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The synthetic method of stannous chloride

A synthesis method and technology of stannous chloride, applied in stannous chloride, tin halide and other directions, can solve the problems of large amount of sewage, leakage of toxic and harmful gases such as chlorine gas, and high cost, and achieve the effect of reliable process

Active Publication Date: 2019-12-13
LIANYUNGANG JINDUN AGROCHEMICAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the present invention is to solve the problems such as waste of resources, high cost, large amount of sewage, difficulty in recycling tin-containing slag, leakage of toxic and harmful gases such as chlorine gas, etc. existing in the existing stannous chloride synthesis method, and provide a kind of stannous chloride resolve resolution

Method used

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  • The synthetic method of stannous chloride
  • The synthetic method of stannous chloride

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Experimental program
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Effect test

Embodiment 1

[0022] 1.97Kg of deionized water, 1.26Kg of 20wt.% hydrochloric acid, 0.77Kg of anhydrous tin tetrachloride and 50g of 1% ruthenium carbon catalyst were added to the reactor in sequence, the system was heated up to 110°C, 1.5MPa hydrogen gas was introduced, and 125°C Insulation reaction for 2 hours, after the reaction is completed, filter out the metal solid impurities; utilize the atmospheric pressure evaporation method to concentrate the formed tin protochloride solution until the temperature of the concentrated solution reaches 136 ° C, then pour out the concentrated solution and crystallize at room temperature; The obtained crystals were filtered under reduced pressure, and the filter cake was dried under vacuum at 80° C. with a vacuum degree of -0.05 MPa and a drying temperature of 50° C. for 12 hours to obtain white stannous chloride crystals with a content of 99.15%.

Embodiment 2

[0024] Add 1.97Kg of deionized water, 1.26Kg of 20wt.% hydrochloric acid, 0.77Kg of anhydrous tin tetrachloride and 50g of 1% rhodium carbon catalyst into the reactor in turn, raise the temperature of the system to 120°C, feed 3MPa hydrogen, and keep it warm at 130°C React for 6 hours, after the reaction is completed, filter out the metal solid impurities; utilize the atmospheric pressure evaporation method to concentrate the stannous chloride solution formed until the temperature of the concentrated solution reaches 136 ° C, then pour out the concentrated solution and crystallize at room temperature; The crystals were filtered under reduced pressure, the filter cake was dried at 80°C, the vacuum degree was -0.1MPa, the drying temperature was 90°C, and vacuum dried for 12 hours, and the white crystals of stannous chloride with a content of 99.33% were obtained.

Embodiment 3

[0026] Add 1.97Kg of deionized water, 1.26Kg of 20wt.% hydrochloric acid, 0.77Kg of anhydrous tin tetrachloride and 50g of 1% platinum-carbon catalyst into the reactor in sequence, raise the temperature of the system to 130°C, and feed 1.5MPa hydrogen gas into the reactor at 135°C Insulation reaction for 2 hours, after the reaction is completed, filter out the metal solid impurities; utilize the atmospheric pressure evaporation method to concentrate the formed tin protochloride solution until the temperature of the concentrated solution reaches 136 ° C, then pour out the concentrated solution and crystallize at room temperature; The obtained crystals were filtered under reduced pressure, and the filter cake was dried under vacuum at 80° C. with a vacuum degree of -0.05 MPa and a drying temperature of 50° C. for 12 hours to obtain white stannous chloride crystals with a content of 99.5%.

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Abstract

The invention discloses a synthetic method of stannous chloride. The method comprises the following steps: by using anhydrous stannic tetrachloride and hydrochloric acid with concentration of 20 wt% as raw materials, adding a precious metal catalyst, heating to 110 to 140 DEG C, introducing hydrogen with the pressure intensity of 1.5 to 3MPa, performing heat insulation reaction for 2 to 6 hours at125 to 135 DEG C, and performing press filtration to obtain a stannous chloride solution and a dilute hydrochloric acid solution with required concentrations; then performing concentration and crystallization to obtain a stannous chloride crystal. According to the synthetic method of stannous chloride disclosed by the invention, by using hydrogen as a reducing agent, a catalyst can be reacted andrecycled for being reused, and the phenomenon that tin is used as the reducing agent in a conventional process is avoided, so that the interference of impurity elements carried by metal tin on the quality of a product is effectively eliminated. The method disclosed by the invention has the advantages of stable process, strong operability, low cost, environment-friendly property, high security andthe like, and can be applied to industrial popularization.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis method of stannous chloride. Background technique [0002] At present, the synthetic process route of oxadiazone suitable for industrialization mainly uses 2,4-dichlorophenol as raw material, through esterification, nitration, hydrolysis, etherification, reduction, diazotization, secondary reduction, alkalization, hydrazide Chemical, photochemical, and cyclization, a total of 11 steps of reaction to obtain oxadiazone. Among them, the diazotization and secondary reduction equations are as follows: [0003] [0004] In this step reaction, 2,4-dichloro-5-isopropoxyaniline is used as raw material to generate 2,4-dichloro-5-isopropoxyaniline diazonium salt through one reduction, and then use Tin acts as a secondary reducing agent to directly generate 2,4-dichloro-5-isopropoxyphenylhydrazine hydrochloride. This step reaction is except generating...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/06
CPCC01G19/06C01P2006/80
Inventor 杨建孙建祝曹现朝石卫兵孙益群
Owner LIANYUNGANG JINDUN AGROCHEMICAL CO LTD
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