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Method for preparing acetaldoxime by adopting continuous method

A technology of acetaldehyde oxime and acetaldehyde, which can be used in oxime preparation, organic chemistry and other directions, and can solve problems such as discontinuous reaction process

Pending Publication Date: 2021-02-26
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Overcome technical difficulties such as discontinuous traditional process and long reaction process

Method used

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  • Method for preparing acetaldoxime by adopting continuous method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024]First configure the mass concentration of 50% hydroxylamine hydrochloride aqueous solution, 40% acetaldehyde aqueous solution, 20% ammonia water, and fill 20-40 mesh quartz sand in the jacketed reactor; connect the jacketed reactor to the refrigerator, and set the refrigeration temperature -5℃; The molar ratio of hydroxylamine hydrochloride aqueous solution, acetaldehyde, and ammonia water is 1:1.05:1.1; under normal pressure, use a metering pump to separate hydroxylamine hydrochloride aqueous solution 2.32g / min, acetaldehyde aqueous solution 1.93g / min, and ammonia 1.56 g / min was fed into the reactor at the same time; running for 20 minutes, reaction temperature 15.4°C, reaction pressure 0.01MPa, pH=7.1, outlet GC detection, hydroxylamine hydrochloride conversion rate ≥99.7%, acetaldoxime selectivity ≥99.4%.

Embodiment 2

[0026]First configure the mass concentration of 50% hydroxylamine hydrochloride aqueous solution, 40% acetaldehyde aqueous solution, 20% ammonia water, and fill 20-40 mesh quartz sand in the jacketed reactor; connect the jacketed reactor to the refrigerator, and set the refrigeration temperature -5℃; The molar ratio of hydroxylamine hydrochloride aqueous solution, acetaldehyde and ammonia water is 1:1.05:1.1; under normal pressure, the hydroxylamine hydrochloride aqueous solution 4.18g / min, the acetaldehyde aqueous solution 3.47g / min and ammonia 2.81 g / min was fed into the reactor at the same time; running for 20 minutes, the reaction temperature was 24.6°C, the reaction pressure was 0.01MPa, pH=7.2, and the outlet GC test showed that the conversion of hydroxylamine hydrochloride was ≥99.4%, and the selectivity of acetaldoxime was ≥99.3%.

Embodiment 3

[0028]First configure the mass concentration of 50% hydroxylamine hydrochloride aqueous solution, 40% acetaldehyde aqueous solution, 20% ammonia water, and fill 20-40 mesh quartz sand in the jacketed reactor; connect the jacketed reactor to the refrigerator, and set the refrigeration temperature -5℃; The molar ratio of the three materials of hydroxylamine hydrochloride aqueous solution, acetaldehyde and ammonia water is 1:1.05:1.1; under normal pressure, the hydroxylamine hydrochloride aqueous solution is 3.48g / min, the acetaldehyde aqueous solution 2.9g / min, and the ammonia water are 2.34 by the metering pump. g / min was fed into the reactor at the same time; running for 20 minutes, the reaction temperature was 20.4°C, the reaction pressure was 0.01MPa, pH=7.1, and the outlet GC test showed that the conversion rate of hydroxylamine hydrochloride was ≥99.6%, and the selectivity of acetaldoxime was ≥99.4%.

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Abstract

The invention discloses a method for preparing acetaldoxime by adopting a continuous method, which comprises the steps of filling quartz sand into a reactor, introducing a hydroxylamine hydrochlorideaqueous solution, acetaldehyde and ammonia water serving as raw materials into the reactor, controlling reaction temperature and reaction pressure, adjusting the pH, and collecting the obtained reaction liquid. GC detection shows that that the conversion rate of hydroxylamine hydrochloride is greater than or equal to 99%, and the acetaldoxime selectivity is greater than or equal to 99%. The methodfor continuously synthesizing acetaldoxime has the characteristics of simplicity in operation, safety, reliability, complete hydroxylamine hydrochloride reaction, high selectivity and the like.

Description

Technical field[0001]The invention belongs to the field of fine chemical synthesis, and specifically relates to a method for preparing acetaldoxime.Background technique[0002]Acetaldoxime is very soluble in water and forms miscibility with water. Acetaldoxime is an important organic synthesis reagent and analytical reagent, as well as a reducing agent and a new type of deoxidizer with excellent deoxidizing effect. It has the characteristics of low price, low pollution and low toxicity. In the 1990s, acetaldoxime replaced the highly toxic hydrazine as a deoxidizer for boiler water, and its deoxidizing effect was much higher than that of hydrazine, about forty times that of hydrazine, so it was widely used. Acetaldoxime is an important intermediate for the synthesis of pesticides methomyl and thiodicarb. This pesticide is a good broad-spectrum insecticide. As its dosage continues to increase, the market for acetaldoxime has also increased.Summary of the invention[0003]The purpose of th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C249/08C07C251/38
CPCC07C249/08
Inventor 厉秉志王庆吉王蕊李进王炳春王贤彬
Owner CHINA CATALYST HLDG CO LTD
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