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Method for separating and purifying nonane diacid

A technique for separation and purification of azelaic acid, which is applied in the separation/purification of carboxylic acid compounds, organic chemistry, preparation of carboxylic acid by ozonation, etc. It can solve the problems of azelaic acid loss and other problems, and achieve short contact time, compact equipment, and good The effect of color

Active Publication Date: 2010-09-15
SICHUAN SIPO CHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the first extraction with water in this process, the water phase is cooled and crystallized to precipitate crude azelaic acid crystals and then extracted with an organic solvent, and solid-liquid separation is carried out after crystallization, which will result in a large amount of azelaic acid loss.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Get the oxidized liquid (the azelaic acid content is about 70% of the 100kg oleic acid ozonation-oxidation reaction gained, the suberic acid content is about 3%, the palmitic acid and stearic acid content are about 10%, the pelargonic acid content is lower than 1.5%) ), put it in a rectification tower, and distill under reduced pressure under the conditions of 100-1000pa and 70-110°C to remove the C 2 -C 9 The monoacid, the residue is transferred to a thin film evaporator, distilled at 80pa, 190°C to remove heavy components such as asphalt; add the distilled crude azelaic acid to 500kg of water at a temperature of 60°C for extraction Operation, azelaic acid and other water-soluble substances dissolved in hot water, C 10-18 The saturated monocarboxylic acid is separated from the water layer, stirred, allowed to stand for stratification, and the upper oil layer is separated by overflow; the extracted water layer is extracted with 500kg aromatic hydrocarbons at a temperat...

example 2

[0023] Get 100kg oleic acid ozonation-oxidative decomposition gained oxidation solution (azelaic acid content is about 68%, suberic acid content is about 3.5%, palmitic acid and stearic acid content are about 12%, nonanoic acid content is less than 2%), Put it in a rectification tower for rectification, and distill under reduced pressure at 400-1200pa and 70-110°C to remove the C 2 ~C 9 Monoacid, transfer the residue to a thin film evaporator and distill at 140pa, 210°C to remove heavy components such as asphalt; add the distilled crude azelaic acid to 500kg of water at a temperature of 85°C, stir, and azelaic acid and other water-soluble substances dissolved in hot water, C 10-18 The saturated monocarboxylic acid is separated from the water layer, and the upper oil layer is separated after standing for stratification, and the extracted water layer is carried out with 500kg of aromatic hydrocarbons at a temperature of 85°C to carry out extraction, and the residual monoacid in...

example 3

[0025] Get 100kg of crude azelaic acid (azelaic acid content is about 70%, suberic acid content is about 3%, palmitic acid and stearic acid content are about 10%, pelargonic acid content is lower than 1.5%), it is placed in refining Distillation column rectification, vacuum distillation under the conditions of 800-2000pa, 90-150℃, to remove the C 2 ~C 9 Monoacid, transfer the residue to a thin film evaporator, distill at 140pa, 210°C to remove heavy components such as asphalt; add the distilled crude azelaic acid to 500kg of water at a temperature of 85°C for extraction , azelaic acid and other water-soluble substances dissolved in hot water, C 10-18 The saturated monocarboxylic acid is separated from the water layer, stirred, allowed to stand for stratification, and the upper oil layer is separated by overflow; the extracted water layer is extracted with 500kg aromatic hydrocarbons at a temperature of 85°C, and a small amount of monohydric acid remaining in the aqueous solut...

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Abstract

The invention discloses a separation purification method of azelaic acid, belonging to the separation purification technical field of organic compound, which comprises depressurizing and distilling the oxidation solution obtained by treating ozonation-oxidation decomposition on unsaturated fatty acid to remove solvent and pelargonic acid, transferring left oxidation solution to a film evaporator to be distilled to obtain crude azelaic acid, extracting and recrystallizing the crude azelaic acid to obtain azelaic acid crystal. In the recrystallization of azelaic acid, the low-carbon dibasic acid of C<4>-C<8> in azelaic acid is dissolved in cold water, to be discharged along with crystallization mother liquor, and the left azelaic acid in the recrystallization mother liquor is recovered by the film separator. The obtained azelaic acid is transferred to a rising film evaporator to be dried and dehydrated and the dehydrated azelaic acid is evaporated by film to obtain the azelaic acid. Thewhole process can confirm the yield of azelaic aicd and obtain high-quality azelaic acid, while the whole system is sealed and the process has better environmental compatibility.

Description

technical field [0001] The invention relates to the technical field of separation and purification of organic compounds, in particular to a separation and purification method of azelaic acid. Background technique [0002] Azelaic acid is an important fine chemical raw material, and its industrial application is very extensive. The industrial use of azelaic acid is mainly for the production of azelaic acid plasticizers, and secondly for the synthesis of fragrances, lubricating oils and polyamides. In addition, it can also be used for the manufacture of electrolytic capacitors, skin protection and skin protection. disease treatment. The high added value of azelaic acid depends on the following quality indicators: the content of azelaic acid in the product should meet the requirements of the application field, the content of ketoacids and monoacids in the product should be as low as possible, and the acid value should be 587-594mgKOH / g. At the same time, the product must hav...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C55/18C07C51/42C07C51/34
Inventor 朱进杜俊超周一民谢小俊
Owner SICHUAN SIPO CHEMICAL CO LTD
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