阅读说明：本技术 一种制备聚乙烯醇缩丁醛用的磺化炭催化剂及其应用 (Sulfonated carbon catalyst for preparing polyvinyl butyral and application thereof ) 是由 王钧伟 石旵东 张元广 吴秀银 崔晓峰 郑学根 杨森 于 2020-11-30 设计创作，主要内容包括：本发明公开了一种制备聚乙烯醇缩丁醛用的磺化炭催化剂及其应用,涉及高分子化工技术领域,所述催化剂的制备方法具体为：将活性炭颗粒在110℃下干燥2小时,然后在130℃-180℃条件下浸泡于浓硫酸中进行磺化,磺化9-14h后洗涤至中性,干燥后即得磺化活性炭催化剂。采用磺化活性炭为催化剂,与传统使用液体酸催化剂相比,克服了传统液体酸对设备的腐蚀问题,并且生产条件温和可靠,稳定安全,大量降低了废水的产生,降低了对环境的污染。(The invention discloses a sulfonated carbon catalyst for preparing polyvinyl butyral and an application thereof, relating to the technical field of polymer chemical industry, wherein the preparation method of the catalyst comprises the following steps: drying the activated carbon particles at 110 ℃ for 2 hours, then soaking the activated carbon particles in concentrated sulfuric acid at 130-180 ℃ for sulfonation, washing the sulfonated activated carbon particles to be neutral after 9-14 hours of sulfonation, and drying the sulfonated activated carbon particles to obtain the sulfonated activated carbon catalyst. Compared with the traditional liquid acid catalyst, the sulfonated activated carbon catalyst has the advantages of overcoming the corrosion problem of the traditional liquid acid to equipment, along with mild and reliable production conditions, stability, safety, great reduction in the generation of waste water and reduction in the pollution to the environment.)

1. The sulfonated carbon catalyst for preparing the polyvinyl butyral is characterized by being prepared by the following method: drying the activated carbon particles at 110 ℃ for 2 hours, then soaking the activated carbon particles in concentrated sulfuric acid at 130-180 ℃ for sulfonation, washing the sulfonated activated carbon particles to be neutral after 9-14 hours of sulfonation, and drying the sulfonated activated carbon particles to obtain the sulfonated activated carbon catalyst.

2. A method for preparing polyvinyl butyral by using the catalyst of claim 1, wherein the method comprises the steps of adding polyvinyl alcohol and n-butyraldehyde into a mixed solvent of water and ethanol, then adding a sulfonated activated carbon catalyst, adding water after the reaction is finished, and separating out a target product.

Technical Field

The invention relates to the technical field of polymer chemical industry, in particular to a catalyst for preparing polyvinyl butyral and application thereof.

Background

Polyvinyl Butyral (PVB) is a condensation product obtained by reacting butyraldehyde with Polyvinyl alcohol (PVA) under the catalysis of a strong acid. PVB molecules contain longer branched chains, have good flexibility, excellent transparency, extremely strong adhesive force, good light resistance, heat resistance, cold resistance, water resistance, film forming property, solubility, miscibility, high tensile strength, impact resistance and the like, and are widely applied to the fields of safety glass interlayers, photovoltaic module packaging films, vacuum aluminized paper, paint ceramic stained paper, aluminum foil paper, adhesives and the like. With the rapid development of industries such as automobiles, buildings and the like, the demand for high-quality PVB resin is more vigorous, and the demand volume is exponentially increased.

Besides being related to the purity and polymerization degree of raw materials, the quality of PVB resin is mainly influenced by a production process and a post-treatment process, wherein the most important problems are that the local rate of an acetal reaction is too high, PVB is separated out in a compact block mass, impurities such as raw materials, catalysts and solvents are easy to be entrained, and uneven intermolecular crosslinking reaction causes the quality of a PVB product to be reduced. In addition, the PVB production in China mostly adopts a two-step precipitation method of inorganic acid catalysis. Although the method uses water as a solvent, the production cost is low, the inorganic acid seriously corrodes equipment, so the equipment investment is high, the post-treatment needs to be carried out by the working procedures of neutralization, water washing and the like, the catalyst and salt substances generated by the catalyst are removed, the operation is complicated, a large amount of time and water resources are consumed, and a large amount of waste water is generated and needs to be treated.

Disclosure of Invention

The invention aims to overcome the defects of the prior art, and provides a sulfonated carbon catalyst for preparing polyvinyl butyral and application thereof, so as to solve the technical problem that a hydrochloric acid catalyst corrodes equipment and the like in the prior art.

The invention is realized by the following technical scheme:

the invention provides a sulfonated carbon catalyst for preparing polyvinyl butyral, which is prepared by the following method: drying the activated carbon particles at 110 ℃ for 2 hours, then soaking the activated carbon particles in concentrated sulfuric acid at 130-180 ℃ for sulfonation, washing the sulfonated activated carbon particles to be neutral after 9-14 hours of sulfonation, and drying the sulfonated activated carbon particles to obtain the sulfonated activated carbon catalyst.

The invention also provides a method for preparing polyvinyl butyral by using the catalyst, which is characterized by comprising the steps of adding polyvinyl alcohol and n-butyraldehyde into a mixed solvent of water and ethanol, then adding a sulfonated activated carbon catalyst, adding water after the reaction is finished, and separating out and separating a target product.

Compared with the prior art, the invention has the following advantages: the invention provides a sulfonated carbon catalyst for preparing polyvinyl butyral and application thereof, wherein sulfonated active carbon is selected as the catalyst, compared with the traditional liquid acid catalyst, the product is generated by a one-step method, the product is easier to separate and purify after reaction, the process flow is simplified, the industrial cost is reduced, meanwhile, the sulfonated carbon is used as the catalyst, the corrosion problem of the traditional liquid acid to equipment is solved, the production condition is mild and reliable, the sulfonated carbon catalyst is stable and safe, the generation of waste water is greatly reduced, and the pollution to the environment is reduced.

Detailed Description

The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

Drying the activated carbon particles at 110 ℃ for 2 hours, then soaking the activated carbon particles in concentrated sulfuric acid at 150 ℃ for sulfonation for 12 hours, then taking out the activated carbon particles, washing the activated carbon particles to be neutral, and drying the activated carbon particles to obtain the sulfonated carbon catalyst. Dissolving 4g of PVA in a mixed solvent of ethanol and water (V ethanol: V water: 1.25: 1), adding 2.8g of n-butyraldehyde, then adding 0.2g of the prepared sulfonated activated carbon catalyst to carry out synthetic reaction of polyvinyl butyral, and continuously stirring and reacting at the reaction temperature of 70 ℃ for 12 hours, wherein the acetal degree of the obtained product polyvinyl butyral reaches 80%.

Example 2

Drying the activated carbon particles at 110 ℃ for 2 hours, then soaking the activated carbon particles in concentrated sulfuric acid at 140 ℃ for sulfonation for 10 hours, then taking out the activated carbon particles, washing the activated carbon particles to be neutral, and drying the activated carbon particles to obtain the sulfonated carbon catalyst. Dissolving 4g of PVA in a mixed solvent of ethanol and water (V ethanol: V water: 1.25: 1), adding 2.4g of n-butyraldehyde, then adding 0.2g of the prepared sulfonated activated carbon catalyst to carry out synthetic reaction of polyvinyl butyral, and continuously stirring and reacting at the reaction temperature of 80 ℃ for 10 hours to obtain the product polyvinyl butyral with the acetalization degree of 76%.

Example 3

Drying the activated carbon particles at 110 ℃ for 2 hours, then soaking the activated carbon particles in concentrated sulfuric acid at 150 ℃ for sulfonation for 10 hours, then taking out the activated carbon particles, washing the activated carbon particles to be neutral, and drying the activated carbon particles to obtain the sulfonated carbon catalyst. Dissolving 4g of PVA in a mixed solvent of ethanol and water (V ethanol: V water: 1.1: 1), adding 2.4g of n-butyraldehyde, then adding 0.2g of the prepared sulfonated activated carbon catalyst to carry out synthetic reaction of polyvinyl butyral, and continuously stirring and reacting at the reaction temperature of 70 ℃ for 12 hours, wherein the acetal degree of the obtained product polyvinyl butyral reaches 78%.

Example 4

Drying the activated carbon particles at 110 ℃ for 2 hours, then soaking the activated carbon particles in concentrated sulfuric acid at 150 ℃ for sulfonation for 12 hours, then taking out the activated carbon particles, washing the activated carbon particles to be neutral, and drying the activated carbon particles to obtain the sulfonated carbon catalyst. Dissolving 4g of PVA in a mixed solvent of ethanol and water (V ethanol: V water: 1.1: 1), adding 2.8g of n-butyraldehyde, then adding 0.25g of the prepared sulfonated activated carbon catalyst to carry out synthetic reaction of polyvinyl butyral, and continuously stirring and reacting at 75 ℃ for 12 hours to obtain the product polyvinyl butyral with the acetalization degree of 81%.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.