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A kind of refining method of long-chain mixed dibasic acid

A technology of mixed dibasic acid and refining method, which is applied in the field of refining long-chain mixed dibasic acid, can solve the problems of inability to effectively remove pigments and impurities, complicated solvent recovery, poor product appearance, etc., and achieves simple and effective discharge problems, The effect of protecting the environment and high productivity

Active Publication Date: 2019-05-31
CATHAY R&D CENT CO LTD +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its disadvantages are: the process requires two or more decolorization of activated carbon, resulting in a large loss of dibasic acid and low yield
Chinese patent application CN102795984A uses the recombination of ethanol to refine dodecane dibasic acid as raw material, and reacts with excess liquid caustic soda to generate long carbon chain dibasic acid. This process has the defect of dibasic acid and ethanol esterification caused by ethanol process. Moreover, decolorization with activated carbon alone cannot effectively remove pigments and impurities, the appearance of the product is poor, and the recovery of solvents is also relatively complicated.

Method used

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  • A kind of refining method of long-chain mixed dibasic acid
  • A kind of refining method of long-chain mixed dibasic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Take 100 grams of the by-product mixed dibasic acid obtained in the extraction process of dodecane dibasic acid, add 1800 grams of water, raise the temperature to 90 ° C, add caustic soda, adjust the pH to 5.7, stir, and the mixed dibasic acid is almost completely dissolved.

[0057] Add 3 grams of macroporous powder sugar carbon to the above solution, stir for 1 hour, and filter while hot to obtain a filtrate.

[0058] The obtained filtrate was stirred, cooled down at room temperature and precipitated. After the temperature dropped to 40°C, it was maintained for one hour, and then filtered to obtain a precipitate of large particles. Wash with 50g of cold water.

[0059] The obtained precipitate was added into 1000 g of water, heated to 80° C., stirred, and after adding 7 g of sodium hydroxide, the precipitate was completely dissolved.

[0060] In the obtained filtrate, add sulfuric acid with a concentration of 30% by mass, adjust the pH to 3.0, cool down to 50°C, fil...

Embodiment 2

[0063] Take 100 grams of the by-product mixed dibasic acid obtained in the extraction process of dodecane dibasic acid, add 400 grams of water, heat up to 90 ° C, add caustic soda, adjust the pH to 6.7, stir, and the mixed dibasic acid is almost completely dissolved.

[0064] The obtained filtrate was stirred, cooled down at room temperature and precipitated. After the temperature dropped to 30°C, it was maintained for one hour, and then filtered to obtain a precipitate of large particles. Wash with 50g of cold water.

[0065] The obtained precipitate was added into 1200 g of water, heated to 80° C., stirred, and after adding 2 g of sodium hydroxide, the precipitate was completely dissolved. Add 3 grams of macroporous powdered sugar carbon into the resulting solution, stir for 1 hour, and filter while hot to obtain a filtrate.

[0066] In the obtained filtrate, add sulfuric acid with a concentration of 45% by mass, adjust the pH to 3.5, cool down to 40° C., filter to obtain ...

Embodiment 3

[0069] Take 100 grams of the by-product mixed dibasic acid obtained in the extraction process of dodecane dibasic acid, add 200 grams of water, heat up to 95 ° C, add caustic soda, adjust the pH to 6.2, stir, and the mixed dibasic acid is almost completely dissolved.

[0070] Add 1 gram of macroporous powdered sugar carbon to the above solution, stir for 1 hour, and filter while hot to obtain a filtrate.

[0071] The obtained filtrate was stirred, cooled down at room temperature and precipitated. After the temperature dropped to 40°C, it was maintained for one hour, and then filtered to obtain a precipitate of large particles. Wash with 50g of cold water.

[0072] The obtained precipitate was added into 1000 g of water, heated to 80° C., stirred, and after adding 5 g of sodium hydroxide, the precipitate was completely dissolved. Add 3 grams of macroporous powdered sugar carbon into the resulting solution, stir for 1 hour, and filter while hot to obtain a filtrate.

[0073] ...

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Abstract

The invention discloses a refining method of a long-chain mixed dibasic acid, which comprises the following steps: (1) adding a mixed dibasic acid solid into water, heating, adding alkali to adjust the pH value, dissolving the mixed dibasic acid, and then lowering the temperature Precipitation and separation to obtain solid I; (2) Put solid I into water, heat up, and after solid I is completely dissolved, add acid to adjust the pH to precipitate the mixed dibasic acid, separate the solid, and obtain the refined long-chain mixed dibasic acid after drying. a. The invention completes the solidification of the oil phase and the secondary precipitation process in the water phase by controlling each process condition of the refining process, and obtains a high-quality, high-yield mixed dibasic acid finished product. The process of the invention can simply and effectively solve the problem of discharge of by-products in the production of long-chain dibasic acids, which not only protects the environment, but also increases profits for enterprises.

Description

technical field [0001] The invention relates to a method for treating long-chain dibasic acids, in particular to a method for refining long-chain mixed dibasic acids. Background technique [0002] Long chain dicarboxylic acids (Long chain dicarboxylic acids) refer to aliphatic dicarboxylic acids (DCn for short) containing more than 10 carbon atoms in the carbon chain, including saturated and unsaturated dicarboxylic acids. The fine chemical products used in the chemical industry are synthetic high-grade spices, high-performance nylon engineering plastics, high-grade nylon hot-melt adhesives, high-temperature dielectrics, high-grade paints and coatings, high-grade lubricating oils, cold-resistant plasticizers, resins, medicines and pesticides, etc. important basic raw materials. Due to the broad development potential of the downstream products of long-chain dibasic acids, the demand for long-chain dibasic acids at home and abroad will continue to increase, and its market pot...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/02C07C51/42C07C51/43C07C55/21C07C55/02C07C57/13
CPCC07C51/02C07C51/42C07C51/43C07C55/21C07C55/02C07C57/13
Inventor 戴端芳杨晨秦兵兵杨希伟李乃强刘修才
Owner CATHAY R&D CENT CO LTD