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Preparation method of trimethyl borate

A technology of trimethyl borate and boric acid, which is applied in the field of preparation of trimethyl borate, can solve the problems of long preparation period and low purity of trimethyl borate, and achieves the improvement of single-pass conversion rate, high separation efficiency and low energy consumption. Effect

Inactive Publication Date: 2020-03-06
NINGXIA BEST PHARMA CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the technical problem to be solved by the present invention, the preparation period of trimethyl borate is long, and the defect of low purity provides a kind of preparation method thereof

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A preparation method for trimethyl borate, comprising the following steps:

[0016] 1), first heat and dehydrate the boric acid solids to obtain metaboric acid and pyroboric acid solids, then add methanol and hydrogen chloride to react for 20 minutes to obtain trimethyl borate, the molar ratio of methanol, hydrogen chloride and boric acid is 8:4:1;

[0017] 2), heating and distilling the obtained reaction solution, in the presence of sulfuric acid, the molar ratio of trimethyl borate to sulfuric acid is 1:1, methanol and trimethyl borate form an azeotrope, and the distillation raffinate is cooled to obtain boric acid;

[0018] 3) Put the azeotropic liquid into the azeotropic distillation column, add N,N-dimethylacetamide for extractive distillation, heat up the temperature of the azeotropic distillation column to 80°C for rectification, and control the reflux ratio to 9 : 1; the quality of N,N-dimethylacetamide is 20-25% of the azeotropic liquid, and the anhydrous metha...

Embodiment 2

[0020] A preparation method for trimethyl borate, comprising the following steps:

[0021] 1), first heat and dehydrate the boric acid solids to obtain metaboric acid and pyroboric acid solids, then add methanol and hydrogen chloride to react for 20-30 minutes to obtain trimethyl borate, the molar ratio of methanol, hydrogen chloride and boric acid is 9:4: 1;

[0022] 2), heating and distilling the obtained reaction solution, in the presence of sulfuric acid, the molar ratio of trimethyl borate to sulfuric acid is 1:4, methanol and trimethyl borate form an azeotrope, and the distillation raffinate is cooled to obtain boric acid;

[0023] 3) Put the azeotropic liquid into the azeotropic rectification tower, add N,N-dimethylacetamide for extractive rectification, heat up the temperature of the azeotropic rectification tower to 90°C for rectification, and control the reflux ratio to 10 : 1; the quality of N,N-dimethylacetamide is 20-25% of the azeotropic liquid, and the anhydrou...

Embodiment 3

[0025] A preparation method for trimethyl borate, comprising the following steps:

[0026] 1), first heat and dehydrate the boric acid solids to obtain metaboric acid and pyroboric acid solids, then add methanol and hydrogen chloride to react for 20-30 minutes to obtain trimethyl borate, the molar ratio of methanol, hydrogen chloride and boric acid is 9:4: 1;

[0027] 2), the obtained reaction solution is heated and distilled. In the presence of sulfuric acid, the molar ratio of trimethyl borate to sulfuric acid is 1:3, methanol and trimethyl borate form an azeotrope, and the distillation raffinate is cooled to obtain boric acid;

[0028] 3) Put the azeotropic liquid into the azeotropic rectification tower, add N,N-dimethylacetamide for extractive rectification, heat up the temperature of the azeotropic rectification tower to 86°C for rectification, and control the reflux ratio to 9.5 : 1; the quality of N,N-dimethylacetamide is 20-25% of the azeotropic liquid, and the anhydr...

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PUM

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Abstract

The invention discloses a preparation method of trimethyl borate. The preparation method of the trimethyl borate comprises the following steps: 1) preparing metaboric acid and pyroboric acid solids byusing boric acid solution, and adding methanol and hydrogen chloride into the metaboric acid and pyroboric acid solids so as to be subjected to reaction, thereby obtaining a reaction solution of trimethyl borate; 2) heating the reaction solution so as to be subjected to heated distillation, thereby forming an azeotrope by the methanol and the trimethyl borate in the presence of sulfuric acid, performing distillation on residual liquid, and cooling the distilled liquid so as to obtain boric acid; and 3) introducing the azeotrope into an azeotropic rectification column, adding N,N-dimethylacetamide so as to be subjected to extractive distillation, cooling anhydrous methanol at the bottom of the azeotropic rectification column for reuse, and collecting trimethyl borate at the top of the azeotropic rectification column. According to the preparation method of the trimethyl borate, the metaboric acid and the pyroboric acid are prepared by performing heated dehydration on the boric acid; andthen, the metaboric acid and the pyroboric acid react with the methanol so as to produce the trimethyl borate. In addition, the catalysts, namely the hydrogen chloride and the sulfuric acid, are sequentially added, so that the reaction time is 1.2-1.5 hours; and moreover, the rectification conditions are strictly controlled, so that a product purity up to 98.5% can be achieved. Therefore, the preparation method of the trimethyl borate has very good industrialization prospects.

Description

technical field [0001] The invention relates to the technical field of preparation of organic borates, in particular to a preparation method of trimethyl borate. Background technique [0002] Trimethyl borate is widely used as a solvent, dehydrating agent, plastic, paint, spray paint, etc. The preparation method of present trimethyl borate generally adopts the reaction preparation of boric acid and methanol, the existence of water is arranged in the product obtained by this method, brings certain difficulty with the separation and purification of product, so the product prepared by conventional method, obtains The yield is not high, the purity is not enough, the preparation cycle is long, and the use requirements cannot be fully met. Contents of the invention [0003] Among the technical problems to be solved by the present invention, the preparation cycle of trimethyl borate is long and the defect of low purity is provided, and a preparation method thereof is provided. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/04
CPCC07F5/04
Inventor 郑志浩杨彬张顺利
Owner NINGXIA BEST PHARMA CHEM CO LTD
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