CN113893850A - Catalyst for purifying dimethyldichlorosilane and preparation method and application thereof - Google Patents
Catalyst for purifying dimethyldichlorosilane and preparation method and application thereof Download PDFInfo
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- CN113893850A CN113893850A CN202111256368.0A CN202111256368A CN113893850A CN 113893850 A CN113893850 A CN 113893850A CN 202111256368 A CN202111256368 A CN 202111256368A CN 113893850 A CN113893850 A CN 113893850A
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- catalyst
- dimethyldichlorosilane
- silicon
- palladium
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- 239000003054 catalyst Substances 0.000 title claims abstract description 88
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title abstract description 19
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 29
- 150000001875 compounds Chemical class 0.000 claims abstract description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 17
- 239000010703 silicon Substances 0.000 claims abstract description 17
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000746 purification Methods 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 10
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 39
- 239000007789 gas Substances 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 22
- 239000011701 zinc Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 13
- 238000004537 pulping Methods 0.000 claims description 11
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 229910052725 zinc Inorganic materials 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 7
- 150000001412 amines Chemical class 0.000 claims description 6
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 4
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 4
- 238000002161 passivation Methods 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- 229910002666 PdCl2 Inorganic materials 0.000 claims description 2
- RBYGDVHOECIAFC-UHFFFAOYSA-L acetonitrile;palladium(2+);dichloride Chemical compound [Cl-].[Cl-].[Pd+2].CC#N.CC#N RBYGDVHOECIAFC-UHFFFAOYSA-L 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 2
- YJVFFLUZDVXJQI-UHFFFAOYSA-L palladium(ii) acetate Chemical compound [Pd+2].CC([O-])=O.CC([O-])=O YJVFFLUZDVXJQI-UHFFFAOYSA-L 0.000 claims description 2
- QJPQVXSHYBGQGM-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 QJPQVXSHYBGQGM-UHFFFAOYSA-N 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 1
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 1
- 239000007858 starting material Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 18
- 239000001257 hydrogen Substances 0.000 abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 14
- 238000009835 boiling Methods 0.000 abstract description 8
- 229930195735 unsaturated hydrocarbon Natural products 0.000 abstract description 7
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 abstract description 6
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000004913 activation Effects 0.000 abstract description 3
- 239000011203 carbon fibre reinforced carbon Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 42
- 238000003756 stirring Methods 0.000 description 30
- 239000002808 molecular sieve Substances 0.000 description 28
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 26
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 20
- 238000010438 heat treatment Methods 0.000 description 20
- 239000000843 powder Substances 0.000 description 20
- 239000002002 slurry Substances 0.000 description 20
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 16
- 229910001868 water Inorganic materials 0.000 description 16
- 239000008367 deionised water Substances 0.000 description 14
- 229910021641 deionized water Inorganic materials 0.000 description 14
- 239000000178 monomer Substances 0.000 description 14
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 13
- 238000002156 mixing Methods 0.000 description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 10
- 239000006227 byproduct Substances 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 10
- 238000000576 coating method Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 238000001816 cooling Methods 0.000 description 10
- 229910052878 cordierite Inorganic materials 0.000 description 10
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 10
- 238000001914 filtration Methods 0.000 description 10
- 229910052760 oxygen Inorganic materials 0.000 description 10
- 239000001301 oxygen Substances 0.000 description 10
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Inorganic materials [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 7
- PFMKUUJQLUQKHT-UHFFFAOYSA-N dichloro(ethyl)silicon Chemical compound CC[Si](Cl)Cl PFMKUUJQLUQKHT-UHFFFAOYSA-N 0.000 description 3
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- KTQYJQFGNYHXMB-UHFFFAOYSA-N dichloro(methyl)silicon Chemical compound C[Si](Cl)Cl KTQYJQFGNYHXMB-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000004383 yellowing Methods 0.000 description 2
- -1 2-methyl 2-butylene) Chemical compound 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- 229910001297 Zn alloy Inorganic materials 0.000 description 1
- 229910007570 Zn-Al Inorganic materials 0.000 description 1
- URBHJJGWUIXBFJ-UHFFFAOYSA-N [C].[Cl] Chemical class [C].[Cl] URBHJJGWUIXBFJ-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- ULYZAYCEDJDHCC-UHFFFAOYSA-N isopropyl chloride Chemical compound CC(C)Cl ULYZAYCEDJDHCC-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000013468 resource allocation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/60—Platinum group metals with zinc, cadmium or mercury
-
- 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
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention belongs to the technical field of dimethyl dichlorosilane purification treatment, and particularly relates to a catalyst for purifying dimethyl dichlorosilane and a preparation method and application thereof. The raw materials of the catalyst comprise a palladium-containing compound, an aluminum-containing precursor and a silicon-containing precursor; the catalyst can obviously reduce the bond breaking activation energy of silicon-hydrogen bonds, silicon-silicon bonds, carbon-chlorine bonds, carbon-carbon unsaturated silicon methyl bonds and silicon-chlorine bonds, so that substances which are difficult to separate are converted into substances which are easy to separate, substances such as chlorocarbon compounds, unsaturated hydrocarbons, ethylhydrogen dichlorosilane and the like generate products with boiling points higher than that of dimethyldichlorosilane, the products are easy to remove in the subsequent rectification link, the purity of a finished dimethyldichlorosilane product can be obviously improved, and the influence of impurities in the dimethyldichlorosilane on the quality of downstream products is reduced. The catalyst provided by the invention has the advantages of good dispersibility, high activity, high repeated utilization rate and wide application range.
Description
Technical Field
The invention belongs to the technical field of dimethyl dichlorosilane purification treatment, and particularly relates to a catalyst for purifying dimethyl dichlorosilane and a preparation method and application thereof.
Background
In recent years, the organic silicon industry in China is rapidly developed, the market demand is increased every year, the total yield of organic silicon monomers leap forward to the first in the world, and the demand of high-quality organic silicon monomers is increased day by day. Along with the continuous expansion of the production scale of the domestic organic silicon monomer and the continuous improvement of the requirement on sustainable development, the amount of the by-products which are difficult to treat and generated in the production of the organic silicon monomer is increased, and the amount of the by-products which are difficult to treat and generated in the production of the organic silicon monomer is increased, so that on one hand, the by-products are easy to react with moisture in the air to generate hydrogen chloride to pollute the environment; on the other hand, recycling of the by-products has become a bottleneck to prevent the resource allocation of the organosilicon monomer industry and the development of the organosilicon monomer industry to the high-end.
Dimethyldichlorosilane is the most commonly used silicone monomer, and in addition to the target product, many byproducts are generated in the production process of the silicone monomer, such as monomethyltrichlorosilane, monomethyldichlorosilane, chlorocarbon compounds, unsaturated hydrocarbons, ethyldichlorosilane, high-boiling substances, low-boiling substances, and the like, and the total content of the byproducts is 15-25%. The reduction of the content of the by-product in the dimethyldichlorosilane not only can greatly improve the purity of the organic silicon monomer, but also can further improve the yield of the organic silicon monomer and the utilization rate of downstream silicon atoms, thereby bringing greater economic benefit. The monomethyl trichlorosilane, the monomethyl hydrogen dichlorosilane, the high boiling residue and the low boiling residue in the dimethyl dichlorosilane can be effectively separated by a subsequent continuous rectification process. For the separation of byproducts such as chlorocarbon compounds, unsaturated hydrocarbons and the like, a phase separation method is mostly adopted to remove the byproducts after a hydrolysis unit in foreign countries, but the technological process is long, the effect is general, and the ultra-high-purity dimethyldichlorosilane cannot be obtained; in China, a deep purification technology for dimethyldichlorosilane is not available for a while. Under the existing process technology, the dimethyl dichlorosilane purified by continuous rectification still contains trace chlorine carbon compounds which are not easy to remove, such as substances of isopropyl chloride, unsaturated hydrocarbon (such as 2-methyl 2-butylene), ethyl hydrogen dichlorosilane and the like, the substances are easy to cause instability of downstream products, the problems of color difference, yellowing and the like, and the ethyl dichlorosilane is easy to cause the downstream polymers to form a three-dimensional network structure in the using process, so that the quality of terminal products is influenced.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects that in the prior art, dimethyldichlorosilane cannot be deeply purified, the contained byproducts are still more, downstream products are affected and the like, so that the catalyst for purifying dimethyldichlorosilane, the preparation method and the application thereof are provided.
Therefore, the invention provides the following technical scheme.
The invention provides a catalyst for purifying dimethyldichlorosilane, which comprises a palladium-containing compound, an aluminum-containing precursor and a silicon-containing precursor.
The feedstock of the catalyst also includes a zinc-containing compound.
In the raw materials of the catalyst, the molar ratio of palladium in a palladium-containing compound, silicon in a silicon-containing precursor and aluminum in an aluminum-containing precursor is (4-6): (75-85): (3-4);
the molar ratio of palladium in the palladium-containing compound to zinc in the zinc-containing compound is 1: (0.5-3).
The raw material of the catalyst also comprises amines;
the amine may be, but is not limited to, at least one of cetyltrimethylammonium bromide, ethylenediamine, triethylamine, hexamethylenediamine, n-butylamine, and ammonia.
The palladium-containing compound may be, but is not limited to, Pd (NO)3)2·2H2O、Pd(OAc)2、PdCl2、Pd(MeCN)2Cl2、Pd(PPh3)2、Pd(TFA)2At least one of;
the zinc-containing compound can be, but is not limited to, Zn (NO)3)2、ZnCl2And Zn (CH)3COO)2At least one of (1).
The aluminum-containing precursor can be, but is not limited to, aluminum-containing compounds such as aluminum oxide, aluminum chloride, pseudo-boehmite and the like;
the silicon-containing precursor can be, but is not limited to, a silicon-containing compound such as tetraethoxysilane, silicon dioxide and the like.
The invention also provides a preparation method of the catalyst, which comprises the following steps,
the raw materials are uniformly mixed, the pH value is adjusted to 9-10, then the mixture is placed at the temperature of 130-220 ℃ for crystallization, and the catalyst is obtained after washing, roasting, reduction and passivation.
Further, the catalyst of the invention is prepared under alkaline conditions.
The preparation method also comprises the steps of pulping and drying between the roasting step and the reduction step;
preferably, the roasting step is carried out at a temperature rise rate of 1-5 ℃ to 700 ℃;
the temperature of the reduction is 450-550 ℃;
the temperature of the passivation is 450-550 ℃.
In addition, the invention provides an application of the catalyst or the catalyst prepared by the method in the purification treatment of the dimethyldichlorosilane.
The application comprises the following steps of,
the dimethyl dichlorosilane gas containing impurities and hydrogen chloride gas form mixed gas, the mixed gas reacts under the action of a catalyst, and the purified dimethyl dichlorosilane is obtained after rectification.
The reaction temperature is 200-400 ℃, preferably 220-280 ℃;
the pressure of the reaction is not higher than 0.2 MPa;
the volume ratio of the impurity-containing dimethyldichlorosilane gas to the hydrogen chloride gas is 1: (1-3), preferably 1:2 or 1: 1.5;
the mass ratio of the catalyst to the mixed gas is (1-10): 100, preferably (2-5): 100.
the impurities in the impurity-containing dimethyldichlorosilane gas generally include monomethyltrichlorosilane, monomethyldichlorosilane, chlorocarbon compounds, unsaturated hydrocarbons, ethyldichlorosilane, high boiling substances, low boiling substances, and the like.
The technical scheme of the invention has the following advantages:
1. the invention provides a catalyst for purifying dimethyldichlorosilane, which comprises raw materials of a palladium-containing compound, an aluminum-containing precursor and a silicon-containing precursor; the catalyst can obviously reduce the bond breaking activation energy of silicon-hydrogen bonds, silicon-silicon bonds, carbon-chlorine bonds, carbon-carbon unsaturated silicon methyl bonds and silicon-chlorine bonds, so that substances which are difficult to separate are converted into substances which are easy to separate, substances such as chlorocarbon compounds, unsaturated hydrocarbons, ethylhydrogen dichlorosilane and the like generate products with boiling points higher than that of dimethyldichlorosilane, the products are easy to remove in the subsequent rectification link, the purity of a finished dimethyldichlorosilane product can be obviously improved, and the influence of impurities in the dimethyldichlorosilane on the quality of downstream products is reduced. The catalyst provided by the invention has the advantages of good dispersibility, high activity, high repeated utilization rate and wide application range.
2. According to the catalyst provided by the invention, the zinc-containing compound is added into the catalyst, so that a Pd-Zn alloy or a Pd-Zn-Al alloy is formed between metals, the reaction is promoted, and the reaction rate is increased.
The catalyst has stronger selectivity to polar monomers and low molecular weight monomers, and the palladium-containing compound is uniformly dispersed in the molecular sieve and on the surface of the molecular sieve, thereby being beneficial to reducing the activation energy of reaction molecules and improving the catalytic activity of the reaction. The porosity of the silicon-aluminum molecular sieve can also improve the specific surface area of the catalyst, so as to improve the reaction activity, and because the palladium-containing compound is loaded on the pore channels or the surface of the porous molecular sieve, the content of palladium has a more proper range, and the too high content of palladium can block the pore channels of the molecular sieve, so that the specific surface area of the catalyst is reduced, and the activity of the catalyst is reduced.
The amine substance is used as a raw material and added into the catalyst, on one hand, the amine substance can be used as a pH regulator to accurately control the pH value of an intermediate product, and is beneficial to synthesizing a molecular sieve with a perfect structure; on the other hand, the molecular sieve can be used as a template agent to guide the synthesis of the molecular sieve with a specific porous structure.
3. The preparation method of the catalyst provided by the invention comprises the steps of mixing the raw materials, crystallizing at 130-220 ℃, washing, roasting, reducing and passivating to obtain the catalyst, and by controlling the crystallization temperature, the yield of the catalyst in the later reaction period can be effectively controlled, and the method plays an important role in forming the catalyst with a corresponding structure subsequently.
4. The catalyst provided by the invention is applied to the purification treatment of dimethyldichlorosilane, impurities in the dimethyldichlorosilane, such as chlorocarbon compounds, unsaturated hydrocarbons and ethylhydrogen dichlorosilane, can be efficiently removed, the impurities can be converted into high-boiling-point substances under the action of the catalyst, and the high-boiling-point substances are removed from the dimethyldichlorosilane by a rectification method in the later treatment, so that the quality of downstream products is improved, and the problems of color difference, yellowing and the like of the products are reduced. Compared with the method for purifying the dimethyldichlorosilane in the prior art, the catalyst provided by the invention is directly mixed with the mixed gas, so that the process flow is simplified, the removal temperature is reduced, and the energy consumption is reduced.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
This comparative example provides a catalyst for the purification of dimethyldichlorosilane starting from TEOS, Pd (NO) in a molar ratio of 8:0.5:0.36:10003)2·2H2O、AlCl3And H2O。
The preparation method of the catalyst comprises the following steps,
adding AlCl at room temperature3Water and Pd (NO)3)2·6H2Mixing O according to the proportion, stirring for 30min, adding TEOS, continuously stirring for 20min, adding triethylamine to adjust pH to 9-10, continuously stirring for 2h, transferring the solution to a hydrothermal kettle, and crystallizing at 200 ℃ for 48 h;
then cooling and filtering the obtained crystallized product, washing the crystallized product with deionized water and ethanol for three times respectively, and drying the product at the temperature of 100 ℃ for 12 hours to obtain palladium-loaded molecular sieve raw powder; and then placing the molecular sieve raw powder in a muffle furnace, heating to 600 ℃ at the heating rate of 2 ℃/min, roasting for 8h, then uniformly dispersing in silica sol, pulping to obtain slurry, coating the slurry on the surface of cordierite, drying for 12h at 100 ℃, then placing in a hydrogen atmosphere, reducing for 2h at 500 ℃, and passivating for 2h in a 5% oxygen atmosphere to obtain the catalyst.
Example 2
This example provides a catalyst for purifying dimethyldichlorosilane, which comprises Tetraethoxysilane (TEOS), Pd (NO) and tetraethyl orthosilicate (TEOS) in a molar ratio of 8:0.5:0.5:0.36:10003)2·2H2O、Zn(NO3)2·6H2O、AlCl3And H2O。
The preparation method of the catalyst comprises the following steps,
adding AlCl at room temperature3Deionized water, Pd (NO)3)2·2H2O and Zn (NO)3)2·6H2Mixing O according to the above proportion, stirring for 30min, adding TEOS, stirring for 20min, adding Triethylamine (TEA) to adjust pH to 9-10, stirring for 2h, transferring the solution to a hydrothermal kettle, and crystallizing at 200 deg.C for 48 h;
then cooling and filtering the obtained crystallized product, washing the crystallized product with deionized water and ethanol for three times respectively, and drying the product at the temperature of 100 ℃ for 12 hours to obtain palladium-loaded molecular sieve raw powder; and then placing the molecular sieve raw powder in a muffle furnace, heating to 600 ℃ at the heating rate of 2 ℃/min, roasting for 8h, then uniformly dispersing in silica sol to prepare slurry, coating the slurry on the surface of cordierite, then drying at 100 ℃ for 12h, then placing in a hydrogen atmosphere, reducing at 500 ℃ for 2h, and passivating for 2h in a 5% oxygen atmosphere to obtain the catalyst.
Example 3
This example provides a catalyst for purifying dimethyldichlorosilane, which comprises TEOS and Pd (NO) at a molar ratio of 8:0.5:0.25:0.36:10003)2·2H2O、Zn(NO3)2·6H2O、AlCl3And H2O。
The preparation method of the catalyst comprises the following steps,
adding AlCl at room temperature3Deionized water, Pd (NO)3)2·2H2O and Zn (NO)3)2·6H2Mixing O according to the above proportion, stirring for 30min, adding TEOS, stirring for 20min, adding Triethylamine (TEA) to adjust pH to 9-10, stirring for 2h, transferring the solution to a hydrothermal kettle, and crystallizing at 200 deg.C for 48 h;
then cooling and filtering the obtained crystallized product, washing the crystallized product with deionized water and ethanol for three times respectively, and drying the product at the temperature of 100 ℃ for 12 hours to obtain palladium-loaded molecular sieve raw powder; and then placing the molecular sieve raw powder in a muffle furnace, heating to 600 ℃ at the heating rate of 2 ℃/min, roasting for 8h, then uniformly dispersing in silica sol, pulping to obtain slurry, coating the slurry on the surface of cordierite, drying for 12h at 100 ℃, then placing in a hydrogen atmosphere, reducing for 2h at 500 ℃, and passivating for 2h in a 5% oxygen atmosphere to obtain the catalyst.
Example 4
This example provides a catalyst for purifying dimethyldichlorosilane, which comprises TEOS and Pd (NO) at a molar ratio of 8:0.5:1.5:0.36:10003)2·2H2O、Zn(NO3)2·6H2O、AlCl3And H2O。
The preparation method of the catalyst comprises the following steps,
adding AlCl at room temperature3Water, Pd (NO)3)2·2H2O andZn(NO3)2·6H2mixing O according to the proportion, stirring for 30min, adding TEOS, continuously stirring for 20min, adding triethylamine to adjust pH to 9-10, continuously stirring for 2h, transferring the solution to a hydrothermal kettle, and crystallizing at 200 ℃ for 48 h;
then cooling and filtering the obtained crystallized product, washing the crystallized product with deionized water and ethanol for three times respectively, and drying the product at the temperature of 100 ℃ for 12 hours to obtain palladium-loaded molecular sieve raw powder; and then placing the molecular sieve raw powder in a muffle furnace, heating to 600 ℃ at the heating rate of 2 ℃/min, roasting for 8h, then uniformly dispersing in silica sol, pulping to obtain slurry, coating the slurry on the surface of cordierite, drying for 12h at 100 ℃, then placing in a hydrogen atmosphere, reducing for 2h at 500 ℃, and passivating for 2h in a 5% oxygen atmosphere to obtain the catalyst.
Example 5
This example provides a catalyst for purifying dimethyldichlorosilane, which comprises TEOS and Pd (NO) at a molar ratio of 8:0.5:0.5:0.36:10003)2·2H2O、Zn(NO3)2·6H2O、AlCl3And H2O。
The preparation method of the catalyst comprises the following steps,
adding AlCl at room temperature3Deionized water, Pd (NO)3)2·2H2O and Zn (NO)3)2·6H2Mixing O according to the above proportion, stirring for 30min, adding TEOS, stirring for 20min, adding n-butylamine, adjusting pH to 9-10, stirring for 2h, transferring the solution to a hydrothermal kettle, and crystallizing at 200 deg.C for 48 h;
then cooling and filtering the obtained crystallized product, washing the crystallized product with deionized water and ethanol for three times respectively, and drying the product at the temperature of 100 ℃ for 12 hours to obtain palladium-loaded molecular sieve raw powder; and then placing the molecular sieve raw powder in a muffle furnace, heating to 600 ℃ at the heating rate of 2 ℃/min, roasting for 8h, then uniformly dispersing in silica sol, pulping to obtain slurry, coating the slurry on the surface of cordierite, drying for 12h at 100 ℃, then placing in a hydrogen atmosphere, reducing for 2h at 500 ℃, and passivating for 2h in a 5% oxygen atmosphere to obtain the catalyst.
Example 6
This example provides a catalyst for purifying dimethyldichlorosilane, which comprises TEOS and Pd (NO) at a molar ratio of 8:0.5:0.5:0.36:10003)2·2H2O、Zn(NO3)2·6H2O、AlCl3And H2O。
The preparation method of the catalyst comprises the following steps,
adding AlCl at room temperature3Water, Pd (NO)3)2·2H2O and Zn (NO)3)2·6H2Mixing O according to the proportion, stirring for 30min, adding TEOS, continuously stirring for 20min, adding a mixed solution of triethylamine and n-butylamine with a molar ratio of 1:1, adjusting the pH to 9-10, continuously stirring for 2h, transferring the solution to a hydrothermal kettle, and crystallizing for 48h at 200 ℃;
then cooling and filtering the obtained crystallized product, washing the crystallized product with deionized water and ethanol for three times respectively, and drying the product at the temperature of 100 ℃ for 12 hours to obtain palladium-loaded molecular sieve raw powder; and then placing the molecular sieve raw powder in a muffle furnace, heating to 600 ℃ at the heating rate of 2 ℃/min, roasting for 8h, then uniformly dispersing in silica sol, pulping to obtain slurry, coating the slurry on the surface of cordierite, drying for 12h at 100 ℃, then placing in a hydrogen atmosphere, reducing for 2h at 500 ℃, and passivating for 2h in a 5% oxygen atmosphere to obtain the catalyst.
Example 7
This example provides a catalyst for purifying dimethyldichlorosilane, which comprises TEOS and Pd (NO) at a molar ratio of 8:0.5:0.5:0.36:10003)2·2H2O、Zn(NO3)2·6H2O、AlCl3And H2O。
The preparation method of the catalyst comprises the following steps,
adding AlCl at room temperature3Water, Pd (NO)3)2·2H2O and Zn (NO)3)2·6H2Mixing O according to the proportion, stirring for 30min, adding TEOS, continuously stirring for 20min, adding a mixed solution of triethylamine and n-butylamine with a molar ratio of 1:0.5, adjusting the pH value to 9-10, continuously stirring for 2h, transferring the solution to a hydrothermal kettle, and crystallizing for 48h at 200 ℃;
then cooling and filtering the obtained crystallized product, washing the crystallized product with deionized water and ethanol for three times respectively, and drying the product at the temperature of 100 ℃ for 12 hours to obtain palladium-loaded molecular sieve raw powder; and then placing the molecular sieve raw powder in a muffle furnace, heating to 600 ℃ at the heating rate of 2 ℃/min, roasting for 8h, then uniformly dispersing in silica sol, pulping to obtain slurry, coating the slurry on the surface of cordierite, drying for 12h at 100 ℃, then placing in a hydrogen atmosphere, reducing for 2h at 500 ℃, and passivating for 2h in a 5% oxygen atmosphere to obtain the catalyst.
Example 8
This example provides a catalyst for purifying dimethyldichlorosilane, which comprises TEOS and Pd (NO) at a molar ratio of 8:0.5:6:0.36:10003)2·2H2O、Zn(NO3)2·6H2O、AlCl3And H2O。
The preparation method of the catalyst comprises the following steps,
adding AlCl at room temperature3Deionized water, Pd (NO)3)2·2H2O and Zn (NO)3)2·6H2Mixing O according to the proportion, stirring for 30min, adding TEOS, continuously stirring for 20min, adding a mixed solution of triethylamine and n-butylamine with a molar ratio of 1:0.5, adjusting the pH value to 9-10, continuously stirring for 2h, transferring the solution to a hydrothermal kettle, and crystallizing for 48h at 200 ℃;
then cooling and filtering the obtained crystallized product, washing the crystallized product with deionized water and ethanol for three times respectively, and drying the product at the temperature of 100 ℃ for 12 hours to obtain palladium-loaded molecular sieve raw powder; and then placing the molecular sieve raw powder in a muffle furnace, heating to 600 ℃ at the heating rate of 2 ℃/min, roasting for 8h, then uniformly dispersing in silica sol, pulping to obtain slurry, coating the slurry on the surface of cordierite, drying for 12h at 100 ℃, then placing in a hydrogen atmosphere, reducing for 2h at 500 ℃, and passivating for 2h in a 5% oxygen atmosphere to obtain the catalyst.
Comparative example 1
The comparative example provides a catalyst for purifying dimethyldichlorosilane, the raw materials of which comprise TEOS and AlCl in a molar ratio of 8:0.36:10003And H2O。
The preparation method of the catalyst comprises the following steps,
mixing aluminum chloride and water according to the proportion at room temperature, stirring for 30min, adding TEOS, continuously stirring for 20min, dropwise adding triethylamine, adjusting pH to 9-10, continuously stirring for 2h, transferring the solution to a hydrothermal kettle, and crystallizing at 200 ℃ for 48 h;
then cooling and filtering the obtained crystallized product, washing the crystallized product with deionized water and ethanol for three times respectively, and drying the product at the temperature of 100 ℃ for 12 hours to obtain palladium-loaded molecular sieve raw powder; and then placing the molecular sieve raw powder in a muffle furnace, heating to 600 ℃ at the heating rate of 2 ℃/min, roasting for 8h, then uniformly dispersing in silica sol, pulping to obtain slurry, coating the slurry on the surface of cordierite, drying for 12h at 100 ℃, then placing in a hydrogen atmosphere, reducing for 2h at 500 ℃, and passivating for 2h in a 5% oxygen atmosphere to obtain the catalyst.
Comparative example 2
This comparative example provides a catalyst for the purification of dimethyldichlorosilane starting from TEOS, Zn (NO) in a molar ratio of 8:0.5:0.36:10003)2·6H2O、AlCl3And H2O。
The preparation method of the catalyst comprises the following steps,
adding AlCl at room temperature3Water and Zn (NO)3)2·6H2Mixing O according to the proportion, stirring for 30min, adding TEOS, continuously stirring for 20min, adding triethylamine to adjust pH to 9-10, continuously stirring for 2h, transferring the solution to a hydrothermal kettle, and crystallizing at 200 ℃ for 48 h;
then cooling and filtering the obtained crystallized product, washing the crystallized product with deionized water and ethanol for three times respectively, and drying the product at the temperature of 100 ℃ for 12 hours to obtain palladium-loaded molecular sieve raw powder; and then placing the molecular sieve raw powder in a muffle furnace, heating to 600 ℃ at the heating rate of 2 ℃/min, roasting for 8h, then uniformly dispersing in silica sol, pulping to obtain slurry, coating the slurry on the surface of cordierite, drying for 12h at 100 ℃, then placing in a hydrogen atmosphere, reducing for 2h at 500 ℃, and passivating for 2h in a 5% oxygen atmosphere to obtain the catalyst.
Test examples
The experimental example provides the application of the catalyst obtained in each example and comparative example in the purification treatment of the dimethyldichlorosilane, and specifically comprises the following steps,
the catalysts provided by each embodiment and comparative example are respectively placed in a fixed bed reactor, dimethyldichlorosilane gas containing impurities such as low-boiling-point substances, high-boiling-point substances and the like generated in the process of synthesizing dimethyldichlorosilane monomer by a direct method is fully mixed with hydrogen chloride gas to form mixed gas, the mixed gas is introduced into the fixed bed reactor, the pressure in the fixed bed reactor is normal pressure, the temperature is 280 ℃, the volume ratio of the dimethyldichlorosilane gas containing impurities to the hydrogen chloride gas is 1:2, the speed of the mixed gas entering the fixed bed reactor is 10-60g/h, preferably 20-40g/h, in the test, the speed of the mixed gas entering the fixed bed reactor is 30g/h, the mixed gas reacts under the action of the catalyst, and then the purified dimethyldichlorosilane is obtained after rectification treatment; the above operations were repeated three times for each of the catalysts of examples and comparative examples, and the average of the three times was taken as the final performance of each catalyst, and the average contents of impurities in dimethyldichlorosilane before and after purification are shown in Table 1, respectively;
TABLE 1 results of performance testing of dimethyldichlorosilanes obtained with the catalyst preparations of the various examples
The experimental results in table 1 show that the catalyst provided by the invention can effectively reduce impurities in dimethyldichlorosilane and improve the purity of dimethyldichlorosilane.
According to the experimental data of the comparative example 1 and the comparative example 2, the invention can improve the catalytic effect of the catalyst and reduce the impurity content in the dimethyldichlorosilane by adding palladium and zinc into 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 of the invention may be made without departing from the spirit or scope of the invention.
Claims (10)
1. The catalyst for purifying the dimethyldichlorosilane is characterized in that raw materials of the catalyst comprise a palladium-containing compound, an aluminum-containing precursor and a silicon-containing precursor.
2. The catalyst of claim 1 wherein the feedstock further comprises a zinc-containing compound.
3. The catalyst of claim 2, wherein the molar ratio of palladium in the palladium-containing compound, silicon in the silicon-containing precursor, and aluminum in the aluminum-containing precursor is (4-6): (75-85): (3-4);
the molar ratio of palladium in the palladium-containing compound to zinc in the zinc-containing compound is 1: (0.5-3).
4. The catalyst of any one of claims 1 to 3, wherein the starting material for the catalyst further comprises an amine;
the amine is at least one of ethylenediamine, triethylamine, hexamethylenediamine, n-butylamine and ammonia water.
5. The catalyst according to any one of claims 2 to 4, characterized in thatCharacterized in that the palladium-containing compound is Pd (NO)3)2、Pd(OAc)2、PdCl2、Pd(MeCN)2Cl2、Pd(PPh3)2、Pd(TFA)2At least one of;
the zinc-containing compound is Zn (NO)3)2、ZnCl2And Zn (CH)3COO)2At least one of (1).
6. A process for preparing a catalyst according to any one of claims 1 to 5, comprising the steps of,
the raw materials are uniformly mixed, the pH value is adjusted to 9-10, then the mixture is placed at the temperature of 130-220 ℃ for crystallization, and the catalyst is obtained after washing, roasting, reduction and passivation.
7. The method according to claim 6, further comprising a step of pulping and drying between the roasting and the reduction step;
preferably, the roasting step is carried out at a temperature rise rate of 1-5 ℃ to 700 ℃;
the temperature of the reduction is 450-550 ℃;
the temperature of the passivation is 450-550 ℃.
8. Use of a catalyst according to any one of claims 1 to 4 or a catalyst obtainable by a process according to any one of claims 5 to 7 in a dimethyldichlorosilane purification process.
9. Use according to claim 8, characterized in that it comprises the following steps,
the dimethyl dichlorosilane gas containing impurities and hydrogen chloride gas form mixed gas, the mixed gas reacts under the action of a catalyst, and the purified dimethyl dichlorosilane is obtained after rectification.
10. Use according to claim 9, wherein the reaction temperature is 200-400 ℃, preferably 220-280 ℃;
the pressure of the reaction is not higher than 0.2 MPa;
the volume ratio of the impurity-containing dimethyldichlorosilane gas to the hydrogen chloride gas is 1: (1-3);
the mass ratio of the catalyst to the mixed gas is (1-10): 100.
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