Catalytic preparation method of dicyclopentadiene dioxide by quaternary ammonium heteropoly phosphato tungstate

A technology of dicyclopentadiene dioxide and phosphotungstic heteropoly acid, which is applied in the direction of organic chemistry, can solve the problems of serious equipment corrosion, complicated reaction process, poor practicability, etc., and achieves high safety, short process and easy operation. Effect

Active Publication Date: 2010-05-12
SICHUAN DONGFANG INSULATING MATERIAL
View PDF0 Cites 16 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the traditional methods for preparing olefin epoxides include the chlorohydrin method and the peracid method. These methods have the disadvantag

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0025] Preparation of phosphotungstic heteropoly acid quaternary ammonium salt catalyst:

[0026] Take cetyltrimethylammonium bromide, etc. to prepare quaternary ammonium phosphotungstate as an example:

[0027] Add 20 g of tungstic acid (80 mmol) and 85 ml of 30% by mass hydrogen peroxide (832.5 mmol) aqueous solution to the reactor, stir and heat to 60°C, react for 80 minutes, cool to room temperature, and then 2.32 g 85% phosphoric acid (20mmol) was dissolved in 9ml of water and added to the reaction solution. The reaction solution was diluted with 210ml of distilled water and then stirred for 50 minutes; 14.6g of cetyltrimethylammonium bromide (40mmol) was dissolved Add 500ml of chloroform to the above reaction solution by dropwise addition, and continue to stir for 80 minutes, stand still for layering, separate the organic phase and distill under reduced pressure to remove the solvent in the organic phase, and the remainder is heated at 60℃ The quaternary ammonium phosphotung...

Example Embodiment

[0030] Example 1:

[0031] Add 125ml 1,2-dichloroethane, 25ml (0.185mol) dicyclopentadiene, 0.99g (5.1×10 -4 mol) Catalyst 2. Add 27.2ml of 50% (0.472mol) hydrogen peroxide by weight percentage dropwise into the reaction flask, and make the temperature in the reactor not exceed 50℃. After the addition of hydrogen peroxide, keep it at 60℃ Continue the reaction for 12 hours under the conditions, use a pipette to directly take 2ml samples from the reactor for analysis, distill under reduced pressure to recover 1,2-dichloroethane, cool to room temperature to remove the water in the reactor, and then use 250ml ethyl acetate The ester is divided into two times to dissolve the residue and filtered to obtain the catalyst. The filtrate is distilled under reduced pressure to recover the ethyl acetate organic solvent to obtain a crude product, which is then recrystallized with a mixed solvent of ethyl acetate and petroleum ether in a volume ratio of 1:4 The white powdery solid was vacuum dr...

Example Embodiment

[0032] Example 2:

[0033] Put 54ml toluene, 18.0ml (0.1335mol) dicyclopentadiene, 1.0g (5.1×10 -4 mol) Catalyst 3, 33ml of hydrogen peroxide with a concentration of 30% (0.3232mol) by weight. After the hydrogen peroxide is added dropwise, continue the reaction at 80°C for 6 hours, and use a pipette to directly take 2ml sample from the reactor To be analyzed, filter the reacted materials, distill the filtrate under reduced pressure to recover toluene, remove the remaining water after cooling to room temperature, and then dissolve the residue twice with 100ml ethyl acetate and filter to obtain the catalyst, and distill the filtrate under reduced pressure The crude product is obtained after the ethyl acetate organic solvent is recovered, and then recrystallized with a mixed solvent of ethyl acetate and petroleum ether in a volume ratio of 1:5 to obtain a white powdery solid, and the others are the same as in Example 1 and omitted.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a catalytic preparation method of dicyclopentadiene dioxide by quaternary ammonium heteropoly phosphato tungstate, which is characterized by comprising the following steps: epoxidation reaction: adding the raw materials of dicyclopentadiene, solvent I and quaternary ammonium heteropoly phosphato tungstate in a reactor, heating the temperature to 30-80 DEG C, stirring and dropwise adding aqueous hydrogen peroxide solution, and reacting for 3-36h under the temperature of 30-80 DEG C after dropwise adding; post-treatment: cooling the reacted materials to room temperature, evaporating solvent I by reduced pressure distillation and separating and removing water to obtain the mixture of the product and the quaternary ammonium heteropoly phosphato tungstate catalyst, dissolving and filtering the mixture by ethyl acetate to obtain filter cake, namely the recovered quaternary ammonium heteropoly phosphato tungstate catalyst, recovering ethyl acetate by performing reduced pressure distillation on filtrate to obtain the crude product, performing recrystallization on the crude product by solvent II, and drying to obtain the product. The invention has the advantages of convenient operation, high safety, small pollution, simple post treatment, and high product yield and purity.

Description

technical field [0001] The invention belongs to organic epoxy compounds, and relates to a method for preparing dicyclopentadiene dioxide by catalyzing a quaternary ammonium salt of phosphotungstic heteropolyacid. Background technique [0002] Dicyclopentadiene dioxide (or Dicyclopentadiene Dioxide, domestic trade name R-122, EP 207; English name: Dicyclopentadiene dioxide; Bicyclopentadienedioxide) is an alicyclic epoxide with excellent performance. It has excellent weather resistance, heat resistance, high hardness, and good electrical insulation performance. It is used in high temperature resistant casting materials, glass fiber reinforced plastics, adhesives, laminated materials, and electronic device packaging. Dicyclopentadiene dioxide is generally prepared by epoxidation of dicyclopentadiene, and the raw materials are easily available. In the prior art, the traditional methods for preparing olefin epoxides include the chlorohydrin method and the peracid method. These ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07D493/08
Inventor 吴学明李学超唐安斌李建学杨波
Owner SICHUAN DONGFANG INSULATING MATERIAL
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap