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Treatment method of crystallization mother liquor in adipic acid crystallization refining process

A processing method and technology for crystallization mother liquor, which can be used in organic chemistry methods, separation/purification of carboxylic acid compounds, organic chemistry, etc., and can solve problems such as difficulty in processing crystallization mother liquor

Pending Publication Date: 2021-03-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The present invention aims to solve the problem of difficult treatment of the crystallization mother liquor in the adipic acid crystallization refining process in the prior art, and provides a treatment method for the crystallization mother liquor in the adipic acid crystallization refining process. Effective removal of other impurities in the diacid mixture

Method used

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  • Treatment method of crystallization mother liquor in adipic acid crystallization refining process

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Get 100g adipic acid crystallization mother liquor, by weight, the typical composition of described crystallization mother liquor is adipic acid (15%), glutaric acid (30%), water (40%), other impurity (15%), Other impurities are mainly succinic acid, esters, polymers, catalysts and other reaction by-products or impurities such as catalysts entrained in the mother liquor, add 10g of methanol, stir evenly, stand at 20°C for 20min, then separate layers, and obtain a light liquid in the upper layer after liquid separation Phase 93g and lower heavy liquid phase 17g.

[0040] The above-mentioned light liquid phase was evaporated under reduced pressure, with an evaporation rate of 40%, to obtain 37.2g of condensate, which was crystallized at 20°C for 40 minutes, and solid-liquid separation obtained 41g of mixed crystals of adipate and glutaric acid, and the impurity content was 0.5w% according to liquid chromatography analysis. The steam condensate can recover methanol and wat...

Embodiment 2

[0043] Take 100g of adipic acid crystallization mother liquor, in parts by weight, the composition of the crystallization mother liquor is the same as that of Example 1, add 20g of methanol, stir evenly, leave to stand at 5°C for 5min and then separate layers, after liquid separation, 102g of the upper light liquid phase and the lower layer are obtained. Heavy liquid phase 18g.

[0044] The above-mentioned light liquid phase was evaporated under reduced pressure, the evaporation volume was 55%, and 56.1 g of condensate was obtained, which was crystallized at 5° C. for 15 minutes, and 44 g of mixed crystals of adipic acid and glutaric acid were obtained by solid-liquid separation. According to liquid chromatography analysis, the impurity content was 0.4w%. The steam condensate can recover methanol and water.

[0045] For the convenience of comparison, the main process conditions and experimental results are listed in Table 1.

Embodiment 3

[0047] Take 100g of adipic acid crystallization mother liquor, in parts by weight, the composition of the crystallization mother liquor is the same as that of Example 1, add 5g of methanol, stir evenly, leave to stand at 50°C for 50min, then separate layers, and obtain 84g of the upper light liquid phase and the lower layer after liquid separation Heavy liquid phase 16g.

[0048] The above-mentioned light liquid phase was evaporated under reduced pressure, with an evaporation rate of 35%, to obtain 29.4g of condensate, crystallized at 50°C for 50min, and obtained 20g of adipate-glutaric acid mixed crystals by solid-liquid separation, and the impurity content was 0.01w% according to liquid chromatography analysis. The steam condensate can recover methanol and water.

[0049] For the convenience of comparison, the main process conditions and experimental results are listed in Table 1.

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Abstract

In order to solve the problem that the crystallization mother liquor is difficult to treat in the adipic acid crystallization refining process in the prior art, the invention provides the treatment method of the crystallization mother liquor in the adipic acid crystallization refining process. The method can effectively remove other impurities in the mixture of adipic acid and glutaric acid in thecrystallization mother liquor. According to the technical schemes, the treatment method of the crystallization mother liquor in the adipic acid crystallization refining process comprises the following steps of: (1) mixing the crystallization mother liquor with an additive; (2) performing still standing and layering to obtain a light liquid phase 1 and a heavy liquid phase 2; (3) evaporating the light liquid phase 1 to obtain a material 3; and (4) crystallizing and separating the material 3 to obtain adipic acid and glutaric acid mixed crystals and mother liquor 4. According to the method, a solvent in the crystallization mother liquor is water or basically water, the additive comprises C1-C3 alcohol, and the weight ratio of the additive to the crystallization mother liquor is greater than0 and less than 0.3.

Description

technical field [0001] The invention relates to a method for treating mother liquor produced by a crude adipic acid crystallization separation process, belonging to the field of chemical industry, and specifically refers to a method for treating the mother liquor produced by a process for preparing refined adipic acid from crude adipic acid crystallization. Background technique [0002] Adipic acid (Adipic acid) is an important basic organic chemical raw material. Its biggest use is to produce nylon 66 salt, and it can also be used to produce polyurethane, plasticizer, polyamide, synthetic leather, lubricant, etc. [0003] Usually adipic acid comes from the catalytic oxidation reaction of cyclohexane. Cyclohexane is first catalyzed and oxidized to cyclohexanone and cyclohexanol. After separation and purification, it is further oxidized to adipic acid with nitric acid; or cyclohexane is directly oxidized by air to obtain adipic acid. Adipic acid, glutaric acid, succinic acid...

Claims

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Application Information

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IPC IPC(8): C07C51/50C07C55/14C07C55/12C07C51/43
CPCC07C51/50C07C51/43C07B2200/13C07C55/14C07C55/12
Inventor 陈燕鑫干丰丰
Owner CHINA PETROLEUM & CHEM CORP
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