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Method for continuously producing p-nitrobenzyl alcohol in tubular reactor

A tubular reactor, technology of p-nitrobenzyl alcohol, applied in chemical instruments and methods, series/parallel reaction, preparation of nitro compounds, etc., can solve the problems of long reaction time, low heat and mass transfer efficiency, etc. Improved safety factor, simplified post-processing process, and reduced side reactions

Pending Publication Date: 2020-07-14
新乡市巨源生物科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] The above synthesis methods are all carried out in traditional tank reactors. Due to the low heat and mass transfer efficiency of tank reactors, the reaction time is long, which brings the above-mentioned safety, environmental protection, product quality, product yield and cost, etc. various problems

Method used

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  • Method for continuously producing p-nitrobenzyl alcohol in tubular reactor
  • Method for continuously producing p-nitrobenzyl alcohol in tubular reactor
  • Method for continuously producing p-nitrobenzyl alcohol in tubular reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0077] Using benzyl chloride as the benzyl halide, dichloromethane as the alkyl halide, sulfur trioxide as the acidic dehydrating agent, and sodium hydroxide as the base, in figure 1 The continuous production test in the production equipment shown is 3h, and the process conditions adopted are as follows:

[0078] a> the feed flow rate of benzyl chloride is set at 1.77Kg / min;

[0079] b> the weight ratio of each raw material is set as, benzyl chloride: methylene chloride: mixed acid: sulfur trioxide: concentrated nitric acid: water (or reclaimed water): sodium hydroxide=100:670:350:32:55:250 :38;

[0080] c>The reaction temperature is set as: nitrification reaction (first tubular reactor) temperature 0~5℃, hydrolysis reaction (second tubular reactor) temperature 35~40℃;

[0081] d> Crystallization and filtration temperature: the internal temperature of the three-in-one is -13~-15°C;

[0082] e> Drying temperature, vacuum degree and time: the internal temperature of the three...

Embodiment 2

[0085] With embodiment 1, benzyl bromide is used as benzyl halide, ethylene dichloride as alkyl halide, sulfur trioxide as acidic dehydrating agent, without alkaline / neutral / acidic aqueous solution, in figure 1 The continuous production test in the production equipment shown is 3h, and the process conditions adopted are as follows:

[0086] a> the feed flow rate of benzyl chloride is set at 2.40Kg / min;

[0087] b> the weight ratio of each raw material is set as, benzyl bromide: methylene chloride: mixed acid: sulfur trioxide: concentrated nitric acid: water (or recycled water) = 100: 600: 250: 24: 42: 300;

[0088] c>The reaction temperature is set as: nitration reaction (first tubular reactor) temperature 10-15°C, hydrolysis reaction (second tubular reactor) temperature 70-75°C;

[0089] d> Crystallization and filtration temperature: the internal temperature of the three-in-one is set to -13~-15°C;

[0090] e> Drying temperature, vacuum degree and time: the internal tempera...

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Abstract

The invention discloses a method for continuously producing p-nitrobenzyl alcohol in a tubular reactor. The method comprises the following steps: in the presence of an acidic dehydrating agent, continuously pumping mixed acid of concentrated sulfuric acid and concentrated nitric acid and benzyl halide into a first tubular reactor according to a certain proportion to finish nitration reaction; immediately and continuously feeding nitration reaction liquid into a first-stage liquid-liquid separator for liquid-liquid separation, pressurizing an obtained alkyl halide layer by using a pump, continuously feeding the alkyl halide layer into a second tubular reactor, and carrying out hydrolysis reaction on the alkyl halide layer and an alkaline, neutral or acidic aqueous solution; after the reaction is completed, performing online pH adjustment on the hydrolysis reaction liquid and performing continuous liquid-liquid separation through a second-stage liquid-liquid separator, introducing an obtained alkyl halide layer to a film evaporator to be continuously concentrated, introducing a concentrated solution to a crystallization kettle, and obtaining a p-nitrobenzyl alcohol finished productthrough freezing crystallization, filtering and drying. The by-product mixed acid and the recycled water are recycled.

Description

technical field [0001] The invention belongs to the technical field of green synthesis of fine chemical products, and in particular relates to a method for continuously producing p-nitrobenzyl alcohol. Background technique [0002] p-nitrobenzyl alcohol is an important intermediate in organic synthesis, widely used in the pharmaceutical industry, and can be used to produce p-aminobenzyl alcohol, p-nitrobenzaldehyde, penem antibiotics and other products. Among them, p-aminobenzyl alcohol is not only an intermediate for synthesizing antitumor drugs, but also an important intermediate for preparing photosensitive materials, alcohol oxidase, and molecular probes for labeling proteins and DNA, and has a good application prospect. p-Nitrobenzaldehyde is the main intermediate for the preparation of fine chemicals such as medicines, dyes, and pesticides. [0003] The synthetic method of p-nitrobenzyl alcohol is mainly divided into two categories: one is the p-nitrohalogen benzyl me...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/11C07C201/12C07C205/19B01J19/00
CPCC07C201/08C07C201/12B01J19/0046B01J19/0053B01J2219/00094C07C205/11C07C205/19
Inventor 杨栽根蒲鹏曹子领于会武化成文
Owner 新乡市巨源生物科技有限公司
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