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CN-121990960-A - Method for continuously producing dicumyl peroxide

CN121990960ACN 121990960 ACN121990960 ACN 121990960ACN-121990960-A

Abstract

The application relates to the field of fine organic synthesis, in particular to a method for continuously producing dicumyl peroxide. The application adopts the fiber with specific diameter and surface contact angle as the material of the coalescing filter element coalescing layer to treat the raffinate oil phase, so that most of alkali in the raffinate oil phase can be removed, the alkali content of the raffinate oil phase can be effectively controlled, and the recycling oil phase with lower alkali content can be obtained. The process can reduce the investment of alkali, lower the process cost, realize higher selectivity and purity and reduce the generation of byproducts. The method for continuously producing the dicumyl peroxide has the advantages of good economy, high selectivity and less byproducts, and can meet the industrial production requirements.

Inventors

  • LIU SHISHUI
  • WANG JUNCHENG
  • ZHOU JINGKAI

Assignees

  • 万华化学集团股份有限公司

Dates

Publication Date
20260508
Application Date
20260104

Claims (10)

  1. 1. The method for continuously producing the dicumyl peroxide is characterized by comprising the following steps of: introducing oxygen-containing gas into the first mixed solution containing the first reaction raw material and alkali to perform oxidation reaction to form oxidation reaction solution; adding a second reaction raw material into the oxidation reaction liquid to form a second mixed liquid; Separating the second mixed solution from the first oil and water to form a first oil phase and a first water phase; Extracting the first oil phase by adopting alkali solution, and separating oil from water to form a raffinate oil phase and a second water phase; mixing the raffinate oil phase with water to form an oil-water mixture, and performing coalescence separation through a coalescence filter element to form a recycling oil phase and a third water phase, wherein the material of a coalescence layer of the coalescence filter element comprises hydrophilic fibers and hydrophobic fibers, the diameters of the hydrophilic fibers and the hydrophobic fibers are respectively and independently 0.1-2 mu m, the surface contact angle of the hydrophilic fibers is 10-60 degrees, and the surface contact angle of the hydrophobic fibers is 110-160 degrees; And recycling the recycled oil phase to the oxidation reaction step for oxidation reaction.
  2. 2. The process of claim 1, wherein the mass ratio of the raffinate oil phase to the water is (1-20): 1.
  3. 3. The method of claim 1, wherein in the step of mixing the raffinate oil phase with water, the mixing conditions include a stirring intensity of 2kW/m 3 ~8kW/m 3 and a residence time of 1h to 5h.
  4. 4. The method of claim 1, wherein the conditions of coalescing separation further comprise a residence time of 1h to 5h.
  5. 5. The process of any one of claims 1-4, wherein the first reactant feedstock and the second reactant feedstock each independently comprise diisopropylbenzene; optionally, the diisopropylbenzene comprises at least one of m-diisopropylbenzene and p-diisopropylbenzene; Optionally, each of the first reaction raw material and the second reaction raw material independently further comprises at least one of m-mono-hydrogen peroxide diisopropylbenzene and p-mono-hydrogen peroxide diisopropylbenzene; Optionally, the addition amount of the second reaction raw material is 90-110 wt% of the consumption amount of the diisopropylbenzene in the first reaction raw material in the oxidation reaction.
  6. 6. The method of any one of claims 1-4, wherein one or more of the following characteristics are met: (1) The oxygen-containing gas comprises air; (2) The alkali comprises at least one of sodium hydroxide and sodium carbonate; (3) The pH of the oxidation reaction liquid is 9-11.
  7. 7. The method according to any one of claims 1 to 4, wherein the conditions for the oxidation reaction comprise a reaction temperature of 80 ℃ to 90 ℃ and a reaction time of 5 hours to 15 hours.
  8. 8. The method of any of claims 1-4, wherein the first oil-water separation and the second oil-water separation comprise at least one of centrifugal separation, coalescing separation, and sedimentation separation.
  9. 9. The method of any one of claims 1-4, wherein one or more of the following characteristics are met: (1) The alkali solution comprises at least one of sodium hydroxide aqueous solution and sodium carbonate aqueous solution; (2) In the alkali solution, the mass concentration of alkali is 5-10wt%; (3) The extraction conditions comprise extraction temperature of 10-50 ℃, optionally 15-25 ℃; (4) The extraction conditions comprise that an extraction tower is adopted for multistage countercurrent extraction, and 3-7 stages of countercurrent extraction can be selected; (5) The mass ratio of the first oil phase to the alkali solution is 1 (0.8-1.5).
  10. 10. The method of any one of claims 1-4, wherein the base content of the reclaimed oil phase is 500ppm to 1500ppm, optionally 500ppm to 1000ppm.

Description

Method for continuously producing dicumyl peroxide Technical Field The application relates to the field of fine organic synthesis, in particular to a method for continuously producing dicumyl peroxide. Background The dicumyl peroxide is an important fine chemical process route, and the produced dicumyl peroxide can be used for producing resorcinol after being cracked, and is widely applied to the fields of wood adhesives, meta-alpha resin, ultraviolet absorbers and the like. However, this process route produces by-products of 3- (2-hydroxy-2-propyl) -1- (2-hydroperoxy-2-propyl) benzene or 4- (2-hydroxy-2-propyl) -1- (2-hydroperoxy-2-propyl) benzene during oxidation, and particularly when the alkali concentration in the reaction system is too high, the by-product utilization value is relatively low, resulting in a decrease in process route economy. Meanwhile, the oxidation reaction liquid contains components such as unreacted raw materials, reaction intermediates, alkali liquor and the like besides the dicumyl peroxide and the byproducts, and purification and separation are needed. After oil-water separation, the separation of the dihydrobenzene in the oil phase and other raw materials (such as unreacted raw materials, reaction intermediates and the like) can be realized through alkali extraction, wherein the dihydrobenzene enters the alkali water phase, the other raw materials remain in the raffinate oil phase, and the recycling of the raffinate oil phase to the reaction system is beneficial to improving the economy. However, the raffinate oil phase dissolves a large amount of sodium hydroxide, and the pH of the reaction system can be obviously improved when the raffinate oil phase is recycled to the reaction system, so that a large amount of byproduct 3- (2-hydroxy-2-propyl) -1- (2-hydroperoxy-2-propyl) benzene or 4- (2-hydroxy-2-propyl) -1- (2-hydroperoxy-2-propyl) benzene is caused. Thus, there is a need to provide an economical and low-byproduct process for continuously producing cumene hydroperoxide. Disclosure of Invention Based on this, the main object of the present application is to provide an economical and low-by-product continuous process for producing cumene hydroperoxide, which meets the industrial production needs. In a first aspect, the present application provides a method for continuously producing cumene hydroperoxide, comprising the steps of: introducing oxygen-containing gas into the first mixed solution containing the first reaction raw material and alkali to perform oxidation reaction to form oxidation reaction solution; adding a second reaction raw material into the oxidation reaction liquid to form a second mixed liquid; Separating the second mixed solution from the first oil and water to form a first oil phase and a first water phase; Extracting the first oil phase by adopting alkali solution, and separating oil from water to form a raffinate oil phase and a second water phase; mixing the raffinate oil phase with water to form an oil-water mixture, and performing coalescence separation through a coalescence filter element to form a recycling oil phase and a third water phase, wherein the material of a coalescence layer of the coalescence filter element comprises hydrophilic fibers and hydrophobic fibers, the diameters of the hydrophilic fibers and the hydrophobic fibers are respectively and independently 0.1-2 mu m, the surface contact angle of the hydrophilic fibers is 10-60 degrees, and the surface contact angle of the hydrophobic fibers is 110-160 degrees; And recycling the recycled oil phase to the oxidation reaction step for oxidation reaction. In some embodiments, the mass ratio of the raffinate oil phase to the water is (1-20): 1. In some embodiments, in the step of mixing the raffinate oil phase with water, the mixing conditions include a stirring intensity of 2kW/m 3~8kW/m3 and a residence time of 1h to 5h. In some embodiments, the conditions for coalescing separation further include a residence time of 1h to 5h. In some embodiments, the first reactant feedstock and the second reactant feedstock each independently comprise diisopropylbenzene; optionally, the diisopropylbenzene comprises at least one of m-diisopropylbenzene and p-diisopropylbenzene; Optionally, each of the first reaction raw material and the second reaction raw material independently further comprises at least one of m-mono-hydrogen peroxide diisopropylbenzene and p-mono-hydrogen peroxide diisopropylbenzene; Optionally, the addition amount of the second reaction raw material is 90-110 wt% of the consumption amount of the diisopropylbenzene in the first reaction raw material in the oxidation reaction. In some embodiments, one or more of the following features are satisfied: (1) The oxygen-containing gas comprises air; (2) The alkali comprises at least one of sodium hydroxide and sodium carbonate; (3) The pH of the oxidation reaction liquid is 9-11. In some embodiments, the oxidation reaction conditions inclu