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A kind of semi-continuous synthesis method of trimethyl borate-methanol azeotrope

A trimethyl borate, semi-continuous technology, applied in the chemical industry, can solve the problems of low conversion rate, difficult to discharge water, etc., and achieve the effect of stable product quality

Active Publication Date: 2021-05-18
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The present invention aims at the problem of low conversion rate caused by the accumulation of water in the reaction system existing in the existing industrial production of trimethyl borate technology, and proposes a method for semi-continuous production of trimethyl borate-methanol azeotrope
The invention solves the problem that the water in the reaction system is difficult to discharge in the traditional process, and realizes the efficient conversion of raw materials

Method used

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  • A kind of semi-continuous synthesis method of trimethyl borate-methanol azeotrope

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Butanol (C 4 h 10 0) Extracted by the first storage tank 1 through the feed pump 2, the first valve 3 is opened, the second valve 4 is closed, n-butanol is introduced into the first premix tank 5 with a volume of 25L, and the After adding 15L of n-butanol in 5, close the first valve 3, start stirring, add 1.67kg boric acid to the first premix tank 5 at the same time, stir and heat to 85°C, stir and keep warm for 0.5h, open the bottom valve and pass through the first inlet The feed pump 7 continuously imports the mixed solution into the continuous stirring and heating reactor 8 (volume is 30L), and the control flow rate is 15L / h; after opening the valve at the bottom of the first premixing tank 5, open the second valve 4, and the positive Butanol is introduced into the second premixing tank 6 for a new round of boric acid and n-butanol mixing process; the temperature of the mixed solution rises to 130°C after entering the reactor 8, and the generated gas enters the firs...

Embodiment 2

[0025] Triethanolamine (C 6 h 15 NO 3) is extracted from the first storage tank 1 through the feed pump 2, the first valve 3 is opened, the second valve 4 is closed, and triethanolamine is introduced into the first premix tank 5 with a volume of 25L, and the first premix tank 5 is added After 15L of triethanolamine, close the first valve 3 and start stirring. At the same time, add 3.5kg of boric acid to the first premix tank 5, stir and heat to 90°C, stir and keep warm for 1 hour, open the bottom valve and pass the first feed pump 7 to mix The liquid is continuously introduced into the continuously stirring and heated reactor 8 (volume is 30L), and the control flow rate is 5L / h; after opening the valve at the bottom of the first premixing tank 5, open the second valve 4, and triethanolamine is imported into the second premixing tank. A new round of boric acid and triethanolamine mixing process is carried out in the mixing tank 6; the temperature of the mixed solution rises t...

Embodiment 3

[0027] ethanolamine (C 2 h 7 NO) is extracted from the first storage tank 1 through the feed pump 2, the first valve 3 is opened, the second valve 4 is closed, the ethanolamine is introduced into the first premix tank 5 with a volume of 25 L, and the first premix tank 5 is added After 15L of ethanolamine, close the first valve 3, start stirring, and add 4.2kg of boric acid to the first premix tank 5 at the same time, stir and heat to 90°C, stir and keep warm for 1 hour, open the bottom valve and pass the mixed solution through the first feed pump 7 Continuously import in the reactor 8 (capacity is 30L) of continuous stirring and heating, control flow rate is 10L / h; After opening the valve at the bottom of the first premix tank 5, open the second valve 4, ethanolamine is imported into the second premix tank In 6, a new round of boric acid and ethanolamine mixing process is carried out; after the mixed solution enters the reaction kettle 8, the temperature rises to 180°C, and t...

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Abstract

A method for semi-continuously synthesizing trimethyl borate-methanol azeotrope. After the boric acid and conversion agent are mixed and heated in the premixing tank, the mixture is introduced into the stirred and heated reactor, and the gas generated in the reactor is condensed and separated; the product flows from the reactor into the mixing tank and mixed with methanol, and the mixed material is introduced into the second A rectifying tower, the first rectifying tower overhead gas is condensed to obtain trimethyl borate-methanol azeotrope. The bottom product of the first rectification tower is introduced into the second rectification tower; the gas at the top of the second rectification tower is condensed to obtain methanol, the methanol is recycled and reused, and the bottom product of the second rectification tower is cooled and recycled for reuse. The molecular formula of the transforming agent is C x h 2x+2+z o y N z , O exists in the form of hydroxyl, x is a natural number between 2 and 8, y is a natural number between 1 and 3, and z is a natural number not greater than 1. This method solves the problem that the water generated in the traditional trimethyl borate preparation process is not easy to discharge, and is easy to realize the digitization and automation of the process.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to a method for semi-continuously synthesizing trimethyl borate-methanol azeotrope. Background technique [0002] Trimethyl borate is an important organoboride, which can be used as organic solvent, dehydrating agent, plasticizer, catalyst and additive for lithium battery electrolyte, and can also be used for the synthesis of sodium borohydride, high-purity boron for photoelectricity and nuclear power Use high-purity boric acid and other high-end boron-containing fine chemicals as raw materials. [0003] The production method of trimethyl borate is mainly: react boron-containing inorganic substances (boric anhydride, metaboric acid, pyroboric acid, boric acid, etc.) with methanol to obtain trimethyl borate-methanol azeotrope, and then add The extractant is subjected to extractive distillation to obtain trimethyl borate. Such as: [0004] CN102002064A discloses a preparatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/04
CPCC07F5/04
Inventor 宁桂玲李长伟田朋林源
Owner DALIAN UNIV OF TECH
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