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Recycling method of purifying, refining and crystallizing mother liquor of dodecanedioic acid

A technology of dodecanedioic acid and crystallization mother liquor, which is applied in chemical instruments and methods, separation/purification of carboxylic acid compounds, preparation of hydroxyl compounds, etc., can solve the problems of low recovery rate of dodecanedioic acid, poor quality of recovered products, Deal with the problem of high cost, and achieve the effect of benefiting the growth of crystal nuclei, increasing product yield and improving solubility

Active Publication Date: 2015-03-25
山东广通新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has high processing costs, low recovery rate of dodecanedioic acid, and poor quality of recovered products, resulting in a huge waste of resources

Method used

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  • Recycling method of purifying, refining and crystallizing mother liquor of dodecanedioic acid
  • Recycling method of purifying, refining and crystallizing mother liquor of dodecanedioic acid
  • Recycling method of purifying, refining and crystallizing mother liquor of dodecanedioic acid

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Experimental program
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Effect test

Embodiment 1

[0067] A method for recycling dodecanedioic acid purification and refining crystallization mother liquor of the present invention comprises the following steps:

[0068] ①. Recycling solvent methanol

[0069] Dodecanedioic acid content is 2000 liters of crystallization mother liquors of 30 g / liter, drop into methanol and reclaim still kettle, under stirring, at first add the industrial liquid caustic soda of 30wt%, dodecanedioic acid: NaOH (molar ratio)=1 : 2.5, then, heat up and distill, collect and recover methanol, and recycle for the recrystallization purification process; in the whole process of recovering solvent methanol, use industrial liquid caustic soda to adjust the pH value of the material in the methanol recovery still, and keep the pH ≥ 8 .

[0070] ②. The residual material at the bottom of the distillation tank is dissolved and diluted

[0071] After the recovery of methanol, add water to dissolve the residual material at the bottom of the distillation tank, a...

Embodiment 2

[0081] A method for recycling dodecanedioic acid purification and refining crystallization mother liquor of the present invention comprises the following steps:

[0082] ①. Recycling solvent methanol

[0083] Dodecanedioic acid content is 2000 liters of crystallization mother liquors of 40 g / liter, drop into the methanol reclaiming distillation still, under stirring, at first add the industrial liquid caustic soda of 30wt%, dodecanedioic acid: NaOH (molar ratio)=1 : 2.6, then, heat up and distill, collect and recover methanol, and recycle for the recrystallization purification process; in the whole process of recovering solvent methanol, use industrial liquid caustic soda to adjust the pH value of the material in the methanol recovery still, and keep the pH ≥ 8 .

[0084] ②. The residual material at the bottom of the distillation tank is dissolved and diluted

[0085] After the recovery of methanol, add water to dissolve the residual material at the bottom of the distillatio...

Embodiment 3

[0095] A method for recycling dodecanedioic acid purification and refining crystallization mother liquor of the present invention comprises the following steps:

[0096] ①. Recycling solvent methanol

[0097] Dodecanedioic acid content is 2000 liters of crystallization mother liquors of 50 g / liter, drop into methanol and reclaim still kettle, under stirring, at first add the industrial liquid caustic soda of 30wt%, dodecanedioic acid: NaOH (molar ratio)=1 : 2.7, then, heat up and distill, collect and recover methanol, and recycle for recrystallization and purification process; in the whole process of recovering solvent methanol, adjust the pH value of the material in the methanol recovery still with industrial liquid caustic soda, and keep the pH ≥ 8 .

[0098] ②. The residual material at the bottom of the distillation tank is dissolved and diluted

[0099] After the recovery of methanol, add water to dissolve the residual material at the bottom of the distillation tank, adj...

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Abstract

The invention provides a recycling method of mother liquor purifying, refining and crystallizing mother liquor of dodecanedioic acid, and belongs to the separation treatment method of non-acyclic dicarboxylic acid containing 12 carbon atoms. The recycling method comprises the steps of (1) recovering a solvent which is methanol; (2) distilling to dissolve and dilute materials residual at the bottom of a kettle; (3) performing acidification under a high temperature, and crystallizing; (4) drying. The recycling method of mother liquor purifying, refining and crystallizing mother liquor of dodecanedioic acid has the advantages that the recovered dodecanedioic acid product has a good color and luster and is of high purity, and moreover, the recovery yield is raised, the device investment is saved, the operation is simple and convenient, the resource can be saved, and the environment is protected; the recovery yield of the dodecanedioic acid product is not less than 97.0%; the product quality meets the technical indexes that the total acid is not less than 99.7wt% (percentage by weight), single acid is not less than 99.3wt%, ash content is not greater than 0.003wt%, the total nitrogen is not greater than 0.004wt%, ferric oxide is not greater than 0.0002wt%, and water content is not greater than 0.17wt%.

Description

technical field [0001] The invention relates to a method for recycling and utilizing dodecanedioic acid purification and crystallization mother liquor. It belongs to the separation and treatment method of acyclic dicarboxylic acid with 12 carbon atoms. Background technique [0002] Dodecanedioic Acid (Dodecanedioic Acid) is also known as Lauric Acid. It is an industrial product developed earlier among long-chain dibasic acids. It is mainly used in the synthesis of polymer materials, spices, medicines, etc. Among them, it is one of the most important uses to synthesize long carbon chain nylon (also known as polyamide resin) engineering plastics through polycondensation reaction between polycondensation monomer and diamine. [0003] Nylon is a class of polymer compounds containing amide groups (-NHCO-) ​​in the main chain of the molecule. Because the molecular structure of nylon contains a large number of amide groups, and the end of the macromolecule is an amino or carbox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/21C07C51/42C07C31/04C07C29/80C07C29/94
CPCC07C29/80C07C29/92C07C51/42C07C51/43C07C55/21C07C31/04
Inventor 郝本清房宁
Owner 山东广通新材料有限公司
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