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A kind of preparation method of large particle pentaerythritol co-production potassium formate

A technology of pentaerythritol and large particles, which is applied in the field of preparation of large particle pentaerythritol co-production potassium formate, can solve the problems of product purity affecting filtration performance, different crystal particle sizes, uncontrolled cooling rate, etc., and achieve regular crystal shape, uniform distribution, The effect of low equipment requirements

Active Publication Date: 2021-11-19
武汉中能恒信工程技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the cooling and crystallization process of pentaerythritol in industry adopts simple natural cooling method, and the cooling rate is uncontrolled. The crystallization products have different crystal particle sizes and irregular shapes, which directly affect the filtration performance and product purity.

Method used

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  • A kind of preparation method of large particle pentaerythritol co-production potassium formate

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preparation example Construction

[0023] Such as figure 1 As shown, the present invention provides a kind of preparation method of large particle pentaerythritol co-production potassium formate, comprises the following steps: step 1, industrial formaldehyde solution is diluted to certain concentration, and the potassium hydroxide solution of certain concentration and acetaldehyde solution are proportional Slowly add to the formaldehyde solution to react, and keep the low temperature reaction; step 2, the solution obtained after the low temperature reaction in step 1, after raising the reaction temperature, to obtain a condensation liquid, add an appropriate amount of formic acid solution dropwise to the condensation liquid, adjust Solution pH value; Step 3, the solution obtained after adjusting the pH value in Step 2 is subjected to vacuum distillation to remove a part of solvent; Step 4, The first mother liquor obtained in Step 3 is crystallized by cooling and filtered to obtain the second mother liquor, and t...

Embodiment 1

[0037] A. Take 118.0511g of 34.00% formaldehyde solution, add water to make 160g / L solution;

[0038] B. Weigh 13.0502g of potassium hydroxide solid, add water to make 160g / L solution, take 10.1512g of acetaldehyde solution (the mass content of acetaldehyde is 99%) at the same time, add the two slowly to the solution obtained in step A, and keep the reaction temperature during The temperature is 10-15°C, and the dropwise reaction time is 1h; the molar ratio of formaldehyde: acetaldehyde: potassium hydroxide = 4:1:1.3 is added in proportion.

[0039] C. After the dropwise addition, raise the reaction temperature to 35° C., and the reaction time is 1 h. After the reaction, use formic acid to adjust the pH value of the solution to 6;

[0040] D. Distill the solution obtained in step C under reduced pressure, the vacuum degree is 0.09Mpa, the distillation temperature is 80°C to 90°C, and 80% of the liquid is controlled to evaporate, and the obtained mother liquor is crystallized ...

Embodiment 2

[0043] A. Take 118.0511g of 36.00% formaldehyde solution, add water to make 170g / L solution;

[0044] B. Weigh 13.0502g potassium hydroxide solid, add water and be mixed with 160g / L solution, get 10.1512 acetaldehyde solution (acetaldehyde content is 99%) simultaneously, both slowly add in the solution that A step obtains. During the period, keep the reaction temperature at 20-25°C, and the dropwise reaction time is 1h; add the molar ratio formaldehyde: acetaldehyde: potassium hydroxide = 4.1:1:1.15 in proportion;

[0045] C. After the dropwise addition, raise the reaction temperature to 38°C, and the reaction time is 1.2h. After the reaction, use formic acid to adjust the pH of the solution to a range of 6.25.

[0046] D. The solution obtained in step C is subjected to vacuum distillation, the vacuum degree is 0.095Mpa, the distillation temperature is 80°C to 90°C, and 82.5% of the liquid is controlled to evaporate, and the obtained mother liquor is cooled and crystallized a...

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Abstract

The invention provides a method for preparing large-particle pentaerythritol co-production potassium formate. The industrial formaldehyde solution is diluted, potassium hydroxide solution and acetaldehyde solution are added to the formaldehyde solution in proportion to react, and the reaction process is kept at low temperature; all reactants are added , increase the reaction temperature, and react by adding formic acid solution dropwise to the condensation liquid to adjust the pH value of the solution; the resulting solution is distilled under reduced pressure to produce pentaerythritol crystals, and the solvent and by-products are removed; the mother liquor is controlled to cool and crystallize, filter, and the filtrate is washed and dried to obtain large Granular pentaerythritol product, after filtration, the mother liquor is evaporated and crystallized, filtered, washed and dried to obtain potassium formate powder. The present invention uses potassium hydroxide or alkaline potassium salt as an alkali source to produce pentaerythritol through two-step variable temperature reaction crystallization, the production process is stable, and the by-product potassium formate has higher added value; the yield of pentaerythritol produced is over 96%, and the obtained The purity of pentaerythritol is close to 98%; the technological process is simple, the equipment requirement is low, and the operation is safe.

Description

technical field [0001] The invention relates to the field of preparation of fine chemicals in the chemical industry, in particular to a method for preparing large-particle pentaerythritol co-production potassium formate. Background technique [0002] Most of the pentaerythritol currently on the market is prepared by Cannizzaro condensation of formaldehyde and acetaldehyde under alkaline conditions. According to the different alkaline solutions used in the production process, it can be divided into sodium method and calcium method. The "calcium method" using calcium hydroxide as a basic catalyst and the "sodium method" using sodium hydroxide as a basic catalyst have relatively mature production technologies in China. There are more than 30 production enterprises, with an installation capacity of 1000-10000t / a and a total production capacity of 75500t / a. The raw material cost of the calcium method is low, but the post-treatment must add precipitation and filtration steps to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/38C07C29/78C07C31/24C07C51/41C07C53/06
CPCC07C29/38C07C29/78C07C51/412C07C31/245C07C53/06C07C31/24
Inventor 邓宏卫刘毅於佳龙秉文王声光刘祎
Owner 武汉中能恒信工程技术有限公司
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