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A kind of method utilizing micro reaction system to synthesize polyvinyl butyral

A technology of polyvinyl butyral and polyvinyl alcohol, applied in chemical instruments and methods, chemical/physical/physicochemical processes, chemical/physical processes, etc., can solve problems affecting product quality, low mixing performance, and reaction energy consumption Advanced problems, to achieve the effect of improving batch stability, reducing process energy consumption, and achieving effective control

Active Publication Date: 2016-11-02
TSINGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to overcome the problem of low mixing performance in traditional stirred reactors, an initial reaction temperature of 5-15°C is generally used to reduce the reaction rate. Since the dissolution temperature of PVA reaches 90°C, such a low reaction temperature results in high energy consumption for the reaction.
More importantly, many studies have shown that the result of low temperature reaction is that the degree of acetalization of PVB increases slowly. When the degree of acetalization reaches 20% to 30%, the hydrophobic PVB molecules are precipitated in the form of precipitation, and the solid-phase PVB after precipitation Continue to react with butyraldehyde in the solution to form a PVB product with a high degree of acetalization under the condition of rising temperature, but because the solid-liquid two-phase reaction process in the conventional stirred reactor is difficult to accurately control, the batch stability of the reaction is not good, serious affect product quality

Method used

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  • A kind of method utilizing micro reaction system to synthesize polyvinyl butyral
  • A kind of method utilizing micro reaction system to synthesize polyvinyl butyral
  • A kind of method utilizing micro reaction system to synthesize polyvinyl butyral

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Reaction device: There is a microstructure distribution plate with a diameter of 0.04mm mesh inside the microreactor.

[0042] Reaction conditions: the mass fraction of polyvinyl alcohol in raw material A is 12%, the mass ratio of n-butyraldehyde and polyvinyl alcohol is 0.65:1, the solvent of raw material A is water; The mass fraction of HCl is 10% in raw material B, reaction The mass ratio of HCl and polyvinyl alcohol in raw material A is controlled to be 0.08:1; the reaction temperature of the hemiacetal reaction is 50°C, and the time is 0.53s; the reaction temperature of the acetal reaction is 75°C, and the time is 0.5h.

[0043] Reaction result: the degree of acetalization of the product polyvinyl butyral is 74.4%, the hydroxyl value is 21.8%, and the viscosity of the PVB ethanol solution is 70 mPa·s.

[0044] The microstructure distribution plate in the above-mentioned microreactor is located between the inlets of the two raw materials, and is used to separate the t...

Embodiment 2

[0046] Reaction device: There is a microstructure distribution plate with a diameter of 0.04mm mesh inside the microreactor.

[0047] Reaction conditions: the mass fraction of polyvinyl alcohol in raw material A is 8.5%, the mass ratio of n-butyraldehyde and polyvinyl alcohol is 1:1, the solvent of raw material A is water; The mass fraction of HCl in raw material B is 10%, and the reaction The mass ratio of HCl and polyvinyl alcohol in raw material A is controlled to be 0.12:1; the reaction temperature of the hemiacetal reaction is 30°C, and the time is 2.8s; the reaction temperature of the acetal reaction is 45°C, and the time is 1.5h.

[0048] Reaction result: the degree of acetalization of the product polyvinyl butyral is 78.0%, the hydroxyl value is 18.4%, and the viscosity of the PVB ethanol solution is 105 mPa·s.

Embodiment 3

[0050] Reaction device: There is a microstructure distribution plate with a length of 2mm and a width of 0.03mm inside the microreactor.

[0051] Reaction conditions: the mass fraction of polyvinyl alcohol in raw material A is 3%, the mass ratio of n-butyraldehyde and polyvinyl alcohol is 1.3:1, the solvent of raw material A is water; The mass fraction of HCl in raw material B is 20%, reaction The mass ratio of HCl and polyvinyl alcohol in raw material A is controlled to be 0.05:1; the reaction temperature of the hemiacetal reaction is 55°C, and the time is 1.2s; the reaction temperature of the acetal reaction is 40°C, and the time is 2h.

[0052] Reaction result: the degree of acetalization of the product polyvinyl butyral is 77.5%, the hydroxyl value is 19.3%, and the viscosity of the PVB ethanol solution is 96 mPa·s.

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Abstract

The invention relates to a method for synthesizing polyvinyl butyral by using a micro reaction system. The micro reaction system consists of a micro reactor, a tubular reactor and a collecting kettle which are connected in sequence, wherein a micro structure distribution plate or micro channels are arranged inside the micro reactor; screening holes or through holes are formed in the micro structure distribution plate. The method comprises the following steps: adding a raw material A and a raw material B into the micro reactor to react so as to generate a reaction liquid C, feeding the reaction liquid C into the tubular reactor for aldolization so as to generate suspension D of polyvinyl butyral, and feeding the suspension D into the collecting kettle, wherein the raw material A is a mixed solution of polyving alcohol and n-butanal, and the raw material B is a HCl solution. Most hemiacetal reaction can be completed before PVB is deposited by virtue of the characteristic that reaction can be enhanced by using the micro reactor, so that the consistency of the acetal degree of a product and the batch stability of the product can be ensured, and the product quality can be improved.

Description

technical field [0001] The invention belongs to the technical field of resin synthesis, in particular to a method for synthesizing polyvinyl butyral by using a micro reaction system. Background technique [0002] Polyvinyl butyral (PVB) is a high molecular polymer, because of its good flexibility, solubility, light resistance, water resistance, heat resistance, film-forming properties, high tensile strength and impact strength, The glass transition temperature is low and the refractive index is similar to that of glass. It was synthesized by American scientists in 1935 and used as an adhesive layer for automobile windshields. In addition to this, it is also used as a sealing material for architectural coatings, bulletproof glass, and photovoltaic panels for solar cells. Among all its downstream uses, laminated glass accounted for 85% of the total. In 2012, the total global consumption of PVB was 270,000 tons. With the rapid development of the automobile industry, construc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/00C08F16/06C08F8/28C08F2/01
Inventor 骆广生唐安斌王凯徐康林林茜妍陈小强
Owner TSINGHUA UNIV