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A kind of polyvinyl butyral synthesis process based on microdispersion technology

A polyvinyl butyral synthesis process technology, applied in the field of polyvinyl butyral synthesis process, can solve problems such as difficult precise control, affecting product quality, strong randomness of reaction, etc., to achieve enhanced dissolution and reaction, and guaranteed Batch stability, guaranteed high acetalization effect

Active Publication Date: 2018-02-16
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction between the solid-liquid phase proceeds very slowly, and it takes a long time to reach the reaction limit. In this process, the reaction is highly random and difficult to accurately control. The batch stability of the reaction cannot be guaranteed, which seriously affects the product. quality

Method used

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  • A kind of polyvinyl butyral synthesis process based on microdispersion technology

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Process device: use a stirred tank as the mixer 1, use a membrane dispersion device filled with a 5μm metal sintered film as a microdisperser 2, use a single-row tubular tubular reactor 3 with a temperature control jacket, and use a heat exchange clamp The set of stirred tank is used as collection tank 4.

[0037] Reaction conditions: the mass fraction of PVA in the PVA aqueous solution A is 10%; the mass fraction of HCl in the HCl aqueous solution B is 31%, and the mass ratio of HCl to PVA in the mixed material liquid C is 0.08:1; The mass ratio of butyraldehyde D to PVA is 0.70:1. The mixing temperature of the mixer 1 is 25°C; the operating temperature of the microdisperser 2 is 50°C, and the material residence time is 7s; the reaction temperature of the tubular reactor 3 is 50°C, and the reaction time is 2min; the collection temperature of the collector 4 The temperature was 55°C and the collection time was 6.0h.

[0038] Reaction result: The acetal degree of the produc...

Embodiment 2

[0040] Reaction device: use a microchannel mixer as the mixer 1, use a micro-mesh dispersing device with a diameter of 500 μm as a microdisperser 2, use a single-row tubular tubular reactor 3 with a temperature control jacket, and use a heat exchanger The jacketed stirred tank is used as the collecting tank 4.

[0041] Reaction conditions: the mass fraction of PVA in the PVA aqueous solution A is 8%; the mass fraction of HCl in the HCl aqueous solution B is 36%, and the mass ratio of HCl to PVA in the mixed material liquid C is 0.25:1; added to the mixed material liquid C The mass ratio of n-butyraldehyde D to PVA is 0.63:1. The mixing temperature of the mixer 1 is 20°C; the operating temperature of the microdisperser 2 is 30°C, and the material residence time is 20s; the reaction temperature of the tubular reactor 3 is 75°C, and the reaction time is 5 minutes; the collection temperature of the collector 4 The temperature is 75°C and the collection time is 3.5h.

[0042] Reaction...

Embodiment 3

[0044] Reaction device: a static mixer is used as the mixer 1, a membrane dispersion device filled with a 20μm metal sintered film is used as a microdisperser 2, a single-row tubular tubular reactor 3 with a temperature control jacket is used, and a heat exchange is used The jacketed stirred tank is used as the collecting tank 4.

[0045] Reaction conditions: the mass fraction of PVA in the PVA aqueous solution A is 12%; the mass fraction of HCl in the HCl aqueous solution B is 30%, and the mass ratio of HCl to PVA in the mixed material liquid C is 0.10:1; added to the mixed material liquid C The mass ratio of n-butyraldehyde D to PVA is 0.60:1. The mixing temperature of the mixer 1 is 23°C; the operating temperature of the microdisperser is 42°C, and the material residence time is 10s; the reaction temperature of the tubular reactor 3 is 50°C, and the reaction time is 30min; the collection temperature of the collecting tank 4 is The collection time is 9.0h at 50°C.

[0046] Reac...

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Abstract

The invention relates to a polyvinyl butyral (PVB) synthesis process based on microdispersion technology. A process device includes a mixer, a microdisperser, a tubular reactor and a collection kettle that are connected in series in order. The process includes: firstly mixing a PVA aqueous solution with an HCl aqueous solution evenly by the mixer, then dispersing n-butyraldehyde into the mixed solution in the form of droplets in the microdisperser, quickly completing the vast majority of hemiacetal reaction and part of acetal reaction before PVB precipitate formation, then completing the vast majority of acetal reaction in the tubular reactor, and finally completing acetal reaction through the collection kettle and collecting the product. The process provided by the invention utilizes the microdisperser to realize rapid and even dispersion of butyraldehyde liquid drops in the mixed solution, reinforces the dissolution and reaction of n-butyraldehyde, and utilizes the tubular reactor to realize effective control of product acetalization degree, thereby ensuring product high acetalization degree, homogeneity and product batch stability. The catalyst concentrated hydrochloric acid is uniformly mixed at the early stage, and the water consumption of the whole process is reduced.

Description

Technical field [0001] The invention belongs to the technical field of resin synthesis, and particularly relates to a polyvinyl butyral synthesis process based on micro-dispersion technology. Background technique [0002] Polyvinyl butyral (PVB) is a condensation product of polyvinyl alcohol (PVA) and n-butyraldehyde under acid catalysis. At present, almost all high-end cars use PVB laminated glass as the front windshield. The demand for PVB coatings and adhesives in the construction market is also increasing at a rate of more than 20% per year. Although the application range of PVB membranes is very narrow, due to its special effects, PVB membranes are still widely used internationally as interlayer films for laminated glass. In addition, PVB is also needed as an intermediate consumable for the adhesive in the production process of solar cell photovoltaic panels and LED substrates, and the requirements for PVB quality are higher. The higher the quality of PVB, the higher the p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F16/06C08F8/28
CPCC08F8/28C08F16/06
Inventor 骆广生王凯林茜妍
Owner TSINGHUA UNIV
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