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High-double bond content allyl polyether production method

A technology of allyl polyether and production method, which is applied in the fields of ether preparation, alkylene oxide preparation ether, organic chemistry, etc. It can solve the problems of difficult catalyst preparation, wide molecular weight distribution, low double bond content, etc., and achieve improved safety , time shortening, and the effect of speeding up the reaction

Active Publication Date: 2015-11-18
扬州晨化新材料股份有限公司
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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 propose an allyl polyether with a double bond content of more than 98% in view of the defects of the prior art products such as low double bond content, poor reactivity, many by-products, wide molecular weight distribution, and difficulty in catalyst preparation. production method

Method used

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  • High-double bond content allyl polyether production method
  • High-double bond content allyl polyether production method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Preparation of catalyst sodium allyl alcohol solution in allyl alcohol:

[0025] Inject 300kg of propylene alcohol into two external circulation stirred reactors equipped with refrigerated condensate reflux, start the stirring and external circulation pump, after nitrogen replacement, open the hydrogen discharge valve and nitrogen automatic replenishment valve, and continue to heat up to 50°C Add 10kg of sodium metal to react, open the jacket of the reaction kettle and the cooling water of the external circulation cooler to ensure the reaction temperature is 60-65°C, after adding the sodium metal, keep it warm for the reaction, when the hydrogen analyzer shows that no hydrogen is produced, cool down to 40°C and exit Feed to obtain 310kg of catalyst sodium acrylate propylene alcohol solution.

[0026] (2) Preparation of allyl polyether:

[0027] Pump 6kg of the catalyst sodium acrylate propylene alcohol solution in step (1) and 52kg of propylene alcohol into the rea...

Embodiment 2

[0031] (1) Preparation of catalyst sodium allyl alcohol solution in allyl alcohol:

[0032] Pump a certain amount of 250kg of propylene alcohol into two external circulation stirred reactors equipped with refrigerated condensate reflux, start the stirring and external circulation pump, after nitrogen replacement, open the hydrogen discharge valve and nitrogen automatic replenishment valve, and raise the temperature to 50°C Afterwards, add 10kg of sodium metal continuously for reaction, open the jacket of the reaction kettle and the cooling water of the external circulation cooler to ensure the reaction temperature is 70-75°C. ℃ discharge to obtain 260 kg of catalyst sodium acrylate allyl alcohol solution.

[0033] (2) Preparation of allyl polyether:

[0034] Pump 52kg of the catalyst sodium acrylate propylene alcohol solution in step (1) and up to 8kg of propylene alcohol into the reaction kettle. After replacing the air with nitrogen, feed 1942kg of epoxy compound to react, ...

Embodiment 3

[0037] (1) Preparation of catalyst sodium allyl alcohol solution in allyl alcohol:

[0038]Pump a certain amount of 200kg of propylene alcohol into two external circulation stirred reactors equipped with refrigerated condensate reflux, start the stirring and external circulation pump, after nitrogen replacement, open the hydrogen discharge valve and nitrogen automatic replenishment valve, and raise the temperature to 50°C Afterwards, add 10kg of sodium metal continuously for reaction, open the jacket of the reactor and the cooling water of the external circulation cooler to ensure the reaction temperature is 65-70°C. °C discharge to obtain 210 kg of catalyst sodium acrylate allyl alcohol solution.

[0039] (2) Preparation of allyl polyether:

[0040] Pump 56kg of the catalyst sodium acrylate propylene alcohol solution in step (1) and 5kg of propylene alcohol into the reaction kettle. After replacing the air with nitrogen, 3942kg of epoxy compounds are introduced to react, and...

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Abstract

The invention discloses a high-double bond content allyl polyether production method and belongs to the technical field of polyether compound synthesis in organic chemistry. In an anoxic environment, at a temperature of 110-140 DEG C, under catalysis action of an allyl alcohol solution of sodium allylate, allyl alcohol and an epoxy compound are mixed and undergo a reaction, the reaction product is aged and cooled to form an allyl polyether crude product, the allyl polyether crude product and water are mixed, the mixture is neutralized and filtered, and a liquid phase is collected and is allyl polyether. The prepared allyl polyether has molecular weight of 200-8000, double bond content greater than or equal to 98% and a molecular weight distribution coefficient less than or equal to 1.05. In catalyst preparation, an outer circulation reaction vessel with two condensers utilizing a freezing liquid for condensation is used so that a reaction rate is accelerated, an allyl alcohol loss is less than 0.2% and environmental pollution is reduced.

Description

technical field [0001] The invention relates to a preparation technology of allyl polyether, which belongs to the technical field of synthesis of polyether compounds in organic chemistry. Background technique [0002] Allyl polyether is a block / random copolymer formed by the reaction of propylene alcohol and epoxy compounds (such as ethylene oxide, propylene oxide or butylene oxide). It is a synthetic polyether-modified polysiloxane, The main raw material of silicon modified polyether. Polyether modified polysiloxane is water-soluble and oil-soluble; it not only has various excellent properties of traditional siloxane products, such as high and low temperature resistance, anti-aging, hydrophobicity, electrical insulation, low surface tension, etc., but also It has special properties such as lubrication, softness, spreadability and emulsion stability provided by polyether chain segments, and can be used as polyurethane foam stabilizer, textile auxiliary agent, oil field demu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C08G65/30C07C43/178C07C41/03
Inventor 房连顺董晓红张秀英曹志利颜梅刘敏
Owner 扬州晨化新材料股份有限公司
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