Synthesis device of 4-chloroacetoacetate

A chloroacetoacetate and synthesis device technology, applied in the chemical industry, can solve the problems of difficult control of chlorination depth, long reaction time, low product yield, etc., achieve long moving distance, many bubbles, and shorten reaction time Effect

Active Publication Date: 2020-11-06
茂名立强化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003]The current industrialized production method is the diketene method, using diketene as the starting material, through two steps of chlorination and esterification to synthesize ethyl 4-chloroacetoacetate, the raw material Both are cheap and easy to get, but their inherent disadvantage is that the product yield is low, only 75%-88%, resulting in high cost
The diketene method is used to synthesize ethyl 4-chloroacetoacetate. The existing industrial production is mainly through batch production. First, chlorine gas is introduced to carry out stirring chlorination. After chlorination, ethanol is added to carry out stirring esterification. There is a long reaction time. , the depth of chlorination is difficult to control, there are many by-products, and the yield is low.

Method used

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  • Synthesis device of 4-chloroacetoacetate
  • Synthesis device of 4-chloroacetoacetate
  • Synthesis device of 4-chloroacetoacetate

Examples

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preparation example Construction

[0093] The present invention also provides a kind of preparation method of 4-chloroacetoacetate, and specific technical scheme comprises:

[0094] 1) Diketene and organic solvent are mixed in a molar ratio of 0.5-50:1 to form a solution, and the above solution enters the first cavity of the reactor through the first feed pipe.

[0095] 2) Feed in chlorine gas, which enters the second cavity in the first material storage through the second feeding pipe, and enters the first cavity in the reactor through the first through hole, and the chlorine gas is introduced for 30 minutes.

[0096]3) Pass in ethanol, ethanol enters the third chamber in the second material storage through the third feed pipe, enters the first chamber in the reactor from the first through hole through the second through hole and the branch pipe, and the ethanol enters The time is 30 minutes.

[0097] 4) Discharge the above-mentioned reaction liquid through the discharge pipe, first perform fractional distill...

Embodiment 1

[0102] Such as image 3 The device for synthesizing 4-chloroacetoacetate shown includes a reactor 120 and a first material storage 220 disposed inside the reactor.

[0103] Wherein the reactor 120 comprises a first side wall 121, a first end wall 123, a second end wall 124 and a first cavity 122, and the first cavity 122 consists of the first side wall 121, the first end wall 123 and the second end wall. The wall 124 surrounds it; wherein the first end wall 123 is provided with a first feed port 3, and the first feed port 3 is provided with a first feed pipe 4, so that the first feed pipe 4 and the first cavity 122 ; the second end wall 124 is provided with a discharge port 5 , and a discharge pipe 6 is provided on the discharge port 5 , so that the discharge pipe 6 communicates with the first cavity 122 .

[0104] The first material storage 220 is arranged in the first cavity 122 of the reactor 120, including a second side wall 221, a third end wall 223 and a second cavity 2...

Embodiment 2

[0114] Except that the diameter of the first through hole 224 of the first material storage 220 is set along the axial direction of the first material storage 220 from the tapered large-diameter end to the small-diameter end, the geometric sequence is set in descending order, and the common ratio of the geometric sequence is 1.5, other The conditions are the same as in Example 1.

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Abstract

The present invention relates to a synthesis device of 4-chloroacetoacetate. The synthesis device comprises a reactor, a reactor, a material storage device, a material discharging pipe and two material feeding pipes, and the reactor comprises a side wall, an end wall and a cavity formed through surrounding; the material storage device is arranged in a cavity of the reactor and comprises a side wall, an end wall and a cavity formed through surrounding, and a plurality of through holes are formed in the side wall; the first feeding pipe is communicated with the cavity of the reactor, and the second feeding pipe is communicated with the cavity of the material storage device; and the discharge pipe is communicated with the cavity of the reactor. During reaction, gas can generate a large numberof bubbles through the through holes, the bubbles can generate a vortex stirring effect, and the gas can quickly react with diketene so that the reaction rate is increased, the reaction time is shortened, the production efficiency is improved, and meanwhile, the generation of a byproduct 2-chloroacetoacetate is reduced.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a synthesis device of 4-chloroacetoacetate. Background technique [0002] Ethyl 4-chloroacetoacetate is a colorless or light yellow transparent liquid. It is an important intermediate for the production of raw materials such as niclodipine, oxiracetam, and atorvastin calcium, and has a large market demand. [0003] The current industrialized production method is the diketene method. Diketene is used as a starting material to synthesize ethyl 4-chloroacetoacetate through two steps of chlorination and esterification. On the low side, only 75%-88%, resulting in high costs. The diketene method is used to synthesize ethyl 4-chloroacetoacetate. The existing industrial production is mainly through batch production. First, chlorine gas is introduced for stirring and chlorination. After chlorination, ethanol is added for stirring and esterification. The reaction time is long. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J4/00C07C51/58C07C67/08C07C67/54
CPCB01J4/001C07C67/08C07C51/58C07C67/54C07C69/72C07C59/21
Inventor 从海彬
Owner 茂名立强化学有限公司
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