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CN-122011246-A - Polyvinyl butyral resin and preparation method and application thereof

CN122011246ACN 122011246 ACN122011246 ACN 122011246ACN-122011246-A

Abstract

The invention provides a polyvinyl butyral resin, a preparation method and application thereof, wherein the preparation method comprises the following steps: reacting polyvinyl alcohol solution with butyraldehyde, crushing and curing to obtain polyvinyl butyral resin. In the invention, after the reaction of polyvinyl alcohol and butyraldehyde is finished, PVB resin is in a wet state, the PVB resin is conveyed to a high-speed cutting type superfine wet pulverizer, and agglomerated loose resin particles generated by the reaction are scattered and pulverized through high-speed shearing and cutting actions, so that the agglomeration of PVB resin is reduced, the particle size distribution of PVB resin particles is narrowed, the uniformity is good, the dispersion time is short, the local overheating and molecular chain degradation possibly caused by dry pulverization are avoided, and the inherent performance of PVB resin is better maintained. The preparation method of the invention realizes the whole process continuous production from reaction, crushing to aging, greatly improves the efficiency, has low energy consumption and can effectively eliminate dust.

Inventors

  • ZHU FUHAI
  • GU XIAO
  • ZHU XIONGBING
  • YUAN HAIFENG

Assignees

  • 亿光年高分子材料(江苏)有限公司

Dates

Publication Date
20260512
Application Date
20251120

Claims (10)

  1. 1. A method for preparing a polyvinyl butyral resin, comprising the steps of: reacting polyvinyl alcohol solution with butyraldehyde, crushing and curing to obtain polyvinyl butyral resin.
  2. 2. The method of claim 1, wherein the comminuting is carried out under shear; preferably, the shear rate is 10-50 m/s; Preferably, the shearing pressure is 0.2-1.5 MPa; Preferably, the shearing time is 0.1-10 s; preferably, the pulverizing adopts a high-speed cutting type superfine wet pulverizer.
  3. 3. The method according to claim 1 or 2, wherein the polyvinyl alcohol solution is obtained by immersing polyvinyl alcohol in water; preferably, the soaking comprises normal temperature soaking and high temperature soaking; preferably, the normal temperature soaking time is 1-3 h; preferably, the high temperature soaking temperature is 80-100 ℃; Preferably, the high temperature soaking time is 2-4 h; Preferably, the mass fraction of the polyvinyl alcohol solution is 10-18%.
  4. 4. A method of preparation according to any one of claims 1 to 3, wherein the temperature of the reaction is 40 to 70 ℃; preferably, the reaction time is 3-6 h.
  5. 5. The method of any one of claims 1-4, wherein the method of reacting comprises adding butyraldehyde to a polyvinyl alcohol solution; Preferably, the mass ratio of the polyvinyl alcohol to the butyraldehyde is 1 (0.3-0.6); Preferably, the butyraldehyde is added in two portions; preferably, the reaction is carried out under the action of a catalyst; Preferably, the catalyst comprises an acidic catalyst; Preferably, the acidic catalyst comprises any one or a combination of at least two of hydrochloric acid, dilute sulfuric acid, phosphoric acid, hydrobromic acid, hydroiodic acid, chloroacetic acid, sulfamic acid, benzenesulfonic acid, o-toluenesulfonic acid, m-toluenesulfonic acid, ethylbenzenesulfonic acid or m-benzenedisulfonic acid; preferably, the mass ratio of the polyvinyl alcohol to the catalyst is 1 (0.05-0.2).
  6. 6. The method of any one of claims 1-5, wherein the reaction further requires the addition of a surfactant; Preferably, the surfactant comprises any one or a combination of at least two of sodium dodecyl sulfate, sodium laureth sulfate, potassium perfluorooctyl sulfonate, cocamidopropyl betaine, dodecyl dimethyl amine oxide, sodium monolauryl phosphate, oleyl polyoxyethylene ether phosphate, potassium isooctyl phosphate, sodium dodecyl benzene sulfonate or sodium xylene sulfonate; preferably, the mass ratio of the polyvinyl alcohol to the surfactant is 100 (1-5).
  7. 7. The method according to any one of claims 1 to 6, wherein the curing is performed in an aging tank; Preferably, the curing temperature is 30-40 ℃; Preferably, the curing time is 2-3 h; Preferably, the post-curing further comprises a post-treatment step; Preferably, the post-treatment comprises washing and/or drying; preferably, the washing comprises washing with an alkaline solution and washing with water; preferably, the alkaline solution comprises any one or a combination of at least two of sodium hydroxide, ammonia water, sodium carbonate or sodium bicarbonate; preferably, the alkaline solution has a pH of 7-10; Preferably, the number of times of washing with water is 4 to 5 times; Preferably, the drying temperature is 65-75 ℃; preferably, the drying time is 6-8 h; preferably, the polyvinyl butyral resin has a water content of 1% or less.
  8. 8. The preparation method according to any one of claims 1 to 7, characterized in that it comprises in particular the following steps: (1) Soaking polyvinyl alcohol in water for 1-3 h deg.c, heating to 80-100 deg.c and stirring at constant temperature for 2-4 h to obtain polyvinyl alcohol solution; (2) Adding partial butyraldehyde into the polyvinyl alcohol solution, and adding the rest butyraldehyde after phase transition, and then adding a catalyst and a surfactant for reaction at 40-70 ℃ for 3-6 h; (3) Screening and crushing the mixed solution obtained in the step (2) by using a high-speed cutting type superfine wet pulverizer, wherein the shearing speed is 10-50 m/s, the pressure is 0.2-1.5 MPa, and the time is 0.1-10 s; (4) Transferring the PVB resin treated in the step (3) to an aging kettle, curing at 30-40 ℃ for 2-3 h ℃, adding an alkaline solution, centrifuging to obtain a PVB resin filter cake, washing with water for 4-5 times, and drying at 65-75 ℃ for 6-8 h to obtain the polyvinyl butyral resin.
  9. 9. A polyvinyl butyral resin prepared by the preparation method of any one of claims 1 to 8.
  10. 10. Use of the polyvinyl butyral resin according to claim 9 in safety glass, optical films or coatings.

Description

Polyvinyl butyral resin and preparation method and application thereof Technical Field The invention belongs to the technical field of polyvinyl butyral resin, and particularly relates to polyvinyl butyral resin, and a preparation method and application thereof. Background Polyvinyl butyral (PVB) resins are widely used in automotive and architectural laminated glass interlayer films, coatings, adhesives, and other industries because of their excellent adhesion to glass, metal, and other materials, high transparency, good toughness, and film forming properties. The width of the particle size distribution of the PVB resin has important and profound effects on material properties, processing and end-use applications. In conventional PVB resin production processes, the process flow generally includes the preparation of an aqueous solution of polyvinyl alcohol, condensation reaction with butyraldehyde, washing and purification of the formed PVB resin precipitate, and final drying and crushing. Wherein, drying and crushing are key post-treatment procedures for determining the granularity distribution, the processing performance and the application field of the final product. In the traditional PVB resin production process, resin crushing work is generally carried out after drying, the hardness of the dried resin is increased, the surface structure becomes compact, a large amount of time and cost are consumed during crushing to cope with the large material cohesion, stronger impact and friction are caused on equipment correspondingly, the crushing time is long, if the crushing time is insufficient, the particle size distribution of the PVB resin is uneven, the molecular weight distribution is wider, and the application of the PVB resin in the high-end field is influenced. CN107022041a discloses a high viscosity polyvinyl butyral and a method for preparing the same, which regulates the product viscosity by mixing PVA with different degrees of polymerization. However, the process eventually still employs conventional washing, drying post-treatment steps. The dried high-viscosity resin has longer molecular chain and stronger cohesive force, so that the crushing difficulty is further increased, and products with uneven granularity are more easily obtained due to insufficient crushing, thereby affecting the processing uniformity in high-viscosity application scenes. CN115505056a discloses a method for preparing polyvinyl butyral resin for electronic ceramics, which adopts an advanced tubular reactor to improve the uniformity of reaction. Nevertheless, it follows the traditional path of centrifugal drying in post-processing. This patent aims at obtaining a resin suitable for electronic ceramics, which has extremely high requirements on the purity and particle size distribution of the resin, but conventional dry grinding inevitably introduces metal abrasion impurities, and has the problem of wide particle size distribution, which is a potential defect for the electronic ceramic field in which precision reliability is sought. CN108299578A discloses a preparation method of polyvinyl butyral resin with high acetalization degree, which comprises the following steps of S1 preparing raw materials of polyvinyl alcohol, water, n-butyraldehyde, dispersing agent and hydrochloric acid, S2 leaching the polyvinyl alcohol by using desalted water at 15-30 ℃, S3 leaching the polyvinyl alcohol obtained after leaching and filtering in the step S2, S4 mixing the polyvinyl alcohol obtained after leaching with water at 85-100 ℃ to prepare a polyvinyl alcohol solution, S5 cooling the polyvinyl alcohol solution to 40-50 ℃, sequentially adding n-butyraldehyde and dispersing agent, S6 cooling the mixed solution in the step S5 to 8-15 ℃, dropwise adding hydrochloric acid, carrying out heat preservation reaction for 1.5-2.5 h, S7 heating to 37-50 ℃, carrying out heat preservation reaction for 0.7-1.2 h, S8 heating to 65-70 ℃, carrying out heat preservation reaction for 1-1.5 h, cooling the mixed solution to 40-45 ℃, transferring the mixed solution into a water-washing kettle, carrying out water washing with 35-40 ℃ brine, carrying out water-conditioning on the mixed solution to obtain the polyvinyl butyral resin, and washing the polyvinyl butyral resin with water at the pH of which the mixed solution is washed by using sodium hydroxide at 35-40 ℃ to 5310 ℃ to be dried to obtain the polyvinyl butyral resin after washing with water, and washing the polyvinyl butyral resin with water at the pH of the mixed solution after the mixed solution is washed with water at 5-10-5 to be washed with water to be dried to be 5. The patent provides for the preparation of high acetalization degree PVB resins by specific raw material treatments and reaction schemes, which are optimized during the reaction stage, but do not pulverize the wet PVB resin, and still form hard lumps after drying, which makes it difficult to obtain PVB resins with narrower steps in particle