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Method for preparing dicyclopentadiene dioxide DCPDDO and 2-phenyl-2-propanol

A technology of dicyclopentadiene and propanol dioxide is applied in chemical instruments and methods, hydrogenation preparation, oxygen-containing functional group reduction preparation, etc., to achieve the effects of improved reaction process safety, high product yield, and simple process control.

Pending Publication Date: 2022-05-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, excessive organic peroxides bring many problems to product separation and purification, and also bring many adverse effects on catalyst activity.

Method used

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  • Method for preparing dicyclopentadiene dioxide DCPDDO and 2-phenyl-2-propanol
  • Method for preparing dicyclopentadiene dioxide DCPDDO and 2-phenyl-2-propanol
  • Method for preparing dicyclopentadiene dioxide DCPDDO and 2-phenyl-2-propanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Embodiment 1: Preparation of titanium silicon molecular sieve catalyst

[0049] At room temperature and under stirring conditions, add 10 grams of hexadecylamine to 112 ml of water and 110 milliliters of ethanol successively in the reactor, and stir; Add it to the above solution, stir for 30 minutes, crystallize for 12 hours, add 18.7 grams of carbon nanofibers, continue stirring for 10 to 72 hours, heat up the reactor, crystallize the reaction material at 200°C for 1 day, filter to obtain a solid, and extract the catalyst with ethanol template agent, and then washed with pure water until the eluent was neutral. After drying the washed solid at 110° C. for 12 hours, Ti-HMS supported by carbon nanofibers was obtained.

[0050] Add 3 times the volume of pure water, 1.2 grams of Mg(OH) 2 , room temperature, stirred for 48 hours, separated the solid, washed with pure water until the washing liquid was neutral, dried at 80°C for 20 hours, and then calcined at 400°C for 20 ...

Embodiment 2～9

[0052] Embodiment 2~9: Tank reactor, the mixed solution of main product DCPDDO and 2-phenyl-2-propanol obtained by catalytic oxidation:

[0053] Get titanium-silicon molecular sieve catalyst, cumene hydroperoxide CHP, and solvent are fed into 500 milliliters of reaction kettles according to technological requirements, rectify and separate solvent, 2-phenyl-2-propanol after the reaction is completed, and then separate DCPDDO, The crystallization mother liquor is mixed with fresh reaction raw materials and put into the reactor to continue the reaction of the next batch. The effects of temperature, pressure, material ratio, and reaction time on the yield of the reaction product DCPDDO were investigated. The catalyst compositions used in Examples 2-9 are shown in Table 1, and the experimental results are shown in Table 2.

[0054] Table 1 Catalyst mass percent composition

[0055]

[0056] *Note: C—indicates carbon nanofiber.

[0057] Table 2 Batch Reaction Synthesis of DCPDD...

Embodiment 10～17

[0059] Examples 10-17: Catalytic oxidation synthesis of DCPDDO and 2-phenyl-2-propanol mixed solution by fixed-bed continuous reaction process

[0060] Take 40 grams of titanium-silicon molecular sieve catalyst, fill it into a 100 ml isothermal fixed-bed reactor, use cumene hydroperoxide CHP as the oxidant, and inject the reaction feed liquid into the reactor through a metering pump. The reaction product is separated from the solvent and 2-phenyl-2-propanol by rectification, DCPDDO is separated by crystallization, the crystallization mother liquor is mixed with fresh reaction raw materials and re-entered the reactor, and the effects of temperature, pressure, material ratio and space velocity on the reaction product are investigated. The influence of DCPDDO yield, the catalyst compositions used in Examples 10-17 are shown in Table 3, and the experimental results are shown in Table 4.

[0061] Table 3 Catalyst mass percent composition

[0062]

[0063] *Note: C—indicates carbo...

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Abstract

The invention discloses a method for preparing dicyclopentadiene dioxide (DCPDDO) and 2-phenyl-2-propanol, which comprises the following steps: with a titanium silicalite molecular sieve as a catalyst, in the presence of an inert solvent, reacting DCPD with CHP to generate dicyclopentadiene dioxide and 2-phenyl-2-propanol; then adopting a double-tower series rectification separation process, collecting the solvent and 2-phenyl-2-propanol at the tops of a first rectification tower and a second rectification tower, and collecting DCPDDO at the bottom of the second tower; dCPDDO collected in a tower kettle is subjected to crystallization separation, solid DCPDDO is obtained, unreacted raw materials or monooxidized dicyclopentadiene in crystallization mother liquor is mixed with fresh reaction raw materials again, and the mixture enters a reactor for continuous reaction. According to the preparation process disclosed by the invention, unreacted raw materials or monooxidized dicyclopentadiene can be reused, the product yield is high, the discharge amount of waste liquid is remarkably reduced, the process operation is safe, and a green reaction process is provided for synthesizing DCPDDO.

Description

technical field [0001] The invention belongs to the technical field of catalytic oxidation synthesis of organic epoxy compounds and olefin catalytic oxidation, specifically, it relates to a kind of preparation and separation of (3,4), (8,9) with dicyclopentadiene as raw material and titanium silicon molecular sieve as catalyst. )-diepoxy-tricyclic[5,2,1,0 2,6 ] Decane (commonly known as dicyclopentadiene dioxide DCPDDO), 2-phenyl-2-propanol method. Background technique [0002] Dicyclopentadiene (DCPD), scientific name: tricyclic [5,2,1,0 2,6 ]Decadiene-3,8 is an important component in the C5 fraction of petroleum cracking, accounting for about 14% to 19% of the C5 fraction. The epoxidation reaction product of dicyclopentadiene is dicyclopentadiene dioxide (DCPDDO), scientific name (3,4), (8,9)-diepoxy-tricyclo[5,2,1,0 2,6 ] Decane is an alicyclic epoxide with excellent performance. Compared with ordinary epoxy resins, dicyclopentadiene dioxide has better performance in ...

Claims

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Application Information

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IPC IPC(8): C07D493/08C07C29/132C07C29/19C07C33/20B01J29/89B01J35/06
CPCC07D493/08C07C29/132C07C29/19B01J29/89B01J2229/20B01J2229/42B01J35/58C07C33/20
Inventor 翁羽飞孙荣华范存良周飞奚军蒋方红许艾娜曹强
Owner CHINA PETROLEUM & CHEM CORP
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