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A kind of preparation method of glyoxylic acid monohydrate crystal

A technology of glyoxylic acid monohydrate and crystallization, which is applied in the field of glyoxylic acid, can solve the problems of low purity of glyoxylic acid crystals, low yield of glyoxylic acid products, and no production and application value, etc., to achieve a strong Market competitiveness, convenient operation and control, and good herbicidal effect

Active Publication Date: 2018-07-03
WUHAN UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity of glyoxylic acid crystals obtained by crystallization is not high, and the color is difficult to reach white. Only one crystallization is performed, and the yield of glyoxylic acid products is not high, which does not have practical production and application value.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A preparation method of glyoxylic acid monohydrate crystals. The concrete steps of described preparation method are:

[0024] Step 1. Heat the crude glyoxylic acid to 50-60°C, put in a precipitant, the molar ratio of the precipitant to the oxalic acid in the crude glyoxylic acid is 1-2:1, stir for 1-2 hours, and cool down naturally to At room temperature, filter with suction to obtain filtrate Ⅰ. Under the condition of 50-60°C, add activated carbon to the filtrate I, the activated carbon is 1-3 wt% of the filtrate I, stir for 2-3 hours, cool down to normal temperature naturally, and suction filter to obtain filtrate II.

[0025] Step 2: Concentrate the filtrate II under reduced pressure at 50-55°C until the concentration of glyoxylic acid is 55-59 wt%, to obtain crystallization mother liquor.

[0026] Step 3. Transfer the crystallization mother liquor into a jacketed crystallization kettle, and under stirring conditions, lower the crystallization mother liquor in the ...

Embodiment 2

[0035] A preparation method of glyoxylic acid monohydrate crystals. Except following parameter, all the other are with embodiment 1:

[0036] In this embodiment: the precipitation agent is zirconium carbonate; the drying atmosphere is a nitrogen atmosphere.

[0037] The total yield of the present embodiment is 85.81~86.9%, the purity is 98.25~99.55% and the appearance is all white: the yield, purity and appearance of the glyoxylic acid monohydrate crystals obtained by the three crystallizations are as shown in Table 2 stated;

[0038] Table 2

[0039] product name

Embodiment 3

[0041] A preparation method of glyoxylic acid monohydrate crystals. Except following parameter, all the other are with embodiment 1:

[0042] In this embodiment: the precipitation agent is zinc oxide; the drying atmosphere is an oxygen atmosphere.

[0043] The total yield of the present embodiment is 85.21~87.01%, the purity is 98.19~99.65% and the appearance is all white: the yield, purity and appearance of the glyoxylic acid monohydrate crystals obtained by the three crystallizations are shown in Table 3 stated;

[0044] table 3

[0045] product name

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Abstract

The invention relates to a preparation method of glyoxalic acid monohydrate crystals. The technical scheme is as follows: the method comprises the following steps: heating a glyoxalic acid crude product, adding a precipitant, stirring, cooling, and carrying out vacuum filtration to obtain a filtrate I; adding activated carbon into the filtrate I, cooling, and carrying out vacuum filtration to obtain a filtrate II; concentrating the filtrate II under reduced pressure until the glyoxalic acid concentration is 55-67 wt%, thereby obtaining a crystallizing mother solution; transferring the crystallizing mother solution into a jacket crystallizing kettle, cooling, adding glyoxalic acid monohydrate crystals, keeping the temperature, cooling to -5 to 10 DEG C, and keeping the temperature to obtain a crystalline liquid; filtering the crystalline liquid to obtain a filtrate III and a filter cake; carrying out vacuum drying on the filter cake to obtain the glyoxalic acid monohydrate crystal crystals; treating the filtrate III by the process for treating the filtrate II to obtain a filtrate IV and glyoxalic acid monohydrate crystals; and treating the filtrate IV by the process for treating the filtrate II, thereby obtaining a filtrate V and the glyoxalic acid monohydrate crystals. The method is simple in technique, convenient to operate and suitable for industrial production. The prepared glyoxalic acid monohydrate crystals have the advantages of high purity and high yield.

Description

technical field [0001] The invention belongs to the technical field of glyoxylic acid. Specifically relates to a preparation method of glyoxylic acid monohydrate crystals. Background technique [0002] Glyoxalic acid (CHOCOOH) is the simplest aldehyde acid, which has both aldehyde and carboxylic acid functional groups and corresponding chemical properties. It is an important fine chemical raw material and is widely used in spices, medicine, paper industry, leather, In the fields of coloring, plastics, pesticides, coatings, food additives, biochemistry, organic and spectroscopy, preparations such as vanillin, ethyl vanillin, jasmonal, allantoin, hydroxyphenylglycine, p-hydroxyphenylacetic acid, Chemical products such as acetophenone, 2-hydroxyquinoxaline, mandelic acid and hydroxyphosphine carboxylic acid. With the continuous development and expansion of downstream products of glyoxylic acid, the demand for glyoxylic acid is growing rapidly. [0003] Glyoxylic acid current...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/43C07C51/50C07C59/153
CPCC07C51/43C07C51/50C07C59/153
Inventor 叶龙邓支华宋磊鲍应元杨飞周拥军
Owner WUHAN UNIV OF SCI & TECH
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