A green synthesis device for 4-chloroacetoacetates

A green synthesis, chlorine technology, applied in chemical methods, organic chemistry, ketene/polyketene preparation, etc. to react liquid and gas medium, can solve problems such as loss of raw materials, and reduce the generation and contact of by-products. Large area, difficult to integrate effect

Active Publication Date: 2021-08-17
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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  • A green synthesis device for 4-chloroacetoacetates
  • A green synthesis device for 4-chloroacetoacetates
  • A green synthesis device for 4-chloroacetoacetates

Examples

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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 and 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 drople...

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Abstract

The invention discloses a green synthesis device for 4-chloroacetoacetate, which comprises a sealed heat-insulating shell, a conductive cylinder is arranged inside the heat-insulating shell, and the upper and lower ends of the conductive cylinder are connected with the inner cavity of the heat-insulating shell. The upper and lower sides are sealed and fixedly connected. An electrostatic generator is installed outside the insulation shell. The output end of the electrostatic generator is connected to the side of the conductive cylinder through a cable, and the cable runs through the insulation shell. The upper part of the inner cavity of the conductive cylinder is equipped with an electrostatic Sprayer, a precooler is installed on the outside of the conductive cylinder; this green synthesis device of 4-chloroacetoacetates electrostatically atomizes the diketene solution to increase the contact area between the diketene solution droplets and chlorine gas, and double The downward movement distance of the diketene solution droplet determines the reaction time of the diketene solution droplet and chlorine gas, the reaction time of diketene solution and chlorine gas is easy to control, reduces the generation of by-products, and avoids the loss of raw materials.

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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Patent Type & Authority Patents(China)
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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