CN110270328B - Three-phase copper-based catalyst and preparation method and application thereof - Google Patents
Three-phase copper-based catalyst and preparation method and application thereof Download PDFInfo
- Publication number
- CN110270328B CN110270328B CN201810222432.5A CN201810222432A CN110270328B CN 110270328 B CN110270328 B CN 110270328B CN 201810222432 A CN201810222432 A CN 201810222432A CN 110270328 B CN110270328 B CN 110270328B
- Authority
- CN
- China
- Prior art keywords
- particles
- based catalyst
- phase copper
- cuo
- ball milling
- 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.)
- Active
Links
- 239000010949 copper Substances 0.000 title claims abstract description 135
- 239000003054 catalyst Substances 0.000 title claims abstract description 85
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000002245 particle Substances 0.000 claims abstract description 110
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 21
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims description 30
- 238000000498 ball milling Methods 0.000 claims description 23
- 230000015572 biosynthetic process Effects 0.000 claims description 14
- 239000000853 adhesive Substances 0.000 claims description 12
- 230000001070 adhesive effect Effects 0.000 claims description 12
- 239000010410 layer Substances 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims description 7
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 7
- 239000011230 binding agent Substances 0.000 claims description 6
- 239000011258 core-shell material Substances 0.000 claims description 6
- 239000002356 single layer Substances 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- 239000012792 core layer Substances 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- 239000012188 paraffin wax Substances 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920000193 polymethacrylate Polymers 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- 230000001788 irregular Effects 0.000 claims 2
- 238000006243 chemical reaction Methods 0.000 abstract description 23
- 230000000694 effects Effects 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000000376 reactant Substances 0.000 abstract description 3
- 239000011863 silicon-based powder Substances 0.000 abstract description 3
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 26
- 239000002994 raw material Substances 0.000 description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 4
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000007036 catalytic synthesis reaction Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000005751 Copper oxide Substances 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229940024463 silicone emollient and protective product Drugs 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0027—Powdering
- B01J37/0036—Grinding
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/16—Preparation thereof from silicon and halogenated hydrocarbons direct synthesis
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a three-phase copper-based catalyst and a preparation method and application thereof. The three-phase copper-based catalyst mainly comprises Cu2An agglomerate of O particles with CuO particles and Cu particles, wherein the CuO particles and the Cu particles surround the Cu2And setting O particles. In the three-phase copper-based catalyst, the ultrafine nano Cu particles with highest activity are exposed at the outer layer of the aggregate and are most directly mixed with reactants Si powder and CH3Cl contacts to trigger the reaction, and CuO and Cu are arranged in the inner layer of the agglomerate2The O particles are gradually converted into Cu to participate in the reaction, so that the continuity of the whole reaction process is ensured, and meanwhile, the three-phase copper catalyst has higher reaction activity, can maintain stable dimethyldichlorosilane selectivity, improves the reaction rate and the production efficiency of the dimethyldichlorosilane synthesis reaction, and reduces the cost.
Description
Technical Field
The invention relates to a catalyst for synthesizing methyl chlorosilane and a preparation method thereof, in particular to a three-phase copper-based catalyst and a preparation method and application thereof, belonging to the technical field of catalysts.
Background
The organosilicon material is a large class of macromolecular compounds which take Si-O bonds as main chains and introduce organic groups on Si atoms as side chains, and has a semi-inorganic and semi-organic structure, so the organosilicon material has a plurality of excellent performances and special functions. The organosilicon monomer is a basic raw material for preparing organosilicon materials, and the dimethyldichlorosilane obtained by the direct synthesis method accounts for more than 90 percent of the total usage of the organosilicon monomer.
In industrial production, methyl chlorosilane is synthesized from metallic silicon and gas-phase chloromethane by a direct method under the catalysis condition, and the specific catalytic reaction process comprises the following steps:
commercial silicone products are mixtures of various functionalities, available in the general formula MenHmSiCl4-(n+m)Wherein n is 0 to 4; m is 0 to 4, and n + m is 0 to 4. Wherein the dimethyl dichlorosilane Me is used2SiCl2The amount of the component (B) is maximum and accounts for about 90 percent (mass percent) of the methyl chlorosilane.
The biggest difficulty of organosilicon production is monomer synthesis, and the problems of improving synthesis efficiency and reducing cost are constant subjects in the field. The yield and dimethyl selectivity of the organosilicon monomer synthesis are affected, and besides the production device, the raw material quality and the synthesis process, the catalyst is a key factor.
The prior art and reports prove that copper element is the most effective catalyst for synthesizing methyl chlorosilane by a direct method, and Cu-Cu is taken as a mainstream catalyst system2The O-CuO (three-phase copper for short) three-phase mixed catalyst powder has the advantages of long reaction period, high yield of the dimethyldichlorosilane, good activity and the like, and the catalytic reaction effect is related to the three-phase proportion and the characteristics of the powder, such as three-phase distribution mode, morphology, granularity, specific surface area and the like.
The existing three-phase copper catalyst system is Cu or Cu2O and CuO are processed by ball millingThe catalyst is prepared by crushing and mixing (as shown in figure 1), the particle size distribution range of three phase particles is 1-50 micrometers, the three phase particles are in disordered and uniform distribution in macro and micro, the powder is flaky or granular in shape, the disordered distribution causes instability and difficulty in sustaining of the reaction process, the activity and dimethyl selectivity of the catalyst are required to be improved, and the stable synthesis reaction process of the dimethyldichlorosilane and the high production efficiency are difficult to maintain. For example, during the reaction, the Cu phase preferentially participates in the reaction, in which case Cu2O, CuO and copper oxide are not available to participate in the reaction and are separated and carried out by a cyclone system, the Cu which is preferentially reacted is placed on the outer layer of the agglomerate, and then the Cu on the inner layer of the agglomerate is placed on the outer layer of the agglomerate2The O participates in the reaction step by step, thereby ensuring the continuity and the continuity of the reaction and obtaining better catalytic effect.
Disclosure of Invention
The invention mainly aims to provide a three-phase copper-based catalyst, and a preparation method and application thereof, so as to overcome the defects of the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention discloses a three-phase copper-based catalyst, which mainly comprises Cu2An agglomerate of O particles with CuO particles and Cu particles, wherein the CuO particles and the Cu particles surround the Cu2And setting O particles.
The embodiment of the invention also provides a preparation method of the three-phase copper-based catalyst, which comprises the following steps: mixing Cu2Placing the O particles, the CuO particles and the Cu particles into vibration ball milling equipment, adding an adhesive in the vibration ball milling process, controlling the addition of the adhesive within 1wt%, and performing vibration ball milling on the mixed material for 10-30 min to obtain the three-phase copper-based catalyst.
The embodiment of the invention also provides application of the three-phase copper-based catalyst in a dimethyl dichlorosilane synthesis process.
Compared with the prior art, in the three-phase copper-based catalyst, the ultrafine nano Cu particles with the highest activity are exposed at the outer layer of the aggregate and are most directly contacted with the reactants Si powder and CH3Cl contactAnd plays a triggering role in reaction, and CuO and Cu are arranged in the inner layer of the aggregate2The O particles are gradually converted into Cu to participate in the reaction, so that the continuity of the whole reaction process is ensured, and meanwhile, the three-phase copper catalyst has higher reaction activity, can maintain stable dimethyldichlorosilane selectivity, improves the reaction rate and the production efficiency of the dimethyldichlorosilane synthesis reaction, and reduces the cost.
Drawings
FIG. 1 is a schematic diagram of the structure of a three-phase copper catalyst system of the prior art;
fig. 2 is a schematic structural diagram of a three-phase copper catalyst in an exemplary embodiment of the invention.
Detailed Description
In view of the deficiencies in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide technical solutions of the present invention. The technical solution, its implementation and principles, etc. will be further explained as follows.
The embodiment of the invention discloses a three-phase copper-based catalyst, which mainly comprises Cu2An agglomerate of O particles with CuO particles and Cu particles, wherein the CuO particles and the Cu particles surround the Cu2And setting O particles.
Further, the agglomerates have a core-shell structure, wherein Cu2The O particles are distributed in the core layer, and the CuO particles and the Cu particles are distributed in the shell layer.
Further, in the agglomerates, CuO particles surround Cu2The O particles are disposed and the Cu particles are disposed around the CuO particles.
Furthermore, the agglomerate comprises 50-85% by mass: 0% -45%: 5 to 35 percent of Cu2O particles, CuO particles, and Cu particles.
More preferably, the Cu2The particle size of the O particles is 1-50 μm.
Preferably, the particle size of the CuO particles is 0.01 to 0.5 μm.
Preferably, the particle size of the Cu particles is 0.01 to 0.5 μm.
More preferably, the Cu2O particlesThe CuO particles and the Cu particles are spherical, spheroidal or irregular-shaped particles.
More preferably, the Cu2The particle diameters of the O particles, the CuO particles and the Cu particles are different from each other.
Further, the three-phase copper-based catalyst also comprises a binder.
Preferably, the binder includes any one or a combination of two or more of spindle oil, paraffin powder, stearic acid, polymethacrylates, and polyethylene glycol, but is not limited thereto.
Preferably, the content of the binder in the three-phase copper-based catalyst is below 1 wt%.
The embodiment of the invention also provides a preparation method of the three-phase copper-based catalyst, which comprises the following steps: mixing Cu2Placing the O particles, the CuO particles and the Cu particles into vibration ball milling equipment, adding an adhesive in the vibration ball milling process, controlling the addition of the adhesive within 1wt%, and performing vibration ball milling on the mixed material for 10-30 min to obtain the three-phase copper-based catalyst.
In some more specific embodiments, the preparation method comprises: mixing Cu2And placing the O particles, the CuO particles and the Cu particles into vibration ball milling equipment, wherein the CuO particles and the Cu particles are simultaneously added, an adhesive is added in the vibration ball milling process, and the mixed material is subjected to vibration ball milling for 10-30 min to obtain the three-phase copper-based catalyst, wherein the three-phase copper-based catalyst comprises an aggregate with a single-layer core-shell structure.
In some more specific embodiments, the preparation method comprises: mixing Cu2And placing the O particles, the CuO particles and the Cu particles into vibration ball milling equipment, wherein the Cu particles are put after the CuO particles are put for 10-30 min, and an adhesive is put in the vibration ball milling process, and the mixed material is subjected to vibration ball milling for 10-30 min to obtain the three-phase copper-based catalyst, wherein the three-phase copper-based catalyst comprises an aggregate with a double-layer core-shell structure.
The embodiment of the invention also provides application of the three-phase copper-based catalyst in a dimethyl dichlorosilane synthesis process.
The technical solution, the implementation process and the principle thereof will be further explained with reference to the specific embodiments as follows.
Specifically, the method for preparing the three-phase copper-based catalyst can comprise the following steps:
1) preparation of Cu by oxidation2O or purchase of high purity Cu2O powder with the grain diameter below 150um is subjected to ball milling treatment, and when the grain diameter reaches below 50 microns, the ball milling is stopped to obtain the required Cu2And (4) O raw material.
2) According to the requirements of the particle size, CuO or Cu ultrafine powder is prepared by adopting electric explosion, plasma discharge or an extraction method.
3) According to the proportion, first Cu2Placing the three raw material powders into a vibration ball mill, adding adhesive in the vibration process, wherein the addition amount of the adhesive is within 1%, and vibrating for 10-30 minutes
4) For the aggregate with a single-layer shell-core structure, Cu and CuO powder are added simultaneously according to the proportion and vibrated for 10 to 30 minutes.
5) For the aggregate with the double-layer shell-core structure, the CuO powder is added in proportion and vibrated for 10-30 minutes, and then the Cu powder is added in proportion and continuously vibrated for 10-30 minutes
6) And (4) putting the mixed powder into a mixer for further mixing uniformly, weighing and packaging.
Each batch of the three-phase copper-based catalyst prepared by the method is used in a fluidized bed (the use of the three-phase copper-based catalyst in the fluidized bed is referred to in the references of organosilicon synthesis process and product application, chemical industry publishers, Happy Sonmin), the difference with the traditional commercial catalyst (the three-phase copper catalyst prepared by CN103127936A, CN103599782A and CN 106140160A) is evaluated, and the performance under the conditions of different raw materials and reaction temperatures is evaluated (the following test data are average values of data obtained by carrying out multiple tests on multiple batches of samples).
Example 1
Three-phase copper-based catalysts were prepared with reference to the contents of the components in tables 1 and 2, and counted as catalyst a and catalyst C, respectively,
table 1 shows the partial raw material ratios of the three-phase copper-based catalyst in example 1
Table 2 shows the proportions of the respective raw materials of the three-phase copper-based catalyst in example 1
The method for catalytically synthesizing the dimethyldichlorosilane is characterized in that the catalyst A, the catalyst C and the catalyst provided in CN103127936A refer to organic silicon synthesis process and product application, chemical industry publishers, Happy Sonmin, record methods, the synthesis reaction temperature is 285-293 ℃, and 421 silicon is used as a synthesis raw material; the catalytic synthesis performance was tested and recorded, and the results are shown in table 3;
table 3 shows the catalytic performance of the catalysts provided in catalyst A, catalyst C and CN103127936A
Example 2
Referring to the contents of the components in Table 4, three-phase copper-based catalysts were prepared, each designated as catalyst B,
table 4 shows the partial raw material ratios of the three-phase copper-based catalyst in example 2
The catalyst B and the catalyst provided in CN103599782A are catalyzed and synthesized into the dimethyldichlorosilane by the method recorded in chemical industry publishers, Happy Sonmin, according to the organosilicon synthesis process and product application, wherein the synthesis reaction temperature is 295-300 ℃, and 411 silicon is used as a synthesis raw material; the catalytic synthesis performance is tested and recorded, and the result is shown in table 5;
table 5 shows the catalytic performance of catalysts B and CN103599782A
Example 3
Referring to the contents of the components in Table 6, three-phase copper-based catalysts were prepared, each designated as catalyst D,
table 6 shows the partial raw material ratios of the three-phase copper-based catalyst in example 3
The catalyst D and the catalyst provided in CN106140160A are catalyzed and synthesized into the dimethyldichlorosilane by the method recorded in chemical industry publishers, Happy Sonmin, which refers to organosilicon synthesis process and product application, the synthesis reaction temperature is 285-290 ℃, and 321 silicon is used as a synthesis raw material; the catalytic synthesis performance is tested and recorded, and the result is shown in table 7;
table 7 shows the catalytic performance of catalyst D and the catalyst provided in CN106140160A
In the three-phase copper-based catalyst, the ultrafine submicron Cu particles with highest activity are exposed at the outer layer of the aggregate and are most directly mixed with reactants Si powder and CH3Cl contacts to trigger the reaction, and CuO and Cu are arranged in the inner layer of the agglomerate2The O particles are gradually converted into Cu to participate in the reaction, so that the continuity of the whole reaction process is ensured, and meanwhile, the three-phase copper catalyst has higher reaction activity, can maintain stable dimethyldichlorosilane selectivity, improves the reaction rate and the production efficiency of the dimethyldichlorosilane synthesis reaction, and reduces the cost.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (15)
1. The three-phase copper-based catalyst is characterized by mainly comprising Cu2The agglomerates are formed by O particles, CuO particles and Cu particles, wherein the agglomerates have a core-shell structure, and the Cu particles2O particles are distributed in the core layer, CuO particles and Cu particles are distributed in the shell layer, and in the agglomerates, the CuO particles and the Cu particles surround the Cu2And setting O particles.
2. The three-phase copper-based catalyst according to claim 1, characterized in that: in the agglomerates, CuO particles surround Cu2The O particles are disposed and the Cu particles are disposed around the CuO particles.
3. The three-phase copper-based catalyst according to claim 1, characterized in that: the mass ratio of the aggregate is 50% -85%: 0% -45%: 5% -35% of Cu2O particles, CuO particles, and Cu particles.
4. The three-phase copper-based catalyst according to claim 1, characterized in that: the Cu2The particle size of the O particles is 1-50 μm.
5. The three-phase copper-based catalyst according to claim 1, characterized in that: the particle size of the CuO particles is 0.01-0.5 μm.
6. The three-phase copper-based catalyst according to claim 1, characterized in that: the particle size of the Cu particles is 0.01-0.5 mu m.
7. The three-phase copper-based catalyst according to claim 1, characterized in that: the Cu2The O particles, the CuO particles and the Cu particles are spherical or quasi-sphericalGranular with irregular or irregular shape.
8. The three-phase copper-based catalyst according to claim 1, characterized in that: the Cu2The particle diameters of the O particles, the CuO particles and the Cu particles are different from each other.
9. The three-phase copper-based catalyst according to claim 1, further comprising a binder.
10. The three-phase copper-based catalyst according to claim 9, wherein: the binder comprises any one or the combination of more than two of spindle oil, paraffin powder, stearic acid, polymethacrylate and polyethylene glycol.
11. The three-phase copper-based catalyst according to claim 9, wherein: the content of the binder in the three-phase copper-based catalyst is less than 1 wt%.
12. The method of preparing a three-phase copper-based catalyst according to claim 1, comprising: mixing Cu2Placing the O particles, the CuO particles and the Cu particles into vibration ball milling equipment, adding an adhesive in the vibration ball milling process, controlling the addition of the adhesive within 1wt%, and performing vibration ball milling on the mixed material for 10-30 min to obtain the three-phase copper-based catalyst.
13. The method according to claim 12, characterized by comprising: mixing Cu2And placing the O particles, the CuO particles and the Cu particles into vibration ball milling equipment, wherein the CuO particles and the Cu particles are simultaneously added, an adhesive is added in the vibration ball milling process, and the mixed material is subjected to vibration ball milling for 10-30 min to obtain the three-phase copper-based catalyst, wherein the three-phase copper-based catalyst comprises an aggregate with a single-layer core-shell structure.
14. The method according to claim 12, characterized by comprising: mixing Cu2O particles,And placing the CuO particles and the Cu particles into vibration ball milling equipment, wherein the Cu particles are put after the CuO particles are put for 10-30 min, an adhesive is put in the vibration ball milling process, and the mixed materials are subjected to vibration ball milling for 10-30 min to obtain the three-phase copper-based catalyst, wherein the three-phase copper-based catalyst comprises an aggregate with a double-layer core-shell structure.
15. Use of the three-phase copper-based catalyst of any one of claims 1 to 11 in a dimethyldichlorosilane synthesis process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810222432.5A CN110270328B (en) | 2018-03-16 | 2018-03-16 | Three-phase copper-based catalyst and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810222432.5A CN110270328B (en) | 2018-03-16 | 2018-03-16 | Three-phase copper-based catalyst and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110270328A CN110270328A (en) | 2019-09-24 |
| CN110270328B true CN110270328B (en) | 2022-03-15 |
Family
ID=67957932
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810222432.5A Active CN110270328B (en) | 2018-03-16 | 2018-03-16 | Three-phase copper-based catalyst and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110270328B (en) |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1156640A (en) * | 1995-12-01 | 1997-08-13 | 拜尔公司 | Copper-based catalysts, processes for their production and their use and process for production of alkyl halosilanes |
| CN101541415A (en) * | 2006-11-14 | 2009-09-23 | 巴斯夫欧洲公司 | Method for production of a mini suspoemulsion or suspension of sub-micron core/shell particles |
| WO2014187646A1 (en) * | 2013-05-24 | 2014-11-27 | Evonik Industries Ag | Copper oxide/silicon dioxide composite |
| CN104308143A (en) * | 2014-09-16 | 2015-01-28 | 湖南省天心博力科技有限公司 | Production method of ternary copper powder |
| CN104837347A (en) * | 2012-12-13 | 2015-08-12 | 昭和电工株式会社 | Antimicrobial and antiviral composition, and method of producing the same |
| CN104857958A (en) * | 2015-05-15 | 2015-08-26 | 中国科学院过程工程研究所 | Copper-based Cu-Cu2O-CuO catalyst as well as preparation method and application thereof |
| CN105536791A (en) * | 2015-12-30 | 2016-05-04 | 河北工程大学 | Preparation method of octahedral cuprous oxide catalyst for synthesizing methyl chlorosilane monomers |
| CN106140160A (en) * | 2015-04-03 | 2016-11-23 | 浙江新安化工集团股份有限公司 | A kind of preparation method of the copper catalyst for direct synthesis methylchlorosilane |
-
2018
- 2018-03-16 CN CN201810222432.5A patent/CN110270328B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1156640A (en) * | 1995-12-01 | 1997-08-13 | 拜尔公司 | Copper-based catalysts, processes for their production and their use and process for production of alkyl halosilanes |
| CN101541415A (en) * | 2006-11-14 | 2009-09-23 | 巴斯夫欧洲公司 | Method for production of a mini suspoemulsion or suspension of sub-micron core/shell particles |
| CN104837347A (en) * | 2012-12-13 | 2015-08-12 | 昭和电工株式会社 | Antimicrobial and antiviral composition, and method of producing the same |
| WO2014187646A1 (en) * | 2013-05-24 | 2014-11-27 | Evonik Industries Ag | Copper oxide/silicon dioxide composite |
| CN104308143A (en) * | 2014-09-16 | 2015-01-28 | 湖南省天心博力科技有限公司 | Production method of ternary copper powder |
| CN106140160A (en) * | 2015-04-03 | 2016-11-23 | 浙江新安化工集团股份有限公司 | A kind of preparation method of the copper catalyst for direct synthesis methylchlorosilane |
| CN104857958A (en) * | 2015-05-15 | 2015-08-26 | 中国科学院过程工程研究所 | Copper-based Cu-Cu2O-CuO catalyst as well as preparation method and application thereof |
| CN105536791A (en) * | 2015-12-30 | 2016-05-04 | 河北工程大学 | Preparation method of octahedral cuprous oxide catalyst for synthesizing methyl chlorosilane monomers |
Non-Patent Citations (2)
| Title |
|---|
| "Template-free synthesis of Cu@Cu2O core-shell microspheres and their application as copper-based catalysts for dimethyldichlorosilane synthesis";Zailei Zhang et al;《Chemical Engineering Journal》;20121005;第211-212卷;430页第4节 * |
| "由铜精矿制备有机硅单体合成反应三元铜催化剂及其性能";翟延昭等;《过程工程学报》;20141215;第14卷(第6期);第1020-1027页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110270328A (en) | 2019-09-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP7329878B2 (en) | Silicon nitride, ceramic slurry and preparation method | |
| EP2420336B1 (en) | Coated silver nanoparticles and manufacturing method therefor | |
| JP5227828B2 (en) | Method for producing oxidation-resistant copper fine particles and joining method using the same | |
| Liu et al. | Effective reduction of 4-nitrophenol with Au NPs loaded ultrathin two dimensional metal-organic framework nanosheets | |
| JP5578175B2 (en) | Conductive nanocomposite and method for producing the same | |
| JP5620122B2 (en) | Joining material and joining method | |
| JP6462109B2 (en) | Production method of silane trichloride | |
| CN110270328B (en) | Three-phase copper-based catalyst and preparation method and application thereof | |
| CN110028062A (en) | A kind of preparation method of surface modification oil solubility graphene oxide | |
| CN109897341A (en) | A kind of composite material and preparation method of modified graphene reinforced epoxy | |
| US10541067B2 (en) | Carbon nanotube pellets and method for manufacturing same | |
| WO1996022401A1 (en) | Copper-tungsten alloys and process for producing the same | |
| Jin et al. | The preparation of a core/shell structure with alumina coated spherical silica powder | |
| CN107225254A (en) | A kind of aluminum nanoparticles and preparation method thereof | |
| CN113976116B (en) | Variable-speed ball milling preparation of ternary copper Cu-Cu 2 O-CuO catalyst and method thereof | |
| CN101811057B (en) | Powdered catalyst for synthesizing methyl chlorosilane | |
| CN105524193B (en) | A kind of carried metallocene catalyst and preparation method thereof | |
| CN109248709A (en) | Nano silver/polystyrene-acrylic acid shell core three-decker complex microsphere catalyst | |
| CN106478441A (en) | Nano diamond, its manufacture method and the nano-fluid using which | |
| US20100160664A1 (en) | Process for the direct synthesis of alkylhalosilanes | |
| US6395917B1 (en) | Preparation of organohalosilanes | |
| Yan et al. | Highly Monodisperse Sub‐microspherical Poly (glycidyl methacrylate) Nanocomposites with Highly Stabilized Gold Nanoparticles | |
| CN110787800B (en) | Method for preparing superfine ternary copper catalyst at low cost | |
| CN100404131C (en) | Preparation method of silicon-copper contact for synthesizing organic chlorosilane | |
| CN100512957C (en) | Copper catalyst for synthesizing organic silicon monomer and its preparation process |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |