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Low-temperature purification and separation process for fatty acid lower alcohol ester plasticizers based on palm oil

An ester plasticizer, purification and separation technology, used in the preparation of carboxylate, organic chemistry, chemical instruments and methods, etc., can solve the problems of narrow application range and complex process flow, and achieve sufficient and stable sources and simple process methods. , the effect of reducing environmental pollution

Inactive Publication Date: 2018-03-27
北京林氏精化新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, the patent application number CN200810227650.4 discloses a method for separating saturated fatty acid methyl esters from biodiesel, its technological process is more complex than the present invention, and its application range is narrower
There is no report on the low-temperature purification and separation process of fatty acid ester plasticizers based on palm oil, especially the low-carbon alcohol esters of epoxy fatty acids.

Method used

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  • Low-temperature purification and separation process for fatty acid lower alcohol ester plasticizers based on palm oil
  • Low-temperature purification and separation process for fatty acid lower alcohol ester plasticizers based on palm oil
  • Low-temperature purification and separation process for fatty acid lower alcohol ester plasticizers based on palm oil

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Embodiment 1

[0028] A low-temperature purification and separation process for fatty acid low-carbon alcohol ester plasticizers based on palm oil, the separation process is the separation method of fatty acid low-carbon alcohol esters and epoxy fatty acid low-carbon alcohol esters generated in the preparation of plasticizers, the method is as follows :

[0029] (1) melting the homemade fatty acid lower alcohol ester or epoxy fatty acid lower alcohol ester at a separation temperature of 30-40° C., and separating and removing the high melting point solid;

[0030] (2) The remaining liquid fatty acid lower alcohol ester or epoxy fatty acid lower alcohol ester is uniformly mixed with the crystallization solvent at a mixing temperature of 20-50°C in a certain volume ratio;

[0031] (3) Control the cooling rate to 0.02-2°C / min. After cooling down to the crystallization temperature of -20-15°C, the cooling rate is 0.02-2°C / min. Keep the temperature and cultivate the crystal for 1-48 hours, and the...

Embodiment 2

[0041]Add 100 parts of epoxy fatty acid ethyl ester self-made from palm oil into the separation kettle, heat to 30° C., and remove the insoluble solid by suction filtration. Add 2 times the volume of pre-prepared acetone-ethanol solution to the remaining liquid epoxy fatty acid ethyl ester, wherein ethanol accounts for 70 wt%, and the rest is acetone, and mix well at 20°C. Under the condition that the cooling rate is controlled to be 0.5°C / min, the temperature is lowered to 10°C, and the temperature is kept in a water bath at a constant temperature of 10°C for 48 hours, and crystals are precipitated from the solution. Filter and separate the crystal and the solution, wash the crystal with ethanol and dry under reduced pressure to obtain ethyl palmitate with a purity greater than 90%; the solution is distilled under reduced pressure to remove ethanol and acetone to obtain ethyl epoxy fatty acid ethyl ester, wherein the ethyl epoxy oleate content is greater than 90%

Embodiment 3

[0043] Add 100 parts of fatty acid n-decyl esters made by palm oil into the separation kettle, heat to 40° C., and remove the insoluble solids by suction filtration. Add 5 times the volume of pre-prepared butanol solution to the remaining liquid n-decyl fatty acid ester, wherein butanol accounts for 100 wt%, and mix uniformly at 50°C. Under the condition that the cooling rate is controlled at 2°C / min, the temperature is lowered to 15°C, and the temperature is kept in a water bath at a constant temperature of 15°C for 24 hours, and crystals are precipitated from the solution. Centrifuge the crystals and solution, wash the crystals with ethanol and dry under reduced pressure to obtain n-decyl palmitate with a purity of not less than 85%; distill the solution under reduced pressure to remove butanol to obtain n-decyl unsaturated fatty acids, of which n-decyl oleate content Greater than 90%.

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Abstract

The invention discloses a low-temperature purification and separation process for fatty acid lower alcohol ester plasticizers based on palm oil. According to the process, micromolecular alcohol is used as a solvent; programmed cooling is carried out to allow methyl palmitate with a high-melting point to be precipitated through crystallization; and palmitate and unsaturated fatty acid esters in fatty acid lower alcohol esters are almost separated and purified by using the process. The process provided by the invention is low in energy consumption, simple in process, good in operability and friendly to environment. Products obtained through multiple separation operations are high in purity and widely applicable to industrial fields like plastics and rubber, are good substitutes for petroleumproducts and have good development prospects.

Description

technical field [0001] The invention relates to a separation process of fatty acid low-carbon alcohol esters, in particular to a low-temperature purification and separation process of palm oil-based fatty acid low-carbon alcohol ester plasticizers. Background technique [0002] Plasticizer is a chemical additive commonly used in plastic production. Its main function is to increase the plasticity and fluidity of polymers and make plastic products flexible. At present, the most widely used plasticizers are phthalate plasticizers, but these plasticizers are derived from petroleum products, which are non-renewable resources; and contain benzene rings, which are toxic and not easy to degrade. It seriously threatens people's health and living environment. At present, people have successively developed a series of products to replace phthalate plasticizers, such as epoxy vegetable oils, citric acid esters, polybasic fatty acid esters, organic phosphoric acid esters, etc. Among th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/52C07C69/24C07C69/58C07C69/587C07D303/42C07D301/32
CPCC07C67/52C07D301/32C07D303/42C07C69/24C07C69/58C07C69/587
Inventor 林金河李宗起林洪凯
Owner 北京林氏精化新材料有限公司
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