Method for preparing oxidative methyl tin

A technology of methyl tin oxide and tin tetrachloride, which is applied in the direction of tin organic compounds, can solve the problems of incomplete reaction, high reactivity, and low utilization rate of tin raw materials, so as to reduce reaction time, increase contact area, and improve Effect of Reaction Utilization

Active Publication Date: 2012-01-04
HANGZHOU SHENGCHUANG IND
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Problems solved by technology

[0002] In the prior art, the Grignard reagent method is generally used to prepare methyl tin oxide. Due to the high reactivity of the Grignard reagent and the lack of targetness, the utilization rate of the tin raw material is low, the entire reaction is incomplete, and raw materials are wasted. At the same time, harmful substances participating in the reaction Chloromethane is not properly recycled, and the toxic substance trimethyltin oxide formed due to side reactions during the reaction process has a high content, which not only affects the product quality, but also pollutes the environment

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  • Method for preparing oxidative methyl tin

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[0015] The method for preparing methyl tin oxide provided by the present invention uses metal tin, methyl chloride, tin tetrachloride and ammonia water as raw materials, including: a, alkane halogenation reaction of tin; b, stable reaction of the first mixed intermediate; c, The distillation preparation of the second mixed intermediate; d, the oxidation reaction of the third mixed intermediate.

[0016] a. Alkyl halogenation reaction of tin

[0017] The alkane halogenation reaction of tin can be represented by the following chemical equation:

[0018]

[0019] There are often some side reactions in the alkane halogenation reaction of tin, mainly including:

[0020] (CH 3 ) 2 SnCl 2 +Sn+2CH 3 Cl→(CH 3 ) 3 SnCl+SnCl 2

[0021] b, the stable reaction of the first mixed intermediate

[0022] The stabilization reaction can be represented by the following chemical equation:

[0023] (CH 3 ) 3 SnCl+SnCl 4 →(CH 3 ) 2 SnCl 2 +CH 3 SnCl 3

[0024] d, the oxidation...

Embodiment 1

[0029] a. Alkyl halogenation reaction of tin

[0030] Carry out under 130 ℃ and 0.2Mpa condition, reaction time is 1.5h and makes the first mixed intermediate, the catalyzer of this reaction is trimethylamine, and the mass ratio of charging of metal tin, methyl chloride and tin tetrachloride is 50: 40: 10. The dosage of catalyst is 1% of the mass of tin metal.

[0031] Mix metal tin and trimethylamine in advance, and heat it to melt, and then mix the mixture with methyl chloride and tin tetrachloride in the form of mist, which greatly increases the contact area between tin and methyl chloride, and makes the reaction as possible as possible. The formation of dimethyl tin dichloride greatly reduces the formation of trimethyl tin chloride, also improves the reaction utilization rate of tin and methyl chloride, reduces the reaction time, and wherein the utilization rate of tin reaches more than 99%, without The methyl chloride of reaction is reclaimed again, can be used for next ...

Embodiment 2

[0045] a. Alkyl halogenation reaction of tin

[0046] Carried out under the conditions of 140°C and 0.3Mpa, the reaction time is 2h to obtain the first mixed intermediate, the catalyst for this reaction is trimethylamine, and the mass ratio of metal tin, methyl chloride and tin tetrachloride is 40:40:10 , The feed amount of the catalyst is one percent of the mass of tin metal.

[0047] Mix metal tin and trimethylamine in advance, and heat it to melt, and then mix the mixture with methyl chloride and tin tetrachloride in the form of mist, which greatly increases the contact area between tin and methyl chloride, and makes the reaction as possible as possible. The formation of dimethyl tin dichloride greatly reduces the formation of trimethyl tin chloride, also improves the reaction utilization rate of tin and methyl chloride, reduces the reaction time, and wherein the utilization rate of tin reaches more than 99%, without The reacted methyl chloride is reclaimed and can be used...

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Abstract

The invention discloses a method for preparing oxidative methyl tin, taking metallic tin, methyl chloride, stannic chloride and ammonia water as raw materials. The method sequentially comprises: a. under the conditions of 130-150 DEG C and 0.2-0.5MPa, the metallic tin, the methyl chloride and the stannic chloride are mixed together to react for 1.5-3h, so that first mixed intermediate is prepared; b. the obtained first mixed intermediate is compressed into a distillation kettle and added with the stannic chloride to react, so that second mixed intermediate is prepared, and the reaction conditions comprise the temperature is 150-180 DEG C, the pressure intensity is 0.1-0.5MPa, and the reaction time is 0.5-1h; c. reduced pressure distillation and purification are carried out on the second mixed intermediate, and third mixed intermediate is obtained under the conditions that the distillation temperature is 152-158 DEG C and the distillation pressure intensity is 1.0MPa; d. the third mixed intermediate has oxidation reaction at the temperature of 40-50 DEG C with the PH value of 8-8.5; after the reaction is carried out for two hours, the product is washed and processed by vacuum distillation and dehydration, so that the oxidative methyl tin can be obtained. The method has the advantages of environmental protection, high efficiency and high quality.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and relates to a preparation process of methyl tin oxide, in particular to a preparation process of methyl tin oxide composed of dimethyl tin oxide and monomethyl tin oxide. Background technique [0002] In the prior art, the Grignard reagent method is generally used to prepare methyl tin oxide. Due to the high reactivity of the Grignard reagent and the lack of targetness, the utilization rate of the tin raw material is low, the entire reaction is incomplete, and raw materials are wasted. At the same time, harmful substances participating in the reaction Chloromethane is not properly recycled, and the toxic substance trimethyltin oxide formed due to side reactions during the reaction process has a relatively high content, which not only affects product quality, but also pollutes the environment. Contents of the invention [0003] The technical problem to be solved by the present inven...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/22
Inventor 宣依富余成
Owner HANGZHOU SHENGCHUANG IND
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