Recycling method of long carbon chain binary acid purification and refining crystallization mother liquor

A long carbon chain dibasic acid and crystallization mother liquor technology, applied in chemical instruments and methods, separation/purification of carboxylic acid compounds, preparation of hydroxyl compounds, etc., can solve the problem of low recovery rate of long carbon chain dibasic acids and the quality of recycled products Poor, high processing costs and other issues, to achieve the effect of promoting 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 long carbon chain dibasic

Method used

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  • Recycling method of long carbon chain binary acid purification and refining crystallization mother liquor
  • Recycling method of long carbon chain binary acid purification and refining crystallization mother liquor
  • Recycling method of long carbon chain binary acid purification and refining crystallization mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] A kind of recycling method of dodecane dibasic acid purification crystallization mother liquor of the present invention comprises the following steps:

[0067] ①. Recycling solvent methanol

[0068] Be that 2000 liters of crystallization mother liquors of 30 grams per liter of dodecane dibasic acid content, drop into the methanol reclaiming distillation still, under stirring, at first add the industrial liquid caustic soda of 30wt%, dodecane dibasic acid: NaOH (mol ratio) =1:2.5, then, heat up distillation, collect and recover methanol, and recycle it 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.

[0069] ②. The residual material at the bottom of the distillation tank is dissolved and diluted

[0070] After the recovery of methanol, add water to dissolve the residual material at the bottom ...

Embodiment 2

[0080] A kind of recycling method of tridecane dibasic acid purification crystallization mother liquor of the present invention comprises the following operation steps:

[0081] ①. Recycling solvent methanol

[0082] Be 2000 liters of crystallization mother liquor with tridecane dibasic acid content of 40 g / liter, drop into methanol and reclaim still kettle, under stirring, at first add the industrial liquid caustic soda of 30wt%, tridecane dibasic acid: NaOH (molar ratio) =1:2.6, then, heat up distillation, collect and recover methanol, and recycle it for the recrystallization purification process; in the whole process of recovering solvent methanol, use industrial liquid alkali to adjust the pH value of the material in the methanol recovery still, and keep the pH ≥8.

[0083] ②. The residual material at the bottom of the distillation tank is dissolved and diluted

[0084] After the recovery of methanol, add water to dissolve the residual material at the bottom of the disti...

Embodiment 3

[0094] A method for recycling tetradecanedioic acid purification and refining crystallization mother liquor of the present invention comprises the following steps:

[0095] ①. Recycling solvent methanol

[0096] Be 2000 liters of crystallization mother liquors with tetradecane dibasic acid content of 50 grams per liter, drop into methanol reclaiming distillation still, under stirring, at first add the industrial liquid caustic soda of 30wt%, tetradecane dibasic acid: NaOH (molar ratio) =1:2.7, then, heat up distillation, collect and recover methanol, and recycle it 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 distillation kettle, and always maintain the pH ≥8.

[0097] ②. The residual material at the bottom of the distillation tank is dissolved and diluted

[0098] After the recovery of methanol, water is added to dissolve...

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Abstract

The invention discloses a recycling method of long carbon chain binary acid purification and refining crystallization mother liquor, and belongs to a separation treatment method of acyclic dicarboxylic acid with 12 carbon atoms. The method comprises the following operation steps: (1) recovering solvent methanol; (2) dissolving and diluting a residual material at the bottom of a distillation kettle; (3) performing high-temperature acid-out crystallization; (4) drying. The recycling method of the long carbon chain binary acid purification and refining crystallization mother liquor has the advantages that the recovered long carbon chain binary acid product has good color, high purification and high recovery yield, equipment investment is saved, the operation is easy and convenient, the resource is saved, and environment protection is facilitated. By using the method, the long carbon chain binary acid recovery rate is greater than or equal to 97.0 percent. The product quality reaches the following technical indexes that the total acid is greater than or equal to 99.7 percent by weight, the single acid is greater than or equal to 99.3 percent by weight, the ash content is smaller than or equal to 0.003 percent by weight, the total nitrogen is smaller than or equal to 0.004 percent by weight, the ferric oxide is smaller than or equal to 0.0002 percent by weight, and the moisture is smaller than or equal to 0.17 percent by weight.

Description

technical field [0001] The invention relates to a recycling method for purifying and refining crystallization mother liquor of long carbon chain dibasic acid. It belongs to the separation and treatment method of acyclic dicarboxylic acid with 12 carbon atoms. Background technique [0002] Long carbon chain dibasic acids are 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 carboxyl group, it is a kind of crystalline polymer with strong polarity, hydrogen bond formation between molecules and...

Claims

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Application Information

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IPC IPC(8): C07C51/43C07C51/42C07C55/02C07C55/21C07C29/80C07C31/04
Inventor 郝本清
Owner 山东广通新材料有限公司
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