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Recycling method of long-carbon-chain dicarboxylic acid refined crystallization mother liquor

A dibasic carboxylic acid and crystallization mother liquor technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve problems such as difficult to solve the chromaticity of heavy fractions in rectification, lower recovery yield of by-products, waste of acetic acid solvent, etc. Achieve the effects of easy control of product indicators, reduction of recycling costs, and improvement of recycling efficiency

Pending Publication Date: 2020-05-05
ZIBO GUANGTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition to reducing the recovery yield of by-products, it will also increase the difficulty of the subsequent decolorization and purification process, and even adversely affect the quality of by-products
[0026] 3. The method of natural drying wastes solvent resources, occupies valuable land, pollutes the atmosphere and water environment, etc.
With the existing technology, about 0.4 tons of long carbon chain mixed dicarboxylic acids can be produced per ton of rectified heavy components, that is, 0.875 tons of acetic acid gas is released into the air on average for every 1 ton of long carbon chain mixed dicarboxylic acids produced. Caused the waste of acetic acid solvent, caused air environment pollution again
0.375 tons of acetic acid entered the sewage treatment system, which undoubtedly increased the sewage treatment load
[0028] 4. The method of natural drying, neutralization into salt and dissolution, twice decolorization and sulfuric acid acidification and crystallization, the process is cumbersome
Therefore, in the above-mentioned decolorization process, although two decolorizations have been adopted, it is still difficult to solve the problem of the deep chroma of the rectification heavy component. The platinum-cobalt chroma of the mixed long carbon chain dicarboxylic acid obtained by this method is generally more than 85

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0107] Embodiment 1 A kind of recycling method of the refined crystallization mother liquor of dodecane dicarboxylic acid

[0108] Including the following steps:

[0109] In the first step, the mother liquor is crystallized by water crystallization, and the dodecane dicarboxylic acid product is extracted again;

[0110] ①.Water crystallization

[0111] Under ambient temperature, in 5000L reaction kettle, at first drop into the refining crystallization mother liquor 2000L of dodecane dicarboxylic acid, in the crystallization mother liquor, dodecanedioic acid content 40g / L, the length in terms of dodecane dicarboxylic acid The total content of carbon chain dicarboxylic acids is 42g / L. Then add 2000L of deionized water, stir, raise the temperature to 95°C, stir for 30 minutes, then cool down to 30°C, and crystallize for 60 minutes;

[0112] ②. Filtration separation

[0113] The material after water crystallization is filtered through a plate and frame filter press to obtain 7...

Embodiment 2

[0138] Embodiment 2 A kind of recycling method of the refined crystallization mother liquor of dodecane dicarboxylic acid

[0139] Including the following steps:

[0140] In the first step, the mother liquor is crystallized by water crystallization, and the dodecane dicarboxylic acid product is extracted again;

[0141] ①.Water crystallization

[0142] Under ambient temperature, in 5000L reaction kettle, at first drop into the refining crystallization mother liquor 2000L of dodecane dicarboxylic acid, in the crystallization mother liquor, dodecanedioic acid content 40g / L, the length in terms of dodecane dicarboxylic acid The total content of carbon chain dicarboxylic acids is 43g / L. Then add 2000L of deionized water, stir, heat up to 90°C, stir for 30 minutes, then cool down to 28°C, and crystallize for 45 minutes;

[0143] ②. Filtration separation

[0144] The material after water crystallization is filtered through a plate and frame filter press, and the filter cake obta...

Embodiment 3

[0169] Embodiment 3. A kind of recycling method of the refined crystallization mother liquor of dodecane dicarboxylic acid

[0170] Including the following steps:

[0171] In the first step, the mother liquor is crystallized by water crystallization, and the dodecane dicarboxylic acid product is extracted again;

[0172] ①.Water crystallization

[0173] Under ambient temperature, in 5000L reaction kettle, at first drop into the refining crystallization mother liquor 2000L of dodecane dicarboxylic acid, in the crystallization mother liquor, dodecanedioic acid content 40g / L, the length in terms of dodecane dicarboxylic acid The total content of carbon chain dicarboxylic acids is 44g / L. Then add 2000L of deionized water, stir, raise the temperature to 85°C, stir for 30 minutes, then cool down to 25°C, and crystallize for 30 minutes;

[0174] ②. Filtration separation

[0175] The material after water crystallization is filtered through a plate and frame filter press, and the o...

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Abstract

The invention relates to a recycling method of a long-carbon-chain dicarboxylic acid refined crystallization mother liquor. The recycling method comprises the following steps: (1) carrying out watering-out crystallization; (2) carrying out solvent recovery by adopting an azeotropic distillation process; (3) drying heavy components at the bottom of a distillation kettle after solvent recovery by adopting a film evaporation process; and (4) refining and purifying the mixed long-carbon-chain dicarboxylic acid. The refined target long-carbon-chain dicarboxylic acid main product can be extracted from the crystallization mother liquor again, so that the yield of the main product is increased. The solvent acetic acid is all recycled. According to the prepared mixed long-carbon-chain dicarboxylicacid, the total acid content is larger than or equal to 98.00 wt%, the ash content is smaller than or equal to 50ppm, the iron content is smaller than or equal to 5ppm in terms of Fe2O3, the total nitrogen content is smaller than or equal to 80ppm in terms of N element, the moisture content is smaller than or equal to 0.4 wt%, and the platinum-cobalt chromaticity is smaller than 10. The recovery rate of the long-carbon-chain dicarboxylic acid main product in the watering-out crystallization step reaches 72%. The total recovery rate of the mixed long-carbon-chain dicarboxylic acid reaches 90.07%.

Description

technical field [0001] The invention relates to a method for recycling and utilizing long carbon chain dibasic carboxylic acid refined crystallization mother liquor. It belongs to the purification treatment of acyclic dicarboxylic acids with more than 10 carbon atoms. Background technique [0002] Long-chain dicarboxylic acid (along-chain dicarboxylic acid)—a straight-chain dicarboxylic acid with more than 10 carbon atoms in the carbon chain, is an important class of fine chemical products. Main raw materials for synthesizing polyamide resins, polyester resins, hot melt adhesives, spices, weather-resistant plasticizers, lubricating oil additives, coatings, liquid crystals, etc. [0003] Long carbon chain dicarboxylic acids do not exist in nature, and are mainly prepared by organic synthesis and biological fermentation. The organic synthesis method has a long process route, high cost, low yield, potential safety hazards and environmental pollution. [0004] The biological f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/42C07C51/47C07C51/43C07C51/46C07C55/02C07C55/21
CPCC07C51/42C07C51/47C07C51/43C07C51/46C07C55/02C07C55/21
Inventor 房宁王增德李永俊张龙
Owner ZIBO GUANGTONG CHEM