CN103819699A - Preparation method for ultraviolet-proof thin film - Google Patents
Preparation method for ultraviolet-proof thin film Download PDFInfo
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- CN103819699A CN103819699A CN201410075516.2A CN201410075516A CN103819699A CN 103819699 A CN103819699 A CN 103819699A CN 201410075516 A CN201410075516 A CN 201410075516A CN 103819699 A CN103819699 A CN 103819699A
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Abstract
The invention discloses a preparation method for an ultraviolet-proof thin film, and belongs to the technical field of chemical engineering. The preparation method comprises the following technological steps: adding 2-6 g of polyvinyl butyral powder into absolute ethyl alcohol according to the solid-liquid ratio of 1g/10ml, and stirring for completely dissolving the polyvinyl butyral powder, so as to obtain a solution of the polyvinyl butyral and the absolute ethyl alcohol; taking 1-5 g of zinc salt, adding the zinc salt into the solution of the polyvinyl butyral and the absolute ethyl alcohol, and performing ultrasonic treatment for 30 minutes for completely dissolving the zinc salt, so as to obtain a mixed solution; adding an ultrasonic treated alcohol soluble alkali saturated solution into the mixed solution to adjust the pH value of the mixed solution to be 8-10, adding 30-60ml of the absolute ethyl alcohol when sediments occur in the solution to clarify the solution, so as to obtain a polyvinyl butyral thin film solution; preparing the polyvinyl butyral solution into the thin film. The ultraviolet-proof thin film has fluorescence after being observed under an ultraviolet lamp. The ultraviolet-proof thin film prepared by the preparation method has high thermosensitivity, fluorescence and the capability of absorbing ultraviolet light, and is energy-saving, environment-friendly, and simple in technological process; the preparation method is mainly applied to the preparation of the ultraviolet-proof thin film.
Description
Technical field
The invention belongs to technical field of chemical engineering, relate in particular to a kind of technique of preparing antiultraviolet film.
Background technology
Along with expanding economy and population growth, global environment sharply worsens, depletion of the ozone layer, thus make the earth accept more ultraviolet radiation.Ultraviolet ray not only causes the injury to human body, also can cause the aging of the material that is exposed under sunlight simultaneously, causes material or service life of equipment to shorten, so that can not use.Polyvinyl butyral acetal, English name is polyvinyl butyral, is called for short PVB.Polyvinyl butyral acetal is a most important product in the polyvinylacetal of suitability for industrialized production, is the condenses by polyvinyl alcohol (PVA) and butyraldehyde-n reaction gained.Wherein PVA is made by Vinyl Acetate Copolymer (PVAc) hydrolysis.Because above two kinds of reactions all can not be carried out completely, so must contain three kinds of functional groups, i.e. butyral group, alcoholic extract hydroxyl group and vinyl acetate between to for plastic in PVB resin.PVB resin also has good transparency, well fast light, heat-resisting, cold-resistant, water tolerance, solvability, compatibility, film-forming properties, high-tensile and shock-resistance etc., have good cohesive force with metal, glass, timber, pottery, fibre product etc., so be all applied widely and developing rapidly aspect manufacture shatter proof glass, coating, tackiness agent, ceramic membrane marble paper, vacuum aluminium-plated paper and engineering plastics, electronic apparatus material.PVB resin is divided and can be divided into two kinds of high viscosity and low viscosity according to viscosity.Low viscous resin is mainly used in tackiness agent, only accounts for a little part for PVB resin total amount.The overwhelming majority of PVB resin is high viscosity resins, and its maximum purposes is exactly to do the intermediate coat of laminated safety glass.
PVB film has caused very large concern as a kind of Thermo-sensitive film.Its technology of preparing is the emphasis that a lot of people pay close attention to always, existing laminated film function singleness, can not have ultraviolet radiation preventing, save energy, fluorescence property concurrently, the several functions such as response are made in environmental change to external world, and the variation of most of Thin Films inside can not repeat, and has unicity.At present, it is mould material that the method for preparing PVB film is mainly polyvinyl butyral acetal, adopt wet method phase inversion process prepare polyvinyl butyral acetal porous diffusion barrier, by metal plating film or add appropriate chainextender and prepare the methods such as full-bodied polyvinyl butyral acetal (PVB) resin and film.While adopting wet method phase inversion process to prepare polyvinyl butyral film precipitation film forming, easily obtain the PVB film of larger aggregate micella; By the polyvinyl butyral film that adds appropriate chainextender to obtain, its to external world environment conversion to make the susceptibility of response too low.With high costs by metal plating film, complete processing complexity, the problems such as contaminate environment, the therefore stronger sensitivity of preparation, simplified processing process reduces costs, and the PVB film of energy-conserving and environment-protective becomes research worker and endeavours one of technical problem solving.
Summary of the invention
The object of this invention is to provide a kind of preparation method of antiultraviolet film, it can simplify production technique effectively, reduces production costs.
The object of the invention is to realize by following means:
A preparation method for antiultraviolet film, comprises following processing step:
Step 1, get 2～6g polyvinyl butyral powder end, and add dehydrated alcohol according to solid-liquid than the ratio for 1g/10ml, stir it is dissolved completely, obtain the solution of polyvinyl butyral acetal and dehydrated alcohol;
Step 2, get the zinc salt of 1～5g, add solution the ultrasonic 30min of polyvinyl butyral acetal and dehydrated alcohol, zinc salt is dissolved completely, obtain mixing solutions;
Step 3, add through ultrasonic alcohol dissolubility alkali saturated solution and regulate, making the pH value of mixing solutions is 8～11, treats that precipitating appears in solution, then adds 30～60ml dehydrated alcohol to make its clarification obtain polyvinyl butyral film solution;
Step 4, polyvinyl butyral acetal solution is prepared into film.
In described antiultraviolet film solution, contain Zinc oxide nanoparticle.
Described alcohol dissolubility alkali saturated solution is lithium hydroxide and methyl alcohol saturated solution.
The pH value optimum of described mixing solutions is 9.
Described antiultraviolet film has temperature-sensing property.
Described temperature-sensing property in the time that temperature raises film from transparent become opaque, temperature reduce time from opaque become transparent, and can repeat change.
Advantage and effect are compared with prior art: add zinc salt to prepare PVB antiultraviolet film by ultrasonic method, compared with traditional wet method phase inversion process, more can simplify experimentation, improve product purity, the structure of simplified apparatus, reduces production costs.
Innovation of the present invention is that the high-frequency oscillation signal sending by ultrasonic generator diminishes solute particles, the reagent that regulates pH value to adopt is lithium hydroxide and methyl alcohol saturated solution, prepared PVB film not only has Thermo-sensitive and fluorescence, and can absorb UV-light.The product that the present invention obtains can be made respective response, absorb the features such as UV-light ability under temperature variation.The present invention's technique used is succinct, and equipment is simple, easy and simple to handle.
Fig. 1 is the process flow sheet that the present invention prepares antiultraviolet film
Fig. 2 is polyvinyl butyral acetal molecular structure
Fig. 3 is antiultraviolet thin film transmission electron microscope figure
Fig. 4 is antiultraviolet film alternating temperature scanning electron microscope (SEM) photograph
Fig. 5 is antiultraviolet film fluorogram under UV-light
Fig. 6 is antiultraviolet film color variation diagram under extraneous temperature variation
Embodiment
By preparation technology's flow process of the present invention, except special statement, the raw materials used chemical pure that is, following examples are take the preparation method of antiultraviolet film as example, using polyvinyl butyral acetal (being called for short PVB) to be dissolved in dehydrated alcohol adds alcohol dissolubility zinc salt then ultrasonic, regulate the pH value of mixing solutions through ultrasonic alcohol dissolubility alkali saturated solution, prepare antiultraviolet film solution, can obtain identical effect:
Embodiment 1
Take 2g polyvinyl butyral acetal, be dissolved in 20ml dehydrated alcohol, strong stirring 6h is to dissolving completely; Take 1g zinc chloride and join in solution, now solution becomes muddy, puts into ultrasonic machine high frequency ultrasonic, after solute in solution dissolves, obtains mixing solutions.Regulate the pH value to 9 of this mixing solutions by ultrasonic lithium hydroxide and methyl alcohol saturated solution, and continuous stirred solution.In the time that precipitation appears in mixing solutions, add again 30ml dehydrated alcohol to make its clarification, prepare polyvinyl butyral acetal solution.Sheet glass is at the uniform velocity drawn high and is prepared into film in polyvinyl butyral acetal solution, be placed in baking oven and dry, just obtain having the variable light antiultraviolet film of temperature-sensing property.
Embodiment 2
Take 4g polyvinyl butyral acetal, be dissolved in 40ml dehydrated alcohol, strong stirring 6h is to dissolving completely; Take 3g zinc acetate and join in solution, now solution becomes muddy, puts into ultrasonic machine high frequency ultrasonic, after solute in solution dissolves, obtains mixing solutions.Regulate the pH value to 9 of mixing solutions by ultrasonic lithium hydroxide and methyl alcohol saturated solution, and continuous stirred solution.Solution occurs adding 40ml dehydrated alcohol to make its clarification after precipitation again, prepares polyvinyl butyral acetal solution.Sheet glass is at the uniform velocity drawn high and is prepared into film in polyvinyl butyral acetal solution, be placed in baking oven and dry, just obtain having the variable light antiultraviolet film of temperature-sensing property.
Embodiment 3
Take 6g polyvinyl butyral acetal, be dissolved in 60ml dehydrated alcohol, strong stirring 6h is to dissolving completely; Take 5g zinc nitrate and join in solution, now solution becomes muddy, puts into ultrasonic machine high frequency ultrasonic, after solute in solution dissolves, obtains mixing solutions.Regulate the pH value to 9 of mixing solutions by ultrasonic lithium hydroxide and methyl alcohol saturated solution, and continuous stirred solution.Solution occurs adding 50ml dehydrated alcohol to make its clarification after precipitation again, prepares polyvinyl butyral acetal solution.Can polyvinyl butyral acetal solution be prepared into film by membrane equipment, just obtain having the variable light antiultraviolet film of temperature-sensing property.
Embodiment 4
Take 4g polyvinyl butyral acetal, be dissolved in 40ml dehydrated alcohol, strong stirring 6h is to dissolving completely; Take 3g zinc chloride and join in solution, now solution becomes muddy, puts into ultrasonic machine high frequency ultrasonic, after solute in solution dissolves, obtains mixing solutions.Regulate the pH value to 9 of mixing solutions by ultrasonic lithium hydroxide and methyl alcohol saturated solution, and continuous stirred solution.Solution occurs that precipitation adds 30ml dehydrated alcohol to make its clarification again, prepares polyvinyl butyral acetal solution.Can polyvinyl butyral acetal solution be prepared into film by membrane equipment, just obtain having the variable light antiultraviolet film of temperature-sensing property.
Embodiment 5
Take 4g polyvinyl butyral acetal, be dissolved in 40ml dehydrated alcohol, strong stirring 6h is to dissolving completely; Take 4g zinc chloride and join in solution, now solution becomes muddy, puts into ultrasonic machine high frequency ultrasonic, after solute in solution dissolves, obtains mixing solutions.Regulate the pH value to 9 of mixing solutions by ultrasonic lithium hydroxide and methyl alcohol saturated solution, and continuous stirred solution.Solution occurs adding 50ml dehydrated alcohol to make its clarification after precipitation again, prepares polyvinyl butyral acetal solution.Can polyvinyl butyral acetal solution be prepared into film by membrane equipment, just obtain having the variable light antiultraviolet film of temperature-sensing property.
Embodiment 6
Take 5g polyvinyl butyral acetal, be dissolved in 50ml dehydrated alcohol, strong stirring 6h is to dissolving completely; Take 3g zinc chloride and join in solution, now solution becomes muddy, puts into ultrasonic machine high frequency ultrasonic, after solute in solution dissolves, obtains mixing solutions.Regulate the pH value to 9 of mixing solutions by ultrasonic lithium hydroxide and methyl alcohol saturated solution, and continuous stirred solution.Solution occurs adding 50ml dehydrated alcohol to make its clarification after precipitation again, prepares polyvinyl butyral acetal solution.Can polyvinyl butyral acetal solution be prepared into film by membrane equipment, just obtain having the variable light antiultraviolet film of temperature-sensing property.
Embodiment 7
Take 6g polyvinyl butyral acetal, be dissolved in 60ml dehydrated alcohol, strong stirring 6h is to dissolving completely; Take 4g zinc chloride and join in solution, now solution becomes muddy, puts into ultrasonic machine high frequency ultrasonic, after solute in solution dissolves, obtains mixing solutions.Regulate the pH value to 9 of mixing solutions by ultrasonic lithium hydroxide and methyl alcohol saturated solution, and continuous stirred solution.Solution occurs adding 50ml dehydrated alcohol to make its clarification after precipitation again, prepares polyvinyl butyral acetal solution.Can polyvinyl butyral acetal solution be prepared into film by membrane equipment, just obtain having the variable light antiultraviolet film of temperature-sensing property.
Embodiment 8
Take 4g polyvinyl butyral acetal, be dissolved in 40ml dehydrated alcohol, strong stirring 6h is to dissolving completely; Take 3g zinc salt and join in solution, now solution becomes muddy, puts into ultrasonic machine high frequency ultrasonic, after solute in solution dissolves, obtains mixing solutions.Regulate the pH value to 8 of mixing solutions by ultrasonic lithium hydroxide and methyl alcohol saturated solution, and continuous stirred solution.Solution occurs adding 30ml dehydrated alcohol to make its clarification after precipitation again, prepares polyvinyl butyral acetal solution.Can polyvinyl butyral acetal solution be prepared into film by membrane equipment, just obtain having the variable light antiultraviolet film of temperature-sensing property.
Embodiment 9
Take 4g polyvinyl butyral acetal, be dissolved in 40ml dehydrated alcohol, strong stirring 6h is to dissolving completely; Take 3g zinc salt and join in solution, now solution becomes muddy, puts into ultrasonic machine high frequency ultrasonic, after solute in solution dissolves, obtains mixing solutions.Regulate the pH value to 10 of mixing solutions by ultrasonic lithium hydroxide and methyl alcohol saturated solution, and continuous stirred solution.Solution occurs adding 30ml dehydrated alcohol to make its clarification after precipitation again, prepares polyvinyl butyral acetal solution.Can polyvinyl butyral acetal solution be prepared into film by membrane equipment, just obtain having the variable light antiultraviolet film of temperature-sensing property.
Embodiment 10
Take 4g polyvinyl butyral acetal, be dissolved in 40ml dehydrated alcohol, strong stirring 6h is to dissolving completely; Take 3g zinc salt and join in solution, now solution becomes muddy, puts into ultrasonic machine high frequency ultrasonic, after solute in solution dissolves, obtains mixing solutions.Regulate the pH value to 11 of mixing solutions by ultrasonic lithium hydroxide and methyl alcohol saturated solution, and continuous stirred solution.Solution occurs adding 30ml dehydrated alcohol to make its clarification after precipitation again, prepare polyvinyl butyral acetal solution, sheet glass is at the uniform velocity drawn high and is prepared into film in polyvinyl butyral acetal solution, be placed in baking oven and dry, just obtain having the variable light antiultraviolet film of temperature-sensing property.
Can find out by accompanying drawing, polyvinyl butyral acetal has butyral group, alcoholic extract hydroxyl group and three kinds of functional groups of vinyl acetate between to for plastic.Less by particle diameter in the film of ultrasonic preparation is several nanometers.Particle under temperature variation in film can repeatedly be reunited and disperse, and arrow in figure: A is cooling to B, and C is intensification to D.Prepared PVB film solution has fluorescence, can absorb UV-light.Under extraneous temperature variation the variation of film be mainly manifested in opaque become transparent.
Claims (6)
1. a preparation method for antiultraviolet film, comprises following processing step:
Step 1, get 2～6g polyvinyl butyral powder end, and add dehydrated alcohol according to solid-liquid than the ratio for 1g/10ml, stir it is dissolved completely, obtain the solution of polyvinyl butyral acetal and dehydrated alcohol;
Step 2, get the zinc salt of 1～5g, add solution the ultrasonic 30min of polyvinyl butyral acetal and dehydrated alcohol, zinc salt is dissolved completely, obtain mixing solutions;
Step 3, add through ultrasonic alcohol dissolubility alkali saturated solution and regulate, making the pH value of mixing solutions is 8～11, treats that precipitating appears in solution, then adds 30～60ml dehydrated alcohol to make its clarification obtain polyvinyl butyral film solution;
Step 4, polyvinyl butyral acetal solution is prepared into film.
2. the preparation method of antiultraviolet film according to claim 1, is characterized in that, in described antiultraviolet film solution, contains Zinc oxide nanoparticle.
3. the preparation method of antiultraviolet film according to claim 1, is characterized in that, described alcohol dissolubility alkali saturated solution is lithium hydroxide and methyl alcohol saturated solution.
4. the preparation method of antiultraviolet film according to claim 1, is characterized in that, the pH value optimum of described mixing solutions is 9.
5. the preparation method of antiultraviolet film according to claim 1, is characterized in that, described antiultraviolet film has temperature-sensing property.
6. the preparation method of antiultraviolet film according to claim 1, is characterized in that, described temperature-sensing property in the time that temperature raises film from transparent become opaque, temperature reduce time from opaque become transparent, and can repeat change.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110204757A (en) * | 2019-06-18 | 2019-09-06 | 中北大学 | Polyvinyl butyral-carbon dots nano composite membrane preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101161705A (en) * | 2006-10-13 | 2008-04-16 | 中国科学院化学研究所 | Functional polymer nano composite material and preparation method and uses thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101161705A (en) * | 2006-10-13 | 2008-04-16 | 中国科学院化学研究所 | Functional polymer nano composite material and preparation method and uses thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110204757A (en) * | 2019-06-18 | 2019-09-06 | 中北大学 | Polyvinyl butyral-carbon dots nano composite membrane preparation method |
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