Extraction method of tebuconazole intermediate ketene

An extraction method and a technology for ketene, which are applied in the field of extraction of tebuconazole intermediate ketene, can solve the problems of large environmental impact and difficulty in implementing a grinding method, improve the reaction yield and reduce connizzaro. Reaction, the effect of reducing side reaction products

Active Publication Date: 2017-03-08
内蒙古沙洲化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Tebuconazole intermediate enone generally adopts p-chlorobenzaldehyde and pinacolone at home and abroad to condense in methanol solution under the condition of sodium hydroxide catalysis, and it is also reported that p-chl

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Tebuconazole intermediate enone extraction method:

[0017] The preparation method of pinacolone comprises: carry out the condensation reaction of chloropentane and formaldehyde under acidic conditions, catalyze with Zn / Co / Sb composite catalyst, the reaction temperature is 60 ℃, the reaction time is 4h, Zn / Co The ratio between the sum of the amount of substance of each component in the / Sb composite catalyst and the amount of substance of chloropentane is 3:50;

[0018] Using p-chlorobenzaldehyde and pinacolone as raw materials, add a composite catalyst and react in a methanol solvent system for 5 hours, the reaction temperature is 60°C, after the reaction is completed, the temperature is lowered to below 10°C, and the crystallized enone is filtered out. Wash with methanol, the mother liquor is applied mechanically for 5 times, the composite catalyst is a Zn / Co / Sb composite catalyst, and in the Zn / Co / Sb composite catalyst, the molar ratio of Zn:Co:Sb is 0.7:0.5:1.2 . ...

Embodiment 2

[0020] Tebuconazole intermediate enone extraction method:

[0021] The preparation method of pinacolone comprises: carry out condensation reaction under acidic condition by chloropentane and formaldehyde, carry out catalysis with Zn / Co / Sb composite catalyst, reaction temperature is 85 ℃, reaction time is 5h, Zn / Co The ratio between the sum of the amount of substance of each component in the / Sb composite catalyst and the amount of substance of chloropentane is 3:50;

[0022] Using p-chlorobenzaldehyde and pinacolone as raw materials, add a composite catalyst and react in a methanol solvent system for 5 hours, the reaction temperature is 60°C, after the reaction is completed, the temperature is lowered to below 10°C, and the crystallized enone is filtered out. Washing with methanol, the mother liquor is applied mechanically for 5 times, the composite catalyst is a Zn / Co / Sb composite catalyst, and in the Zn / Co / Sb composite catalyst, the molar ratio of Zn:Co:Sb is 1:0.7:1.2 .

Embodiment 3

[0024] Tebuconazole intermediate enone extraction method:

[0025] The preparation method of pinacolone comprises: carry out condensation reaction under acidic condition by chloropentane and formaldehyde, carry out catalysis with Zn / Co / Sb composite catalyst, reaction temperature is 95 ℃, reaction time is 5h, Zn / Co The ratio between the sum of the amount of substance of each component in the / Sb composite catalyst and the amount of substance of chloropentane is 3:50;

[0026] Using p-chlorobenzaldehyde and pinacolone as raw materials, add a composite catalyst and react in a methanol solvent system for 8 hours, the reaction temperature is 60°C, after the reaction is completed, the temperature is lowered to below 10°C, and the crystallized enone is filtered out. Washing with methanol, the mother liquor is applied mechanically for 5 times, the composite catalyst is a Zn / Co / Sb composite catalyst, and in the Zn / Co / Sb composite catalyst, the molar ratio of Zn:Co:Sb is 1.2:0.5:1 .

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Abstract

The application discloses an extraction method of a tebuconazole intermediate ketene, which comprises the following steps of: taking p-chlorobenzaldehyde and pinacolone as raw materials; adding a compound catalyst and carrying out reaction in a methanol solvent system for 5-8 hours at a reaction temperature of 50-60 DEG C; after the reaction is finished, cooling a reactant to a temperature below 10 DEG C; carrying out pumping filtration on crystallized ketene and washing the ketene with methanol; and using mother liquor for many times. The method solves the problems of large product residual amount in the mother liquor and large mother liquor processing amount. The reaction yield is improved by 6%, the mother liquor processing amount is reduced, and the cost is greatly reduced.

Description

technical field [0001] The application belongs to the technical field of biology and new pesticides, and in particular relates to a method for extracting tebuconazole intermediate enone. Background technique [0002] Tebuconazole intermediate enone generally adopts p-chlorobenzaldehyde and pinacolone at home and abroad to condense in methanol solution under the condition of sodium hydroxide catalysis, and it is also reported that p-chlorobenzaldehyde and pinacolone, Sodium hydroxide is directly condensed, but the grinding method is quite difficult to implement in large-scale production, and the impact on the environment is much greater than that in the reactor. Contents of the invention [0003] In order to overcome the deficiencies of the prior art, the invention improves the process and proposes a process for reducing by-products and increasing yield. [0004] To achieve the above object, the present invention provides the following technical solutions: [0005] The em...

Claims

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Application Information

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IPC IPC(8): C07C49/235B01J23/843C07C45/74
CPCB01J23/8435C07C45/74C07C49/235
Inventor 曹爱春赵松雪郁培华
Owner 内蒙古沙洲化学科技有限公司
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