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Synthesis method of tetrahydrofurfuryl alcohol polyoxyethylene ether

A technology of polyoxyethylene ether and tetrahydrofurfuryl alcohol, which is applied in the field of synthesis of tetrahydrofurfuryl alcohol polyoxyethylene ether, can solve the problems that have not been reported in the literature, and achieve the effects of reasonable product distribution, light color and improved selectivity

Inactive Publication Date: 2013-12-11
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It is an important organic synthesis intermediate, which can be used in epoxy resin diluent, chloride stabilizer and fabric finishing agent. It has good reactivity and activity, and can be used in various reagents in paint and coating industry after addition reaction; However, this series of products has not been seen on the market, nor has it been reported in literature.

Method used

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  • Synthesis method of tetrahydrofurfuryl alcohol polyoxyethylene ether
  • Synthesis method of tetrahydrofurfuryl alcohol polyoxyethylene ether

Examples

Experimental program
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Effect test

Embodiment 1

[0015] In this example 1) Add 102g of tetrahydrofurfuryl alcohol, 2.0g of solid potassium hydroxide, 50g of acetone, (the weight ratio of acetone:tetrahydrofurfuryl alcohol = 1:2.04) vacuum with a vacuum pump, using N 2 Replace the air in the reactor. After three replacements, the temperature is raised to 58℃ under vacuum ≥-0.02MPa to start collecting the distilled liquid (the vacuum pipe is connected to the condenser to recover the distilled liquid), and the dehydration temperature is 70℃. The collected liquid is tested , After the water is evaporated ≥ 0.64g, stop vacuuming and close the vacuum valve; 2) Start adding ethylene oxide continuously, control the reaction temperature at 60-80℃, the pressure in the reactor at 0.1-0.55Mpa, add epoxy in total 880 g of ethane (the molar ratio of tetrahydrofurfuryl alcohol: ethylene oxide: catalyst = 1:20:0.04). After the addition is completed, keep holding the reaction until the pressure no longer drops. After the reaction is completed...

Embodiment 2

[0018] In this embodiment 1) Add 102g of tetrahydrofurfuryl alcohol, 3.0g of solid sodium hydroxide, and 100g of acetone (weight ratio of acetone: tetrahydrofurfuryl alcohol = 1:1.02) into the reaction kettle; vacuum with a vacuum pump, using N 2 Replace the air in the reactor, replace it three times, heat up to 58℃ under vacuum ≥-0.02MPa and start collecting the steamed liquid (the vacuum pipe is connected to the condenser to recover the steamed liquid), the dehydration temperature is 100℃, the collected liquid is tested , After the water is evaporated ≥1.0g, stop vacuuming and close the vacuum valve; 2) Start adding ethylene oxide continuously, control the reaction temperature at 60-80℃, the pressure in the reactor at 0.1-0.55Mpa, add epoxy in total 440 g of ethane (the molar ratio of tetrahydrofurfuryl alcohol:ethylene oxide:catalyst=1:10:0.07). After the addition is completed, keep holding the reaction until the pressure no longer drops. After the reaction is completed, the...

Embodiment 3

[0021] Add 204g of tetrahydrofurfuryl alcohol, 2.5g of solid potassium methoxide, 20.4g of acetone (weight ratio of acetone:tetrahydrofurfuryl alcohol = 1:10) into the reaction kettle, vacuum with a vacuum pump, and use N 2 Replace the air in the reactor. After three replacements, the temperature is raised to 58°C under vacuum ≥-0.02MPa to start collecting the distilled liquid (the vacuum pipe is connected to the condenser to recover the distilled liquid), and the dealcoholization temperature is 58°C. It was detected that after methanol was distilled out of ≥1.0g, stop vacuuming, close the vacuum valve, and start adding ethylene oxide continuously, control the reaction temperature at 60-80℃, the pressure in the reactor at 0.1-0.55Mpa, and add ethylene oxide in total 352 g of alkanes (molar ratio of tetrahydrofurfuryl alcohol:ethylene oxide:catalyst=1:4.0:0.02). After the addition is completed, keep holding the temperature and continue to react until the pressure no longer drops....

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Abstract

The invention discloses a synthesis method of tetrahydrofurfuryl alcohol polyoxyethylene ether, and is characterized by comprising the following steps: 1) using water and ethanol contained agent which is commercially available as a dissolvent, using tetrahydrofurfuryl alcohol as a raw material, and adding a catalyst to perform reactions of dealcoholization and dehydration; 2) taking epoxyethane as a chain extender, performing reaction, and preparing tetrahydrofurfuryl alcohol polyoxyethylene ether. The tetrahydrofurfuryl alcohol polyoxyethylene ether synthesized by the method is high in content, good in color quality, and low in residue of tetrahydrofurfuryl alcohol, as well as content of by-product carbowax or polyethylene glycol monomethyl ether.

Description

Technical field [0001] The invention relates to a method for synthesizing tetrahydrofurfuryl alcohol polyoxyethylene ether, and belongs to the technical field of organic compound synthesis. Background technique [0002] Tetrahydrofurfuryl alcohol polyoxyethylene ether itself is a good surfactant. According to the number of ethylene oxide added, the performance of the obtained product is also different. It can be used as a wetting agent, penetrating agent, Different uses such as emulsifier. At the same time, it has an epoxy group, which can open the ring and react with other special substances to form a product with special properties. It is an important organic synthesis intermediate. It can be used as epoxy resin diluent, chloride stabilizer and fabric finishing agent. It has good reactivity and activity. It can be used in various reagents in paint and coating industry after addition reaction; However, this series of products has not been seen on the market, nor has it been re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28
Inventor 马定连王胜利金一丰郭晓峰张敏
Owner ZHEJIANG HUANGMA TECH
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