Preparation method and preparation device for gamma-chloro-methyl butyrate

A technology for preparing methyl chlorobutyrate and a preparation device, which is applied in the field of preparation method and preparation device of methyl γ-chlorobutyrate, can solve problems such as fluctuations in product quality, high labor intensity, and large environmental pollution, and achieve Reduce production costs, reduce labor intensity, and stabilize the preparation process

Inactive Publication Date: 2015-12-09
SHANDONG GUOBANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In industrialized production, the above processes are all completed by batch reactors, which have problems such as high labor intensity and low production efficiency, and manual operation will lead to unstable process conditions and fluctuations in product quality; at the same time, hydrogen chloride, Sulfur dioxide and other waste gas treatment methods are still the traditional way of absorbing hydrogen chloride with water, and then using ammonia water to absorb sulfur dioxide to prepare ammonium bisulfite. Due to unsalable by-products, normal production is affected. At the same time, hydrogen chloride and sulfur dioxide gases leaked during the absorption process are very corrosive and pollute the environment.
[0006] Because the reaction process of gamma-butyrolactone to prepare gamma-chlorobutyric acid methyl ester is a batch process, and the production process needs to be continuously heated, cooled, etc., not only reduces production efficiency, increases energy consumption, but also the hydrogen chloride and The process of sulfur dioxide and other gases cannot be continuously produced, and the method of continuous pressurized rectification cannot be used for subsequent treatment, which also increases the difficulty of efficient resource utilization of waste gas; to change the above problems, this traditional reaction process must be changed

Method used

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  • Preparation method and preparation device for gamma-chloro-methyl butyrate
  • Preparation method and preparation device for gamma-chloro-methyl butyrate
  • Preparation method and preparation device for gamma-chloro-methyl butyrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] figure 1 A schematic structural view of the preparation device of methyl γ-chlorobutyrate provided in this example is shown. For the convenience of description, this figure only provides the structural parts related to the present invention.

[0032] A preparation device for methyl gamma-chlorobutyrate, such as figure 1 As shown, it includes a primary jet mixer 1 , a preheater 2 , a secondary jet mixer 3 , a static mixer 4 and a cooler 5 connected in sequence. The first-stage jet mixer 1 and the second-stage jet mixer 3 have the same structure, and are all existing products. For example, the products of models such as SX / SK / SV / SL can be produced by Qidong mixer factory, and its structure will not be repeated here. The first-stage jet mixer 1 and the second-stage jet mixer 3 are respectively provided with two liquid inlets 6 and one liquid outlet 7, and the preheater 2 and the cooler 5 have the same structure, for example, a tube-and-tube heat exchanger can be used , p...

Embodiment 2

[0035] image 3 A schematic structural view of the preparation device of methyl γ-chlorobutyrate provided in this example is shown. For the convenience of description, this figure only provides the structural parts related to the present invention.

[0036] The preparation device of gamma-chlorobutyric acid methyl ester in the present embodiment is basically identical with the structure in embodiment one, difference is:

[0037] Such as image 3 As shown, the preparation device also includes an automatic flow control system 9, the automatic flow control system 9 is located outside the outer shell 42, the automatic flow control system 9 includes a controller 91, a motor 92 and a flow valve 93, the controller 91 and the motor 92 Electrically connected, the motor 92 is connected to the flow valve 93 in transmission, the cooling medium inlet 45 and the heat medium inlet 47 are respectively provided with flow valves 93 , and the temperature control probe 49 is electrically connect...

Embodiment 3

[0040] (1) Feed γ-butyrolactone 1mol into the first-stage jet mixer with a flow rate of 400g / h, and pass into thionyl chloride 1.3mol with a flow rate of 719g / h simultaneously, and the two materials are in the first-stage jet mixer The mixed liquid is formed in the middle, and the mixed liquid is sprayed out from the first-stage jet mixer and directly enters the preheater, and is heated to 30°C to form a mixed liquid;

[0041] (2) The mixed solution directly enters the secondary jet mixer, and simultaneously delivers 2 mol of methanol to the secondary jet mixer at a flow rate of 297g / h, thereby forming a premixed solution of the mixed solution and methanol in the secondary jet mixer;

[0042] (3) The premixed liquid is sprayed out from the secondary jet mixer and directly enters the static mixer. The premixed liquid is strongly mixed and continuously reacted in the static mixer. The reaction temperature is controlled by the temperature control device of the static mixer, and th...

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PUM

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Abstract

The invention belongs to the technical field of drug intermediate synthesis, and particularly relates to a preparation method and preparation device for gamma-chloro-methyl butyrate. The preparation method comprises the following steps that gamma-butyrolactone and sulfoxide chloride are fed into a first-level jet mixer to be mixed and then sprayed into a preheater, and the temperature is increased to 30-35 DEG C; the mixture enters a second-level jet mixer, and meanwhile methyl alcohol is added in the second-level jet mixer; after mixing is performed, the mixture is sprayed into a static mixer, and the temperature is controlled at 52-55 DEG C; after a reaction is completed, the temperature is lowered, and then the gamma-chloro-methyl butyrate is obtained. The preparation device comprises the first-level jet mixer, the preheater, the second-level jet mixer, the static mixer and a cooler which are sequentially communicated; the first-level jet mixer and the second-level jet mixer are each provided with two liquid inlets and a liquid outlet, and the static mixer comprises a shell and a temperature control device arranged in the shell. According to the preparation method and preparation device for the gamma-chloro-methyl butyrate, continuous production can be achieved, the production efficiency is high, the product yield is high, and the cost is low.

Description

technical field [0001] The invention belongs to the technical field of synthesis of pharmaceutical intermediates, and in particular relates to a preparation method of methyl γ-chlorobutyrate and a preparation device thereof. Background technique [0002] Cyclopropylamine is an aliphatic amine containing a three-membered ring, which is a very important high value-added drug intermediate, quinolone antibacterial drugs Ciprofloxacin (Ciprofloxacin), Sparfloxacin (Sparfloxacin), Barofloxacin (Balofloxacin) Cyclopropylamine and Tomefloxacin (Tomefloxacin) all use cyclopropylamine as the main intermediate or raw material; in addition, cyclopropylamine is also used in the synthesis of plant protection agents and feed additives. [0003] At present, the production process of cyclopropylamine with industrial value is to use γ-butyrolactone as raw material, undergo ring opening, esterification, and then undergo ring closure and Hoffmann degradation reaction to finally generate cyclopr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/63C07C67/03
CPCC07C67/03C07C69/63
Inventor 黄秀泉李进伟杨国泉乔建超廖仕学李琦斌杨俊德
Owner SHANDONG GUOBANG PHARMA
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