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A kind of preparation method of polyvinyl butyral

A technology of polyvinyl butyral and polyvinyl alcohol, which is applied in the field of polymer chemistry and can solve the problems of poor thermal stability of PVB film strength and polyvinyl butyral

Inactive Publication Date: 2017-09-29
宜春市康盛高分子材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the above-mentioned technical problems in the prior art, the invention provides a kind of preparation method of polyvinyl butyral, the preparation method of described this polyvinyl butyral should solve the preparation method in the prior art to obtain The low butyraldehyde group value in polyvinyl butyral affects the strength of PVB film and the technical problems of poor thermal stability of polyvinyl butyral

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 6000kg of deionized water into a 10000L (10T) enamel reactor equipped with a stirring, heating and dripping system. Under stirring at 80r / min, add 750kg of polyvinyl alcohol and heat to 95±1℃. Dissolve polyvinyl alcohol (PVA) in 4h, then cool the dissolved PVA to 20±2℃, add 1500kg hydrochloric acid solution with a mass percent solubility of 2.5% in 30min, after adding acid, cool to 10± 2℃, first drop 300kg of n-butyraldehyde into the acidic PVA solution; dripping time 40min; stirring speed 150r / min; after dripping n-butyraldehyde, keep the reaction at 10±2℃ for 60min; then, at this temperature Next, add the remaining 150kg n-butyraldehyde dropwise for 30 minutes. After the dropwise addition of n-butyraldehyde is completed, the reaction is kept at 10±2°C for 60min; then, the temperature is heated to 64±1°C at a heating rate of 10°C / h, and the reaction is kept at this temperature for 90min. After the completion of the reaction, the reaction mass was cooled to 30°C. T...

Embodiment 2

[0023] Add 6000kg of deionized water into a 10000L (10T) enamel reactor equipped with a stirring, heating and dripping system. Under stirring at 80r / min, add 750kg of polyvinyl alcohol and heat to 95±1℃. Dissolve polyvinyl alcohol (PVA) in 4h, then cool the dissolved PVA to 20±2℃, add 1500kg hydrochloric acid solution with a mass percent solubility of 2.5% in 30min, after adding acid, cool to 10± 2℃, first drop 300kg of n-butyraldehyde into the acidic PVA solution; dripping time 40min; stirring speed 150r / min; after dripping n-butyraldehyde, keep the reaction at 10±2℃ for 60min; then, at this temperature Next, add the remaining 150kg n-butyraldehyde dropwise for 30 minutes. After the dropwise addition of n-butyraldehyde is completed, the reaction is kept at 10±2°C for 60min; then, the temperature is heated to 64±1°C at a heating rate of 10°C / h, and the reaction is kept at this temperature for 90min. After the completion of the reaction, the reaction mass was cooled to 30°C. T...

Embodiment 3

[0027] Add 6000kg of deionized water into a 10000L (10T) enamel reactor equipped with a stirring, heating and dripping system. Under stirring at 80r / min, add 750kg of polyvinyl alcohol and heat to 85±2℃. Dissolve polyvinyl alcohol (PVA) in 4h, then cool the dissolved PVA to 20±2℃, add 1500kg hydrochloric acid solution with a mass percent solubility of 2.5% in 30min, after adding acid, cool to 10± 2℃, first drop 300kg of n-butyraldehyde into the acidic PVA solution; dripping time 40min; stirring speed 150r / min; after dripping n-butyraldehyde, keep the reaction at 10±2℃ for 60min; then, at this temperature Next, add the remaining 150kg n-butyraldehyde dropwise for 30 minutes. After the dropwise addition of n-butyraldehyde is completed, the reaction is kept at 10±2°C for 60min; then, the temperature is heated to 64±1°C at a heating rate of 10°C / h, and the reaction is kept at this temperature for 90min. After the completion of the reaction, the reaction mass was cooled to 30°C. T...

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Abstract

A preparation method of polyvinyl butyral according to the present invention uses polyvinyl alcohol with an alcoholysis degree of 97.0 to 98.5% as a raw material, dissolves it in deionized water and cools it, and under the catalysis of an inorganic acid, first makes the polyvinyl butyral at a low temperature. Vinyl alcohol reacts with a part of n-butyraldehyde, then adds the remaining n-butyraldehyde to continue to react with polyvinyl alcohol, then heats up to 50-70°C at a heating rate of 8-12°C / h to fully acetalize, and the reaction ends Finally, the polyvinyl butyral and the acidic liquid are separated by a centrifuge, and the separated polyvinyl butyral is washed with deionized water and a dilute alkali solution in a vacuum filter washing machine, and then dried by centrifugation and airflow. Polyvinyl butyral is obtained. After the thermal stability test, the polyvinyl butyral obtained by the method of the present invention does not turn yellow within 1.5 hours at a high temperature of 180°C, the butyraldehyde group value (%)>76, and the hydroxyl value (%)>18~19.5 , haze (%) <0.3.

Description

Technical field: [0001] The invention belongs to the field of polymer chemistry, and particularly relates to a polyvinyl butyral, specifically a method for preparing polyvinyl butyral. technical background: [0002] Polyvinyl butyral is formed by the condensation of polyvinyl alcohol (PVA) and n-butyraldehyde in an aqueous solution through inorganic acid catalysis. It is a thermoplastic polymer compound, referred to as PVB. [0003] With the continuous development of my country's national economy, the use of PVB has gradually entered a wider range of fields. Especially with the rapid development of my country's automobile industry and the strict safety requirements imposed by the Ministry of Construction on high-rise building glass, the domestic demand for PVB market has increased significantly every year. However, there is still a certain gap between domestic PVB preparation technology and foreign countries. Therefore, high-quality PVB needs to be imported in large quantities fro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F16/06C08F8/28
Inventor 金东元杨志强吴大利
Owner 宜春市康盛高分子材料科技有限公司