Synthetic method of butyl glycidyl ether

A technology of glycidyl ether and synthesis method, applied in the direction of organic chemistry, etc., which can solve the problems of corrosion of reaction equipment, low epoxy value of the final product, and inability to recycle and use

Active Publication Date: 2013-06-12
ANHUI XINYUAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of this type of acidic catalyst not only has the disadvantages of serious corrosion to the reaction equipment, inconvenient use, and inability to recycle and recycle; it also has poor selectivity in the ring-opening reaction, resulting in many by-products in the intermediate product, making the epoxy of the final product Low value, high total chlorine content

Method used

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  • Synthetic method of butyl glycidyl ether

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 5g of activated carbon and impregnate in 75g of HNO with a mass fraction of 10-30% 3 In the solution, the immersion temperature is 20-40°C, the immersion time is 3-4h, then the activated carbon is taken out and washed to neutrality, filtered and dried to obtain the modified activated carbon; after the modified activated carbon is impregnated in the The catalyst can be obtained by immersing in 75g of toluene solution with 0.5% boron mass fraction, immersing temperature at 30-45°C, and immersing time for 3-4 hours, filtering and drying. The immobilized amount of the activated carbon-supported boron trifluoride catalyst was measured to be 5%.

Embodiment 2

[0024] Take 5g of activated carbon and first impregnate it in 50g of HNO with a mass fraction of 10-30%. 3 In the solution, the immersion temperature is 40-70°C, the immersion time is 2-3h, then the activated carbon is taken out and washed to neutrality, filtered and dried to obtain the modified activated carbon; after the modified activated carbon is impregnated in the The catalyst can be obtained by immersing in 50g of toluene solution with 2% boron mass fraction, immersing temperature at 45-60°C and immersing time for 2.5-3 hours, filtering and drying. It is measured that the immobilized amount of the activated carbon-supported boron trifluoride catalyst is 16%.

Embodiment 3

[0026] Take 5g of activated carbon and impregnate in 25g of HNO with a mass fraction of 10-30% 3 In the solution, the immersion temperature is 70-100°C, the immersion time is 1-2h, then the activated carbon is taken out and washed to neutrality, filtered and dried to obtain the modified activated carbon; after the modified activated carbon is impregnated in the The catalyst can be obtained by immersing in 50g of toluene solution with 5% boron mass fraction at 60-70°C for 1-2.5 hours, filtering and drying. It is measured that the immobilized amount of the activated carbon immobilized boron trifluoride catalyst is 20%.

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Abstract

The invention discloses a synthetic method of butyl glycidyl ether. The method comprises the following steps of performing ring-opening reaction on butanol and epoxy chloropropane to prepare a butyl chlorhydrin ether intermediate and performing ring-closing reaction on the butyl chlorhydrin ether intermediate and sodium hydroxide to prepare butyl glycidyl ether. The catalyst used in the ring-opening reaction is an active carbon immobilized boron trifluoride catalyst, wherein the immobilized amount of boron trifluoride is 5-20%. Through using the active carbon immobilized boron trifluoride catalyst to catalyze the ring-opening reaction of butanol and epoxy chloropropane, the selectivity for main reaction of the ring-opening reaction is high, and side reactions are reduced, so that the epoxide number of the obtained butyl glycidyl ether is high, the content of organochlorine is low and the quality is good. In addition, the solid phase catalyst has low corrosion to devices, can be easily separated from reaction products after ring-opening reaction, and can be recycled after being separated, and therefore, the environmental pollution is avoided.

Description

technical field [0001] The invention relates to the field of synthesis of aliphatic monoglycidyl ether, in particular to a synthesis method of butyl glycidyl ether. Background technique [0002] Butyl glycidyl ether is a linear aliphatic monoepoxy diluent, containing ether bonds and epoxy groups in the molecule, which has the advantages of low viscosity and good dilution effect; it participates in the curing reaction during curing to form a uniform system. It is a commonly used reactive diluent for epoxy resin, and can be widely used in the dilution of epoxy materials such as solvent-free insulating paint, epoxy potting and encapsulation materials, solvent-free epoxy floor coatings and epoxy adhesives, among which high epoxy value The high-quality distillate can also be used as a modified material for fatty amines, imidazoles and other amine curing agents. [0003] The synthesis of butyl glycidyl ether mainly includes one-step method, two-step method and oxidation method. A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/22C07D301/26
Inventor 朱新宝程振朔王传柱
Owner ANHUI XINYUAN CHEM
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