Method and special device for separating trimethyl borate from carbinol mixture

A technology of trimethyl borate and a special device, which is applied in the field of organic matter preparation, can solve the problems of high sulfuric acid concentration, large plate load, and large sulfuric acid consumption, and achieve low equipment investment, convenient recycling and good results.

Active Publication Date: 2012-12-12
江苏宏梓新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This separation technology has the following disadvantages: 1) Due to the large amount of sulfuric acid used; 2) The concentration of sulfuric acid in the ester

Method used

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  • Method and special device for separating trimethyl borate from carbinol mixture

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The theoretical plate number of the extractive distillation column is 15 (the number of plates is counted from top to bottom), and ethylene glycol containing lithium chloride (the mass fraction of lithium chloride is 15%) is used as the salting solvent. The theoretical plate is added, the flow rate is 20g / min, the mixture of trimethyl borate and methanol is added from the ninth theoretical plate, the mass fraction of trimethyl borate is 75%, the mass fraction of methanol is 25%, and the flow rate is 10g / min. The reflux ratio at the top of the extractive distillation column is 0.2, and the temperature at the top of the column is controlled at 68.5~69.0℃. The product at the top of the column is analyzed. The mass fraction of trimethyl borate is 99.6%, and the mass fraction of methanol is 0.4%. The extractive distillation tower tower kettle discharge is methanol, salt, solvent mixture into the solvent recovery tower, the solvent recovery tower has 10 theoretical trays, th...

Embodiment 2

[0024] The theoretical plate number of the extractive distillation column is 40 (the number of plates is counted from top to bottom), and ethylene glycol containing lithium chloride (the mass fraction of lithium chloride is 8%) is selected as the salting solvent. The theoretical plate is added, the flow rate is 5g / min, the mixture of trimethyl borate and methanol is added from the 24th theoretical plate, the mass fraction of trimethyl borate is 75%, the mass fraction of methanol is 25%, and the flow rate is 10g / min . The reflux ratio at the top of the extractive distillation column is 4, the temperature at the top of the column is controlled at 68.5~69.0℃, and the product at the top of the column is analyzed. The mass fraction of trimethyl borate is 99.5%, and the mass fraction of methanol is 0.5%. The extractive distillation tower reactor discharge is methanol, salt, solvent mixture into the solvent recovery tower, the solvent recovery tower has 30 theoretical trays, the feed...

Embodiment 3

[0026] The theoretical plate number of the extractive distillation column is 25 (the number of plates is counted from top to bottom), and ethylene glycol containing lithium chloride (the mass fraction of lithium chloride is 12%) is selected as the salting solvent. The theoretical plate is added, the flow rate is 10g / min, the mixture of trimethyl borate and methanol is added from the 15th theoretical plate, the mass fraction of trimethyl borate is 75%, the mass fraction of methanol is 25%, and the flow rate is 10g / min . The reflux ratio at the top of the extractive distillation column is 2, the temperature at the top of the column is controlled at 68.5~69.0℃, and the product at the top of the column is analyzed. The mass fraction of trimethyl borate is 99.8%, and the mass fraction of methanol is 0.2%. The extractive distillation tower tower kettle discharge is methanol, salt, solvent mixture into the solvent recovery tower, the solvent recovery tower has 20 theoretical trays, t...

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Abstract

The invention discloses a method and a special device for separating trimethyl borate from a carbinol mixture. The method is a salt-adding extraction and rectification method which comprises the following steps of: charging a salt-containing solvent, trimethyl borate and carbinol mixture from the upper part and middle part of an extraction and rectification tower respectively, carrying out salt-adding extraction and rectification, withdrawing pure trimethyl borate from the top of the tower, and obtaining the mixture of carbinol, salt and solvent at a tower kettle; and charging the mixture of carbinol, salt and solvent into a solvent recovering tower from the middle, wherein the distillate on the top of a recovery tower is the carbinol, obtaining the salt-containing solvent at the tower kettle, and repeatedly charging the salt-containing solvent into the extraction and rectification tower to be used. The method is better in effect due to the salt-adding extractant compared with the extractant, has the advantages of being convenient to recycle and easy to realize on the industry, can be used for overcoming the defect that the sold salt in a salt-adding rectification technology is hard to cycle, can be used for greatly improving the separation effect since the relative volatility of the trimethyl borate and the carbinol is increased, has the advantages of being low in equipment investment and low in energy consumption, and can be used for the industrial application for the separation and purification of the trimethyl borate.

Description

technical field [0001] The invention relates to the technical field of organic matter preparation, in particular to a method for separating a mixture of trimethyl borate and methanol by a salt-adding extractive distillation method and a special device thereof. Background technique [0002] Trimethyl borate was first synthesized in 1846. Since the 1960s, a lot of research on its synthesis methods has been carried out abroad, mainly including the reaction method of boron trichloride and methanol, the direct reaction method of boric acid and methanol, the direct reaction method of boron anhydride and alcohol, and the reaction of borax and alcohol. law, etc. In the above method, since boric acid is relatively cheap, and the product of esterification reaction of boric acid and methanol is easier to separate. Therefore, the direct reaction method of boric acid and methanol is the main method of industrial production. In order to improve the conversion rate of boric acid, batch ...

Claims

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Application Information

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IPC IPC(8): C07F5/04C07C31/04C07C29/84C07C29/80
Inventor 钱烽钱兵荣
Owner 江苏宏梓新能源科技有限公司
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