CN112439458A - Catalyst for preparing polyvinyl butyral and application thereof - Google Patents
Catalyst for preparing polyvinyl butyral and application thereof Download PDFInfo
- Publication number
- CN112439458A CN112439458A CN202011372019.0A CN202011372019A CN112439458A CN 112439458 A CN112439458 A CN 112439458A CN 202011372019 A CN202011372019 A CN 202011372019A CN 112439458 A CN112439458 A CN 112439458A
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- CN
- China
- Prior art keywords
- ion exchange
- exchange resin
- acidic ion
- catalyst
- sulfonated
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/08—Ion-exchange resins
- B01J31/10—Ion-exchange resins sulfonated
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/28—Condensation with aldehydes or ketones
Abstract
The invention discloses a catalyst for preparing polyvinyl butyral and application thereof, relating to the technical field of polymer chemical industry, wherein the preparation method of the catalyst specifically comprises the following steps: drying the acidic ion exchange resin at 100-110 ℃ for 2 hours, then soaking the acidic ion exchange resin in concentrated sulfuric acid at 80-120 ℃ for sulfonation for 8-16 hours, and then washing and drying the acidic ion exchange resin to obtain the sulfonated acidic ion exchange resin catalyst. The sulfonated acidic ion exchange resin is used for replacing the traditional liquid inorganic acid catalyst, so that the introduction of impurity ions is avoided, the product quality is improved, and the corrosion of equipment is reduced. The sulfonated ion exchange resin can be recycled, the production cost is reduced, the procedures such as neutralization and the like are omitted, the post-treatment process is simplified, the generation of waste water is reduced, and the sulfonated ion exchange resin is more green and environment-friendly.
Description
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 the reaction of polyvinyl alcohol (PVA) with butyraldehyde under the catalysis of a strong acid. The PVB molecule has the characteristics of long chain length, good flexibility, good transparency, strong adhesive force, light resistance, heat resistance, cold resistance, water resistance, film formation, good solubility, good compatibility and the like. The coating is 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 of high-quality PVB resin is continuously and rapidly increased.
At present, the PVB production in China mostly adopts a two-step precipitation method with inorganic protonic acid as a catalyst, and the catalyst is mainly hydrochloric acid. Although the method takes water as a solvent, the production cost is low, the corrosion of inorganic protonic acid to equipment is serious, the use of a liquid acid catalyst can cause the mixed solution after reaction to be subjected to the processes of neutralization, water washing and the like so as to remove the liquid acid catalyst and miscellaneous substances generated in the reaction process, the process flow is complex, the time is long, and a large amount of wastewater is generated and needs to be treated. In addition, the quality of the PVB resin is related to the purity and polymerization degree of raw materials, and the production process and the post-treatment process are main influencing factors, wherein the most important problems are that the local rate of the acetalization reaction is too high, PVB is separated out in a compact lump, impurities such as raw materials, catalysts and solvents are easy to be entrained, and uneven intermolecular crosslinking reaction causes the quality of the PVB product to be reduced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a 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 catalyst for preparing polyvinyl butyral, which is prepared by the following steps: drying the acidic ion exchange resin at 100-110 ℃ for 2 hours, then soaking the acidic ion exchange resin in concentrated sulfuric acid at 80-120 ℃ for sulfonation for 8-16 hours, and then washing and drying the acidic ion exchange resin to obtain the sulfonated acidic ion exchange resin catalyst.
The invention also provides a method for preparing polyvinyl butyral by using the catalyst, which comprises the steps of adding polyvinyl alcohol and n-butyraldehyde into a mixed solvent of water and ethanol, then adding a sulfonated acidic ion exchange resin 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 catalyst for preparing polyvinyl butyral and application thereof, wherein sulfonated acidic ion exchange resin is used for replacing the traditional liquid inorganic acid catalyst, so that the introduction of impurity ions is avoided, the product quality is improved, and the corrosion of equipment is reduced. The sulfonated ion exchange resin can be recycled, the production cost is reduced, the procedures such as neutralization and the like are omitted, the post-treatment process is simplified, the generation of waste water is reduced, and the sulfonated ion exchange resin is more green and environment-friendly.
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 acidic ion exchange resin at 100 ℃ for 2 hours, then soaking the acidic ion exchange resin in concentrated sulfuric acid at 110 ℃ for sulfonation for 12 hours, and then taking out the acidic ion exchange resin, washing and drying the acidic ion exchange resin to obtain the sulfonated acidic ion exchange resin catalyst. Dissolving 4g of PVA in a mixed solvent of ethanol and water (V ethanol: V water: 1.2: 1), adding 2.6g of n-butyraldehyde, then adding 0.3g of the prepared sulfonated acidic ion exchange resin catalyst to carry out synthetic reaction of polyvinyl butyral, and continuously stirring and reacting at the reaction temperature of 100 ℃ for 12 hours, wherein the acetal degree of the obtained product polyvinyl butyral reaches 68%.
Example 2
Drying the acidic ion exchange resin at 100 ℃ for 2 hours, then soaking the acidic ion exchange resin in concentrated sulfuric acid at 100 ℃ for sulfonation for 10 hours, and then taking out the acidic ion exchange resin, washing and drying the acidic ion exchange resin to obtain the sulfonated acidic ion exchange resin 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 acidic ion exchange resin catalyst to carry out synthetic reaction of polyvinyl butyral, and continuously stirring and reacting at the reaction temperature of 90 ℃ for 10 hours, wherein the acetalization degree of the obtained product polyvinyl butyral reaches 62%.
Example 3
Drying the acidic ion exchange resin at 100 ℃ for 2 hours, then soaking the acidic ion exchange resin in concentrated sulfuric acid at 110 ℃ for sulfonation for 12 hours, and then taking out the acidic ion exchange resin, washing and drying the acidic ion exchange resin to obtain the sulfonated acidic ion exchange resin catalyst. Dissolving 4g of PVA in a mixed solvent of ethanol and water (V ethanol: V water: 1.15: 1), adding 2.6g of n-butyraldehyde, then adding 0.25g of the prepared sulfonated acidic ion exchange resin catalyst to carry out synthetic reaction of polyvinyl butyral, and continuously stirring and reacting at the reaction temperature of 100 ℃ for 12 hours, wherein the acetal degree of the obtained product polyvinyl butyral reaches 65%.
Example 4
Drying the acidic ion exchange resin at 100 ℃ for 2 hours, then soaking the acidic ion exchange resin in concentrated sulfuric acid at 110 ℃ for sulfonation for 12 hours, and then taking out the acidic ion exchange resin, washing and drying the acidic ion exchange resin to obtain the sulfonated acidic ion exchange resin 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 0.32g of the prepared sulfonated acidic ion exchange resin catalyst to carry out synthetic reaction of polyvinyl butyral, and continuously stirring and reacting at the reaction temperature of 95 ℃ for 11h to obtain the product polyvinyl butyral with the acetal degree of 73%.
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.
Claims (2)
1. The catalyst for preparing the polyvinyl butyral is characterized by being prepared by the following method: drying the acidic ion exchange resin at 100-110 ℃ for 2 hours, then soaking the acidic ion exchange resin in concentrated sulfuric acid at 80-120 ℃ for sulfonation for 8-16 hours, and then washing and drying the acidic ion exchange resin to obtain the sulfonated acidic ion exchange resin catalyst.
2. A method for preparing polyvinyl butyral by using the catalyst as described in claim 1, wherein the method comprises adding polyvinyl alcohol and n-butyraldehyde into a mixed solvent of water and ethanol, then adding a sulfonated acidic ion exchange resin catalyst, adding water after the reaction is finished, and separating out the target product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011372019.0A CN112439458A (en) | 2020-11-30 | 2020-11-30 | Catalyst for preparing polyvinyl butyral and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011372019.0A CN112439458A (en) | 2020-11-30 | 2020-11-30 | Catalyst for preparing polyvinyl butyral and application thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112439458A true CN112439458A (en) | 2021-03-05 |
Family
ID=74738113
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011372019.0A Pending CN112439458A (en) | 2020-11-30 | 2020-11-30 | Catalyst for preparing polyvinyl butyral and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112439458A (en) |
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2020
- 2020-11-30 CN CN202011372019.0A patent/CN112439458A/en active Pending
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