more active sites, allowing the catalyst to contact the reactants more effectively, improving the catalytic efficiency, and promoting the diffusion and transmission of the reactants, so that the catalyst can process a large amount of reactants more quickly during the catalytic process, further improving the catalytic performance. DETAILED DESCRIPTION

[0026] In order to make the objectives, technical solutions and advantages of the present invention more clear, the embodiments of the present invention will be described in further detail below.

[0027] Embodiment 1:

[0028] The present invention provides a method for preparing a highly active nanocatalyst material, comprising the following specific steps:

[0029] Step 1, taking materials: weighing the raw materials according to the amount of each component, the raw materials include: platinum acetylacetonate, solvent, anhydrous phloroglucinol, hexadecyltrimethylammonium chloride, titanium nitride mesoporous carrier, temperature resistant agent, volatile solvent;

[0030] The raw materials include, by weight: 4 parts of platinum acetylacetonate, 2 parts of solvent, 3 parts of anhydrous phloroglucinol, 2 parts of hexadecyltrimethylammonium chloride, 4 parts of titanium nitride mesoporous carrier, 2 parts of temperature resistant agent, and 4 parts of volatile solvent;

[0031] The solvent is a mixture of one or more of oleic acid amide and 1-octadecene; the temperature-resistant agent is a mixture of one or more of copper aluminum oxide, zirconium oxide, vanadium titanium, tungsten titanium, platinum, and palladium; the volatile solvent is a mixture of one or more of methanol, ethanol, acetone, ethyl acetate, benzene, and toluene;

[0032] Step 2, stirring: placing platinum acetylacetonate, solvent, anhydrous phloroglucinol, hexadecyltrimethylammonium chloride, a temperature-resistant agent and a volatile solvent in a reaction kettle for mixing to obtain a platinum mixed solution; wherein the stirring speed is 60 r / min and the stirring time is 6 min;

[0033] Step 3, dispersion: placing the platinum mixed solution in an ultrasonic disperser, and adding a titanium nitride mesoporous carrier, so that the platinum mixed solution can be evenly diffused in the pores of the titanium nitride mesoporous carrier by ultrasonic oscillation to obtain a platinum impregnation load; wherein the operating frequency of the ultrasonic disperser is 7 kHz, and the dispersion time is 4 minutes;

[0034] Step 4, rolling: placing the platinum impregnation load in a vacuum roller press for rolling, during which a vacuum operation is performed to remove excess gas in the platinum impregnation load and the platinum residual solution, until the platinum residual solution is completely filled in the pores of the platinum impregnation load to obtain a platinum roller-pressed load; wherein the vacuum pressure of the vacuum roller press is 0.004 Pa, and the rolling pressure is 2 MPa;

[0035] Step 5, drying: drying the platinum support to obtain a platinum nanowire catalyst, and during this process, a plurality of pores are formed in the platinum nanowire catalyst due to the volatilization of the volatile solvent;

[0036] Step 6, soaking: soaking the platinum nanowire catalyst in an anti-corrosion solution to form a protective layer on the outer surface of the platinum nanowire catalyst;

[0037] The raw materials of the antiseptic solution include, by weight: 10 parts of phenol fluorine resin, 10 parts of unsaturated polyester resin, 10 parts of epoxy resin, and 2 parts of adhesive;

[0038] The preparation process of the antiseptic solution is as follows:

[0039] Process 1: mixing phenol fluorine resin, unsaturated polyester resin and epoxy resin to obtain mixture A;

[0040] Process 2: Mixing and heating the mixture A and the binder to obtain an antiseptic solution;

[0041] Step seven, centrifugal drying: centrifugal drying the immersed platinum nanowire catalyst to form a protective film on the surface of the platinum nanowire catalyst.

[0042] Embodiment 2:

[0043] The present invention provides a method for preparing a highly active nanocatalyst material, comprising the following specific steps:

[0044] Step 1, taking materials: weighing the raw materials according to the amount of each component, the raw materials include: platinum acetylacetonate, solvent, anhydrous phloroglucinol, hexadecyltrimethylammonium chloride, titanium nitride mesoporous carrier, temperature resistant agent, volatile solvent;

[0045] The raw materials include, by weight: 8 parts of platinum acetylacetonate, 3 parts of solvent, 4.5 parts of anhydrous phloroglucinol, 4 parts of hexadecyltrimethylammonium chloride, 6 parts of titanium nitride mesoporous carrier, 5 parts of temperature resistant agent, and 5 parts of volatile solvent;

[0046] The solvent is a mixture of one or more of oleic acid amide and 1-octadecene; the temperature-resistant agent is a mixture of one or more of copper aluminum oxide, zirconium oxide, vanadium titanium, tungsten titanium, platinum, and palladium; the volatile solvent is a mixture of one or more of methanol, ethanol, acetone, ethyl acetate, benzene, and toluene;

[0047] Step 2, stirring: placing platinum acetylacetonate, a solvent, anhydrous phloroglucinol, hexadecyltrimethylammonium chloride, a temperature-resistant agent and a volatile solvent in a reaction kettle for mixing to obtain a platinum mixed solution; wherein the stirring speed is 80 r / min and the stirring time is 9 min;

[0048] Step 3, dispersion: placing the platinum mixed solution in an ultrasonic disperser, and adding the titanium nitride mesoporous carrier, so that the platinum mixed solution can be evenly diffused in the pores of the titanium nitride mesoporous carrier by ultrasonic oscillation to obtain a platinum impregnation load; wherein the operating frequency of the ultrasonic disperser is 9.5 kHz, and the dispersion time is 5 minutes;

[0049] Step 4, rolling: placing the platinum impregnation load in a vacuum roller press for rolling, during which a vacuum operation is performed to remove excess gas in the platinum impregnation load and the platinum residual solution, until the platinum residual solution is completely filled in the pores of the platinum impregnation load, to obtain a platinum roller-pressed load; wherein the vacuum pressure of the vacuum roller press is 0.006 Pa, and the rolling pressure is 2.5 MPa;

[0050] Step 5, drying: drying the platinum support to obtain a platinum nanowire catalyst, and during this process, a plurality of pores are formed in the platinum nanowire catalyst due to the volatilization of the volatile solvent;

[0051] Step 6, soaking: soaking the platinum nanowire catalyst in an anti-corrosion solution to form a protective layer on the outer surface of the platinum nanowire catalyst;

[0052] The raw materials of the antiseptic solution include, by weight: 13 parts of phenol fluorine resin, 13 parts of unsaturated polyester resin, 13 parts of epoxy resin, and 4 parts of adhesive;

[0053] The preparation process of the antiseptic solution is as follows:

[0054] Process 1: mixing phenol fluorine resin, unsaturated polyester resin and epoxy resin to obtain mixture A;

[0055] Process 2: Mixing and heating the mixture A and the binder to obtain an antiseptic solution;

[0056] Step seven, centrifugal drying: centrifugal drying the immersed platinum nanowire catalyst to form a protective film on the surface of the platinum nanowire catalyst.

[0057] Embodiment 3:

[0058] The present invention provides a method for preparing a highly active nanocatalyst material, comprising the following specific steps:

[0059] Step 1, taking materials: weighing the raw materials according to the amount of each component, the raw materials include: platinum acetylacetonate, solvent, anhydrous phloroglucinol, hexadecyltrimethylammonium chloride, titanium nitride mesoporous carrier, temperature resistant agent, volatile solvent;

[0060] The raw materials include, by weight: 12 parts of platinum acetylacetonate, 4 parts of solvent, 6 parts of anhydrous phloroglucinol, 6 parts of hexadecyltrimethylammonium chloride, 8 parts of titanium nitride mesoporous carrier, 8 parts of temperature resistant agent, and 6 parts of volatile solvent;

[0061] The solvent is a mixture of one or more of oleic acid amide and 1-octadecene; the temperature-resistant agent is a mixture of one or more of copper aluminum oxide, zirconium oxide, vanadium titanium, tungsten titanium, platinum, and palladium; the volatile solvent is a mixture of one or more of methanol, ethanol, acetone, ethyl acetate, benzene, and toluene;

[0062] Step 2, stirring: placing platinum acetylacetonate, solvent, anhydrous phloroglucinol, hexadecyltrimethylammonium chloride, a temperature-resistant agent and a volatile solvent in a reaction kettle for mixing to obtain a platinum mixed solution; wherein the stirring speed is 100 r / min and the stirring time is 12 min;

[0063] Step 3, dispersion: placing the platinum mixed solution in an ultrasonic disperser, and adding a titanium nitride mesoporous carrier, so that the platinum mixed solution can be evenly diffused in the pores of the titanium nitride mesoporous carrier by ultrasonic oscillation to obtain a platinum impregnation load; wherein the operating frequency of the ultrasonic disperser is 12 kHz, and the dispersion time is 6 minutes;

[0064] Step 4, rolling: placing the platinum impregnation load in a vacuum roller press for rolling, during which a vacuum operation is performed to remove excess gas in the platinum impregnation load and the platinum residual solution, until the platinum residual solution is completely filled in the pores of the platinum impregnation load, to obtain a platinum roller-pressed load; wherein the vacuum pressure of the vacuum roller press is 0.008 Pa, and the rolling pressure is 3 MPa;

[0065] Step 5, drying: drying the platinum support to obtain a platinum nanowire catalyst, and during this process, a plurality of pores are formed in the platinum nanowire catalyst due to the volatilization of the volatile solvent;

[0066] Step 6, soaking: soaking the platinum nanowire catalyst in an anti-corrosion solution to form a protective layer on the outer surface of the platinum nanowire catalyst;

[0067] The raw materials of the antiseptic solution include, by weight: 16 parts of phenol fluorine resin, 16 parts of unsaturated polyester resin, 16 parts of epoxy resin, and 6 parts of adhesive;

[0068] The preparation process of the antiseptic solution is as follows:

[0069] Process 1: mixing phenol fluorine resin, unsaturated polyester resin and epoxy resin to obtain mixture A;

[0070] Process 2: Mixing and heating the mixture A and the binder to obtain an antiseptic solution;

[0071] Step seven, centrifugal drying: centrifugal drying the immersed platinum nanowire catalyst to form a protective film on the surface of the platinum nanowire catalyst.

[0072] The highly active nanocatalyst materials prepared in the above Examples 1-3 were compared to obtain the following data:

[0073] Example 1 Example 2 Example 3 Corrosion resistance grade Sa2 Sa2.5 Sa2 High and low temperature resistance -280℃-1000℃ -280℃-1000℃ -280℃-1000℃

[0074] It can be seen from the above table that the high-activity nanocatalyst materials prepared in Examples 1-3 have good performance in terms of corrosion resistance and high and low temperature resistance. After use, Example 2 has the best effect.

[0075] Although the present invention has been described above with reference to the embodiments, various modifications may be made thereto and parts thereof may be replaced by equivalents without departing from the scope of the present invention. In particular, as long as there is no structural conflict, the various features in the embodiments disclosed in the present invention may be used in combination with each other in any manner, and the fact that these combinations are not exhaustively described in this specification is only for the sake of omitting space and saving resources. Therefore, the present invention is not limited to the specific embodiments disclosed herein, but includes all technical solutions falling within the scope of the claims.

Claims

1. A method for preparing a highly active nanocatalyst material, characterized in that: The specific steps are as follows: Step 1, taking materials: weighing the raw materials according to the amount of each component, the raw materials include: platinum acetylacetonate, solvent, anhydrous phloroglucinol, hexadecyltrimethylammonium chloride, titanium nitride mesoporous carrier, temperature resistant agent, volatile solvent; Step 2, stirring: placing platinum acetylacetonate, a solvent, anhydrous phloroglucinol, hexadecyltrimethylammonium chloride, a temperature-resistant agent and a volatile solvent in a reaction kettle and mixing them to obtain a platinum mixed solution; Step 3, dispersion: placing the platinum mixed solution in an ultrasonic disperser and adding the titanium nitride mesoporous carrier, so that the platinum mixed solution can be evenly diffused in the pores of the titanium nitride mesoporous carrier by ultrasonic oscillation to obtain platinum impregnation loading; Step 4, rolling: placing the platinum impregnation load in a vacuum roller press for rolling, during which a vacuum operation is performed to remove excess gas in the platinum impregnation load and the platinum residual solution, until the platinum residual solution is completely filled in the pores of the platinum impregnation load, thereby obtaining a platinum roller-pressed load; Step 5, drying: drying the platinum support to obtain a platinum nanowire catalyst, and during this process, a plurality of pores are formed in the platinum nanowire catalyst due to the volatilization of the volatile solvent; Step 6, soaking: soaking the platinum nanowire catalyst in an anti-corrosion solution to form a protective layer on the outer surface of the platinum nanowire catalyst; Step seven, centrifugal drying: centrifugal drying the immersed platinum nanowire catalyst to form a protective film on the surface of the platinum nanowire catalyst.

2. The method for preparing a highly active nanocatalyst material according to claim 1, characterized in that: The raw materials in step 1 include, by weight: 4-12 parts of platinum acetylacetonate, 2-4 parts of solvent, 3-6 parts of anhydrous phloroglucinol, 2-6 parts of hexadecyltrimethylammonium chloride, 4-8 parts of titanium nitride mesoporous carrier, 2-8 parts of temperature-resistant agent, and 4-6 parts of volatile solvent.

3. The method for preparing a highly active nanocatalyst material according to claim 2, characterized in that: The solvent is a mixture of one or more of oleic acid amide and 1-octadecene.

4. The method for preparing a highly active nanocatalyst material according to claim 2, characterized in that: The temperature resistant agent is a mixture of one or more of copper aluminum oxide, zirconium oxide, vanadium titanium, tungsten titanium, platinum and palladium.

5. The method for preparing a highly active nanocatalyst material according to claim 2, characterized in that: The volatile solvent is a mixture of one or more of methanol, ethanol, acetone, ethyl acetate, benzene and toluene.

6. The method for preparing a highly active nanocatalyst material according to claim 1, characterized in that: In the step 2, the stirring speed is 60-100 r / min, and the stirring time is 6-12 min.

7. The method for preparing a highly active nanocatalyst material according to claim 1, characterized in that: The working frequency of the ultrasonic disperser in step 3 is 7 to 12 kHz, and the dispersion time is 4 to 6 minutes.

8. The method for preparing a highly active nanocatalyst material according to claim 1, characterized in that: In the step 4, the vacuum pressure of the vacuum roller press is 0.004-0.008 Pa, and the roller pressing pressure is 2-3 MPa.

9. The method for preparing a highly active nanocatalyst material according to claim 1, characterized in that: The raw materials of the anticorrosive solution include, by weight: 10-16 parts of phenol fluorine resin, 10-16 parts of unsaturated polyester resin, 10-16 parts of epoxy resin, and 2-6 parts of adhesive.

10. The method for preparing a highly active nanocatalyst material according to claim 9, characterized in that: The preparation process of the antiseptic solution is as follows: Process 1: mixing phenol fluorine resin, unsaturated polyester resin and epoxy resin to obtain mixture A; Process 2: Mixing and heating the mixture A and the adhesive to obtain an antiseptic solution.