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Green synthesis device of 4-chloroacetoacetate

A green synthesis technology of chloroacetoacetate, applied in the chemical method of reacting liquid and gas medium, preparation of ketene/polyketene, organic chemistry, etc., can solve the problem of raw material loss and reduce by-products The effect of generation, large contact area, and accelerated reaction speed

Active Publication Date: 2020-05-29
山东昌邑灶户盐化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] During the synthesis of 4-chloroacetoacetate esters: the diketene solution is at -15~-30°C, filled with chlorine gas, stirred at low temperature, after the reaction is completed, alcohols are added for esterification reaction, and after the reaction is completed, it is obtained by post-processing and rectification The yield of the product is 80-88%. If the contact time between chlorine gas and the product is too long, it is easy to produce other chlorinated compounds, such as: ethyl 2-chloroacetoacetate, ethyl 2,4-dichloroacetoacetate, 2 , 4 , Ethyl 4-trichloroacetoacetate, etc., causing loss of raw materials

Method used

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  • Green synthesis device of 4-chloroacetoacetate
  • Green synthesis device of 4-chloroacetoacetate
  • Green synthesis device of 4-chloroacetoacetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Please refer to Figure 1-3 , the present embodiment discloses a green synthesis device for 4-chloroacetoacetates, comprising a sealed heat-insulating shell 5, the interior of the heat-insulating shell 5 is provided with a conductive cylinder 12, and the upper and lower ends of the conductive cylinder 12 are connected to The upper and lower sides of the inner cavity of the thermal insulation shell 5 are sealed and fixedly connected. An electrostatic generator 8 is provided outside the thermal insulation shell 5. The output end of the electrostatic generator 8 is connected to the side of the conductive cylinder 12 through a cable, and the cable runs through the thermal insulation shell. Body 5.

[0034] The upper part of the inner cavity of the conductive cylinder 12 is provided with an electrostatic sprayer 9, and a precooler 1 is installed on the outside of the conductive cylinder 12. The liquid outlet of the precooler 1 and the liquid inlet of the electrost...

Embodiment 2

[0049] Embodiment two: if figure 2 As shown, this embodiment discloses a green synthesis device for 4-chloroacetoacetates, the structure of which is roughly the same as that of Embodiment 1, the difference being that the lower part of the inner cavity of the conductive cylinder 12 of this embodiment is set There is a grounding grid 10, the side of the grounding grid 10 is fixedly connected to one end of the grounding wire 4, the other end of the grounding wire 4 runs through and extends to the outside of the heat preservation shell 5, and the end of the grounding wire 4 located outside the heat preservation shell 5 is connected to the ground wire connect.

[0050] Preferably, the ground grid 10 is made of metal or alloy.

[0051] The working process and principle of this embodiment are: the charged diketene droplet moving to the lower part of the inner cavity of the conductive cylinder 12 contacts the grounding grid 10, and the charge on the diketene droplet passes through t...

Embodiment 3

[0052] Embodiment three: as figure 2 with Figure 4 As shown, this embodiment discloses a green synthesis device for 4-chloroacetoacetates. On the basis of Embodiment 1 or Embodiment 2, an ultrasonic vibrator 14 is fixed on the inside of the conductive cylinder 12 in this embodiment. The input end of the ultrasonic vibrator 14 is electrically connected to the output end of the control switch group 6 .

[0053] Preferably, the upper and lower ends of the conductive cylinder 12 are fixed with rubber rings 11 , and the upper and lower ends of the conductive cylinder 12 are sealed and elastically connected to the upper and lower sides of the inner cavity of the thermal insulation shell 5 through the rubber ring 11 .

[0054] The working process and principle of this embodiment are:

[0055] The operation of the ultrasonic vibrator 14 is controlled by the control switch group 6, and the ultrasonic vibrator 14 causes the conductive cylinder 12 to vibrate. When some diketene dropl...

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Abstract

The invention discloses a green synthesis device of 4-chloroacetoacetate. The synthesis device comprises a sealed thermal insulation shell; an electro-conductive barrel is arranged in the thermal insulation shell; the upper end and lower end of the electro-conductive barrel are hermetically and fixedly connected with the upper side and lower side of the inner cavity of the thermal insulation shellrespectively; an electrostatic generator is arranged outside the thermal insulation shell, the output end of the electrostatic generator is connected with the side face of the electro-conductive barrel through a cable, the cable penetrates through the thermal insulation shell, an electrostatic sprayer is arranged in the upper portion of the inner cavity of the electro-conductive barrel, and a pre-cooler is installed outside the electro-conductive barrel. The green synthesis device atomizes a diketene solution through static electricity, the contact area between liquid drops of the diketene solution and chlorine is increased, the time of reactions between the liquid drops of the diketene solution and chlorine is determined by the downward moving distance of the liquid drops of the diketenesolution, the time of reactions between the diketene solution and chlorine is convenient to control, byproducts are reduced, and raw material loss is avoided.

Description

technical field [0001] The invention relates to the technical field of organic synthesis equipment, in particular to a green synthesis device for 4-chloroacetoacetate. Background technique [0002] During the synthesis of 4-chloroacetoacetate esters: the diketene solution is at -15~-30°C, filled with chlorine gas, stirred at low temperature, after the reaction is completed, alcohols are added for esterification reaction, and after the reaction is completed, it is obtained by post-processing and rectification The yield of the product is 80-88%. If the contact time between chlorine gas and the product is too long, it is easy to produce other chlorinated compounds, such as: ethyl 2-chloroacetoacetate, ethyl 2,4-dichloroacetoacetate, 2 , 4 , 4-ethyl trichloroacetoacetate, etc., resulting in loss of raw materials. Contents of the invention [0003] The technical problem to be solved in the present invention is to overcome the existing defects and provide a green synthesis devi...

Claims

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Application Information

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IPC IPC(8): B01J19/24B01J10/00C07C67/46C07C69/716
CPCB01J10/00B01J19/24C07C67/46C07C69/716
Inventor 徐少华高建伟付忠东常永恒姜雯徐英猛姚璐于晓辉
Owner 山东昌邑灶户盐化有限公司
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