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Preparation method of dicyclopentadiene dioxide based on modified nano MgO loaded heteropolyacid catalyst

A technology of dicyclopentadiene dioxide and loaded heteropolyacid, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve the problem that heteropolyacids are easy to fall off. and other problems, to achieve the effect of environmental protection process method, high activity, improved service life and shortened life.

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 selects a silylating agent to chemically react with the hydroxyl on the surface of MgO, introduces quaternary ammonium salt ion groups on the surface of MgO, and undergoes ion exchange reaction. The heteropolyacid or peroxyheteropolyacid as the active component is firmly adsorbed on the surface of the modified nano-MgO carrier, which improves the problem of heteropolyacid shedding and prolongs the service life of the catalyst

Method used

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  • Preparation method of dicyclopentadiene dioxide based on modified nano MgO loaded heteropolyacid catalyst
  • Preparation method of dicyclopentadiene dioxide based on modified nano MgO loaded heteropolyacid catalyst
  • Preparation method of dicyclopentadiene dioxide based on modified nano MgO loaded heteropolyacid catalyst

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Embodiment 1

[0020] Example 1 illustrates the preparation method of the modified nanometer MgO-supported heteropolyacid compound catalyst, and Examples 2-22 illustrate the preparation method of dicyclopentadiene dioxide based on the modified nanometer MgO supported heteropolyacid compound catalyst. The silylating reagents used for catalyst modification treatment in Examples 2-7 have molecular structural formulas as shown in (1)-(6) respectively:

[0021]

[0022]

Embodiment 2～22

[0023] In embodiment 2~22, the definition of dicyclopentadiene dioxide reaction yield:

[0024]

[0025] Example 1

[0026] Nano-MgO is selected as the inorganic oxide carrier, the molecular structure of the silylation reagent used is shown in formula (3), acetonitrile is used as the solvent, and the catalyst is prepared according to the following steps:

[0027](1) According to the molar ratio of inorganic oxide powder to silylation reagent 100:1, the mass ratio of solvent to inorganic oxide powder is 4:1, weigh the above-mentioned raw materials and put them into the reactor, mix and stir to make them react, and the reaction temperature is 90 °C, the reaction time is 10 hours;

[0028] (2) The product in step (1) is filtered, the solid powder is separated from the solution, and the isolated solid powder is washed with the solvent in step (1), and the solvent used for each washing is mixed with the inorganic oxide in step (1). The powder mass ratio is 4:1, remove the unre...

Embodiment 14～22

[0042] Further illustrate the stability of the modified nanometer MgO loaded heteropolyacid compound catalyst used in the present invention, the reaction raw material that drops into every time is identical, and catalyst is reused, and adopts suspension reactor, and concrete steps: to volume is 500ml containing inner cooling plate In the autoclave of tube, drop into the used catalyst 15g of embodiment 2, with 316L stainless steel wire mesh, catalyst adopts hanging basket mode to be fixed on the inner cooling coil of autoclave, drop into 98% dicyclopentadiene 60g, mass percentage is 50 % hydrogen peroxide 74ml, acetone 222ml, reaction temperature 60 ~ 62 ℃, reaction pressure 5MPa, mechanical stirring to ensure that the reaction raw materials and the catalyst fully contact, the materials are mixed evenly, the reaction time is 10h, and the reaction is terminated. The material is cooled to room temperature and discharged. The water and solvent were separated to obtain a crude prod...

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Abstract

The invention discloses a method for preparing dicyclopentadiene dioxide by taking dicyclopentadiene as a raw material, taking a modified nano MgO loaded heteropolyacid type compound as a catalyst andtaking hydrogen peroxide as an oxidizing agent through catalytic oxidation using a suspended bed or a fixed bed reactor in the presence of a solvent. In the preparation method provided by the invention, the catalyst is long in service life, stable in performance, easy to separate and high in product yield, and when the catalyst is used for preparing dicyclopentadiene dioxide, the reaction yield of dicyclopentadiene dioxide is greater than 96%.

Description

technical field [0001] The invention belongs to the field of organic epoxy compounds, and specifically relates to a method for preparing dicyclopentadiene dioxide based on a modified nano-MgO loaded 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. The epoxidation reaction product of dicyclopentadiene Dicyclopentadiene dioxide is an alicyclic epoxide with excellent performance. Compared with ordinary epoxy resins, dicyclopentadiene dioxide has better performance in terms of 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 resistant castables, glass fiber reinforced plastics, adhesives, laminated materials and electronic device packaging. [0003] In the pri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/08B01J31/26B01J27/188B01J23/30B01J27/19
CPCC07D493/08B01J31/26B01J27/188B01J23/30B01J27/19B01J2231/72
Inventor 翁羽飞奚军蒋方红周飞许艾娜
Owner CHINA PETROLEUM & CHEM CORP
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