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Method for jointly preparing dicyclopentadiene dioxide and alkylene oxide by adopting titanium silicalite molecular sieve catalyst

A technology of dicyclopentadiene dioxide and titanium-silicon molecular sieves, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., to solve the problem of organic peroxide separation, high product selectivity, and simple process operation Effect

Pending Publication Date: 2021-07-09
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 jointly preparing dicyclopentadiene dioxide and alkylene oxide by adopting titanium silicalite molecular sieve catalyst
  • Method for jointly preparing dicyclopentadiene dioxide and alkylene oxide by adopting titanium silicalite molecular sieve catalyst
  • Method for jointly preparing dicyclopentadiene dioxide and alkylene oxide by adopting titanium silicalite molecular sieve catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The preparation of the modified Ti-HMS molecular sieve catalyst of embodiment 1

[0044] 500 ml reaction kettle, under room temperature and stirring conditions, put into 25 grams of hexadecylamine, 45 ml of water and 250 ml of ethanol successively, stir; Add diethyl silicate to the above solution and stir for 60 minutes; add 14.2 grams of tetraethyl titanate, stir and crystallize for 10 hours; add 74.9 grams of nano-carbon fibers, and continue stirring for 10 to 72 hours. After heating up, the material in the reaction kettle was crystallized at 200°C for 4 days, and then filtered to obtain a solid, which was extracted with ethanol to remove the template agent in the catalyst, and then washed with pure water until the eluent was neutral. Dry the washed solid at 110°C for 12 hours to obtain Ti-HMS supported by carbon nanofibers;

[0045] Add 300 milliliters of pure water, 3.0 grams of magnesium aluminum hydrotalcite (Mg 6 al 2 (OH) 16 CO 3 .4H 2 (0), room temperatur...

Embodiment 2～8

[0047] Embodiment 2~8 DCPDDO, 1,2-epoxypentane, the synthesis of 2,3-epoxypentane

[0048] 20 grams of the catalyst prepared in Example 1 were respectively packed into two 100 ml double-isothermal bed fixed-bed reactors in series, and the reaction feed liquid was pumped into the reactors through a metering pump. Using a continuous reaction process with two reactors in series, the effects of temperature, pressure, material ratio and space velocity on the reaction yield of DCPDDO, 1,2-epoxypentane or 2,3-epoxypentane were investigated. The first-stage reactor synthesizes dicyclopentadiene dioxide, and the second-stage reactor reacts excess organic peroxide with 1-pentene or 2-pentene to generate 1,2-epoxypentane or 2,3 -Pentene oxide, the used olefin raw material of the two-stage reaction of embodiment 2~5 is 1-pentene, and the used olefin raw material of embodiment 6~8 two-stage reaction is 2-pentene, and the results are shown in Table 1,2.

[0049] Table 1 One stage reaction ...

Embodiment 9～15

[0053] The synthesis of embodiment 9~15 DCPDDO, epoxycyclopentane

[0054] 20 grams of the catalyst prepared in Example 1 were packed into two 50 milliliter double isothermal-bed fixed-bed reactors respectively, and the reaction feed liquid was sent into the reactor by a metering pump, and a two-stage continuous reaction process was adopted to examine the temperature and pressure. , material ratio, space velocity on the reaction product DCPDDO, epoxy cyclopentane reaction yield. The first-stage reactor synthesizes dicyclopentadiene dioxide, and the second-stage reactor reacts excess organic peroxide and cyclopentene in the first-stage reactor to generate epoxycyclopentane. The results are shown in Tables 3 and 4.

[0055] Table 3 one stage reaction process

[0056]

[0057] Table 4 two-stage reaction process

[0058]

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Abstract

The invention discloses a method for jointly preparing dicyclopentadiene dioxide and alkylene oxide by adopting a titanium silicalite molecular sieve catalyst, the method comprises the following steps: reacting DCPD with excessive organic peroxide to generate dicyclopentadiene dioxide, adding olefin with 3-10 carbon atoms into the reaction product, and enabling the excessive organic peroxides to continuously react with the olefin to generate alkylene oxide, so that the organic peroxides in the reaction product are effectively removed. The preparation method is used for synthesizing dicyclopentadiene dioxide, not only is high in DCPD conversion rate and product selectivity and simple in process operation, but also can be used for synthesizing alkylene oxide, organic peroxides in reactants are fully utilized, the problem of separation of the organic peroxides in reaction products is effectively solved, and a green reaction process is provided for synthesizing alkylene oxide.

Description

technical field [0001] The invention belongs to the technical field of catalytic oxidation synthesis of organic epoxy compounds and olefin catalytic oxidation, and specifically relates to a method for jointly preparing dicyclopentadiene dioxide and alkylene oxide by using a titanium-silicon molecular sieve catalyst. Background technique [0002] Dicyclopentadiene 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 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 plas...

Claims

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Application Information

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IPC IPC(8): C07D493/08B01J29/89C07D301/19C07D303/04
CPCC07D493/08B01J29/89C07D301/19C07D303/04
Inventor 翁羽飞周飞奚军蒋方红许艾娜
Owner CHINA PETROLEUM & CHEM CORP
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