Preparation method of dicyclopentadiene dioxide based on modified nano aluminum oxide loaded heteropolyacid type compound catalyst

A technology of dicyclopentadiene dioxide and aluminum oxide, applied in organic compound/hydride/coordination complex catalysts, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc. It can solve the problems that heteropolyacids are easy to fall off, etc., and achieve the effects of environmental protection technology, shortened service life and stable performance

Pending Publication Date: 2020-05-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Aiming at the problem that the heteropolyacid in the existing heteropolyacid catalyst is easy to fall off, the inventor carried out a chemical reaction with the hydroxyl group on the surface of the nano-aluminum oxide through a silylation agent containing a quaternary ammonium salt, and modified the aluminum

Method used

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  • Preparation method of dicyclopentadiene dioxide based on modified nano aluminum oxide loaded heteropolyacid type compound catalyst
  • Preparation method of dicyclopentadiene dioxide based on modified nano aluminum oxide loaded heteropolyacid type compound catalyst
  • Preparation method of dicyclopentadiene dioxide based on modified nano aluminum oxide loaded heteropolyacid type compound catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1 illustrates the preparation method of the modified nano-alumina oxide-supported heteropoly acid compound catalyst, and Examples 2 to 30 illustrate the preparation of dicyclopentadiene dioxide based on the modified nano-aluminum oxide-supported heteropoly acid compound Preparation. The molecular structural formulas of the silylation reagents used in the catalyst modification treatment of Examples 2-7 are as shown in (1) to (6):

[0022]

[0023]

Embodiment 2～22

[0024] In Examples 2-22, the reaction yield of dicyclopentadiene dioxide is defined as:

[0025]

[0026] Example 1

[0027] Select nano aluminum oxide as the inorganic oxide carrier, the molecular structure of the silylation reagent used is shown in the molecular structure (2), benzene is used as the solvent, and the catalyst is prepared according to the following steps:

[0028] (1) According to the molar ratio of inorganic oxide powder to silylation reagent of 300:1 and the mass ratio of solvent to inorganic oxide powder of 4:1, weigh the above-mentioned raw materials into the reactor, mix and stir to make the reaction, the reaction temperature is 50 ℃, the reaction time is 15 hours;

[0029] (2) Filter the product in step (1), separate the solid powder from the solution, and wash the separated solid powder with the solvent in step (1). The solvent used for each wash is the same as the inorganic oxide in step (1). The powder mass ratio is 5:1, remove the unreacted silylation reage...

Embodiment 2～7

[0034] Using dicyclopentadiene as the raw material and hydrogen peroxide as the oxidant, the epoxidation reaction adopts a suspended bed reactor to modify the heteropoly acid type compound and its mass percentage composition in the nano alumina supported heteropoly acid type compound catalyst See Table 1. Specific steps: Into an autoclave with a volume of 500ml containing an inner cooling coil, put the modified nano-alumina oxide-supported heteropoly acid compound catalyst, solvent, and dicyclopentadiene according to the process requirements, turn on the stirring, and heat up the material. After the reaction material reaches the process setting temperature, the hydrogen peroxide is added into the reaction kettle by a metering pump, the cooling water system is turned on, and the cooling water flow is adjusted to ensure that the reaction temperature is within the process setting range. After the reaction is over, turn on the cooling water to cool the material to room temperature....

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Abstract

The invention discloses a method for preparing dicyclopentadiene dioxide by catalytic oxidation of dicyclopentadiene serving as a raw material in the presence of a solvent through a suspended bed or afixed bed reactor by taking a modified nano aluminum oxide loaded heteropolyacid type compound as a catalyst and hydrogen peroxide as an oxidant. Compared with the prior art, the preparation method provided by the invention has the advantages that the catalyst is long in service life, stable in performance, simple to separate and high in product yield, and the reaction yield of dicyclopentadienedioxide is greater than 96%.

Description

Technical field [0001] The invention belongs to the field of organic epoxy compounds. Specifically, it relates to a method for preparing dicyclopentadiene dioxide based on a modified nano-aluminum oxide supported heteropolyacid compound catalyst. Background technique [0002] Dicyclopentadiene is an important component in the C5 fraction of petroleum cracking, accounting for about 14-19% of the C5 fraction. Dicyclopentadiene dioxide, the product of the epoxidation reaction of dicyclopentadiene, is an alicyclic epoxide with excellent performance. Compared with ordinary epoxy resin, dicyclopentadiene dioxide has better performance in high temperature resistance, heat resistance, weather resistance, ultraviolet resistance, electrical insulation, and high strength. Based on the above properties, dicyclopentadiene dioxide is widely used in high-temperature castables, glass fiber reinforced plastics, adhesives, laminates and electronic device packaging. [0003] In the prior art, dicyc...

Claims

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Application Information

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IPC IPC(8): C07D493/08B01J31/18B01J27/188B01J27/19B01J23/30B01J23/28
CPCC07D493/08B01J27/188B01J27/19B01J23/30B01J23/28
Inventor 翁羽飞秦技强周飞奚军蒋方红许艾娜
Owner CHINA PETROLEUM & CHEM CORP
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