Method used for preparing compounds or high-purity compounds having general formula of R(4-m-n)AClmHn, especially silane, and apparatus thereof

A technology of compound and general formula, applied in the field of devices implementing the method, to achieve the effect of simple operation and operation

Inactive Publication Date: 2013-09-04
EVONIK DEGUSSA GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A specific drawback of this method is that a reducing agent must be added

Method used

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  • Method used for preparing compounds or high-purity compounds having general formula of R(4-m-n)AClmHn, especially silane, and apparatus thereof
  • Method used for preparing compounds or high-purity compounds having general formula of R(4-m-n)AClmHn, especially silane, and apparatus thereof
  • Method used for preparing compounds or high-purity compounds having general formula of R(4-m-n)AClmHn, especially silane, and apparatus thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 21

[0138] Alkylaminotrialkoxysilanes having the following general formula are used as catalysts,

[0139] (CH 3 CH 2 O) 3 Si(CH 2 ) 3 N(octyl) 2

[0140] The catalyst was immobilized on spherical SiO in the presence of aqueous ethanol 2 on the carrier material and dried in vacuo. 6.2 g of aminosilane per 100 g of catalyst mass were immobilized.

[0141] The catalyst material was put into the reactor under a nitrogen atmosphere, also with N 2 Flush the distillation column. Then SiCl 4 Fill the still and heat until boiling. After overhead reflux was initiated, trichlorosilane was slowly fed into the reactor, thereby initiating the disproportionation reaction, and the reactor was heated to boil the reactor charge. Due to the formation of gaseous dichlorosilane and trichlorosilane which flows into the column in liquid phase, the distillation column also starts to work, and the temperature in the top and middle of the column drops, wherein an automatic control of the top o...

Embodiment 22

[0146] Catalyst materials obtained by hydrolysis of alkylaminotrialkoxysilanes of the general formula in the presence of water and separation of methanol by careful drying in a downstream vacuum were used in the following examples. The process mode of Example 2.1 was repeated.

[0147] (CH 3 O) 3 Si(CH 2 ) 3 N(C 2 h 5 ) 2

[0148] Tests of the catalyst were carried out in the apparatus and at different reactor heating temperatures. The results obtained are listed in table 2.1 (all data are based on 100g catalyst material):

[0149] Table 2.1:

[0150]

[0151] In a corresponding manner it is also possible to use fixation on SiO 2 Or ceramic carrier (CH 3 O) 3 Si(CH 2 ) 2 N(C 4 h 9 ) 2 as a catalyst.

[0152] According to a third aspect of the present invention, it has now surprisingly been found that hydrogen and formula IIa R wherein p=4 and q=0 are delivered in a simple and economical manner (4-p-q) SiCl p h q A mixture of compounds, namely SiCl 4 ...

Embodiment 31

[0176] with 0.1N-BaCl 2 - Solution impregnation of ZSM5, followed by drying and firing at 450° C. for 1 hour in a hydrogen atmosphere. 10% by weight of salt was applied in this way.

[0177] In a quartz glass reactor with a diameter of 15 mm and a length of 250 mm, 1.3 g of this metal salt-containing zeolite were applied to the frit. via tube furnace The electrons heat up to 845°C. h 2 / SiCl 4 The mixture flows through the reactor at a throughput of 7 l / h. The conversion rate of the reaction was detected by gas chromatography. Table 3.1 shows the proportion of different substances n(H 2 ) / n(SiCl 4 ) SiCl 4 Convert to HSiCl 3 conversion rate.

[0178] chart 3.1

[0179] n(H 2 ) / n(SiCl 4 ) Convert to HSiCl 3 conversion rate (%) 4 17.4 5 19.2 6 20.7 8 23.2

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Abstract

The invention relates to a method used for preparing compounds or high-purity compounds having a general formula of R(4-m-n)AClmHn, and an apparatus suitable for implementing the method, and especially relates to an apparatus for preparing silane having a general formula of HnSiCl4-n through disproportionating highly-chlorinated silane in the presence of a catalyst, and a method thereof, wherein A is Si, Ge, Ti or Sn; n is 1, 2, 3 or 4; and the apparatus used for the method is an assembly composed of at least one distillation tower and at least one bypass reactor which is an external reactor. The invention also relates to a catalyst comprising alkylaminotrialkoxy silane having a general formula of (CxH2x+1O)3Si(CH2)zN(CyH2y+1)2, and a method for preparing trichlorosilane (HSiCl3) through catalytic hydrogenation dehalogenation of tetrachlorosilicane (SiCl4) in the presence of hydrogen. The invention further relates to a method for preparing alkylhydrochlorosilane having a general formula of Ia(R(4-m-n)SiClmHn), wherein m is 1 or 2, n is 1 or 2, the m+n value is not equal to 3, and R represents a C1-5 alkyl group. The invention discloses a method for processing silicon tetrachloride, germanium tetrachloride, titanium tetrachloride or tin tetrachloride containing at least one hydrogen-containing compound which cannot be separated through distillation, and an apparatus thereof. The invention also discloses a continuous method for preparing high-purity silicon tetrachloride, germanium tetrachloride, titanium tetrachloride or tin tetrachloride, and an apparatus and a reactor thereof.

Description

[0001] This application is a divisional application of the application number 200710109791.1, and the filing date of the application number 200710109791.1 is April 10, 2007. Technical field: [0002] The present invention relates to having general formula R (4-m-n) AC1 m h n And the method wherein A is equal to the compound or high-purity compound of silicon, germanium, titanium or tin, and the device suitable for implementing the method. [0003] The present invention also relates to a method for passing at least one general formula (II) R (4-p-q) AC1 p h q The reaction of the compound with general formula (I) R (4-m-n) AC1 m h n The device and method of the silane, and in the formula (II), R is a linear, branched or cyclic optionally substituted hydrocarbon group with 1 to 8 C atoms, preferably methyl, ethyl, propyl, chlorine Methyl, chloroethyl, chloropropyl - just to mention some of the compounds - A represents an element of the Periodic Table of the Elements (PSE)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07F7/12
Inventor P.阿德勒K.博姆汉默尔H.J.霍恩J.卡斯尼茨S.科瑟J.E.朗R.马特赫斯J.蒙凯维奇R.尼科莱T.波普肯H.-P.波普H.劳尔德I.罗弗G.罗沃R.肖尔克J.舒勒R.索南谢恩H.-J.瓦伦西克
Owner EVONIK DEGUSSA GMBH
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