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Method for separating and purifying nonane diacid

A technology for separation and purification of azelaic acid, used in chemical recovery, ozone oxidation to prepare carboxylic acid, etc., can solve the problems of complex distribution of reaction products, high equipment requirements, long separation time, etc., to facilitate large-scale continuous production and implementation Simple conditions and the effect of reducing environmental pollution

Inactive Publication Date: 2007-05-30
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First of all, the trouble caused by the content of the reaction raw materials, because the general oleic acid-containing raw materials contain a considerable part of fatty acids such as linoleic acid, palmitic acid, stearic acid, linolenic acid and other unsaturated double bonds, the composition is quite complicated, If ozone is used to break all the unsaturated bonds, the distribution of reaction products will be more complicated, and the separation problem brought to the later work is obvious; secondly, the complexity of the ozonation reaction itself results in a wider distribution of reaction products
So separation work will be very complicated work
[0007] GB 604281, US 2813113 adopt the method of vacuum distillation, but because the boiling point of long-chain carboxylic acid is high, and relatively similar, the energy consumption during distillation is huge, and the equipment requirement is very high, and the carbonization in the distillation process is serious at the same time, has reduced production greatly. Rate
GB 757355 adopts the water extraction method after azelaic acid rectification, but this method requires the use of a large amount of water, and the purity of the obtained azelaic acid is mostly below 90%.
US 20030032825A1 adopts the method of separation column, but this method requires long separation time and is not suitable for industrial application

Method used

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  • Method for separating and purifying nonane diacid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] a. Stir and mix 50g oleic acid (73% by mass, 0.129mol in moles) and 200ml glacial acetic acid, and place them in a water bath at 26°C with a concentration of 108mg / L and a flow rate of 0.08m 3 / h ozone stirring reaction 2.5h;

[0030] b. Heat up, when the temperature rises to 92°C, the flow rate is changed to 0.10m 3 / h of oxygen for 2 hours of cracking reaction;

[0031] c. Recover glacial acetic acid by rotary evaporation, and then put the residue into 1000-1100ml of hot water at 90-100°C for extraction;

[0032] d, let stand to separate the liquids, put the lower water layer into a refrigerator with a constant temperature of 5°C to cool for 16h, filter, and dry to obtain 17.1g of azelaic acid crude product from the reaction solution, the yield (in terms of oleic acid) is 70.3%, and the melting point is 96- 103°C, 88% purity;

[0033] e. Weigh 10 g of the crude product and put it into 80 g of ethyl acetate, stir and mix for 3 hours at a constant temperature of 24° ...

Embodiment 2

[0035] a. Stir and mix 51g oleic acid (73% by mass, 0.132mol in moles) and 200ml glacial acetic acid, and place them in an ice-water bath at 0°C with a concentration of 101mg / L and a flow rate of 0.10m 3 / h ozone stirring reaction for 1.5h;

[0036] b. Heating up, when the temperature rises to 80°C, the flow rate is changed to 0.10m 3 / h of oxygen, reaction 1.5h;

[0037] c. Recover glacial acetic acid by rotary evaporation, and immediately put the residue into 1100-1200ml of 90-100°C hot water for extraction;

[0038] d, let stand to separate the liquids, put the lower water layer into a refrigerator with a constant temperature of 5°C to cool for 15h, filter, dry and extract 16.8g of the product azelaic acid crude product from the reaction solution, the yield (in terms of oleic acid) is 67.7%, and the melting point 95-103°C, 86% purity;

[0039]e. Weigh 10 g of the crude product and put it into 63 g of ethyl acetate, stir and mix for 4 hours at a constant temperature of 10...

Embodiment 3

[0041] a. Stir and mix 50g oleic acid (73% by mass, 0.129mol in moles) and 200ml glacial acetic acid, and place them in a water bath at 40°C with a concentration of 96mg / L and a flow rate of 0.12m 3 / h of ozone 2h;

[0042] b. Heating up, when the temperature rises to 120°C, the flow rate is changed to 0.10m 3 / h of oxygen, reaction 2.5h;

[0043] c. Rotary evaporation reclaims glacial acetic acid. Immediately put the residue into 1200ml of hot water for extraction after spinning;

[0044] d. Stand still for liquid separation, put the lower water layer into the refrigerator to cool for 16h, filter, dry and extract from the reaction solution to obtain 16.5g of azelaic acid crude product, the yield (calculated as oleic acid) is 67.8%, and the melting point is 96-105°C , with a purity of 79%;

[0045] e. Put 10 g of this crude product in 40 g of ether, stir and mix at a constant temperature of 35 ° C for 2 hours, let it stand and filter, dry and extract from the extract to ob...

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Abstract

The invention discloses a separating purifying method of nonadioic acid, which comprises the following steps: oxidizing oleic acid through ozone; cracking; evaporating solvent; recycling; extracting substrate through hot water; crystallizing water phase after extracting; drying to obtain rough product of nonadioic acid; adding rough product of nonadioic acid into organic solvent; stirring; sucking; drying; obtaining the pure product of nonadioic acid. The invention removes monacid and insoluble impurity with purity of nonadioic acid over 98%, which provides clean manufacturing method.

Description

technical field [0001] The invention relates to a method for separating and purifying azelaic acid Background technique [0002] Azelaic acid, also known as azelaic acid, is a white to yellowish monoclinic prism, needle-like crystal or powder. Molecular formula C 9 h 16 o 4 , molecular weight 188.22, specific gravity 1.0291 (4°C), 1.225 (25°C), melting point 106.5°C, boiling point 286.5°C (13.33kPa), refractive index 1.4303 (111°C), medium-length carbon chain plus two carboxyl groups, giving Azelaic acid has a wide range of uses and is an important intermediate in organic synthesis. [0003] Azelaic acid can be used to synthesize dioctyl azelate (DOZ) plasticizer, synthetic perfume, lubricating oil and polyamide and other products. Dioctyl azelate, didecyl azelate, and tridecyl azelate are good lubricants. Azelaic acid is also used in the production of nylon 69 and nylon 9. Azelaic acid is aminated and hydrogenated to produce aminononanoic acid, which can be directly ...

Claims

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Application Information

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IPC IPC(8): C07C51/34C07C55/18
CPCY02P20/582
Inventor 吾满江·艾力周聪晓黄成坤董昕
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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