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Preparation method of pinacolone

A technology of pinatonone and isopentene, which is applied in the field of pinatone preparation, can solve the problems of hydrochloric acid usage, many by-products, etc., and achieve the effect of high yield

Pending Publication Date: 2017-02-15
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 is about 65%, and the amount of hydrochloric acid used and by-products are more

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The preparation method of pinatone comprises:

[0020] (1), isopentene addition reaction

[0021] Add isopentene to 30% hydrochloric acid, the ratio of isopentene to hydrochloric acid is 1:2.8, heat up for 5 hours to 25°C, then continue to heat up to 65°C in the condensation kettle, and heat up for 5 hours to obtain Chloropentane;

[0022] (2) Condensation reaction between pentane chloride and formaldehyde

[0023] Formaldehyde was added dropwise to chlorpentane, the molar ratio of chlorpentane to formaldehyde was 1:1.2, the temperature was raised to 90°C while adding dropwise, the time of dropping was 6 hours, and then kept for 2.5 hours, separated into layers to obtain Crude pinatone.

[0024] (3), the pinatone crude product is purified

[0025] Add 10% water to the crude product of pinacolone, use steam to directly heat and distill, and rectify in the rectification column with a reflux ratio of 1:2.5.

[0026] The yield of pinatone was 67.8%.

Embodiment 2

[0028] The preparation method of pinatone comprises:

[0029] (1), isopentene addition reaction

[0030] Add isopentene to 30% hydrochloric acid, the ratio of isopentene to hydrochloric acid is 1:2.8, heat up for 4-6 hours to 25°C, then continue to heat up to 65°C in the condensation kettle, and the heating time is 4 hours , to obtain chloropentane;

[0031] (2) Condensation reaction between pentane chloride and formaldehyde

[0032] Formaldehyde was added dropwise to chlorpentane, the molar ratio of chlorpentane to formaldehyde was 1:1.3, the temperature was raised to 90°C while adding dropwise, the time of dropping was 6 hours, and then kept for 1.5 hours, separated into layers to obtain Crude pinatone.

[0033] (3), the pinatone crude product is purified

[0034] Add 10% water to the crude product of pinacolone, use steam to directly heat and distill, and rectify in the rectification column with a reflux ratio of 1:3.

[0035] The yield of pinatone was 67.1%.

Embodiment 3

[0037] The preparation method of pinatone comprises:

[0038] (1), isopentene addition reaction

[0039] Add isopentene to 30% hydrochloric acid, the ratio of isopentene to hydrochloric acid is 1:2.8, heat up for 4 to 6 hours to 25°C, then continue to heat up to 65°C in the condensation kettle, and the heating time is 6 hours , to obtain chloropentane;

[0040] (2) Condensation reaction between pentane chloride and formaldehyde

[0041] Formaldehyde was added dropwise to chlorpentane, the molar ratio of chlorpentane to formaldehyde was 1:1.2, the temperature was raised to 90°C while adding dropwise, the time of dropping was 6 hours, and then kept for 2.5 hours, separated into layers to obtain Crude pinatone.

[0042] (3), the pinatone crude product is purified

[0043] Add 10% water to the crude product of pinacolone, use steam to directly heat and distill, and rectify in the rectification column with a reflux ratio of 1:3.

[0044] The yield of pinatone was 67.3%.

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Abstract

The invention discloses a preparation method of pinacolone. The method includes: (1) isopentene addition reaction: adding isopentene into hydrochloric acid, performing heating for 4-6h to 25DEG C, then further conducting heating to 65DEG C for 4-6h, thus obtaining chloro-tert-pentane; and (2) condensation reaction of chloro-tert-pentane and formaldehyde: adding formaldehyde dropwise into chloro-tert-pentane for 4-6h, and performing heating at the same time to 88-90DEG C, then conducting heat preservation for 1.5-2.5h, and carrying out layering, thus obtaining a pinacolone crude product. The method provided by the invention can achieve high pinacolone yield up to 67% or more.

Description

technical field [0001] The application belongs to the technical fields of biology, new medicine and pesticide, and in particular relates to a preparation method of 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 pinatonone preparation method, to overcome the deficiencies in the prior art. ...

Claims

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Application Information

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IPC IPC(8): C07C45/45C07C49/04C07C17/08C07C19/01
CPCC07C45/45C07C17/08C07C45/82C07C49/04C07C19/01
Inventor 曹爱春赵松雪郁培华
Owner ZHANGJIAGANG CITY ZHENFANG CHEM
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