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Preparation method of plant monophenol glycidyl ether

A technology of glycidyl ether and monophenol, which is applied in the field of plant monophenol to prepare epoxy resin, can solve the problems of poor quality and high epoxy equivalent of plant phenol glycidyl ether

Inactive Publication Date: 2014-10-22
SUZHOU BAOLIRUI BIOLOGICAL MATERIAL TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] But the plant phenol glycidyl ether epoxy equivalent that above-mentioned patent obtains is higher, quality is poorer

Method used

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  • Preparation method of plant monophenol glycidyl ether
  • Preparation method of plant monophenol glycidyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Pass nitrogen into a 1L four-neck flask equipped with a stirring, thermometer and condensing reflux device to replace the air, add 200g of plant monophenol, 100g of epichlorohydrin, and 0.2g of tetraethylammonium bromide, stir and heat up to 50°C, and open Cycloaddition etherification reaction 1h. Keep the temperature constant, add 40 g of sodium hydroxide solution with a mass concentration of 30% dropwise with a constant pressure funnel, the dropwise addition time is 1 h, and keep for 0.5 h after the dropwise addition to complete the initial ring-closing epoxidation dechlorination reaction. Distill under reduced pressure to recover water and excess epichlorohydrin. The temperature was raised to 60° C., and 20 g of sodium hydroxide solution with a mass concentration of 10% was added at one time to carry out a second ring-closing epoxidative dechlorination reaction for 5 hours. Centrifugal filtration to obtain crude plant monophenol glycidyl ether; washing, liquid separ...

Embodiment 2

[0028] Pass nitrogen into a 1L four-neck flask equipped with a stirring, thermometer and condensing reflux device to replace the air, add 150 g of plant monophenols, 150 g of epichlorohydrin, 0.2 g of tetramethylammonium bromide, and 0.2 g of tetraethylammonium bromide g, stirring and raising the temperature to 75°C, the ring-opening addition etherification reaction was carried out for 2 hours. Keeping the temperature constant, add 45 g of sodium hydroxide solution with a mass concentration of 50% dropwise through a constant pressure funnel for 2.5 hours. Distill under reduced pressure to recover water and excess epichlorohydrin. The temperature was raised to 70° C., and 30 g of sodium hydroxide solution with a mass concentration of 20% was added at one time to carry out a second ring-closing epoxidative dechlorination reaction for 3 hours. Centrifugal filtration to obtain crude plant monophenol glycidyl ether; washing, liquid separation, distillation, and repeated filtration...

Embodiment 3

[0030] Pass nitrogen into a 1L four-neck flask equipped with a stirring, thermometer and condensing reflux device to replace the air, add 100g of plant monophenol, 0.5g of benzyltriethylammonium bromide, stir and raise the temperature to 80°C, and etherify by ring-opening addition Reaction 0.5h. Keeping the temperature constant, 50 g of sodium hydroxide solution with a mass concentration of 60% was added dropwise with a constant pressure funnel for 4 hours, and kept for 3 hours after the dropwise addition to complete the initial ring-closing epoxidative dechlorination reaction. Distill under reduced pressure to recover water and excess epichlorohydrin. The temperature was raised to 90° C., and 40 g of sodium hydroxide solution with a mass concentration of 30% was added at one time to carry out a second ring-closing epoxidative dechlorination reaction for 1 hour. Centrifugal filtration to obtain crude plant monophenol glycidyl ether; washing, liquid separation, distillation, a...

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Abstract

The invention discloses a preparation method of plant monophenol glycidyl ether. The preparation method comprises the steps of carrying out ring-opening addition etherification on plant monophenol and epoxy chloropropane under the action of a quaternary ammonium salt catalyst; then, carrying out initial ring-closed epoxidation dechlorination reaction under the action of sodium hydroxide; separating a solvent and excessive epoxy chloropropane, and then, adding sodium hydroxide to carry out secondary ring-closed epoxidation dechlorination reaction to obtain a crude product; refining the crude product to obtain the plant monophenol glycidyl ether with the solid content of more than 99.5%. The method is high in yield; in addition, the prepared plant monophenol glycidyl ether is relatively low in epoxide equivalent, relatively good in quality and beneficial to industrial production.

Description

technical field [0001] The invention relates to a method for preparing epoxy resin by using plant monophenol, in particular to a preparation method of plant monophenol glycidyl ether. Background technique [0002] Plant monophenol is a kind of C 15 Unsaturated linear phenolic compounds, due to their abundant sources, low price, non-toxic and tasteless, plant monophenols have great application prospects and research and development value. The basic structure of plant monophenols is: [0003] R=C 15 h 31-2n , where n=0~3, [0004] plant monophenols [0005] As a derivative of phenol, plant monophenols have the properties of phenol and can react with formaldehyde to synthesize phenolic resins. Due to the existence of long chains, plant monophenols can also be used in the synthesis of polyvinyl chloride (PVC) plasticizers, etc. [0006] Plant monophenol glycidyl ether is an epoxy compound with unsaturated long chain and benzene ring. It has the characteristics of low v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/23C07D301/26
CPCC07D303/23C07D301/26
Inventor 戴志成
Owner SUZHOU BAOLIRUI BIOLOGICAL MATERIAL TECH DEV
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