Preparation method of high-acetalization-degree high-flowability polyvinyl butyral resin

A polyvinyl butyral resin, high fluidity technology, applied in the field of heat-shrinkable polymer materials, can solve the problem of increasing the amount of plasticizer used in processing temperature, affecting the strength and stability of products, and breaking the macromolecular chain of products, etc. problems, to achieve good fluidity, reduce the breakage of product macromolecular chains, and achieve the effect of good resin bonding

Active Publication Date: 2013-04-03
ZHEJIANG DECENT PLASTIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in this method, directly raising the temperature to 45-75°C for 4 hours will easily lead to the breakage of the product's macromolecular chain, thereby affecting the strength and stability of the product, resulting in the need to increase the processing temperature or the amount of plasticizer used for processing into a film, which is difficult and expensive to process. high

Method used

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  • Preparation method of high-acetalization-degree high-flowability polyvinyl butyral resin

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Heat 100g of polyvinyl alcohol to 95°C and dissolve it in 900g of water, then cool down to 45°C and add all proportion of n-butyraldehyde. Continue to cool down the liquid to the reaction temperature of 20°C, add all proportion of hydrochloric acid, the mass ratio of the reaction material is polyvinyl alcohol: hydrochloric acid = 100:50, the mass concentration of hydrochloric acid is 32%, keep the reaction for 1 hour, and then use the reaction solution for 1 hour Gradually raise the temperature to 35°C, keep it warm for 1 hour, then gradually raise the temperature to 50°C for 1 hour again, keep it warm for 1 hour, then cool down and wash the reaction product 6 times with water, then raise the temperature to 45°C, add an appropriate amount of caustic soda solution to adjust the pH To 9, keep warm for 2 hours, fully neutralize and remove acid, and finally wash 8 times again, and the polyvinyl butyral resin after washing is centrifugally dehydrated and dried to obtain a fin...

Embodiment 2

[0023] Heat 100g of polyvinyl alcohol to 95°C and dissolve it in 900g of water, then cool down to 45°C and add all proportion of n-butyraldehyde. Continue to cool down the liquid to the reaction temperature of 25°C, add all proportion of hydrochloric acid, the mass ratio of the reaction material is polyvinyl alcohol: hydrochloric acid = 100:50, the mass concentration of hydrochloric acid is 32%, keep the reaction for 1 hour, and then use the reaction solution for 1 hour Gradually raise the temperature to 40°C, keep it warm for 1 hour, then gradually raise the temperature to 55°C for 1 hour again, keep it warm for 1 hour, then cool down and wash the reaction product 6 times with water, then raise the temperature to 45°C, add an appropriate amount of caustic soda solution to adjust the pH To 9, keep warm for 2 hours, fully neutralize and remove acid, and finally wash 8 times again, and the polyvinyl butyral resin after washing is centrifugally dehydrated and dried to obtain a fin...

Embodiment 3

[0025] Heat 100g of polyvinyl alcohol to 95°C and dissolve it in 900g of water, then cool down to 45°C and add all proportion of n-butyraldehyde. Continue to cool down the liquid to the reaction temperature of 20°C, add all proportion of hydrochloric acid, the mass ratio of the reaction material is polyvinyl alcohol: hydrochloric acid = 100:50, the mass concentration of hydrochloric acid is 32%, keep the reaction for 1 hour, and then use the reaction solution for 1 hour Gradually raise the temperature to 35°C, keep it warm for 1 hour, then gradually raise the temperature to 50°C for 1 hour again, keep it warm for 1 hour, then cool down and wash the reaction product 6 times with water, then raise the temperature to 45°C, add a small amount of caustic soda solution to adjust the pH To 9, keep warm for 2 hours, fully neutralize and remove acid, and finally wash 8 times again, and the polyvinyl butyral resin after washing is centrifugally dehydrated and dried to obtain a finished p...

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Abstract

The invention provides a preparation method of a high-acetalization-degree high-flowability polyvinyl butyral resin, which comprises the following steps: a. condensation reaction: heating polyvinyl alcohol to 95 DEG C, dissolving in water to prepare a 10% solution, cooling the solution to 40-60 DEG C, adding n-butyl aldehyde to carry out reaction, cooling to 20-25 DEG C, adding a catalyst hydrochloric acid to react for 1 hour, sending the mixed reaction solution to a condensation kettle, gradually heating to 35-40 DEG C within 1 hour, keeping the temperature to react for 1 hour, gradually heating to 50-55 DEG C within 1 hour, keeping the temperature to react for 1 hour, and cooling; b. neutralizing treatment: sending the cooled reaction solution to a water washing kettle to carry out water washing 5-6 times, heating to 40-50 DEG C, adding a right amount of caustic soda solution to regulate the pH value to 8-10, and keeping the temperature for 2-3 hours for sufficient neutralization and acid removal; and c. dehydration and drying: washing the reaction solution subjected to neutralization and acid removal with water 6-8 times, and dehydrating and drying with a centrifugal machine to obtain the polyvinyl butyral resin finished product. The polyvinyl butyral resin prepared by the method provided by the invention has the advantages of high acetalization degree and favorable flowability.

Description

technical field [0001] The invention belongs to the technical field of heat-shrinkable polymer materials, in particular to a preparation method of polyvinyl butyral resin with high acetalization degree and high fluidity. Background technique [0002] Polyvinyl butyral resin has superior properties in transparency, film-forming properties, cold resistance, impact resistance, UV resistance, and adhesion to glass, ceramics, etc. Polyvinyl butyral is an essential material for preparing laminated safety glass. With the development of the automobile industry, construction industry and photovoltaic industry, the amount of laminated safety glass is increasing. The demand for polyvinyl butyral resin in the Chinese market is The demand is increasing, but there is no domestic manufacturer that can supply it. Most of them rely on imports, and are mainly monopolized by the three major companies of Monsanto, Dupont and Sekisui in Japan. Therefore, the synthesis of polyvinyl butyral resin ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F16/06C08F8/28C08F16/38C08F6/12C08L29/14
Inventor 范乔乔陈庚叶卫民胡建清
Owner ZHEJIANG DECENT PLASTIC
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