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Preparation method and device of 1-cyano-2-propenyl acetate

A technology of acryl acetate and cyano group, which is applied in the field of preparation of 1-cyano-2-propenyl acetate, can solve the problems of high cost, many side reactions, high toxicity, etc., and achieve improved reaction efficiency, Guaranteed timeliness

Inactive Publication Date: 2020-05-05
SHANDONG XINHECHENG AMINO ACID
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The reaction yields of the two-step preparation of ACA in the above two documents are not ideal, and the main problems are as follows: 1) The activation energy of the esterification reaction is high, the reaction rate is slow, and there are many side reactions; 2) The reaction process is not well controlled, and only Empirical control of reaction residence time
However, the inhibitors disclosed in the prior art are highly toxic or costly, which limits their industrial use

Method used

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  • Preparation method and device of 1-cyano-2-propenyl acetate
  • Preparation method and device of 1-cyano-2-propenyl acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] According to attached figure 1 The flow diagram shown carries out the procedure for the preparation of 1-cyano-2-propenyl acetate. in:

[0058] The esterification reaction tower R1 is a packed reaction tower with a diameter of 0.2m and a height of 2.0m; the distillation tower R2 is a distillation tower with a diameter of 0.1m and a height of 1.0m.

[0059] 1) Esterification reaction of acrolein cyanohydrin

[0060] Acrolein cyanohydrin is sent into the first pipeline 1 at 85.6g / min, the catalyst DMAP formate is mixed with liquid acetic anhydride at 79.5g / min in the second pipeline 2 at 0.36g / min, and phosphoric acid is mixed at 0.45 g / min is added to the second pipeline 2, the second pipeline 2 is communicated with the first pipeline 1, and the time from the phosphoric acid feeding point to the esterification reaction tower R1 is 6min, the catalyst DMAP formate, liquid acetic anhydride, phosphoric acid, The four components of acrolein cyanohydrin are fed into the fee...

Embodiment 2

[0070] According to attached figure 1 The flow diagram shown carries out the continuous preparation of 1-cyano-2-propenyl acetate. in:

[0071] The esterification reaction tower R1 is a multistage stirring reaction tower with a diameter of 0.2m and a height of 2.0m.

[0072] The distillation tower R2 is a distillation tower with a diameter of 0.1 m and a height of 1.0 m.

[0073] 1) Esterification reaction of acrolein cyanohydrin

[0074] Acrolein cyanohydrin is sent into the first pipeline 1 at 78.5g / min, catalyst DMAP acetate is mixed with liquid acetic anhydride at 76.5g / min in the second pipeline 2 at 0.85g / min, and sulfuric acid is mixed at 0.95 g / min is added to the second pipeline 2, the second pipeline 2 is connected with the first pipeline 1, the time from the sulfuric acid feeding point to the esterification reaction tower R1 is 5min, and the four components are added through the first pipeline 1. To the feed inlet of the esterification reaction tower R1, feed in...

Embodiment 3

[0083] According to attached figure 1 The flow diagram shown carries out the continuous preparation of 1-cyano-2-propenyl acetate. in:

[0084] The esterification reaction tower R1 is a multistage stirring reaction tower with a diameter of 0.2m and a height of 2.0m.

[0085] The distillation tower R2 is a distillation tower with a diameter of 0.1 m and a height of 1.0 m.

[0086] 1) Esterification reaction of acrolein cyanohydrin

[0087] Acrolein cyanohydrin is sent into the first pipeline 1 at 95.6g / min, catalyst DMAP butyrate is mixed with liquid acetic anhydride at 55.6g / min in the second pipeline 2 at 2.25g / min, and phosphoric acid is mixed at 0.09 g / min is added to the second pipeline 2, the first pipeline 1 is connected to the second pipeline 2, the time from the phosphoric acid feeding point to the reaction tower is 6min, and the four components are added to the esterification through the first pipeline 1 Feed inlet of reaction tower R1, feed in the tower, feed tem...

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Abstract

The invention provides a preparation method of 1-cyano-2-allyl acetate. The preparation method comprises an esterification reaction and distillation. Acrolein cyanohydrin and liquid acetic anhydride are subjected to the esterification reaction in the presence of a catalyst and inorganic acid to prepare a reaction solution containing ACA, an ACA product is obtained after distillation, and the esterification reaction further comprises the step of introducing gaseous acetic anhydride into a reaction system. The invention further provides a preparation device of 1-cyano-2-allyl acetate. Accordingto the method and the device, acetic anhydride is ingeniously divided into two parts to be fed, one part is separated out to serve as acetic anhydride steam which is fed into an esterification reaction tower from the bottom of the tower, heat required by reaction can be provided, acetic acid can be effectively blown off, the esterification reaction can be accelerated through effective removal of acetic acid, and the reaction efficiency is improved. The device is characterized in that a conductivity meter is arranged in the esterification reaction tower to monitor the reaction process on line,so that the timeliness and effectiveness of reaction process control are guaranteed.

Description

technical field [0001] The invention relates to a preparation method and device of 1-cyano-2-propenyl acetate, belonging to the field of esterification reaction. Background technique [0002] 1-cyano-2-propenyl acetate (ACA, Acrolein Cyanohydrin Acetate) is mainly used as an intermediate in the production of the pesticide glufosinate-ammonium. [0003] There are mainly one-step and two-step synthesis routes for ACA: [0004] One-step method: after acrolein is mixed with NaCN or NaCN aqueous solution, then mixed with acid anhydride, the ACA reaction liquid is obtained through one-pot reaction, and the product ACA is obtained after post-treatment. [0005] H. Ohse and R. Palm [Angew. Chem. 78, p1093] mixed 0.77 mol of acrolein and 1.12 mol of sodium cyanide in water, then added 0.77 mol of acetic anhydride dropwise to the mixture to obtain ACA reaction solution , ACA products can be obtained after post-processing. About 45% of sodium cyanide is excessive in this reaction pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C253/34C07C255/16B01D3/10B01J8/00B01J8/10B01J8/12
CPCB01D3/10B01J8/001B01J8/008B01J8/10B01J8/12B01J2208/00601C07C253/30C07C253/34C07C255/16
Inventor 王志轩陈聪杜振宇李建军
Owner SHANDONG XINHECHENG AMINO ACID
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