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Method for continuously synthesizing 2-nitropropane by adopting slurry reactor

A nitropropane, slurry bed technology, applied in the preparation of nitro compounds, organic chemistry, chemical recovery, etc., can solve the problems of cumbersome operation, unfriendly environment, low yield, etc., and achieves simple process, convenient operation, and economical energy effect

Active Publication Date: 2021-02-05
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To overcome technical problems such as co-production of acetone oxime and intermittent reaction in the prior art, cumbersome operation, low yield and unfriendly to the environment

Method used

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  • Method for continuously synthesizing 2-nitropropane by adopting slurry reactor
  • Method for continuously synthesizing 2-nitropropane by adopting slurry reactor
  • Method for continuously synthesizing 2-nitropropane by adopting slurry reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Take 200 g of the treated TS-1 catalyst and put it into a 2L slurry bed reactor, and add 1.2 L of methanol into the slurry bed reactor, raise the temperature to 70°C, and turn on the circulating pump to circulate. 200g / h acetone-methanol mixture and 212.9g / h27.5% hydrogen peroxide enter the reaction tank at the same time, and feed ammonia gas to control the pH of the reaction system=6~7, control the reaction pressure to 0.2MPa, and the total feed is in the reaction tank After staying for 3 hours, 400 g / h of the reaction solution was extracted through membrane tube separation, and the conversion rate of acetone was 95.4%, the selectivity of 2-nitropropane was 99.6%, and the yield was as high as 95.2%.

Embodiment 2

[0038] Take 200 g of the treated TS-1 catalyst and put it into a 2L slurry bed reactor, and add 1.2 L of methanol into the slurry bed reactor, raise the temperature to 75°C, and turn on the circulation pump to circulate. 200g / h acetone-methanol mixture and 212.9g / h27.5% hydrogen peroxide enter the reaction tank at the same time, and feed ammonia gas to control the pH of the reaction system=6~7, control the reaction pressure to 0.2MPa, and the total feed is in the reaction tank After staying for 5 hours, 400 g / h of the reaction solution was extracted through membrane tube separation, and the conversion rate of acetone was 97.4%, the selectivity of 2-nitropropane was 99.2%, and the yield was as high as 96.8%.

Embodiment 3

[0040] Take 200 g of the treated TS-1 catalyst and put it into a 2L slurry bed reactor, and add 1.2 L of methanol into the slurry bed reactor, raise the temperature to 70°C, and turn on the circulating pump to circulate. 200g / h acetone-methanol mixture and 255.7g / h27.5% hydrogen peroxide enter the reaction tank at the same time, and feed ammonia gas to control the pH of the reaction system=6~7, control the reaction pressure to 0.2MPa, and the total feed is in the reaction tank After staying for 4 hours, 400 g / h of the reaction liquid was extracted through membrane tube separation, and the conversion rate of acetone was 99.1%, the selectivity of 2-nitropropane was 99.5%, and the yield was as high as 98.8%.

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Abstract

The invention discloses a method for continuously synthesizing 2-nitropropane by adopting a slurry reactor, and belongs to a fine chemical synthesis method. The method comprises the following steps of: adding a treated TS-1 catalyst into a slurry bed according to a certain ratio, controlling the temperature and pressure at certain values, simultaneously introducing an acetone-methanol mixed solution, hydrogen peroxide and ammonia gas according to a certain ratio to control the pH value of a reaction system to be 6-7, and separating the reaction solution through a membrane tube. The method hasthe advantages of realization of continuous production, simple process, convenience in operation and no generation of byproducts. The acetone conversion rate is greater than or equal to 95.0%, and the2-nitropropane selectivity is greater than or equal to 99.0%. The method is green, environment-friendly, safe, reliable and energy-saving.

Description

technical field [0001] The invention belongs to fine chemical synthesis methods, in particular to a method for continuously synthesizing 2-nitropropane by using a slurry bed. Background technique [0002] 2-Nitropropane is used as a special solvent for ethylene and epoxy resin coatings, rocket fuel, gasoline additives, etc. It is also used in organic synthesis. This product has a strong dissolving ability, and is an excellent solvent for various cellulose derivatives, vinyl resins, etc. It is also used as a solvent for wax, fat, dyes, etc., a lubricant for grinding pigments, and a cleaning and mordant agent for cotton fabrics. [0003] Chinese patent CN201610208003.3 discloses a method of synthesizing 2-nitropropane by using acetone, ammonia, hydrogen peroxide and a reaction solvent under the action of a titanium-silicon molecular sieve catalyst, and co-producing 30-50% of acetone oxime at the same time. Chinese patent CN201710218837.7 discloses an isohydrazone obtained by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/06C07C205/02
CPCC07C201/06C07C205/02Y02P20/584
Inventor 王庆吉王蕊厉秉志李进王炳春王贤彬
Owner CHINA CATALYST HLDG CO LTD
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