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Process for the preparation of hydrocarbyl halides

A technology of halides and metal halides, which is applied in chemical instruments and methods, tin organic compounds, compounds of group 4/14 elements of the periodic table, etc., can solve the problems of lower economic benefits, expensive, bulky and difficult to use, and achieve Fast and safe operation, low cost and good yield effect

Inactive Publication Date: 2007-09-26
BAERLOCHER ITAL SPA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, such equipment is expensive and often cumbersome, which reduces the economics of the described methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Tributylamine (63.6 g, 0.34 mol) was placed in a 500 ml round bottom flask with stirrer, thermometer well and condenser on top. Tin tetrachloride (89.7 g, 0.34 mol) was slowly added with stirring over 1 hour. The reaction temperature increased from 29°C to 65°C. After the addition was complete, the reaction mass was heated to 100°C with stirring and then cooled to room temperature.

[0051] Preparation of dimethyl tin dichloride

Embodiment 2

[0053]The catalyst prepared above (145 g) was placed in a 1 liter stainless steel autoclave, and then tin pellets (200 g, 1.68 gm-atom (mol)) were added. The autoclave was filled with nitrogen to expel the air and release the nitrogen to the air. Connect a cylinder of methyl chloride to the reaction vessel. Maintain the temperature of the cylinder by placing it in a hot water bath. The catalyst and tin mixture was heated to 185°C with stirring and methyl chloride was introduced until the pressure reached 120 psi. The immediate onset of the reaction was observed by the pressure drop in the reaction vessel. When the pressure dropped to 100 psi, methyl chloride was reintroduced until the pressure reached 120 psi. This step was continued until no pressure drop was observed, indicating completion of the reaction (330 min). After cooling the reaction to about 85°C, the excess methyl chloride was slowly vented off. Fill with nitrogen and vent excess. This ensures that when the ...

Embodiment 3～10

[0055] The steps of Example 2 were repeated using different catalysts, and the preparation of the catalyst was as described in Example 1. When using a complex between phosphine and tin tetrachloride, the amine is replaced by phosphine, all other reaction conditions are similar. The results are shown in Table 1.

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PUM

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Abstract

Described is a process for the preparation of hydrocarbyl metal halides, such as alkyl tin chlorides, in which a reaction between the metal in its metallic state and a hydrocarbyl halide is catalyzed by a dihydrocarbyl sulfoxide or a dihydrocarbyl formamide in the presence of a hydrocarbyl metal halide and wherein the pressure of the reaction vessel is varied during the reaction.

Description

technical field [0001] The present invention relates to a process for the preparation of hydrocarbyl halides such as alkyl tin chlorides (alkyltin chlorides), wherein metal in metallic state and hydrocarbyl halides (halogenated hydrocarbons) are formed by reacting the hydrocarbyl halides with dihydrocarbyl sulfoxides. The reaction is carried out under the catalysis of the complex formed between or dihydrocarbyl formamides, and wherein the pressure of the reaction vessel is changed during the reaction. Background technique [0002] Hydrocarbon-substituted tin halides (tin halides) such as methyl tin chloride are very useful in the preparation of stabilizers for polymers, especially for halogenated polymers such as polyvinyl chloride resins, chlorinated paraffins, etc. . Various methods for preparing hydrocarbyl tin chlorides have been proposed. So far there is no completely satisfactory method. [0003] US 3,901,821 A1 describes a process for the preparation of dimethyltin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/22
CPCC07F7/2216C07F7/2208
Inventor 安德烈亚·科米尼加内什·瓦拉德卡尔·马尤其帕德马卡尔·戈卡莱·阿纳德尚蒂拉尔·卡斯利瓦·拉金德拉阿尼尔·本达尔·吉塔
Owner BAERLOCHER ITAL SPA