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A kind of molecular sieve immobilized catalytic synthesis method of allyl glycidyl ether

A technology of allyl glycidyl ether and a synthesis method, which is applied in the field of molecular sieve immobilized catalysis synthesis of allyl glycidyl ether, can solve the problems of difficulty in recovering allyl alcohol, high production cost, pollute the environment and the like, and achieves selectivity High, easy separation, low equipment corrosion effect

Active Publication Date: 2016-04-20
HUBEI GREENHOME MATERIALS TECH INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a molecular sieve immobilized catalytic synthesis method of allyl glycidyl ether, which solves the technical problems of existing methods such as environmental pollution, many side reactions, and high production costs.
At the same time, it also solves the problem that excessive allyl alcohol is difficult to recycle

Method used

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  • A kind of molecular sieve immobilized catalytic synthesis method of allyl glycidyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The preparation method of molecular sieve immobilized concentrated sulfuric acid and trifluoromethanesulfonic acid mixed catalyst: mix 5 parts of concentrated sulfuric acid and 15 parts of trifluoromethanesulfonic acid evenly in advance, add 50 parts in a certain reaction kettle, wash with distilled water and dry in advance 3A molecular sieve, gradually add the mixture of concentrated sulfuric acid and trifluoromethanesulfonic acid dropwise while stirring, then let it stand for adsorption for 12 hours, then dry it at 120°C for 4 hours, after cooling, wash it in absolute ethanol, and put it in 120°C Dry and set aside.

[0028] In the reaction kettle, add 278 parts of allyl alcohol and 6 parts of immobilized catalyst respectively, start stirring, raise the temperature to 45°C, add 185 parts of epichlorohydrin dropwise, control the reaction temperature at 50-55°C, finish adding in 3 hours, and keep warm React for 2 hours, after the reaction is complete, lower the temperatu...

Embodiment 2

[0030] The preparation method of the mixed catalyst of concentrated sulfuric acid and trifluoromethanesulfonic acid immobilized on molecular sieves: 10 parts of concentrated sulfuric acid and 10 parts of trifluoromethanesulfonic acid are uniformly mixed in advance. Add 50 parts of 3A molecular sieves that have been washed and dried with distilled water in a certain reaction kettle, and gradually add the mixture of concentrated sulfuric acid and trifluoromethanesulfonic acid dropwise while stirring, then let it stand for adsorption for 12 hours, and then red at 120°C for 4 hours. , after cooling, wash in absolute ethanol, and dry at 120°C for later use.

[0031] Add 230 parts of allyl alcohol and 16 parts of immobilized catalyst into the reaction kettle, start stirring, raise the temperature to 45°C, add 185 parts of epichlorohydrin dropwise, control the reaction temperature at 50-55°C, complete the addition in 3 hours, and keep warm for the reaction 2h, the reaction is complet...

Embodiment 3

[0033] Add 230 parts of allyl alcohol to the reaction kettle, use the solid-supported catalyst separated in Example 2, start stirring, raise the temperature to 45°C, add 185 parts of epichlorohydrin dropwise, and control the reaction temperature to 50-60°C for 3h After the addition is completed, keep the temperature for 2 hours. After the reaction is completed, lower the temperature, filter out the immobilized catalyst, and recover 110 parts of excess allyl alcohol under reduced pressure; lower the temperature to 30°C, add 5 parts of benzyltriethylammonium chloride, and drop Add 166 parts of 48% liquid caustic soda, control the reaction temperature at 40-45°C, complete the addition in 1 hour, keep the temperature for 2 hours, and complete the reaction. Add 100 parts of water and 100 parts of cyclohexane dissolved salt, let it stand for stratification, drain the brine, add 50 parts of water for washing, and adjust the pH of the water phase to 6-7, drain the lower water phase and...

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Abstract

A molecular sieve immobilized catalytic synthesis method of allyl glycidyl ether, using allyl alcohol and epichlorohydrin as raw materials, the weight ratio of allyl alcohol and epichlorohydrin is (1.2-2):1, in The ring-opening reaction is carried out under the action of a mixed catalyst of concentrated sulfuric acid and trifluoromethanesulfonic acid loaded on molecular sieves. The temperature of the ring-opening reaction is 50-70°C. The amount of concentrated sulfuric acid added is 10%-30% based on the mass of the molecular sieve. The addition amount of trifluoromethanesulfonic acid is 10%-30%, and the dosage of the catalyst is 1-5% of the total mass of reactants. The invention uses a new type of immobilized catalyst, which has high selectivity for the main reaction of the ring-opening reaction, less side reactions, low corrosion to equipment, easy separation from the reaction product after the end of the ring-opening reaction, and can be recycled after separation , can be recycled at least 10 times, avoiding environmental pollution, reducing production costs, and at the same time solving the problem of smooth recovery and recycling of excess allyl alcohol.

Description

technical field [0001] The invention relates to an allyl glycidyl ether, in particular to a molecular sieve immobilized catalytic synthesis method of an allyl glycidyl ether. Background technique [0002] Allyl glycidyl ether contains both carbon-carbon double bonds and epoxy bonds in its molecule. It is an important polymer monomer and organic synthesis intermediate; it is also widely used in the production of silicone, epoxy resin, chemical fiber, plastic and rubber It is used as additive, solvent, catalyst, crosslinking agent and chain transfer agent, and has important uses in organic chemical industry. [0003] The synthetic method of allyl glycidyl ether mainly contains following three kinds: [0004] The first method is: open-loop and closed-loop two-step method, using allyl alcohol and epichlorohydrin as raw materials, in the Lewis acid catalyst (such as concentrated sulfuric acid, boron trifluoride ether, anhydrous tin tetrachloride, dichloride In the presence of t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/22C07D301/26B01J31/26
CPCY02P20/584
Inventor 杨华胡登华肖华青黄圣
Owner HUBEI GREENHOME MATERIALS TECH INC
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