Method for continuously synthesizing peracetic acid by using microreactor

A technology of microreactor and peracetic acid, applied in chemical instruments and methods, preparation of peroxygen compounds, preparation of organic compounds, etc., can solve problems such as dangerous self-accelerating decomposition reactions, low concentration of peracetic acid, and low production efficiency , to achieve the effect of easy reaction control, short reaction time and high production efficiency

Pending Publication Date: 2022-07-08
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional synthesis of peracetic acid is a batch reaction generation method, the reaction takes 10 to 20 hours, the reaction time is long, the concentration of peracetic acid is low, and the production efficiency is not high. In addition, the important feature of organic peroxy compounds is the self-accelerating decomposition temperature. , high reaction temperature and long reaction time in the production process may lead to dangerous self-accelerating decomposition reaction, explosion or fire in unfavorable environment

Method used

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  • Method for continuously synthesizing peracetic acid by using microreactor
  • Method for continuously synthesizing peracetic acid by using microreactor
  • Method for continuously synthesizing peracetic acid by using microreactor

Examples

Experimental program
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Effect test

Embodiment 1-6

[0025] Experiments were carried out according to this method, 10mol% concentrated sulfuric acid with a concentration of 98wt% was slowly added to acetic anhydride to obtain mixed solution A, the metering pump was turned on, 30wt% hydrogen peroxide first entered the micro-preheater at a stable flow rate, and the hydraulic diameter of the micro-preheater was 1.2mm, the channel length is 35cm, the hydrogen peroxide enters the microsieve reactor after preheating, and the mixed solution A directly enters the microsieve reactor. The hydraulic diameter of the microsieve reactor is 0.5mm, and the channel length is 43cm. The mixed solution A and the hydrogen peroxide are mixed and reacted in the micro-sieve reactor. The heat exchanger controls the reaction temperature to 30-80°C, and the constant flow pump is used to control the flow rate of the reaction liquid to be 1ml / min. The residence time of the reaction is 9min. , and finally the solution obtained is analyzed according to the nat...

Embodiment 7-13

[0030] Using the same micro-preheater and micro-mesh reactor as in Example 1, acetic anhydride solution containing 10mol% concentration of 98wt% concentrated sulfuric acid and 30wt% hydrogen peroxide were input into the microreactor through two pumps for mixing and reaction, and The reaction temperature was controlled at 60°C by a heat exchanger, so that the molar ratio of acetic anhydride and hydrogen peroxide was 1.10:1, and the flow rate of the reaction solution was controlled by a constant flow pump to control the residence time of the material in the reactor to be 3.0 min and 3.6 min respectively. min, 4.5min, 6.0min, 9.0min, 12min and 18min, the product solution was collected from the discharge port, and the peracetic acid content was analyzed according to the national standard (GB 19104-2008). The results are shown in Table 2 below.

[0031]

[0032] As can be seen from the data in Table 2 above, when the residence time is 4.5min, the yield is the best, and it is give...

Embodiment 14-17

[0034] Using the same micro-preheater and micro-sieve reactor as in Example 1, acetic anhydride solution A containing 5mol%, 10mol%, and 15mol% concentration of 98wt% concentrated sulfuric acid and 30wt% hydrogen peroxide were respectively prepared into the micrometer at a stable flow rate. The reactor mixes and reacts, the heat exchanger controls the reaction temperature at 60°C, the constant flow pump is used to control the flow rate of the reaction solution, and the flow rate of the reaction solution is 1ml / min. The acetic acid content, the results are shown in Table 3 below, respectively.

[0035]

[0036] It can be seen from the above table 3 that the content of peracetic acid obtained when the amount of sulfuric acid is 15 mol% is the highest, and it is given priority to use.

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Abstract

The invention provides a method for continuously synthesizing peracetic acid by using a microreactor. According to the method, acetic anhydride (AA) is used as a raw material, concentrated sulfuric acid is used as a catalyst, and hydrogen peroxide (HP) is oxidized in a microreactor to generate peracetic acid (PAA). The concentration of the hydrogen peroxide is 30-50wt%, the molar ratio of the acetic anhydride to the hydrogen peroxide is (1-1.2): 1, the dosage of the catalyst concentrated sulfuric acid is 5-15mol%, the retention time is 3-20 minutes, and the reaction temperature is 30-80 DEG C. The method comprises the following steps: fully mixing acetic anhydride and concentrated sulfuric acid, mixing with hydrogen peroxide preheated by a micro preheater in a micro reactor to initiate a reaction, controlling the reaction temperature through a heat exchanger, and controlling the concentration of generated peracetic acid to be 21-35wt%. According to the invention, continuous preparation of peracetic acid is realized by adopting the microreactor, the process flow is simplified, the reaction period is short, the reaction is easy to control, peracetic acid can be rapidly and conveniently obtained when the device is used and opened, and the safety of the preparation process is improved.

Description

technical field [0001] The invention relates to a preparation method of peracetic acid, in particular to a method for continuously synthesizing peracetic acid by utilizing a microreactor, and belongs to the technical field of chemical product synthesis. Background technique [0002] Organic peroxy compounds are very reactive chemicals. Due to its easy decomposition into highly reactive free radicals and oxygen atoms. It is mainly used as oxidant for organic synthesis, initiator for free radical polymerization, cross-linking agent for polymer materials, bleaching agent and bactericide, etc. [0003] The traditional synthesis of peracetic acid adopts the batch reaction generation method, the reaction is 10 to 20 hours, the reaction time is long, the concentration of peracetic acid is low, and the production efficiency is not high. , high reaction temperature and long reaction time during production may lead to dangerous self-accelerating decomposition reaction, explosion or ...

Claims

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Application Information

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IPC IPC(8): C07C407/00C07C409/26B01J19/00
CPCC07C407/00B01J19/0093C07C409/26Y02P20/10
Inventor 陈光文廉应江韩梅
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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