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Polyvinyl ether synthesis method

A polyvinyl ether and polyvinyl alcohol technology, applied in the field of organic synthesis, can solve the problems of high technical requirements, temperature sensitivity, and restrictions on the wide application of compounds, and achieve the effect of high purity and waste reduction

Active Publication Date: 2015-11-04
宁夏荆洪生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to choose different initiators or cations to control the length of the chain, is also extremely sensitive to temperature, and requires relatively high technical requirements, which further limits the wide application of this type of compound.
Currently, polyvinyl alcohol synthesis technology is relatively mature, the types are relatively diverse, and the market supply is sufficient. However, there is still a lack of relevant literature and patent reports for obtaining different types of polyvinyl ethers from this raw material.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Synthesis of polyvinyl methyl ether:

[0017] In a three-necked flask equipped with a reflux water separation device, add low-viscosity polyvinyl alcohol (average molecular weight: 16,000-20,000, 0.4 mol) and 20 ml of water, and dissolve completely under stirring. After adding strongly acidic cation exchange resin (0.4 mol) and tetrabutylammonium bromide (4 mmol), add methanol (2.0 mol) and 180 ml of toluene, heat to reflux at 110°C to separate water. After detecting that there is no more water in the reaction, the temperature of the reaction system is lowered, and the solid obtained after filtration can be continuously used in the synthesis reaction for 4-6 times to maintain the same activity. The organic layer was washed with saturated brine, and distilled to obtain a 40% toluene solution of polyvinyl methyl ether.

Embodiment 2

[0019] Synthesis of Polyvinyl Ether:

[0020] In a three-necked flask equipped with a reflux water separation device, add low-viscosity polyvinyl alcohol (average molecular weight: 16,000-20,000, 0.4 mol) and 22 ml of water, and dissolve completely under stirring. After adding strongly acidic cation exchange resin (0.4 mol) and trioctylmethylammonium chloride (5 mmol), ethanol (2.5 mol) and 180 ml of toluene were added, and heated at 110°C to reflux to separate water. After detecting that there is no more water coming out of the reaction, the temperature of the reaction system is lowered, and the solid obtained after filtration can be continuously used in the synthesis reaction for 3-4 times to maintain the same activity. The organic layer was washed with saturated brine, and distilled to obtain a 50% toluene solution of polyvinyl ether.

Embodiment 3

[0022] Synthesis of polyvinyl n-butyl ether:

[0023] In a three-necked bottle equipped with a reflux water separation device, add medium-viscosity polyvinyl alcohol (average molecular weight: 110,000-130,000, 0.4 mole) and 30 ml of water, and dissolve completely under stirring. After adding strongly acidic cation exchange resin (0.4 mol) and tetradecyltrimethylammonium chloride (8 mmol), add n-butanol (4.0 mol) and 220 ml p-xylene, heat at 140°C to reflux and separate water . After detecting that there is no more water in the reaction, the temperature of the reaction system is lowered, and the solid obtained after filtration can be continuously used in the synthesis reaction for 4-6 times to maintain the same activity. The organic layer was washed twice with saturated brine, and distilled to obtain an 80% p-xylene solution of polyvinyl n-butyl ether.

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PUM

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Abstract

The invention discloses a polyvinyl ether synthesis method. The method comprises the steps that polyvinyl alcohol is dissolved in water, strong acid cation exchange resin and phase transfer catalyst are added, then, methylbenzene or paraxylene and corresponding alcohol are added, heating is carried out at the temperature of 110-140 DEG C, and backflowing and water diversion are carried out. After a reaction is finished, the system carries out cooling and filtering, organic layer saturated salt water washing is carried out, distillation is carried out, and a methylbenzene or paraxylene solution with 40-80% of polyvinyl ether is obtained. The cation exchange resin and the phase transfer catalyst can be recycled, so that waste is effectively reduced, and environmental protection is achieved. The obtained product is high in purity and has competitive advantages.

Description

technical field [0001] The invention relates to a method for synthesizing polyvinyl ether, which belongs to the technical field of organic synthesis. Background technique [0002] Polyvinyl ether is mainly used in coatings, adhesives, additives, and plasticizers, and those with special structures can also be used as aviation hydraulic oil, hydraulic transmission oil, and shock absorber oil. [0003] The prior art method mainly uses acetylene and alcohol to prepare vinyl ether first, and then obtains polyvinyl ether through free radical or active cationic polymerization or copolymerization. This method needs to choose different initiators or cations to control the length of the chain, is also extremely sensitive to temperature, and requires relatively high technical requirements, which further limits the wide application of this type of compound. Currently, polyvinyl alcohol synthesis technology is relatively mature, the types are relatively diverse, and the market supply is...

Claims

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Application Information

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IPC IPC(8): C08F16/06C08F8/00
CPCY02P20/584
Inventor 杨辉韩连城朱美山
Owner 宁夏荆洪生物科技有限公司
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