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Long-chain mixed dicarboxylic acid purification method

A technology of mixing dibasic acids and dibasic acids, which is applied in the separation/purification of carboxylic acid compounds, chemical instruments and methods, and the preparation of organic compounds, etc. It can solve the problems of poor solubility, poor product appearance, and high-carbon dibasic acids High content and other issues, to achieve the effect of protecting the environment, increasing income, and good quality

Active Publication Date: 2015-08-19
CATHAY (JINXIANG) BIOMATERIAL CO LTD +1
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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
At the same time, this mixed long-chain dibasic acid contains too many high-carbon dibasic acids (more than sixteen carbons), which leads to poor solubility of the product in the anti-rust formula, which affects the anti-rust effect and customer use
Chinese patent application CN102795984A uses ethanol to refine the reorganization of dodecane dibasic acid into raw materials and react 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, and Decolorization with activated carbon alone cannot effectively remove pigments and impurities, the product has poor appearance, and the recovery of solvents is also relatively complicated
Similarly, this product also has the problem of high carbon number dibasic acid content, which affects the final application of the product

Method used

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  • Long-chain mixed dicarboxylic acid purification method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] 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.

[0063] Add 3 grams of macroporous powder sugar carbon to the above solution, stir for 1 hour, and filter while hot to obtain a filtrate.

[0064] 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.

[0065] 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.

[0066] Ozone is passed into the solution to carry out oxidation, and the amount of ozone passed into is controlled at 2% of the dry ...

Embodiment 2

[0070] 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.

[0071] 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.

[0072] 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.

[0073] Ozone is passed into the solution to carry out oxidation, and the amount of ozone passed into is controlled at 5% of the dry weight of solid ...

Embodiment 3

[0077] 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.

[0078] Add 1 gram of macroporous powdered sugar carbon to the above solution, stir for 1 hour, and filter while hot to obtain a filtrate.

[0079] 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.

[0080] 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.

[0081] Pass into ozone in solution and carry out oxidation, feed into the 8% of ozone amount control at solid 1 dry weight, and oxidation temperat...

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Abstract

The present invention relates to a long-chain mixed dicarboxylic acid extraction method, which comprises: (1) adding a mixed dicarboxylic acid solid to water, heating, adding an alkali to adjust the pH value, dissolving, cooling, precipitating, and separating to obtain a solid I; (2) pouring the solid I to water, heating to increase the temperature, and after dissolving the solid I, adding an oxidizing agent to oxidize so as to improve the solution color and reduce the high carbon number dicarboxylic acid content in the solution; and (3) adding an acid to the obtained solution to adjust the pH value so as to precipitate the mixed dicarboxylic acid, separating the solid, and drying to obtain the long-chain mixed dicarboxylic acid finished product. According to the present invention, the second precipitation and the oxidizing process are combined in the water phase to obtain the high quality dicarboxylic acid finished product, wherein the dicarboxylic acid finished product has characteristics of white color, good quality, and low high-carbon-number dicarboxylic acid (dicarboxylic acid having more than or equal to 16 carbon number) content, and is especially suitable for the anti-rust field; and with the extraction process, the by-product discharge problem during the long-chain dicarboxylic acid production can be simply and effectively solved, such that the environment is protected and the enterprise incomes are increased.

Description

technical field [0001] The invention relates to a method for treating mixed long-chain dibasic acids, in particular to a purification method for decolorizing and oxidizing mixed long-chain 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 con...

Claims

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Application Information

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IPC IPC(8): C07C51/02C07C51/42C07C51/487C07C55/21C07C55/02C07C57/13
CPCC07C51/02C07C51/42C07C51/43C07C51/487C07C55/02C07C55/21C07C57/13
Inventor 戴端芳杨晨秦兵兵杨希伟李乃强
Owner CATHAY (JINXIANG) BIOMATERIAL CO LTD
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