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
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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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