Method for continuously producing monochloroacetone by micro-droplet reactor

A chloroacetone and reactor technology, which is applied in the field of continuous production of high-purity monochloroacetone in a microdroplet reactor, can solve the problems of reduced output, high system energy consumption, low purity of monochloroacetone, etc., and achieves a reduction in polychlorinated products. Generate, operate efficiently and continuously, and purify the effect easily

Active Publication Date: 2021-02-12
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this process can obtain monochloroacetone, there are many problems
First, batch operation severely reduces yield
The second, the yield of dichloroacetone is higher than 10%, not only has caused the waste of raw material, more importantly is the difficulty of product purification, and the monochloroacetone purity that obtains is not high
Third, acetone requires a large excess, and the recovery of acetone requires high energy consumption
Mesityl oxide and monochloroacetone are difficult to separate mixtures, so there are still problems of low product purity and high energy consumption of the system
[0004] The monochloroacetone production process reported above all can obtain monochloroacetone, but the common defect of these processes is that the purity is not high

Method used

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  • Method for continuously producing monochloroacetone by micro-droplet reactor

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Experimental program
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Effect test

Embodiment 1

[0023] Prepared into 35wt% HCl solution under normal temperature and pressure, and passed Cl 2 Saturate to form a dispersed phase, Cl in the dispersed phase 2 The molar concentration is 0.02mol / L. The mass fractions of acetone and cyclohexane in the continuous phase were 20% and 80%, respectively. The dispersed phase and the continuous phase were injected by two syringe pumps into a microchannel made of PTFE and a diameter of 1 mm, respectively. The volume flow ratio of the two phases was 1:1, the reaction temperature was 20 °C, and the total volume flow was 2ml / min, the reaction time was 5 min, and the reaction pressure was 0.2 MPa. The liquid-liquid two-phase leaving the microchannel is layered in a liquid-liquid stratifier, and the cyclohexane phase containing monochloroacetone is put into a rectifying tower for rectification separation, and the content of the obtained monochloroacetone is as high as 99.5%.

Embodiment 2

[0025] Prepare 35% HCl solution at normal temperature and pressure, and pass Cl 2 Saturate to form a dispersed phase, Cl in the dispersed phase 2 The molar concentration is 0.02mol / L. The mass fractions of acetone and cyclohexane in the continuous phase were 20% and 80%, respectively. The dispersed phase and the continuous phase were injected into a microchannel made of PTFE and a diameter of 1 mm by two syringe pumps respectively. The volume flow ratio of the two phases was 1:1, the reaction temperature was 30 °C, and the total volume flow was 2ml / min, the reaction time was 5 min, and the reaction pressure was 0.2 MPa. The liquid-liquid two-phase leaving the microchannel is layered in a liquid-liquid stratifier, and the cyclohexane phase containing monochloroacetone is put into a rectifying tower for rectification separation, and the content of the obtained monochloroacetone is as high as 99.1%.

Embodiment 3

[0027] Prepare 35% HCl solution at normal temperature and pressure, and pass Cl 2 Saturate to form a dispersed phase, Cl in the dispersed phase 2 The molar concentration is 0.02mol / L. The mass fractions of acetone and cyclohexane in the continuous phase were 20% and 80%, respectively. The dispersed phase and the continuous phase were injected by two syringe pumps into a microchannel made of PTFE and a diameter of 1mm, respectively. The volume flow ratio of the two phases was 1:2, the reaction temperature was 30 °C, and the total volume flow was 4ml / min, the reaction time was 5 min, and the reaction pressure was 0.2 MPa. The liquid-liquid two-phase leaving the microchannel is layered in a liquid-liquid stratifier, and the cyclohexane phase containing monochloroacetone is put into a rectifying tower for rectification separation, and the content of the obtained monochloroacetone is as high as 99.2%.

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Abstract

The invention discloses a method for continuously producing high-purity monochloroacetone by using a micro-droplet reactor. The method comprises the following steps: reacting acetone in a continuous phase with Cl2 in a dispersion phase by using a hydrochloric acid aqueous solution containing chlorine with a certain concentration as the dispersion phase and a cyclohexane solution containing acetoneas the continuous phase, and rectifying the obtained reaction product to obtain the high-purity monochloroacetone. According to the invention, an HCl solution containing Cl2 is sheared into micro-droplets by the continuous phase in the micro-channel, and the micro-droplets are surrounded by the continuous phase, so that corrosion of the HCl solution to equipment is avoided; and excessive acetonein the continuous phase reacts with Cl2 in the liquid drop on a phase interface to generate monochloroacetone, then monochloroacetone is diffused to a continuous phase main body, and Cl2 is insolublein cyclohexane, so that Cl2 can be effectively prevented from further reacting with monochloroacetone to obtain a by-product; and the high-purity monochloroacetone is continuously and efficiently produced by adopting the micro-droplet reactor, so that the generation of byproducts is greatly reduced, and the process is easy to control.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, in particular to a method for continuously producing high-purity monochloroacetone in a microdroplet reactor. Background technique [0002] Monochloroacetone is an important organic synthesis intermediate, used in the production of dyes, pesticides, drugs, fragrances, antioxidants, desiccants, vinyl photosensitive resins, color motion picture film coupling agents, etc. In the pharmaceutical industry, it is mainly used to produce antibiotics, pain relievers, etc., especially ofloxacin, a new quinolone antibacterial drug. With the rapid increase in the market demand for ofloxacin, the demand for the raw material monochloroacetone also increases rapidly. In the production of pharmaceuticals, the requirements for the purity of monochloroacetone are very high. Monochloroacetone can be obtained from acetone and Cl 2 reaction prepared. Since the hydrogen atom on the α carbon in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/63C07C45/82C07C49/16B01J19/00
CPCB01J19/0093C07C45/63C07C45/82C07C49/16
Inventor 王晓达夏江南邱挺黄智贤葛雪惠
Owner FUZHOU UNIV
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