Synthesis method of high-purity pinacolone

A synthesis method and pinaconone technology are applied in the field of high-purity pinaconone synthesis, which can solve the problems such as the amount of hydrochloric acid used and by-products, and achieve the effect of high purity

Inactive Publication Date: 2017-02-01
ZHANGJIAGANG CITY ZHENFANG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The content of pinacolone produced by most manufacturers is 95%, the yield...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The synthetic method of high-purity pinacolone comprises:

[0022] Isoamyl and 36% hydrochloric acid are added to the addition catalyst zinc chloride, and reacted at 8°C to prepare chloropentane;

[0023] Condensate pentane chloride and formaldehyde under acidic conditions, add a condensation catalyst, and react for 5 hours at 70°C to prepare crude pinacolone. The condensation catalyst is a Zn / Co / Sb composite catalyst, Zn / Co / Sb composite catalyst The molar ratio of each component is 1:1:1, and the purity of the crude product reaches 82%.

[0024] Add 10% water to the crude product of pinacolone, directly heat and distill with steam, and rectify in the rectification tower under the condition of reflux ratio 1:2.5. The total yield of pinatone was 45%.

Embodiment 2

[0026] The synthetic method of high-purity pinacolone comprises:

[0027] Isoamyl and 30% hydrochloric acid are added to the addition catalyst zinc chloride, and reacted at 8°C to prepare chloropentane;

[0028] Condensate pentane chloride and formaldehyde under acidic conditions, add a condensation catalyst, react at 60°C for 5-7 hours to prepare crude pinacolone, the condensation catalyst is Zn / Co / Sb composite catalyst, Zn / Co / Sb composite The molar ratio of each component in the catalyst is 0.7:0.8:1; the purity of the crude product reaches 79%.

[0029] Add 12% water to the crude product of pinacolone, heat and distill directly with steam, and rectify in the rectification tower under the condition of reflux ratio 1:2.2. The total yield of pinatone was 38%.

Embodiment 3

[0031] The synthetic method of high-purity pinacolone comprises:

[0032] Isoamyl and 39% hydrochloric acid are added to the addition catalyst zinc chloride, and reacted at 4°C to prepare chloropentane;

[0033] Condensate pentane chloride and formaldehyde under acidic conditions, add a condensation catalyst, and react at 95°C for 6 hours to prepare crude pinacolone. The condensation catalyst is Zn / Co / Sb composite catalyst, Zn / Co / Sb composite catalyst The molar ratio of each component is 1:1.3:1, and the purity of the crude product reaches 80%.

[0034] Add 8% water to the crude product of pinacolone, heat and distill directly with steam, and rectify in the rectification tower under the condition of reflux ratio 1:2.8. The total yield of pinatone was 41%.

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Abstract

The invention discloses a synthesis method of high-purity pinacolone. The synthesis method of the high-purity pinacolone comprises the following steps: adding isoamylene and 30-39% of hydrochloric acid in zinc chloride as a hydrosilylation catalyst, and reacting at the temperature of 4-8 DEG C to prepare chloro t-pentane; condensing the chloro t-pentane and formaldehyde under an acidic condition, adding a condensation catalyst, and reacting for 5-7 hours at the temperature of 60-95 DEG C to prepare a pinacolone crude product; and adding 8-12% of water in the pinacolone crude product, directly heating and distilling with steam, and rectifying in a rectifying tower. By the method, the problem that a rectifying section is large in energy consumption and low in efficiency is solved, the pinacolone with high content of 98% is increased to be 45% from 15% in total yield, and the rectifying time is shortened to be 12 hours from 16 hours.

Description

technical field [0001] The application belongs to the technical fields of biology, new medicine and pesticide, and in particular relates to a method for synthesizing high-purity pinacolone. Background technique [0002] Because pinatonone is widely used in triazole fungicides (including pesticides and medicines), as well as new herbicides, and some new materials also use pinatonone as the main raw material, the market for pinatonone is also increasing. [0003] Pinacolone is generally used at home and abroad to hydrolyze pinacol and add isopentene with hydrochloric acid to form chloropentane, then react with formaldehyde and then dehydrate to form pinacolone. The content of pinacolone produced by most manufacturers is 95%, the yield is about 65%, and the usage amount and by-products of hydrochloric acid are more. Contents of the invention [0004] The object of the present invention is to provide a kind of synthetic method of high-purity pinacolone, to overcome the defic...

Claims

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Application Information

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IPC IPC(8): C07C45/45C07C49/04
CPCC07C45/45C07C17/08C07C49/04C07C19/01
Inventor 曹爱春赵松雪郁培华
Owner ZHANGJIAGANG CITY ZHENFANG CHEM
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