Method for preparing polychlorinated phenyl trichlorosilane through catalysis of ionic liquid

A technology of polychlorophenyltrichlorosilane and phenyltrichlorosilane, which is applied in the field of synthesis of polychlorophenyltrichlorosilane, can solve the problems of difficult repeated recycling, short catalyst life, complex reaction process, etc. Achieve the effect of good product yield, low reaction temperature and simple process

Inactive Publication Date: 2012-08-15
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method has a high product yield and can effectively inhibit the debenzene reaction, it has disadvantages such as complex reaction process, short catalyst life, difficulty in repeated recycling, waste of resources, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 3 Preparation of ionic liquid:

[0027] Under the protection of nitrogen, 3.1 mol of 1-methylimidazole (254.5 g) and 3.35 mol of chlorobutane (350 mL, 310 g) were stirred and mixed in a 1000 mL three-necked flask with a condenser, and the temperature was raised to React at 80 °C for 48 h under reflux. Then the reaction material was cooled to 0 °C for crystallization for 12 h, the remaining unreacted liquid was poured off, washed with ethyl acetate, and the crude product was rotary evaporated under vacuum at 80 °C to remove the residual ethyl acetate, and then crystallized to obtain 1-butyl chloride -3 Methylimidazolium salt milky yellow solid, then vacuum-dried at 70 °C for 24 h, stored in dry N 2 Reserve under atmosphere.

[0028] In a glove box full of dry nitrogen, take 174.6 g of the intermediate prepared above, and add 81.25 g of anhydrous FeCl in batches under stirring. 3 (The molar ratio of intermediate to anhydrous ferric chloride is 1:0.5). This proces...

Embodiment 2

[0038] Same as Example 1, but change [BMIM]Cl and anhydrous FeCl 3 The mol ratio: 1:1, 1:1.5, 1:2, the results are shown in Table 2.

[0039]

[0040] Table 2: Effect of Catalyst Composition on Reaction

[0041] n([BMIM]Cl):n(FeCl 3 ) PhSiCl 3 Conversion rate ClPhSiCl 3 yield Cl 2 PhSiCl 3 yield Cl 3 PhSiCl 3 yield 1:0.5 74.35 % 56.74 % 11.83 % 2.45 % 1:1 81.72 % 60.40 % 13.87 % 5.23 % 1:1.5 86.59 % 60.91 % 17.00 % 7.50 % 1:2 93.17 % 58.16 % 18.35 % 13.71 %

[0042] It can be seen from Table 2 that with [BMIM]Cl- n FeCl 3 FeCl in ionic liquid 3 With the increase of the molar content, the conversion rate of raw material phenyltrichlorosilane and the yield of dichlorophenyltrichlorosilane gradually increased, while the yield of chlorophenyltrichlorosilane had no obvious change. In addition, we also found that [BMIM]Cl- n FeCl 3 FeCl in ionic liquid 3 The increase of the molar content is beneficial to the fo...

Embodiment 3

[0045] Same as Example 1, but changing the reaction temperature to 60°C and 80°C, the results are shown in Table 3.

[0046]

[0047] Table 3 Effect of reaction temperature on reaction

[0048] temperature reflex PhSiCl 3 Conversion rate ClPhSiCl 3 yield Cl 2 PhSiCl 3 yield Cl 3 PhSiCl 3 yield 40 ℃ 74.35 % 56.74 % 11.83 % 2.45 % 60 ℃ 89.1 % 68.90 % 12.37 % 3.20 % 80 ℃ 99.87 % 76.30 % 16.01 % 5.19 %

[0049] As can be seen from Table 3, along with the raising of reaction temperature, the yield of methyltrichlorosilane and the yield of chlorinated product all increase, and product is with monochlorophenyltrichlorosilane, dichlorophenyl Trichlorosilane is the main content, and the content of trichlorophenyltrichlorosilane is extremely small. When the reaction temperature was 80 ℃, the raw material phenyltrichlorosilane basically realized 100% conversion, the yield of chlorophenyltrichlorosilane was 76.30%, the yield of dic...

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PUM

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Abstract

The method relates to a method for preparing polychlorinated phenyl trichlorosilane through catalysis of ionic liquid, and belongs to the technical field of application of the ionic liquid. According to the method, methyl trichlorosilane is catalyzed and chloridized to prepare polychlorinated phenyl trichlorosilane with Cl2 serving as a chlorinating agent, and (BMIM)Cl-nFeCl3 (n=0.5, 1, 1.5 and 2) acidic ionic liquid serving as a catalyst. According to the method, the technology is simple, the reaction condition is mild, the conversion rate of the raw material is high, and the product yield is high. The (BMIM)Cl-nFeCl3 ionic liquid catalyst can be reutilized through simple liquid-liquid separation, and the catalytic activity of the (BMIM)Cl-nFeCl3 ionic liquid catalyst remains unchanged fundamentally. Compared with the conventional catalyst such as FeCl3 and AlCl3, the (BMIM)Cl-nFeCl3 ionic liquid catalyst can effectively inhibit side reaction, namely the breakage of Si-C bond, and thus the product yield can be improved.

Description

technical field [0001] The present invention relates to a kind of synthetic method of polychlorinated phenyltrichlorosilane, especially refers to 2 As a chlorinating agent, [BMIM]Cl- n FeCl 3 (n=0.5, 1, 1.5, 2) The acidic ionic liquid is used as a catalyst, and the method for catalyzing the synthesis of polychlorophenyltrichlorosilane from chlorinated phenyltrichlorosilane belongs to the technical field of ionic liquid application. [0002] technical background [0003] Polychlorophenyltrichlorosilane is a mixture of different degrees of chlorine substitution on the benzene ring of phenyltrichlorosilane, mainly monochlorophenyltrichlorosilane and dichlorophenyltrichlorosilane, and is a colorless Or light yellow oily liquid. Like phenyltrichlorosilane, polychlorinated phenyltrichlorosilane is rich in Si-Cl bonds, so it is easily hydrolyzed in air to produce HCl gas, which is highly corrosive. [0004] Polychlorophenyl trichlorosilane is mainly used to prepare chloropheny...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/14
CPCY02P20/584
Inventor 姜逸倩殷恒波柳艳君颜晓波付玉军
Owner JIANGSU UNIV
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