CN108097274A - 催化剂及其应用 - Google Patents
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- 239000003054 catalyst Substances 0.000 title claims abstract description 44
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000013312 flour Nutrition 0.000 claims abstract description 12
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 11
- 239000004411 aluminium Substances 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000001119 stannous chloride Substances 0.000 claims abstract description 11
- 235000011150 stannous chloride Nutrition 0.000 claims abstract description 11
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical compound C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 claims abstract description 10
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims abstract description 10
- WPYVAWXEWQSOGY-UHFFFAOYSA-N indium antimonide Chemical compound [Sb]#[In] WPYVAWXEWQSOGY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 238000010189 synthetic method Methods 0.000 claims description 2
- 229910052787 antimony Inorganic materials 0.000 claims 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 15
- 230000000694 effects Effects 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000010949 copper Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910000906 Bronze Inorganic materials 0.000 description 1
- 239000005046 Chlorosilane Substances 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000032696 parturition Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Classifications
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- 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
- B01J35/19—Catalysts containing parts with different compositions
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
- B01J27/10—Chlorides
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- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/08—Halides
- B01J27/122—Halides of copper
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- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/125—Halogens; Compounds thereof with scandium, yttrium, aluminium, gallium, indium or thallium
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- 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
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- Catalysts (AREA)
Abstract
本发明涉及一种催化剂及其应用,该催化剂包括氯化亚铜、铝粉、三氯化锑、硅粉以及铜粉,所述三氯化锑还可更换为锑化铟。本发明提供的催化剂具有更高的活性和二甲选择性(二甲选择性在82~93%之间,氯甲烷一次转换率在38%以上,波动范围为11%),可使二甲基二氯硅烷的合成反应更加平稳,并大幅提升二甲基二氯硅烷的生产效率,降低其生产成本,适于大规模生产和应用。
Description
技术领域
本发明涉及一种催化剂及其应用,属于粉末冶金和化工领域。
背景技术
有机硅新材料是国民经济发展的基础材料之一,它的结构是由硅-氧链接构成主链,硅原子与其它各种有机基团构成侧链,既能保持有机物的特性,又具有无机物的功能,使它与一般有机物相比具有更好的耐高低温、耐气候老化、电气绝缘、耐臭氧,憎水、难燃、无毒无腐蚀和生理惰性等诸多优势,被制作成改性硅橡胶、硅树脂、硅油、玻璃胶、防水剂、脱模剂等超过5000种产品,广泛应用于电子电气、医疗卫生、国防军工、农业生产和快速消费品等诸多领域。
工业上的有机硅产品为多种官能度的混合物,其中以二甲基二氯硅烷的用量最大,约占甲基氯硅烷的90%(质量分数)。制取甲基氯硅烷的方式有多种,现代化工业都是采用直接合成法来批量生产,它是将氯甲烷和硅粉在加热及催化剂的作用下,直接合成甲基氯硅烷的方法。有机硅生产的最大难点在于单体的合成,提高合成的效率以及降低成本是该领域永恒的课题。影响有机硅单体合成的产率和二甲选择性,除了生产装置、原料品质和合成工艺外,催化剂是其关键因素。
现有技术和报道已证实铜元素是当前直接法合成甲基氯硅烷的最有效催化剂,但仅用铜元素作为催化剂不足以获得很好的效果,一般都会在其中复合或添加其它辅助的元素,如锌元素能提高反应的活性增加产量,锡元素可改善二甲基二氯硅烷的获得率(又叫“二甲选择性”),磷元素可降低副反应的发生几率,氧元素延长反应周期稳定反应进程。一些研究人员通过加入磷等元素制造了铜基合金催化剂,这种催化剂在实际生产应用过程中对于反应的活性和二甲选择性不够稳定,尤其是针对不同硅矿石原料的表现不稳定,二甲选择性的范围在75~90%之间,波动范围在15%以上,整个反应过程波动很大,不利于反应过程的控制和操作。
发明内容
本发明的目的在于提供一种催化剂及其应用,可以在不改变现有装置生产现状的条件下,有效的提高二甲基二氯硅烷的选择性。
为达到上述目的,本发明提供如下技术方案:一种催化剂,包括氯化亚铜、铝粉、三氯化锑、硅粉以及铜粉,所述三氯化锑还可更换为锑化铟。
进一步地,在所述催化剂中,所述氯化亚铜的含量为90至96wt%。
进一步地,在所述催化剂中,所述铝粉的含量为0.7至1.0wt%。
进一步地,在所述催化剂中,所述三氯化锑或锑化铟的含量为2.9至4.4wt%。
进一步地,在所述催化剂中,所述硅粉的含量为0.2至0.6wt%。
进一步地,在所述催化剂中,所述铜粉的含量为0.1至0.2%。
进一步地,所述催化剂的形状包括颗粒状、鳞片状中的任意一种或两种以上的组合。
本发明实施例还提供了如所述催化剂于催化合成二甲基二氯硅烷中的用途。
本发明实施例又提供了一种二甲基二氯硅烷的合成方法,包括,采用所述的催化剂作为催化剂,使氯甲烷与硅在250~350℃条件下反应生成二甲基二氯硅烷。
与现有技术相比,本发明的有益效果在于:本发明提供的催化剂具有更高的活性和二甲选择性(二甲选择性在82~93%之间,氯甲烷一次转换率在38%以上,波动范围为11%),可使二甲基二氯硅烷的合成反应更加平稳,并大幅提升二甲基二氯硅烷的生产效率,降低其生产成本,适于大规模生产和应用。
上述说明仅是本发明技术方案的概述,为了能够更清楚了解本发明的技术手段,并可依照说明书的内容予以实施,以下以本发明的较佳实施例详细说明如后。
具体实施方式
下面结合实施例,对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明,但不用来限制本发明的范围。
实施例一
以氯化亚铜、铝粉、三氯化锑、硅粉以及铜粉为原料的催化剂,其中各组分含量(wt%)为氯化亚铜:铝粉:三氯化锑:硅粉:铜粉=94.6:0.7:3.2:0.5:0.9。该催化剂为颗粒状,且其用于合成二甲基二氯硅烷的反应效果为:二甲选择性83至91%,氯甲烷一次转换率为39.5%。
实施例二
以氯化亚铜、铝粉、三氯化锑、硅粉以及铜粉为原料的催化剂,其中各组分含量(wt%)为氯化亚铜:铝粉:三氯化锑:硅粉:铜粉=92:1.3:4.2:1:1.4。该催化剂为颗粒状,且其用于合成二甲基二氯硅烷的反应效果为:二甲选择性81至91%,氯甲烷一次转换率为38%。
实施例三
以氯化亚铜、铝粉、锑化铟、硅粉以及铜粉为原料的催化剂,其中各组分含量(wt%)为氯化亚铜:铝粉:锑化铟:硅粉:铜粉=96:0.7:2.9:0.2:0.1。该催化剂部分为颗粒状,部分为片状,且其用于合成二甲基二氯硅烷的反应效果为:二甲选择性86至93%,氯甲烷一次转换率为41.3%。
综上所述:本发明提供的催化剂具有更高的活性和二甲选择性(二甲选择性在82~93%之间,氯甲烷一次转换率在38%以上,波动范围为11%),可使二甲基二氯硅烷的合成反应更加平稳,并大幅提升二甲基二氯硅烷的生产效率,降低其生产成本,适于大规模生产和应用。
以上所述实施例的各技术特征可以进行任意的组合,为使描述简洁,未对上述实施例中的各个技术特征所有可能的组合都进行描述,然而,只要这些技术特征的组合不存在矛盾,都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。
Claims (9)
1.一种催化剂,其特征在于,包括氯化亚铜、铝粉、三氯化锑、硅粉以及铜粉,所述三氯化锑还可更换为锑化铟。
2.如权利要求1所述的催化剂,其特征在于,在所述催化剂中,所述氯化亚铜的含量为90至96wt%。
3.如权利要求1所述的催化剂,其特征在于,在所述催化剂中,所述铝粉的含量为0.7至1.0wt%。
4.如权利要求1所述的催化剂,其特征在于,在所述催化剂中,所述三氯化锑或锑化铟的含量为2.9至4.4wt%。
5.如权利要求1所述的催化剂,其特征在于,在所述催化剂中,所述硅粉的含量为0.2至0.6wt%。
6.如权利要求1所述的催化剂,其特征在于,在所述催化剂中,所述铜粉的含量为0.1至0.2%。
7.如权利要求1所述的催化剂,其特征在于,所述催化剂的形状包括颗粒状、鳞片状中的任意一种或两种以上的组合。
8.如权利要求1至7中任意一项所述催化剂于催化合成二甲基二氯硅烷中的用途。
9.一种二甲基二氯硅烷的合成方法,其特征在于包括,采用权利要求1至7中任意一项所述的催化剂作为催化剂,使氯甲烷与硅在250~350℃条件下反应生成二甲基二氯硅烷。
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US6090966A (en) * | 1997-05-13 | 2000-07-18 | Shin-Etsu Chemical Co., Ltd. | Preparation of contract mass for alkylhalosilane production and process for producing alkylhalosilanes |
CN1915508A (zh) * | 2005-08-17 | 2007-02-21 | 中国石油天然气股份有限公司 | 一种用于有机氯硅烷合成的硅—铜触体的制备方法 |
CN103316702A (zh) * | 2012-03-22 | 2013-09-25 | 中国科学院过程工程研究所 | 一种铜基催化剂及其制备方法 |
CN103566955A (zh) * | 2012-08-02 | 2014-02-12 | 中国石油天然气股份有限公司 | 一种提高二甲基二氯硅烷选择性的催化剂及其应用 |
CN106000429A (zh) * | 2016-06-15 | 2016-10-12 | 苏州铜宝锐新材料有限公司 | 一种催化剂及其应用 |
-
2017
- 2017-12-18 CN CN201711361905.1A patent/CN108097274A/zh not_active Withdrawn
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6090966A (en) * | 1997-05-13 | 2000-07-18 | Shin-Etsu Chemical Co., Ltd. | Preparation of contract mass for alkylhalosilane production and process for producing alkylhalosilanes |
CN1915508A (zh) * | 2005-08-17 | 2007-02-21 | 中国石油天然气股份有限公司 | 一种用于有机氯硅烷合成的硅—铜触体的制备方法 |
CN103316702A (zh) * | 2012-03-22 | 2013-09-25 | 中国科学院过程工程研究所 | 一种铜基催化剂及其制备方法 |
CN103566955A (zh) * | 2012-08-02 | 2014-02-12 | 中国石油天然气股份有限公司 | 一种提高二甲基二氯硅烷选择性的催化剂及其应用 |
CN106000429A (zh) * | 2016-06-15 | 2016-10-12 | 苏州铜宝锐新材料有限公司 | 一种催化剂及其应用 |
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