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Method for producing dicyclopentadiene dioxide by using molybdenum-based homogeneous catalyst and obtained dicyclopentadiene dioxide

A dipentadiene dioxide, homogeneous catalyst technology, applied in the direction of organic chemistry, can solve the problems of poor product quality, strong equipment corrosion, pollution, etc., and achieve the effect of overcoming organic acid corrosion

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

[0009] The technical problem to be solved by the present invention is that in the prior art, there are dicyclopentadiene dioxide products containing Cl - and Na + , and use peroxyacid as oxidant, the equipment is highly corrosive, and produces a large amount of chlorine-containing and sulfur-containing wastewater and waste residue, serious pollution, poor product quality, high energy consumption, low production efficiency, etc., providing a new homogeneous catalytic An efficient and integrated method for the preparation of dicyclopentadiene dioxide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] At 90°C and 0.1MPa, cumene and air are oxidized in the oxidation tower. By controlling the O in the reaction tail gas 2 The content is less than 6% to adjust the air flow to obtain a cumene hydroperoxide (CHP) oxidation solution with a weight concentration of 20 wt%. According to the requirements of the follow-up reaction, the 20wt% CHP oxidation solution can be concentrated to different concentrations with a maximum concentration of 80wt% by vacuum distillation.

[0077] In the presence of molybdenum isooctanoate catalyst, the above CHP oxidation solution is epoxidized with dicyclopentadiene (DCPD) in the first epoxidation reactor to generate dicyclopentadiene dioxide (DCPDDO) and α,α- Dimethylbenzyl alcohol (DMBA). Where CHP / DCPD=6:1 (mole), CHP / Mo=1500:1 (mole), the reaction time is 2 hours, the reaction temperature is 85° C., and the reaction pressure is 1.0 MPa. The DCPD conversion rate was 99.0%, and the DCPDDO selectivity was 96.5%.

[0078] The reaction materia...

Embodiment 2

[0087] At 100°C and 0.4MPa, cumene and air are oxidized in the oxidation tower. By controlling the O in the reaction tail gas 2 The content is less than 6% to adjust the air flow to obtain a cumene hydroperoxide (CHP) oxidation solution with a weight concentration of 25%. According to the needs of the subsequent reaction, the 25% CHP oxidation solution can be concentrated to different concentrations with a maximum concentration of 80wt% by vacuum distillation.

[0088] In the presence of molybdenum isooctanoate catalyst, the above CHP oxidation solution is epoxidized with dicyclopentadiene (DCPD) in the first epoxidation reactor to generate dicyclopentadiene dioxide (DCPDDO) and α,α- Dimethylbenzyl alcohol (DMBA). Where CHP / DCPD=4:1 (mole), CHP / Mo=2000:1 (mole), the reaction time is 2 hours, the reaction temperature is 90° C., and the reaction pressure is 1.0 MPa. Using online chromatographic quantitative analysis, the conversion rate of DCPD was 98.5%, and the selectivity o...

Embodiment 3

[0099] At 100°C and 0.3MPa, cumene and air are oxidized in the oxidation tower. By controlling the O in the reaction tail gas 2 The content is less than 6% to adjust the air flow to obtain a cumene hydroperoxide (CHP) oxidation solution with a weight concentration of 25%. According to the needs of the subsequent reaction, the 25% CHP oxidation solution can be concentrated to different concentrations with a maximum concentration of 80wt% by vacuum distillation.

[0100] In the presence of molybdenum naphthenate catalyst, the above-mentioned CHP oxidation solution is epoxidized with dicyclopentadiene (DCPD) in the first epoxidation reactor to generate dicyclopentadiene dioxide (DCPDDO) and α, α - Dimethylbenzyl alcohol (DMBA). Where CHP / DCPD=5:1 (mole), CHP / Mo=2000:1 (mole), the reaction time is 3 hours, the reaction temperature is 90° C., and the reaction pressure is 1.0 MPa. The DCPD conversion rate was 99.2%, and the DCPDDO selectivity was 95.6%.

[0101] The reaction mate...

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Abstract

The invention discloses a method for producing dipentadiene dioxide, which comprises the following steps of: 1, reacting cumyl hydroperoxide with dicyclopentadiene in the presence of a homogeneous molybdenum-based homogeneous catalyst to obtain a material I; step 2, adding a monoolefine compound into the material I, and reacting to obtain a material II; step 3, carrying out post-treatment on the material II to respectively obtain dipentadiene dioxide, a monoepoxy compound and alpha, alpha-dimethyl benzyl alcohol; and step 4, carrying out conversion treatment on the alpha, alpha-dimethyl benzyl alcohol. A two-step epoxidation reaction is adopted in the presence of a molybdenum-based homogeneous catalyst to efficiently generate more than two (including two) epoxidation products; the obtained alpha, alpha-dimethyl benzyl alcohol can be treated according to market and comprehensive conditions to obtain cumene or dicumyl peroxide and the like.

Description

technical field [0001] The invention relates to dicyclopentadiene dioxide, in particular to a method for producing dicyclopentadiene dioxide by utilizing a molybdenum-based homogeneous catalyst. Background technique [0002] Epoxy resins generally refer to polymer prepolymers containing two or more epoxy groups, with aliphatic, alicyclic or aromatic segments as the main chain. The molecular structure of epoxy resin is characterized by active epoxy groups in the molecular chain, and the epoxy groups can be located at the end, middle or ring structure of the molecular chain. Due to the active oxygen-containing groups in the molecular structure, they can undergo cross-linking reactions with various types of curing agents to form insoluble, infusible high polymers with a three-way network structure. [0003] As a thermosetting resin, epoxy resin has excellent electrical insulation, heat resistance, water resistance, adhesion, chemical resistance and mechanical properties, and h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/08
CPCC07D493/08
Inventor 金国杰翁羽飞汪超高焕新杨洪云康陈军丁琳黄政
Owner CHINA PETROLEUM & CHEM CORP