Preparation method of pentaerythritol ester

A technology of pentaerythritol ester and pentaerythritol, which is applied in the field of preparation of pentaerythritol ester and can solve problems such as negative influence on comprehensive performance of oil products

Active Publication Date: 2014-01-29
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, more cumbersome processes are often used to remove the residual catalyst, and while removing the catal

Method used

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preparation example Construction

[0019] The embodiment of the present invention discloses a kind of preparation method of pentaerythritol ester, comprises the following steps:

[0020] The pentaerythritol, fatty acid and activated carbon are reacted for the first time under the action of catalyst at 150-220°C and -0.03--0.07MPa vacuum to obtain the first reaction product;

[0021] Refluxing the first reaction product at 220 to 250°C under a vacuum of -0.05 to -0.095MPa to obtain a second reaction product;

[0022] Vacuumize the second reaction product below -0.098MPa, and filter after the third reaction to obtain pentaerythritol ester.

[0023] According to the present invention, in the process of preparing pentaerythritol ester, first react pentaerythritol and fatty acid for the first time, the conditions of the first reaction are 150~220° C. It can ensure the full reaction of pentaerythritol and fatty acid. The fatty acid is preferably one or more of butyric acid, caproic acid, caprylic acid and capric ac...

Embodiment 1

[0031] 15g of pentaerythritol, 80g of butyric acid, and 0.3g of activated carbon were reacted for 5 hours under the action of 0.8g of concentrated sulfuric acid at 160-180°C and -0.03--0.04MPa vacuum to fully react butyric acid and pentaerythritol; ~230°C, -0.05~-0.06MPa under vacuum for 3 hours to remove the residual compound catalyst in the ester molecule; then pull out the excess acid under vacuum below -0.06MPa; at 100~120°C, ~-0.06MPa under vacuum and stirring for 2 hours, then cooled to below 40°C and filtered to obtain pentaerythritol ester; the concentration of sulfuric acid was 98wt%. Experimental results show that the purity of pentaerythritol ester is 99.5wt%.

Embodiment 2

[0033] 18g of pentaerythritol, 80g of hexanoic acid, and 0.8g of activated carbon were reacted for 7 hours under the action of 0.5g of concentrated sulfuric acid at 170 to 200°C and -0.05 to -0.07MPa in vacuum to fully react hexanoic acid and pentaerythritol; ~230°C, -0.07~-0.09MPa under vacuum for 3 hours to remove the remaining combined catalyst in the ester molecule; then pull out the excess acid under -0.08MPa vacuum; at 130~140°C, -0.07~-0.08 Stir under MPa vacuum for 2 hours, then cool down to 30°C and filter to obtain pentaerythritol ester; the concentration of sulfuric acid is 98wt%. Experimental results show that the purity of pentaerythritol ester is 99.52wt%.

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Abstract

The invention provides a preparation method of pentaerythritol ester. The preparation method comprises following steps: pentaerythritol, a fatty acid and active carbon are reacted for a first time at a temperature of 150 to 220 DEG C, under a pressure of -0.03 to -0.07MPa so as to obtain a first reaction product; the first reaction product is subjected to reflux at a temperature of 220 to 250 DEG C, under a pressure of -0.05 to -0.095MPa so as to obtain a second reaction product; and the second reaction product is subjected to third reaction under a pressure of -0.098MPa so as to obtain pentaerythritol ester. Technological parameters of the esterification step are adjusted, so that residual catalyst is removed, production technology is simplified, purity of the obtained product is increased, more excellent combination properties of the obtained product are ensured, and coking resistance at high temperature and low temperature stability of the obtained product under harsh conditions are achieved.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of pentaerythritol ester. Background technique [0002] Pentaerythritol ester has excellent thermal stability and oxidation stability because there is no active hydrogen atom at the carbon atom of the alcohol end in the molecule. Therefore, pentaerythritol ester has excellent high and low temperature performance, high flash point, and low pour point. It is used as aviation engine oil, high temperature chain oil, synthetic air compressor oil and refrigerating machine oil base oil compatible with environmentally friendly refrigerants; it can also be blended with polyalphaolefin oil to improve polyalphaolefin oil to make rubber shrinkage and The defect of poor compatibility of additives can be used as base oil for internal combustion engine oil, gear oil and other oil products. [0003] As pentaerythritol ester, it is often used in harsh working condi...

Claims

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Application Information

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IPC IPC(8): C07C69/33C07C67/08C07C67/48
CPCC07C67/08C07C69/33
Inventor 梅莉刘月皞李霞李玉平熊瑶马楷
Owner CHINA PETROLEUM & CHEM CORP
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