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Synthesis method of polyvinyl butyral resin

A technology of polyvinyl butyral resin and synthesis method, which is applied in the field of polymer materials, can solve problems such as uneven precipitation of resin, uneven degree of acetalization, and difficulty in post-processing, so as to improve reaction conversion rate and operability Strong, easy to industrialize the effect of production

Active Publication Date: 2020-08-07
HENAN ACADEMY OF SCI CHEM RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the problems existing in the prior art, the purpose of the present invention is to provide an improved synthesis method of polyvinyl butyral resin, aiming at solving the unevenness of resin in the early stage of reaction Precipitation leads to problems such as low conversion rate, uneven degree of acetalization and post-processing difficulties, which better meet the needs of industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028](1) Add 1,000 parts of deionized water and 90 parts of PVA1799 polyvinyl alcohol into a reactor equipped with electric stirring, temperature control and reflux condensing device, stir and heat up to 90°C until the polyvinyl alcohol is completely dissolved to form a uniform solution ;

[0029] (2) Adjust the temperature of the reaction system to 40°C, add 0.5 parts of emulsifier sodium dodecylsulfonate, and stir until a uniform solution is formed;

[0030] (3) Keep the temperature of the reaction system at 40°C, add 55 parts of n-butyraldehyde and 12 parts of oxalic acid mixture, and keep the temperature at 40°C for 3 hours;

[0031] (4) Keep the temperature of the reaction system at 40°C, add 6 parts of 30% hydrochloric acid by mass percent, gradually increase the temperature of the reaction system to 70°C within 0.5 hours, and keep the temperature at 70°C for 4 hours;

[0032] (5) Regulating the temperature of the reaction system to 30° C., adding a mass percent concen...

Embodiment 2

[0035] (1) Add 1,000 parts of deionized water and 100 parts of PVA1799 polyvinyl alcohol into a reactor equipped with electric stirring, temperature control and reflux condensing device, stir and heat up to 95°C until the polyvinyl alcohol is completely dissolved to form a uniform solution ;

[0036] (2) Adjust the temperature of the reaction system to 30°C, add 1.5 parts of emulsifier sodium lauryl sulfate, and stir until a uniform solution is formed;

[0037] (3) Keep the reaction system temperature at 30°C, add 65 parts of n-butyraldehyde and 6 parts of formic acid mixture, keep the temperature at 40°C for 3 hours;

[0038] (4) Keep the temperature of the reaction system at 30°C, add 15 parts by mass of 30% hydrochloric acid, gradually increase the temperature of the reaction system to 65°C within 0.5 hours, and keep the temperature at 65°C for 3 hours;

[0039] (5) Regulating the temperature of the reaction system to 30° C., adding a mass percent concentration of 3% potas...

Embodiment 3

[0042] (1) Add 1,000 parts of deionized water and 110 parts of PVA1799 polyvinyl alcohol into a reactor equipped with electric stirring, temperature control and reflux condensing device, stir and heat up to 90°C until the polyvinyl alcohol is completely dissolved to form a uniform solution ;

[0043] (2) Adjust the temperature of the reaction system to 40°C, add 0.5 parts of emulsifier sodium dodecylbenzenesulfonate, and stir until a uniform solution is formed;

[0044] (3) Keep the temperature of the reaction system at 40°C, add 80 parts of n-butyraldehyde and 15 parts of maleic acid mixture, and keep the temperature at 40°C for 3 hours;

[0045] (4) Keep the temperature of the reaction system at 40°C, add 8 parts of 30% sulfuric acid by mass percentage, gradually increase the temperature of the reaction system to 70°C within 0.5 hours, and keep the temperature at 70°C for 3 hours;

[0046] (5) Regulating the temperature of the reaction system to 30° C., adding a mass percen...

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Abstract

The invention discloses a synthesis method of polyvinyl butyral resin, and belongs to the field of high polymer material preparation. The method comprises the following steps: dissolving polyvinyl alcohol in deionized water, adding an emulsifier, adding n-butyraldehyde to react with an organic acid, then adding an inorganic acid, carrying out a heating reaction, performing neutralizing with an alkaline solution, adjusting the pH value of the reaction solution to 7-9, carrying out solid-liquid separation, treating the solid resin with a stabilizer solution, washing, filtering, and performing drying to obtain the polyvinyl butyral resin. The condensation reaction of polyvinyl alcohol and n-butyraldehyde is catalyzed step by step by adopting organic acid and inorganic acid; the early condensation reaction speed is effectively controlled, resin can be stably separated out from a water phase, the main chain acetal uniformity is improved, inorganic acid is adopted for catalysis in the middleand later periods of the reaction, the condensation reaction speed can be increased, the conversion rate of n-butyraldehyde is increased, and the acetal degree of the resin is improved. The synthesismethod is simple, high in operability and easy for industrial production. The resin can be used in the fields of safety glass, coatings, adhesives and the like.

Description

technical field [0001] The invention relates to the field of macromolecule materials, more specifically, to a synthesis method of polyvinyl butyral resin. Background technique [0002] Polyvinyl butyral (PVB) is one of the most important categories of polyvinyl acetal products. It is a condensation product obtained by reacting polyvinyl alcohol (PVA) and n-butyraldehyde under the action of an acidic catalyst. Usually white to slightly yellow powdery solid, insoluble in water, soluble in alcohols, ketones, esters and aromatic hydrocarbon solvents. PVB resin has excellent transparency, aging resistance, water resistance and impact resistance, and has good adhesion to different substrates such as metal, glass, wood, ceramics and fabrics. Therefore, it is used in safety glass, photovoltaic materials, It has been widely used in many industries such as coatings, adhesives, ceramic film decals and engineering plastics. [0003] The industrial production methods of polyvinyl butyr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F16/06C08F8/28
CPCC08F8/28C08F16/06
Inventor 周文欣胡志刚张卫红王建余立明侯静魏红宇
Owner HENAN ACADEMY OF SCI CHEM RES INST CO LTD
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