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Preparation method of polyvinyl butyral

A polyvinyl butyral and polyvinyl alcohol technology, which is applied in the field of preparation of polyvinyl butyral (PVB), can solve the problems of cross-linking reaction products, uneven distribution of acetal groups, affecting product quality and the like

Inactive Publication Date: 2014-09-17
四川宝利丰科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem with this method is that the distribution of acetal groups is uneven, and it is prone to cross-linking reactions between molecules and product agglomeration, etc., which affects the quality of the product.

Method used

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  • Preparation method of polyvinyl butyral
  • Preparation method of polyvinyl butyral
  • Preparation method of polyvinyl butyral

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 100 parts of PVA (unless otherwise specified, the parts used for each material are parts by weight) and 900 parts of deionized water into a three-necked flask equipped with a stirrer, reflux condenser and thermostat, raise the temperature to 92°C and stir until All the PVA was dissolved, and after cooling to 62°C, 60 parts of butyraldehyde was added and stirred thoroughly to obtain a uniformly mixed PVA-butyraldehyde mixed solution. Add a small amount of dilute hydrochloric acid with a pH value of 1 to a four-necked flask equipped with a stirrer, reflux condenser and constant temperature instrument, keep the temperature at 25°C, and then use a constant pressure dropping funnel to the four-necked flask at a substantially uniform speed at the same time Slowly add a mixed solution of dilute hydrochloric acid and PVA-butyraldehyde with a concentration of 15% dropwise, so that the two mixed liquids are added dropwise at the same time within about 1 hour, and continue to r...

Embodiment 2

[0024] Add 100 parts of PVA and 800 parts of deionized water into a three-necked flask equipped with a stirrer, reflux condenser and a thermostat, raise the temperature to 94°C and stir until the PVA is completely dissolved. After cooling to 64°C, add 62 parts of butyraldehyde through Thoroughly stir to obtain a uniformly mixed PVA-butyraldehyde mixed solution. Add a small amount of dilute hydrochloric acid with a pH value of 2 to a four-necked flask equipped with a stirrer, a reflux condenser and a constant temperature instrument, keep the temperature at 27°C, and then use a constant pressure dropping funnel to the four-necked flask at a substantially uniform speed at the same time Slowly add a mixed solution of dilute hydrochloric acid and PVA-butyraldehyde with a concentration of 12% dropwise, so that the two mixed liquids are added dropwise at the same time within about 1 hour, and continue to react under stirring until the degree of acetalization basically does not change ...

Embodiment 3

[0026] Add 100 parts of PVA and 1000 parts of deionized water into a three-necked flask equipped with a stirrer, reflux condenser and thermostat, raise the temperature to 92°C and stir until the PVA is completely dissolved. After cooling to 62°C, add 63 parts of butyraldehyde through Thoroughly stir to obtain a uniformly mixed PVA-butyraldehyde mixed solution. Add a small amount of dilute hydrochloric acid with a pH value of 0.72 to a four-necked flask equipped with a stirrer, reflux condenser and constant temperature instrument, keep the temperature at 20°C, and then use a constant pressure dropping funnel to the four-necked flask at a substantially uniform speed at the same time Slowly add a mixed solution of dilute hydrochloric acid and PVA-butyraldehyde with a concentration of 7% dropwise, so that the two mixed liquids are added dropwise at the same time within about 1 hour, and continue to react under stirring until the degree of acetalization basically does not change (a...

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Abstract

The invention provides a preparation method of polyvinyl butyral (PVB). The preparation method comprises the following steps: mixing the aqueous solution of polyvinyl alcohol having the mass fraction content of 7-12.5% with butyraldehyde 0.4-0.8 times the weight of the polyvinyl alcohol to obtain a polyvinyl alcohol-butyraldehyde mixed solution; under the conditions of less than or equal to 35 DEG C and a system pH value kept in the range of 0.1 to 4, simultaneously adding the polyvinyl alcohol-butyraldehyde mixed solution and an acidic aqueous solution, in such a manner of keeping the solutions in disperse state, to a reaction container, mixing and carrying out a low-temperature polymerization reaction of the first step; next, increasing the reaction system to the range of 45-75 DEG C at a rate of less than or equal to 0.5 DEG C per minute, further carrying out a high-temperature polymerization reaction of the second step until the reaction terminates, and adding an alkali aqueous solution so that the pH value of the reaction system is greater than 7, and carrying out solid-liquid separation, thereby obtaining the polyvinyl butyral product. The PVB obtained by the method is high in degree of acetalization and high in butyraldehyde utilization rate; the obtained PVB is in the form of a fine powder of even particles; the reactions are easy to operate and control; the repeatability is high; besides, the after-treatment is simple; the preparation method has great significance for cost saving and environmental protection, and is especially suitable for continuous industrial production.

Description

technical field [0001] The present invention relates to a preparation method of polyvinyl butyral (PVB), in particular to a fine powder PVB product with uniform particle size and high acetalization degree obtained by self-dispersion and gradual polymerization of polyvinyl alcohol and butyral Methods. Background technique [0002] Polyvinyl butyral (PVB) resin has been widely used as the main material of safety glass interlayer because of its excellent bonding performance and optical properties. [0003] For the preparation of PVB materials, the one-step method represented by U.S. Monsanto Company that has been reported / used at present is to form polyvinyl acetate by polymerization of vinyl acetate, and add an acidic catalyst in the obtained methanol solution to carry out alcoholysis to obtain polyvinyl acetate. Vinyl alcohol (PVA), then suspend it in a mixed solvent of ethyl acetate and ethanol, add hydrochloric acid and butyraldehyde for acetalization reaction, and contin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F16/06C08F8/28
Inventor 李晶晶刘明杨琴罗芩
Owner 四川宝利丰科技有限公司
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