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Preparation method of neo-pentyl polyhydric alcohol heptanoic acid ester

A technology of neopentyl polyol and alcohol heptanoate, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, organic chemistry, etc., can solve the problems of limited lifespan, and save high energy consumption, water washing and phase separation , the effect of avoiding dangerous and harmful factors

Inactive Publication Date: 2015-11-04
NANTONG BAICHUAN NEW MATERIAL CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Even though some solid catalysts can be recycled, as the active components of the solid-supported catalysts are continuously eluted during use, in fact these catalysts can be reused for a limited lifespan

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A kind of preparation method of neopentyl polyhydric alcohol heptanoate adopts trimethylol propane and heptanoic acid as raw material, and concrete steps comprise:

[0045] Step S1: For the current batch of trimethylolpropane and heptanoic acid purchased, since the number of hydroxyl groups contained in one molecule of trimethylolpropane is 3, the theoretical molar ratio of heptanoic acid to trimethylolpropane is 3;

[0046] Step S2: Set the molar ratio of heptanoic acid and trimethylolpropane in this small test. According to the experience obtained from previous synthesis, the more suitable molar ratio of trimethylolpropane and heptanoic acid is 1.05:3;

[0047] Step S3: For a small test, first put a magnetic stirrer in a 500mL three-necked bottle, put in 1.2mol (156.216g) of heptanoic acid, then put in 0.42mol (56.351g) of trimethylolpropane accordingly, and turn on the oil bath The temperature rise switch of the heater is used to heat the materials in the kettle...

Embodiment 2

[0057] A method for producing ditrimethylolpropane heptanoate, adopting ditrimethylolpropane and heptanoic acid as raw materials, the specific steps comprising:

[0058] Step S1: For the current batch of ditrimethylolpropane and heptanoic acid purchased, there are 4 hydroxyl groups in a ditrimethylolpropane molecule, and the theoretical molar ratio of heptanoic acid to ditrimethylolpropane is 4;

[0059] Step S2: Set the molar ratio of heptanoic acid and ditrimethylolpropane in this small test, and combine the experience and theoretical molar ratio obtained from the previous synthesis, the molar ratio of ditrimethylolpropane and heptanoic acid is more appropriate is 1.05:4;

[0060] Step S3: For a small test, in a 500mL three-necked bottle, first put a magnetic stirrer, put in 1.2mol (156.216g) of heptanoic acid, and then put in 0.315mol (78.854g) of ditrimethylolpropane accordingly, and turn on the oil The temperature rise switch of the bath heater heats the materials i...

Embodiment 3

[0070] A kind of preparation method of neopentyl polyol enanthate, adopt pentaerythritol and heptanoic acid as raw material, concrete steps are as follows:

[0071] Step S1: For the current batch of pentaerythritol and heptanoic acid purchased, there are 4 hydroxyl groups in one pentaerythritol molecule, so the theoretical molar ratio of heptanoic acid to pentaerythritol is 4;

[0072] Step S2: Set the molar ratio of heptanoic acid and pentaerythritol in this small test, first adopt the theoretical molar ratio of the two 1:4;

[0073] Step S3: For a small test, first put a magnetic stirrer in a 500mL three-necked bottle, put in 1.2mol (156.216g) of heptanoic acid, and then put in 0.3mol (40.845g) of pentaerythritol accordingly, and turn on the temperature rise of the oil bath heater Switch on and off to heat the materials in the kettle. When the temperature in the kettle rises to 110°C, add 1% (1.97g) p-toluenesulfonic acid with a total mass of 197.061g of heptanoic acid ...

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Abstract

The invention relates to a preparation method of a neo-pentyl polyhydric alcohol heptanoic acid ester. According to the preparation method, neo-pentyl polyhydric alcohol and heptylic acid are obtained via different batches; theoretical molar ratio required by complete esterification with heptylic acid is determined based on the number of hydroxy groups in neo-pentyl polyhydric alcohol or mixed neo-pentyl polyhydric alcohol molecules, or a plurality of pilot tests are carried out based on experience molar ratio of neo-pentyl polyhydric alcohol or mixed neo-pentyl polyhydric alcohol with heptylic acid; when the acid value of a pilot test sample is 1.5mgKOH / g or lower, and separation performance of a synthetic liquid with water is excellent, testing is stopped, and the raw material batch and the raw material ratio are used for large-scale production. The preparation method is capable of realizing full utilization of the raw materials, and avoiding troubles caused by product postprocessing.

Description

technical field [0001] The invention belongs to the field of organic chemical raw material production, in particular to a preparation process of neopentyl polyol enanthate. Background technique [0002] Among the many fatty acid esters, there is a type of fatty acid ester with a special structure of quaternary carbon atoms, also known as neopentyl structure. Typical examples are: pentaerythritol fatty acid ester, dipentaerythritol fatty acid ester, trimethylolpropane fatty acid ester Ester, ditrimethylolpropane fatty acid ester, neopentyl glycol fatty acid ester, they are favored by people. Because there is no hydrogen atom on the β carbon atom of the carbonyl of these neopentyl fatty acid esters, it cannot form a six-atom ring resonance structure with the carbon and hydrogen of the alcohol part of the ester group. Only high energy can destroy such an ester structure. , which makes the anti-oxidation and anti-elimination reaction stability of neopentyl polyol fatty acid est...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/56C07C69/33
CPCC07C67/08C07C67/56C07C69/33
Inventor 薛建军孙百亚潘洁肖春生
Owner NANTONG BAICHUAN NEW MATERIAL CO LTD