CN104193662A - Preparing method of peracetic acid - Google Patents

Abstract

The invention provides a continuous synthesis method of peracetic acid. The method includes: a step of measuring acetic acid and hydrogen peroxide with the ratio of the acetic acid to the hydrogen peroxide being 0.4-1.1; a step of mixing the acetic acid and the hydrogen peroxide; a step of feeding the liquid under cooling conditions into an immobilized reactor filled with a solid acid catalyst; and a step of allowing the reaction time of the acetic acid and the hydrogen peroxide in the immobilized reactor to be 1-3 h by adjusting the flow rate so as to obtain the peracetic acid. By the continuous reaction catalyzed by the solid acid and increasing the using amount of the catalyst, the reaction time is shortened, the reaction temperature is lowered, the reaction efficiency is increased, operation is simplified, safety is enhanced, and the peracetic acid with a high concentration is obtained rapidly and conveniently.

Description

A kind of preparation method of peracetic acid

technical field

The invention belongs to the field of chemical industry, in particular to a kind of peracetic acid, specifically a kind of preparation method of peracetic acid.

Background technique

Peracetic acid is a very versatile strong oxidizing agent, which can be used as a bleaching agent for paper, paraffin, wood, and starch. In the pharmaceutical industry, it is used as a disinfectant for drinking water, food and preventing infectious diseases. In the organic industry, it is used as an oxidizing agent and epoxy oxidizing agent for the manufacture of propylene oxide, glycerin, caprolactam, etc.

The synthesis of traditional peracetic acid adopts a batch reaction production mode, a large amount of sulfuric acid is used as a catalyst, and the reaction takes 20-30 hours. The reaction time is long, the concentration of peracetic acid is low, and the production efficiency is low. The obtained peracetic acid contains sulfuric acid. Strong acidity.

Zheng Xiaobing (CN1803771A), Zhang Xiaofeng (Fine Chemical Intermediates 2008, Vol38, No.4, p34) and others solved the problem of low peracetic acid concentration and long reaction time by raising the reaction temperature and vacuum distillation, but the temperature was high, Peracetic acid is easy to decompose, has poor safety, and the operation is complex and the production efficiency is relatively low.

Contents of the invention

For the above-mentioned defectives in the prior art, the technical problem to be solved by this invention is to provide a kind of preparation method of peracetic acid, and the preparation method of described this peracetic acid will solve the problem that the preparation method in the prior art obtains. The technical problems of peracetic acid are easy to decompose, poor safety, and low production efficiency.

A method for continuously synthesizing peroxyacetic acid of the present invention comprises a step of measuring acetic acid and hydrogen peroxide, the ratio of said acetic acid to hydrogen peroxide is 0.4 to 1:1, mixing acetic acid and hydrogen peroxide, and cooling the liquid Import into an immobilized reactor equipped with a solid acid catalyst, and adjust the flow rate so that the reaction time of the mixed liquid of acetic acid and hydrogen peroxide in the immobilized reactor is 1-3 hours to obtain peracetic acid.

Further, the concentration of the hydrogen peroxide is 20-70%, preferably 30-50%.

Further, the cooling condition refers to a controlled temperature of 0-30°C, preferably 10-15°C.

Further, the solid acid catalyst is acidic cation exchange resin, or perfluorosulfonic acid resin, or immobilized sulfuric acid.

The invention discloses a method for continuous synthesis of peroxyacetic acid. Through the continuous reaction catalyzed by solid acid, the amount of catalyst is increased, the reaction time is shortened, the reaction temperature is reduced, the reaction efficiency is improved, the operation is simplified, and the production capacity is increased. Safety, quick and convenient access to high concentration peracetic acid.

Compared with the prior art, the technical progress of the present invention is remarkable. The method solves the technical problems of low efficiency, low content and strong acidity of synthesizing peracetic acid by using concentrated sulfuric acid as a catalytic reaction. The present invention shortens the reaction time, increases the concentration of peracetic acid and enhances the safety of the reaction through the continuous synthesis method of peracetic acid. It is a process for continuous preparation of peracetic acid with short production time, moderate temperature, high concentration and good production safety.

Detailed ways

In order to enable those skilled in the art to better understand the present invention, the present invention will be further described below through examples, but these examples do not limit the scope of the present invention.

Example 1

Mix 500kg (8.3mol) of acetic acid with 500kg (14.7mol) of 30% hydrogen peroxide and pump it into an immobilized reactor (diameter 400mm, length 8m) equipped with 001×7 type cation exchange resin, with a clamp Cool the jacket to control the temperature to 10-15°C, and control the reaction solution to stay in the fixed-bed reactor for 2-3 hours to obtain peracetic acid with a concentration of 25-30%.

Example 2

Mix 500kg (8.3mol) of acetic acid with 500kg (14.7mol) of 50% hydrogen peroxide and pump it into an immobilized reactor (diameter 400mm, length 8m) equipped with 001×7 type cation exchange resin, with a clamp Cool the jacket to control the temperature to 10-15°C, and control the reaction solution to stay in the fixed-bed reactor for 2-3 hours to obtain peracetic acid with a concentration of 35-45%.

Example 3

Mix 880kg (14.7mol) of acetic acid with 500kg (14.7mol) of 70% hydrogen peroxide and pump it into an immobilized reactor (diameter 400mm, length 8m) equipped with PFSA E87-05 perfluorosulfonic acid resin. Cool with a jacket to control the temperature to 0-5°C, and control the reaction solution to stay in the fixed-bed reactor for 1-2 hours to obtain peracetic acid with a concentration of 50%-58%.

Example 4

Mix 352kg (5.9mol) of acetic acid with 500kg (14.7mol) of 20% hydrogen peroxide and pump it into a fixed-bed reactor (diameter 400mm, length 8m) equipped with a solid-loaded sulfuric acid catalyst, and cool it with a jacket Control the temperature to 25-30°C, and control the reaction solution to stay in the fixed-bed reactor for 2-3 hours to obtain peracetic acid with a concentration of 15-18%.

Claims (4)

1. the method for the synthetic Peracetic Acid of serialization, it is characterized in that: comprise a step that measures acetic acid and hydrogen peroxide, described acetic acid and the ratio of hydrogen peroxide are 0.4 ~ 1:1, acetic acid is mixed with hydrogen peroxide, under cooling conditions, liquid is imported in the immobilization reactor that solid acid catalyst is housed, by regulating flow velocity, the acetic acid described in making and the reaction times of the mixing liquid of hydrogen peroxide in immobilization reactor are 1-3 hour, obtain Peracetic Acid.

2. the method for the synthetic Peracetic Acid of a kind of serialization according to claim 1, is characterized in that: the concentration of described hydrogen peroxide is 20 ~ 70%, and preferred concentration is 30 ~ 50%.

3. the method for the synthetic Peracetic Acid of a kind of serialization according to claim 1, is characterized in that: under described cooling conditions, refer to and control 0 ~ 30 DEG C of temperature, preferred temperature is 10 ~ 15 DEG C.

4. the method for the synthetic Peracetic Acid of a kind of serialization according to claim 1, is characterized in that: described solid acid catalyst is acidic cation-exchange resin or perfluorinated sulfonic resin or immobilized sulfuric acid.