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Method and system for continuous kettle type industrial production of crude acetal product

A production method and technology of continuous kettle, applied in the field of continuous kettle industrial production method and system of crude acetal, can solve the problems of material and energy loss, unsuitability for large-scale industrial production, prolonging production cycle, etc., to achieve acetal The content is increased, which is beneficial to large-scale industrial production and the effect of inhibiting side reactions

Active Publication Date: 2020-04-17
LIER CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Auxiliary operations such as loading and unloading are required in the batch production process, which will easily cause material and energy losses, increase production costs, prolong the production cycle, and the product quality is not easy to stabilize
Batch-type production is likely to cause the volatilization of toxic, flammable and explosive solvents, which will have a certain impact on human health and increase the risk level of safety production
Batch kettle production is not suitable for large-scale industrial production

Method used

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  • Method and system for continuous kettle type industrial production of crude acetal product
  • Method and system for continuous kettle type industrial production of crude acetal product
  • Method and system for continuous kettle type industrial production of crude acetal product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Load the crude acetal product into the continuous tank reactor 100 for pre-filling and laying the bottom, start stirring, and keep warm at 25-30°C; then turn on the diethyl methylphosphinate supply pump 200 and adjust the flow rate to 36.2kg / h, and turn on the propylene The mixed solution of aldehyde and glacial acetic acid is supplied to the pump 300 and the flow rate is adjusted to 28.8kg / h. At the same time, the flow rate of the heat exchange medium introduced into the heat exchange structure is controlled to keep the temperature in the continuous tank reactor 100 stable at 25-30°C. Reaction; the reaction product is discharged from the overflow port 11 to the temporary storage tank 400 for crude acetal. After testing, the conversion rate of diethyl methylphosphonite into acetal is 97%.

Embodiment 2

[0064] Add crude acetal to the continuous tank reactor 100 for pre-filling and laying the bottom, start stirring, keep warm at 20-25°C; then start the diethyl methylphosphinate supply pump 200 and adjust the flow rate to 36.2kg / h, and start the acrolein The mixed solution with glacial acetic acid is supplied to the pump 300 and the flow rate is adjusted to 28.8kg / h. At the same time, the flow rate of the heat exchange medium introduced into the heat exchange structure is controlled to keep the temperature in the continuous tank reactor 100 stable at 20-25°C for reaction The reaction product is discharged from the overflow port 11 to the crude acetal temporary storage tank 400. After testing, the conversion rate of diethyl methylphosphonite into acetal is 97%.

Embodiment 3

[0066] Add crude acetal to the continuous tank reactor 100 for pre-filling and bottoming, start stirring, keep warm at 15-20°C; then turn on the diethyl methylphosphinate supply pump 200 and adjust the flow rate to 36.2kg / h, and turn on the propylene The mixed solution of aldehyde and glacial acetic acid is supplied to the pump 300 and the flow rate is adjusted to 28.8kg / h. At the same time, the flow rate of the heat exchange medium introduced into the heat exchange structure is controlled to keep the temperature in the continuous tank reactor 100 stable at 15-20°C. Reaction; the reaction product is discharged from the overflow port 11 to the temporary storage tank 400 for crude acetal. After testing, the conversion rate of diethyl methylphosphonite into acetal is 96%.

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Abstract

The invention discloses a method and a system for continuous kettle type industrial production of a crude acetal product, and belongs to the technical field of chemical production. A feeding mode of simultaneously, preferably and continuously adding corresponding reaction materials in the same proportion is adopted, and particularly, the temperature is controlled, so that the whole reaction process is continuously carried out; compared with a feeding mode of dropwise adding an acrolein-weak acid mixture into diethyl methylphosphite in the prior art that, the feeding mode of the invention realizes the continuous kettle type reaction process for preparing the crude acetal product, so the problems existing in the intermittent kettle type production process are effectively solved; and the production efficiency of the crude acetal product is effectively improved, the production cost is reduced, and meanwhile, large-scale industrial production is facilitated.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a method and system for continuous-kettle industrial production of crude acetal. Background technique [0002] Acetal is an intermediate of glufosinate-ammonium in fine chemical products. At present, there are many literature reports on how to prepare glufosinate, such as "Preparation Method of Glufosinate", Yan Haichang, He Hongdong, Pesticides, 2002, 41(9), P46-48. However, the traditional preparation methods generally have the problems of many reaction steps, low reaction yield and high production cost. [0003] Hoechst's patent document "Method and intermediate for preparing glufosinate", notification number CN1267305A, uses methyl phosphonite as raw material, acid anhydride as condensation agent, and acrolein addition reaction in the presence of alcohol. The production method of acetal is produced by the batch-kettle Michel (Michael) addition method. Zhejiang ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/32B01J19/18B01J4/00
CPCC07F9/3264C07F9/3211B01J19/18B01J19/0066B01J4/001B01J2204/002B01J2219/00033
Inventor 张飞辛杨杨王志豪张万君曾柏清彭启才周波程柯尹英遂
Owner LIER CHEM CO LTD
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