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A method for refining long-chain dibasic acid

A long-chain dibasic acid and dibasic acid salt technology, which is applied in the separation/purification of carboxylic acid compounds, carboxylate salt preparation, organic chemistry, etc., can solve the problems of acetone instability, dangerous implementation, environmental pollution, etc., and achieve The effect of less material consumption, low energy consumption and simple process

Active Publication Date: 2016-08-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the nitrogen content in the long-chain dibasic acid product obtained by this method is lower than 12ppm, due to the use of acetone or butanone with a low boiling point solvent (acetone 56.1°C, butanone 79.6°C), the sealing performance of the device during the treatment process has been raised. Higher requirements, especially the use of air to purge the crystalline dibasic acid containing solvent during the implementation of the method. This process is more dangerous to implement, and it is easy to form an explosive gas mixture, and the ketone solvent in the mixture is difficult to recover, which will inevitably affect the environment. create pollution
And acetone is unstable in the presence of acid, and it is easy to generate mesityl oxide, which affects the purity and application of the final product

Method used

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  • A method for refining long-chain dibasic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Take 2000ml and get C by fermenting Candida tropicalis 12 h 22 o 4 Fermentation broth (concentration: 160g / L), heated at 95°C, adding sodium hydroxide solution, adjusting the pH value to 10, standing for about 2 hours, and removing the supernatant liquid wax. C 12 h 22 o 4 The temperature of the salt solution was lowered to 80° C., and filtered through a ceramic microfiltration membrane to obtain a dodecanoic dibasic acid salt filtrate.

[0038] with H 2 SO 4 After adjusting the pH value of the dodecane dibasic acid salt filtrate to 6.2, carbon dioxide was introduced into it to adjust the pH value to 3.8, and 1.7 g of activated carbon was added, stirred slowly for 1 h, and filtered to remove solids. with H 2 SO 4 Adjust the pH value of the dodecane dibasic acid salt liquid phase to 3.0, and heat it to 80°C to obtain C 12 h 22 o 4 The aqueous crystallization solution was filtered to obtain a wet filter cake, which was washed with deionized water until neutral...

Embodiment 2

[0040] Take 2000ml and get C by fermenting Candida tropicalis 13 h 24 o 4 Add sodium hydroxide solution to the fermentation broth (concentration: 156g / L), adjust pH to 9, heat to 70°C, filter through ceramic microfiltration membrane, remove bacteria and residual liquid wax to obtain filtrate.

[0041] with H 2 SO 4 After adjusting the pH value of the tridecane dibasic acid salt filtrate to 6.0, carbon dioxide was introduced into it to adjust the pH value to 4.2, and 1.5 g of activated carbon was added, stirred slowly for 1.5 h, and filtered to remove solids. With 50wt%H 2 SO 4 Adjust the pH value of the tridecane dibasic acid salt liquid phase to 3.5, and heat it to 85°C to obtain C 13 h 22 o 4 The aqueous crystallization solution was filtered to obtain a wet filter cake, which was washed with deionized water until neutral. The filter cake was mixed with 1500ml deionized water for beating, filtered and dried to obtain tridecanedioic acid product. The product quality ...

Embodiment 3

[0043] Take 2000ml and get C by fermenting Candida tropicalis 14 h 24 o 4 Add sodium hydroxide solution to the fermentation broth (concentration: 152g / L), adjust pH to 8.5, heat to 80°C, filter through ceramic microfiltration membrane, remove bacteria and residual liquid wax to obtain filtrate.

[0044] with H 2 SO 4 After adjusting the pH value of the fourdecane dibasic acid salt filtrate to 6.5, carbon dioxide was introduced into it to adjust the pH value to 4.5, and 2.5 g of activated carbon was added, stirred slowly for 2 hours, and filtered to remove solids. With 50wt%H 2 SO 4 Adjust the pH value of the tetradecane dibasic acid salt liquid phase to 3.0, and heat it to 87°C to obtain C 14 h 22 o 4 The aqueous crystallization solution was filtered to obtain a wet filter cake, which was washed with deionized water until neutral. The filter cake was mixed with 1400ml deionized water for beating, filtered and dried to obtain tetradecanedibasic acid product. The produ...

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Abstract

The invention discloses a refining method for long-chain dicarboxylic acid. The method comprises the following steps: converting long-chain dicarboxylic acid in terminated long-chain dicarboxylic acid fermentation broth into long-chain dicarboxylic acid salt and carrying out filtering to eliminate thalli; then adjusting the pH value of a liquid phase to 5.0 to 7.0; introducing carbon dioxide into a system and carrying out filtering to remove solids; and carrying out acidification, separation, washing, drying and the like so as to obtain a long-chain dicarboxylic acid product. The method has mild treatment conditions, does not use any organic solvent, is simple and safe to operate and poses no pollution to operators and the environment. The long-chain dicarboxylic acid obtained after treatment of the method can satisfy the requirement that total N is less than 30 [mu]g / g .

Description

technical field [0001] The invention relates to a method for refining long-chain dibasic acids, in particular to a method for removing total nitrogen in the long-chain dibasic acid product process obtained from C10-C18 normal alkane fermentation liquid. Background technique [0002] The long-chain dibasic acid molecule general formula that the present invention refers to is C n h 2n-2 o 4 , where n is 10-18, which is a metabolite obtained by fermentation of microorganisms using liquid wax, etc. Dibasic acids refer to organic compounds with carboxyl groups at both ends of the straight carbon chain, and dibasic acids with more than 10 carbon atoms are usually called long-chain dibasic acids, and the abbreviated forms are: DC11~DC18. Long-chain dibasic acid is an important organic intermediate with a wide range of applications. [0003] The main production process of long-chain dibasic acid is divided into vegetable oil cracking method, organic synthesis method and biologic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/02C07C51/50C07C55/21C07C55/02
CPCC07C51/02C07C51/42C07C51/50C07C55/02C07C55/21
Inventor 高大成李晓姝
Owner CHINA PETROLEUM & CHEM CORP