Refining method of C11-C18 long-chain diacid

A C11-C18, long-chain dibasic acid technology, used in granular long-chain dibasic acid crystallization products, high-purity polymerization grade field, can solve the problem of low yield, achieve high crystallization yield and good fluidity Effect

Inactive Publication Date: 2012-06-20
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In summary, recrystallization of long-chain dibasic acids with organic solvents as a solvent can effectively improve product quality, but the existing organic solvent recrystallization method has the disadvantage of low yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0029]Weigh 30g of crude long-chain dibasic acid, put it into a 1L three-hole flask equipped with a stirring device, then add 100mL of ethanol with a concentration of 95% by volume, and then heat it to 60°C while stirring on a digital constant temperature heating mantle , continue heating for 20 minutes to ensure that the long-chain dibasic acid is completely dissolved. Add 6g of activated carbon, stir at a constant temperature for 60 minutes under closed system conditions, then filter while hot and collect the filtrate. The filtrate is cooled naturally in the crystallization cup. When the temperature drops to 52 degrees Celsius, add 2g of granular seed crystals, continue to slowly cool down while stirring, keep the temperature constant after dropping to 30 degrees Celsius, and start slowly adding in batches with a concentration of 40%, 30 %, 20% and 15% dilute ethanol 25mL each, then add 200mL dilute ethanol with a concentration of 5%, and finally lower the temperature to roo...

example 2

[0030] Example two, a refining method of C11-C18 long-chain dibasic acid, adopts the following steps:

[0031] Weigh 40g of crude long-chain dibasic acid, put it into a 1L three-hole flask equipped with a stirring device, then add 100mL of 95% ethanol, and then heat it to 70°C while stirring on a digital constant temperature heating mantle to make the long-chain dibasic acid The crude product was completely dissolved. Add 10 g of activated clay, stir at a constant temperature for 80 minutes under a closed system, then filter while hot and collect the filtrate. After the filtrate is moved into the crystallization cup, start to cool down naturally. When the temperature drops to 55 degrees Celsius, add 4g granular seed crystals, continue to slowly cool down while stirring, keep the temperature constant after dropping to 40 degrees Celsius, and start to add dilute ethanol solution continuously and slowly. The concentration of dilute ethanol was provided by a gradient mixer. The i...

example 3

[0032] Example three, a refining method of C11-C18 long-chain dibasic acid, adopts the following steps:

[0033] Weigh 25g of crude long-chain dibasic acid, put it into a 1L three-hole flask equipped with a stirring device, then add 100mL of ethanol with a concentration of 85%, and then heat it to 55°C while stirring on a digital constant temperature heating mantle The crude chain dibasic acid is completely dissolved, and the system is kept airtight. Add 3g of activated carbon and stir at constant temperature for 120 minutes, then filter while hot. The filtrate begins to cool down naturally. When the temperature drops to 50 degrees Celsius, add 2g of seed crystals, continue to cool down slowly while stirring, keep the temperature constant after dropping to 45 degrees Celsius, and start adding slowly in batches. Concentrations are 60%, 40% and 20% respectively Each 25mL of dilute ethanol was added, and then 300mL of dilute ethanol with a concentration of 10% was added, and the...

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Abstract

The invention provides a refining method of C11-C18 long-chain diacids. granular long-chain diacid crystals are obtained by using methanol and ethanol as organic solvents and adopting a crystallization mode of cooling crystallization with seeding materials combined with flowing addition of dilute solvent aqueous solutions. The method has the advantages of high product purity and high crystallization yield; alcohol solvents are low in price and simple in recovery, which greatly reduces the refining cost of crude products.

Description

technical field [0001] The present invention relates to a refining method of C11-C18 long-chain dibasic acid, specifically refers to recrystallization of long-chain dibasic acid crude product in methanol, ethanol and other alcohol solvents to obtain high-purity polymerization grade, granular long A method for chain dibasic acid crystallization products belongs to the technical field of biochemical industry. Background technique [0002] C11-18 long-chain dibasic acid refers to a straight-chain dibasic carboxylic acid containing 11-18 carbon atoms. It is a chemical raw material with important uses and is widely used in the synthesis of high-grade spices, high-performance engineering plastics, and high-grade lubricating oil. , hot melt adhesives, paints and coatings and other products. [0003] At present, there are mainly two methods for producing long-chain dibasic acids: synthetic method and microbial fermentation method. Foreign countries mainly use chemical synthesis, w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/43
Inventor 张建华唐蕾张宏建陈旭升曹付明毛忠贵
Owner JIANGNAN UNIV
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