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Method for semi-continuously synthesizing trimethyl borate-methanol azeotrope

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

Active Publication Date: 2020-06-05
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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  • Method for semi-continuously synthesizing 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

The invention discloses a method for semi-continuously synthesizing trimethyl borate-methanol azeotrope. The method comprises the following steps: mixing and heating boric acid and a transforming agent in a premixing tank, introducing a mixture into a stirred and heated reaction kettle, condensing gas generated in the reaction kettle, and separating; flowing a product into a mixing tank from the reaction kettle to be mixed with methanol, introducing the mixed material into a first rectifying tower, and obtaining the trimethyl borate-methanol azeotrope after tower top gas of the first rectifying tower is condensed; introducing bottom products of the first rectifying tower into a second rectifying tower; condensing tower top gas of the second rectifying tower to obtain methanol, recycling the methanol, and cooling and recycling a bottom product of the second rectifying tower. The molecular formula of the transforming agent is CxH2x+2+zOyNz, O exists in the form of hydroxyl, x is a natural number ranging from 2 to 8, y is a natural number ranging from 1 to 3, and z is a natural number not larger than 1. The method solves the problem that water generated in a traditional trimethyl borate preparation process is not easy to discharge, and digitization and automation of the process are easy to realize.

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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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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