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Treatment method of mixture containing long-chain dicarboxylic acid, long-chain dicarboxylic acid dibutyl ester mixture and application thereof

A long-chain dibasic acid and dibutyl acid technology, which is applied in the field of recycling and reuse of mixtures, can solve problems such as waste of resources, and achieve the effect of solving waste of resources

Pending Publication Date: 2020-06-12
CATHAY R&D CENT CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The butyl esterification technology is suitable for industrial production. It can not only solve the problem of resource waste of the mixture containing long-chain dibasic acids discharged during the industrial fermentation and preparation of long-chain dibasic acids, but also convert the mixed long-chain dibasic acids produced after the butyl esterification reaction. Dibutyl dibasic acid can be directly used in products such as cold-resistant plasticizers

Method used

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  • Treatment method of mixture containing long-chain dicarboxylic acid, long-chain dicarboxylic acid dibutyl ester mixture and application thereof
  • Treatment method of mixture containing long-chain dicarboxylic acid, long-chain dicarboxylic acid dibutyl ester mixture and application thereof
  • Treatment method of mixture containing long-chain dicarboxylic acid, long-chain dicarboxylic acid dibutyl ester mixture and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0106] Take DC12 (dodecane dibasic acid) fermentation broth, extract and refine DC12, and dry the mixture containing long-chain dibasic acid (extraction and refining example 1) at 110°C until the water content is 1 wt%, to obtain 1.626kg of dry matter, dry The effective acid content in the substance is 81.34wt%, the content of long-chain dibasic acids (composed of DC10, DC11, DC12, DC13, DC14 and DC15) is 71.76%, and the content of heteroacids is 9.58%. The mass ratio of long-chain dibasic acid to heteroacid is 7.5:1.

[0107] The above dry matter was added to a 5L reaction kettle, and 1.25kg of n-butanol and 58g of p-toluenesulfonic acid monohydrate were added simultaneously. Under the condition that the liquid phase temperature was 120°C, the esterification was refluxed for 5 hours, and 460 g of the mixed solution of n-butanol and water was separated. The acid value of the reaction solution was tested, and the esterification rate was 60.2%. Add 500 g of n-butanol, continue ...

Embodiment 2

[0112] Take DC13 (tridecane dibasic acid) fermentation broth, extract and refine DC13, and dry the mixture containing long-chain dibasic acid (extraction and refining example 1) at 110°C until the water content is 1 wt%, to obtain 1.205kg of dry matter, wherein The effective acid content is 73.18wt%, the long-chain dibasic acid content is 62.35% (composed of DC11, DC12, DC13, DC14 and DC15), and the heteroacid content is 10.83%. The mass ratio of long-chain dibasic acid and heteroacid is 5.8:15.8:1.

[0113] The above-mentioned dry matter was added into a 5L reaction kettle, and 1.755kg of n-butanol and 51g of p-toluenesulfonic acid monohydrate were added at the same time. Under the condition that the liquid phase temperature was 125°C, the esterification was refluxed for 7 hours, and 582 g of the mixed solution of n-butanol and water was separated, and the acid value of the reaction solution was detected to calculate the esterification rate.

[0114] Under the conditions of ...

Embodiment 3

[0118] Take DC11 (undecane dibasic acid) fermentation broth, extract and refine DC11, and dry the mixture containing long-chain dibasic acid (extraction and refining example 1) at 110°C until the water content is 1 wt%, to obtain 1.931kg of dry matter, dry The effective acid content in the substance is 78.04wt%, the long-chain dibasic acid content is 51.94% (composed of DC10, DC11, DC12, DC13, DC14 and DC15), and the heteroacid content is 26.1%. The mass ratio of long-chain dibasic acid and heteroacid is 2:1.

[0119]The above dry matter was added into a 5L reaction kettle, and 1.855kg of n-butanol and 60g of 98% concentrated sulfuric acid were added simultaneously. Under the condition that the liquid phase temperature was 118° C., the esterification was refluxed for 4 hours, and 665 g of the mixed solution of n-butanol and water was separated. The acid value of the reaction solution was tested, and the esterification rate was 68.9%. Add 700g of n-butanol, continue to reflux ...

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Abstract

The invention provides a treatment method of a mixture containing long-chain dicarboxylic acid, a long-chain dicarboxylic acid dibutyl ester mixture and application thereof. The treatment method comprises the step of carrying out butyl esterification on the mixture containing the long-chain dicarboxylic acid to obtain mixed long-chain dicarboxylic acid dibutyl ester. The mixture containing the long-chain dicarboxylic acid, which is discharged in the process of extracting and refining the long-chain dicarboxylic acid from the long-chain dicarboxylic acid fermentation liquor, is effectively utilized, so that resource waste is avoided. The long-chain dicarboxylic acid dibutyl ester mixture obtained after the mixture containing long-chain dicarboxylic acid is subjected to a butyl esterification reaction and purification is low in chromaticity, can be directly applied to a cold-resistant plasticizer, and can effectively improve the low-temperature flexibility of a polymer. The treatment method of the mixture containing the long-chain dicarboxylic acid is suitable for industrial large-scale production, has low requirements on equipment, is simple and convenient to operate, solves the problem of treatment and reutilization of discharge in the production process of the long-chain dicarboxylic acid, and has economic value.

Description

technical field [0001] The invention relates to a recovery and reuse method for a mixture containing long-chain dibasic acids. Background technique [0002] Plasticizers generally refer to a class of small molecular substances with high boiling point, low volatility, and miscibility with polymers, which have the behavior of changing the mechanical properties of polymers. The main function of the plasticizer is to weaken the secondary bond between the polymer molecules, that is, the van der Waals force, thereby increasing the mobility of the polymer molecular chain, reducing the crystallinity of the polymer molecular chain, increasing the plasticity of the polymer, and the performance The hardness, modulus, softening temperature and embrittlement temperature of the polymer decrease, while the elongation, flexibility and flexibility increase. Plasticizers can be some high-boiling, non-volatile viscous liquids or low-melting solids, which generally do not chemically react with...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/34C07C69/50C07C69/24C07C69/675C08K5/11C08K5/101C08K13/02C08L27/06
CPCC07C67/08C08K5/11C08K5/101C08K13/02C08K2201/014
Inventor 樊爱龙周喜龙张淑华刘修才
Owner CATHAY R&D CENT CO LTD
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