Preparation method of pentaerythritol tetrabasic acid ester

A technology for pentaerythritol tetra and pentaerythritol, which is applied in the field of preparation of pentaerythritol tetrabasic acid ester, can solve the problems of complex process, influence on high temperature performance of products, decomposition of pentaerythritol tetrabasic acid ester, etc., and achieves simple process, improved product appearance, and increased oxidation temperature. Effect

CN106631782AActive Publication Date: 2017-05-10CHINA PETROLEUM & CHEM CORP
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Publication Date
2017-05-10
Patent Text Reader

Abstract

The invention provides a preparation method of pentaerythritol tetrabasic acid ester. The method includes the steps of: a) mixing pentaerythritol, fatty acid and a catalyst to perform an esterification reaction to prepare a pentaerythritol tetrabasic acid ester crude product; and b) mixing the pentaerythritol tetrabasic acid ester crude product with a solid adsorbent to purify the crude product to obtain the pentaerythritol tetrabasic acid ester. Compared with the prior art, the preparation method can effectively remove impurities in the reaction system, so that the pentaerythritol tetrabasic acid ester has excellent high temperature performance. A test result proves that the content of impurity elements in the pentaerythritol tetrabasic acid ester prepared through the method is lower than 1 ppm. In addition, the pentaerythritol tetrabasic acid ester has better oxidizing performance, wherein the initial oxidization temperature thereof is increased by more than 10 DEG C in the same base oil.
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Description

technical field

[0001] The invention relates to the technical field of chemical industry, more specifically, relates to a preparation method of pentaerythritol tetrabasic acid ester. Background technique

[0002] Pentaerythritol tetrabasic acid ester is an important neopentyl polyol ester. Due to its large number of ester groups and no hydrogen atom on the β-position of the quaternary carbon atom, it can form a six-membered ring resonance structure with hydroxyl oxygen, and has good Oxidation stability, thermal stability, low temperature fluidity and viscosity temperature properties, widely used in aviation lubricants, automotive lubricants, air compressor oils and fire-resistant hydraulic oils and other fields.

[0003] The synthesis method of pentaerythritol tetrabasic acid ester mainly contains esterification method, acid chloride method and transesterification method, wherein, esterification method has advantages such as simple process, low cost, becomes the most commonl...

Examples

preparation example Construction

[0022] The invention provides a kind of preparation method of pentaerythritol tetrabasic acid ester, comprises the following steps:

[0023] a) Pentaerythritol, fatty acid and catalyst are mixed, carry out esterification reaction, obtain pentaerythritol tetrabasic acid ester crude product;

[0024] b) mixing the crude product of pentaerythritol tetrabasic acid ester with a solid adsorbent, and performing refining treatment to obtain pentaerythritol tetrabasic acid ester.

[0025] The present invention firstly mixes pentaerythritol, fatty acid and catalyst. In the present invention, the fatty acid is preferably selected from one or more saturated fatty acids with 1 to 10 carbon atoms, more preferably one or more saturated fatty acids with 4 to 10 carbon atoms, More preferably, it is one or more of butyric acid, pentanoic acid, hexanoic acid, heptanoic acid, octanoic acid and capric acid. In the present invention, the source of the fatty acid is not particularly limited, and c...

Embodiment 1

[0039](1) Mix 136g of pentaerythritol, 48.96g of n-valeric acid, 17.28g of n-heptanoic acid, 663.6g of 3,3,5-trimethylhexanoic acid and 5.1g of stannous oxide at 200°C and -0.05MPa vacuum , reflux reaction for 5h, and then vacuum deacidification to obtain 660g crude pentaerythritol tetrabasic ester, the acid value of the crude pentaerythritol tetrabasic ester tested by GB / T7304 was 0.5mgKOH / g.

[0040] (2) Mix the above-mentioned pentaerythritol tetrabasic acid ester crude product with 16.5g activated clay, stir at 100°C for 1h, filter the activated clay to obtain pentaerythritol tetrabasic acid ester, test the acid value of pentaerythritol tetrabasic acid ester is less than 0.1mgKOH / g .

[0041] The obtained pentaerythritol tetrabasic acid ester is carried out the accelerated oxidation test of oil product, experimental result shows, the impurity element content of the pentaerythritol tetrabasic acid ester that embodiment 1 obtains is less than 1ppm, and oxidation performance ...

Embodiment 2

[0044] (1) Mix 136g of pentaerythritol, 48.96g of n-valeric acid, 19.5g of n-octanoic acid, 663.6g of 3,3,5-trimethylhexanoic acid and 5.1g of stannous oxide, at 210°C and -0.06MPa vacuum, Reflux for 6 hours, and then carry out vacuum deacidification to obtain 662g of crude pentaerythritol tetrabasic ester. The acid value of the crude pentaerythritol tetrabasic ester was tested to be 0.5 mgKOH / g.

[0045] (2) Mix the above crude pentaerythritol tetrabasic acid ester with 6.62g of 5A molecular sieve and 6.62g of alumina, stir for 2h under vacuum at 110°C, filter the solid adsorbent to obtain pentaerythritol tetrabasic acid ester, test pentaerythritol tetrabasic acid ester The acid value of the acid ester is less than 0.1mgKOH / g.

[0046] The obtained pentaerythritol tetrabasic acid ester is carried out the accelerated oxidation test of oil product, and experimental result shows, the impurity element content of the pentaerythritol tetrabasic acid ester obtained in embodiment 2 i...