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Method and device for continuously preparing pivaloyl chloride

A technology for crude pivaloyl chloride and pivaloyl chloride, which is applied to the preparation of carboxylic anhydrides and organic chemistry, can solve the problems of long separation reaction time, many by-product impurities, and long time, and achieve shortened reaction time, high conversion efficiency, High conversion effect

Active Publication Date: 2019-03-08
山东民基新材料科技有限公司
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Problems solved by technology

The above-mentioned several pivaloyl chloride preparation techniques are comparatively perfect with the first kind, can make the pivaloyl chloride that meets the standard, but pivaloyl chloride is made by the reaction of pivalic acid and chlorinating agent still has big problem, wherein existing chlorination The reaction devices are all batch reaction devices, which have problems such as low reaction efficiency, long time, high energy consumption, low product conversion rate, and many impurities.
[0004] The existing pivaloyl chloride production processes are all batch-type, adopting the method of tank reaction-separation-rectification purification. After the single-pot reaction, the separation reaction time is long, the operation is complicated, and there are many by-product impurities; in the production process and control of reaction conditions On the one hand, there are technical problems to be solved, and there is no report on the continuous production of pivaloyl chloride

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  • Method and device for continuously preparing pivaloyl chloride

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Embodiment 1

[0029] This embodiment relates to a kind of method for continuously preparing pivaloyl chloride, and concrete steps are as follows:

[0030] (1) Feed the raw materials: feed the raw material pivalic acid through the pivalic acid delivery pipe at a flow rate of 167kg / h, and add phosphorus trichloride into the raw material mixer through the phosphorus trichloride delivery pipe at a flow rate of 93.5kg / h. The feed time of a kind of raw material is 2 hours;

[0031] (2) Chlorination reaction: Stir the raw materials in step (1) evenly and transport them to the 4 2- / ZrO 2 -Sm 2 o 3 In the microchannel reactor of the catalyst, the pressure is 20kPa, the temperature is 40°C, the residence time is 20s, and the chlorination reaction solution is obtained;

[0032] (3) Preparation of crude pivaloyl chloride: the chlorination reaction solution prepared in step (2) first enters the chromatography tank for chromatography, the lower phosphorous acid phase is separated into the crude pho...

Embodiment 2

[0037] This embodiment relates to a kind of method for continuously preparing pivaloyl chloride, and concrete steps are as follows:

[0038] (1) Feed raw materials: feed raw pivalic acid through the pivalic acid delivery pipe at a flow rate of 167kg / h, and add phosphorus trichloride into the raw material mixer through the phosphorus trichloride delivery pipe at a flow rate of 50kg / h. The feeding time of raw materials is 2 hours;

[0039] (2) Chlorination reaction: Stir the raw materials in step (1) evenly and transport them to the 4 2- / ZrO 2 -Sm 2 o 3 In the microchannel reactor of the catalyst, the pressure is 25kPa, the temperature is 45°C, the residence time is 24s, and the chlorination reaction solution is obtained;

[0040] (3) Preparation of crude pivaloyl chloride: the chlorination reaction solution prepared in step (2) first enters the chromatography tank for chromatography, the lower phosphorous acid phase is separated into the crude phosphorous acid storage tan...

Embodiment 3

[0045] This embodiment relates to a kind of method for continuously preparing pivaloyl chloride, and concrete steps are as follows:

[0046] (1) Feed the raw materials: feed pivalic acid as the raw material through the pivalic acid delivery pipe at a flow rate of 167kg / h, and add phosphorus trichloride into the raw material mixer through the phosphorus trichloride delivery pipe at a flow rate of 92kg / h. The feeding time of raw materials is 2 hours;

[0047] (2) Chlorination reaction: Stir the raw materials in step (1) evenly and transport them to the 4 2- / ZrO 2 -Sm 2 o 3 In the microchannel reactor of the catalyst, the pressure is 20kPa, the temperature is 50°C, the residence time is 25s, and the chlorination reaction solution is obtained;

[0048] (3) Preparation of crude pivaloyl chloride: the chlorination reaction solution prepared in step (2) first enters the chromatography tank for chromatography, the lower phosphorous acid phase is separated into the crude phosphor...

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Abstract

The invention relates to a method and a device for continuously preparing pivaloyl chloride. The specific operation method comprises the following steps: adding raw materials pivalic acid and phosphorus trichloride to a raw material mixer respectively, uniformly stirring the raw materials, and then conveying the raw materials into a microchannel reactor with a solid catalyst to prepare a chlorination solution; feeding the prepared chlorination solution into two chromatography tanks for chromatography respectively to prepare a crude product of pivaloyl chloride; finally, feeding the crude product of pivaloyl chloride into a rectification section to obtain a pure product of pivaloyl chloride. The microchannel reactor is adopted to replace an original chlorination reactor, so that the reaction is more thorough, the conversion rate is high, and purity is high; a continuous reaction is adopted to replace the original intermittent reaction, and reaction time is greatly shortened to 0.5 hoursfrom 12 hours in the prior art.

Description

technical field [0001] The present invention relates to a kind of method for preparing pivaloyl chloride and equipment thereof, more specifically, relate to a kind of method for continuously preparing pivaloyl chloride and equipment thereof. Background technique [0002] Pivaloyl chloride, also known as trimethylacetyl chloride, is commonly used as a pharmaceutical and pesticide intermediate. It is an intermediate for the production of carbamate insecticide thabicarb and herbicide isoxazolone, and for the synthesis of amides and phenolic ester drugs. It is also widely used in the production of (hydroxy) ampicillin, cephalosporin (hydroxy) ampicillin, cefazolin, dipivaloyl adrenaline and other drugs. [0003] There have been many reports on the preparation process of pivaloyl chloride, and the main industrial production processes are as follows: (1) pivalic acid is prepared from isobutene and carbon monoxide as initial raw materials, and pivaloyl chloride is prepared by react...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/56C07C53/42
CPCC07C51/56C07C53/42
Inventor 张海朋韦兵李建军杨中原李萍林苗苗王建芹祝新涛张瑞扈世琳陈凯黄超鹏
Owner 山东民基新材料科技有限公司
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