CN1373119A - Process for synthesis of pentaerythritol tetraheptanoate by catalysis of phosphotungstic acid - Google Patents
Process for synthesis of pentaerythritol tetraheptanoate by catalysis of phosphotungstic acid Download PDFInfo
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- CN1373119A CN1373119A CN 02110015 CN02110015A CN1373119A CN 1373119 A CN1373119 A CN 1373119A CN 02110015 CN02110015 CN 02110015 CN 02110015 A CN02110015 A CN 02110015A CN 1373119 A CN1373119 A CN 1373119A
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- acid
- tetramethylolmethane
- catalysis
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- pentaerythritol
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A process for catalytically synthesizing pentaerythritol tetraheptanoate is characterized by that the pentaerythritol and heptanoic acid in a mole ratio of 1:(5-7) are used as raw materials and the phosphotungstic acid is used as catalyst. Its advantages are high catalytic effect, high esterifying rate, short reaction time and low cost.
Description
Technical field:
The present invention relates to a kind of processing method of polyvalent alcohol esterification, concrete is a kind of method of synthesis of pentaerythritol tetraheptanoate by catalysis of phosphotungstic acid.
Background technology:
Pentaerythritol tetraheptanoate is a kind of polyol ester with potentiality to be exploited.Because the special chemical structure of polyvalent alcohol, make by such ester as the lubricating oil of base oil also to have good viscosity temperature characteristic, lubricity and excellent low temperature viscosity characteristic except having excellent heat-resistant quality and oxidation stability.General esterification is to carry out under the katalysis of the vitriol oil or strong phosphoric acid, especially the esterification of polyol ester, as pentaerythritol ester etc., because the branch of its molecule is more, steric effect is big, the esterification difficulty, not only require the reaction times at 10～16h, and must control vacuum tightness well in the entire reaction stage, and the difficult control of condition, product is difficult purifies etc.; Spent acid not only can etching apparatus in addition, and causes environmental pollution.
Summary of the invention:
The present invention is intended to overcome above-mentioned the deficiencies in the prior art, provides a kind of and can effectively shorten esterification time, the method for the synthesis of pentaerythritol tetraheptanoate by catalysis of phosphotungstic acid that reduces production costs.
The present invention adopts tetramethylolmethane and enanthic acid to make raw material, and with phosphomolybdic acid catalyst, the mol ratio of tetramethylolmethane and enanthic acid is 1: 5-7; Phospho-wolframic acid is counted the 1-3% of tetramethylolmethane weight according to weight percent.
Step of the present invention is: (1) is added to tetramethylolmethane, enanthic acid, phospho-wolframic acid in the there-necked flask that has the water trap reflux in proportion, is heated to 120-160 ℃, refluxes about 2 hours, does not only appear as to there being the globule; (2) after reaction finishes, precipitate and isolate catalyzer, inclining reaction solution; (3) underpressure distillation depickling obtains pentaerythritol tetraheptanoate.
Heteropoly compound is the multinuclear macromolecular compound that a class contains oxo bridge, and its feature is the catalytic activity height, and selectivity is good, and reproduction speed is fast.The present invention adopts synthesis of pentaerythritol tetraheptanoate by catalysis of phosphotungstic acid, and the result shows that this catalyzer has catalytic activity and stability preferably.
The inventive method excellent catalytic effect, the esterification yield height has shortened the reaction times, has optimized reaction conditions, has reduced production cost.
Embodiment:
The mol ratio of tetramethylolmethane and enanthic acid is 1: 5; Phospho-wolframic acid is counted 1% of tetramethylolmethane weight according to weight percent.Can obtain pentaerythritol tetraheptanoate by abovementioned steps.
Claims (2)
1, a kind of method of synthesis of pentaerythritol tetraheptanoate by catalysis of phosphotungstic acid is characterized in that adopting tetramethylolmethane and enanthic acid to make raw material, and with phosphomolybdic acid catalyst, the mol ratio of tetramethylolmethane and enanthic acid is 1: 5-7; Phospho-wolframic acid is counted the 1-3% of tetramethylolmethane weight according to weight percent.
2, the method for synthesis of pentaerythritol tetraheptanoate by catalysis of phosphotungstic acid as claimed in claim 1, it is characterized in that: (1) is added to tetramethylolmethane, enanthic acid, phospho-wolframic acid in the there-necked flask that has the water trap reflux in proportion, be heated to 120-160, refluxed about 2 hours, and only do not appear as to there being the globule; (2) after reaction finishes, precipitate and isolate catalyzer, inclining reaction solution; (3) underpressure distillation depickling obtains pentaerythritol tetraheptanoate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02110015 CN1373119A (en) | 2002-02-07 | 2002-02-07 | Process for synthesis of pentaerythritol tetraheptanoate by catalysis of phosphotungstic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02110015 CN1373119A (en) | 2002-02-07 | 2002-02-07 | Process for synthesis of pentaerythritol tetraheptanoate by catalysis of phosphotungstic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1373119A true CN1373119A (en) | 2002-10-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02110015 Pending CN1373119A (en) | 2002-02-07 | 2002-02-07 | Process for synthesis of pentaerythritol tetraheptanoate by catalysis of phosphotungstic acid |
Country Status (1)
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| CN (1) | CN1373119A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086420A (en) * | 2014-06-30 | 2014-10-08 | 海盐县精细化工有限公司 | Method for preparing high-quality pentaerythritol high-carbon fatty acid ester by adopting extraction process |
| CN113698372A (en) * | 2021-09-29 | 2021-11-26 | 安徽中烟工业有限责任公司 | Preparation method of alkyl carboxylic acid furfuryl ester |
-
2002
- 2002-02-07 CN CN 02110015 patent/CN1373119A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104086420A (en) * | 2014-06-30 | 2014-10-08 | 海盐县精细化工有限公司 | Method for preparing high-quality pentaerythritol high-carbon fatty acid ester by adopting extraction process |
| CN104086420B (en) * | 2014-06-30 | 2016-05-11 | 海盐县精细化工有限公司 | Produce the method for high-quality pentaerythrite high-carbon fatty acid ester with extraction process |
| CN113698372A (en) * | 2021-09-29 | 2021-11-26 | 安徽中烟工业有限责任公司 | Preparation method of alkyl carboxylic acid furfuryl ester |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |