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1,3-cyclohexanedione preparation process

A production process and technology of cyclohexanedione, which is applied in the field of production technology of 1,3-cyclohexanedione, can solve problems such as poor safety and low production efficiency, achieve improved efficiency and service life, reduce emissions, reduce The effect of discharge

Pending Publication Date: 2020-02-21
湖北广富林生物制剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Aiming at the problems existing in the prior art, the present invention provides a production process of 1,3-cyclohexanedione, which solves the problems of low production efficiency and poor safety in the existing 1,3-cyclohexanedione production process

Method used

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  • 1,3-cyclohexanedione preparation process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: The technological process of 1,3-cyclohexanedione is as follows:

[0024] (1) Mixing: under stirring conditions, successively drop 450 parts by weight of water, 150 parts by weight of resorcinol, 50 parts by weight of sodium hydroxide (caustic soda), and a load-type compound containing 1 part by weight of active nickel into the batching tank. Catalyst slurry (including newly input catalyst and recycled catalyst), after the solid raw materials are fully mixed and dissolved, mixed solution A is obtained;

[0025] (2) Hydrogenation: Adjust the temperature of the microtubular reactor to 60°C, open the discharge valve of the batching kettle, the high-pressure diaphragm pump of the microtubular reactor and the valve of the buffer tank of the hydrogen compressor, and inject hydrogen, and the reaction pressure of the fixed system is 1.5Mpa, make the mixed solution A slowly flow through the microtubular reactor, and the time for the mixed solution A to flow through...

Embodiment 2

[0031] (1) Mixing: In the batching kettle, according to the proportioning of the process requirements, 440 parts by weight of water, 130 parts by weight of resorcinol, 40 parts by weight of sodium hydroxide (caustic soda), containing 1 weight part The loaded catalyst slurry (comprising the catalyst of new drop-in and the catalyst of recycling) of active nickel, treats that solid raw material is fully mixed and dissolved, obtains mixed solution A;

[0032] (2) Hydrogenation: Adjust the temperature of the microtubular reactor to 80°C, open the discharge valve of the batching kettle, the high-pressure diaphragm pump of the microtubular reactor and the valve of the buffer tank of the hydrogen compressor, and the reaction pressure of the fixed system is the reaction pressure of the fixed system is 1.5Mpa, make the mixed solution A slowly flow through the microtubular reactor, and the time for the mixed solution A to flow through the microtubular reactor is 80s;

[0033] (3) Materia...

Embodiment 3

[0038] (1) Mixing: In the batching kettle, according to the proportioning of the process requirements, 460 parts by weight of water, 150 parts by weight of resorcinol, 40 parts by weight of sodium hydroxide (caustic soda), containing 1 weight part The loaded catalyst slurry (comprising the catalyst of new drop-in and the catalyst of recycling) of active nickel, treats that solid raw material is fully mixed and dissolved, obtains mixed solution A;

[0039] (2) Hydrogenation: Adjust the parallel micro-tubular reactor to a temperature of 70°C, open the discharge valve of the batching kettle, the high-pressure diaphragm pump of the micro-tubular reactor and the valve of the buffer tank of the hydrogen compressor, and the reaction pressure of the fixed system is the fixed system The reaction pressure is 1.5Mpa, so that the mixed solution A slowly flows through the microtubular reactor, and the time for the mixed solution A to flow through the microtubular reactor is 60s;

[0040] (...

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Abstract

The invention discloses a 1,3-cyclohexanedione preparation method, which comprises: mixing water, resorcinol, sodium hydroxide and a catalyst, pumping the mixture into a micro-tube reactor, introducing hydrogen into the micro-tube reactor by using a hydrogen compressor buffer tank, making the reacted materials enter a settling separator, and separating, wherein the excessive hydrogen returns to the hydrogen compressor buffer tank so as to be cyclically utilized through a hydrogen collecting pipe at the upper portion of the settling separator; and dividing the materials settled to the bottom ofthe settling separator into a catalyst slurry and a mixed solution B, making the catalyst re-enter a material preparing kettle so as to be cyclically utilized through a valve at the bottom of the settling separator, sucking the mixed solution B into an acidification kettle, and carrying out acid precipitation to obtain the 1,3-cyclohexanedione. According to the invention, the production process increases the reaction speed, reduces the generation of side reactions, increases the yield of 1,3-cyclohexanedione to more than 94% by recycling the hydrogen and the catalyst, and improves the production efficiency and the safety.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a production process of 1,3-cyclohexanedione. Background technique [0002] 1,3-cyclohexanedione, also known as hexadecyl oxirane, is mainly used as a pharmaceutical intermediate for organic synthesis, and is an intermediate of herbicides sulcotrione and mesotrione. The existing 1,3-cyclohexanedione synthesis method generally uses resorcinol and hydrogen as raw materials: put resorcinol and sodium hydroxide solution into a high-pressure reactor, add a nickel catalyst, and 100 atmospheric pressure hydrogen reaction 10-12h. Then lower the temperature, release the pressure, filter out the catalyst, acidify the filtrate with concentrated hydrochloric acid, cool to 0°C, and filter out the crystals, that is, 1,3-cyclohexanedione resorcinol. Due to the excessive hydrogen used in the reduction reaction, the excess hydrogen will be discharged into the air after the reaction ...

Claims

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Application Information

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IPC IPC(8): C07C45/00C07C49/713C07C45/51C07C49/403B01J19/00
CPCC07C45/006C07C45/512B01J19/0093C07C2601/14C07C49/713C07C49/403Y02P20/584
Inventor 张晓臣李萍张强牛巍
Owner 湖北广富林生物制剂有限公司