Immobilized catalytic synthesis method of allyl glycidyl ether molecular sieve

A technology for the synthesis of allyl glycidyl ether and its synthesis method, which is applied in the field of molecular sieve immobilized catalytic synthesis of allyl glycidyl ether, which can solve the problems of difficult recovery of allyl alcohol, high production cost, and environmental pollution, and achieve selectivity High, easy to separate, low corrosion effect of equipment

Active Publication Date: 2015-05-06
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 existin

Method used

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  • Immobilized catalytic synthesis method of allyl glycidyl ether molecular sieve

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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

The invention relates to an immobilized catalytic synthesis method of an allyl glycidyl ether molecular sieve. According to the method, allyl alcohol and epoxy chloropropane at a feed weight ratio of (1.2-2): 1 are adopted as raw materials and are subjected to ring-opening reaction in the presence of a mixed catalyst of concentrated sulfuric acid and trifluoromethanesulfonic acid which are immobilized on the molecular sieve at an ring-opening reaction temperature of 50-70 DEG C, wherein the addition of concentrated sulfuric acid is 10%-30% of mass of the molecular sieve, the addition of trifluoromethanesulfonic acid is 10%-30% of mass of the molecular sieve, and the usage amount of the catalyst is 1-5% of the total mass of the reactants. The novel immobilized catalyst is high in main ring-opening reaction selectivity, small in secondary reactions and low in device corrosion; after the ring-opening reaction is completed, the catalyst easily separates from reaction products and can be recycled for at least 10 times after being separated, the environmental pollution is avoided, the production cost is decreased and meanwhile, the problem that excessive allyl alcohol is smoothly recovered and recycled is solved.

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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IPC IPC(8): C07D303/22C07D301/26B01J31/26
CPCY02P20/584C07D303/22B01J31/26B01J2231/48C07D301/26
Inventor 杨华胡登华肖华青黄圣
Owner HUBEI GREENHOME MATERIALS TECH INC
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