CN113845678B - Preparation method of high-transparency flame-retardant polyvinyl alcohol film - Google Patents
Preparation method of high-transparency flame-retardant polyvinyl alcohol film Download PDFInfo
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- CN113845678B CN113845678B CN202111208343.3A CN202111208343A CN113845678B CN 113845678 B CN113845678 B CN 113845678B CN 202111208343 A CN202111208343 A CN 202111208343A CN 113845678 B CN113845678 B CN 113845678B
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
- C08K5/175—Amines; Quaternary ammonium compounds containing COOH-groups; Esters or salts thereof
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
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Abstract
The invention belongs to the technical field of polymer chemistry, and discloses a preparation method of a transparent flame-retardant polyvinyl alcohol film, which comprises the following method steps: the transparent flame-retardant polyvinyl alcohol film is prepared from a mixed solution of L-aspartic acid dissolved by acid and polyvinyl alcohol, and the solution is centrifugally stirred for several hours under the heating condition and then cast into a film, and finally heated and dried, and the specific preparation method comprises the following steps: under the heating condition, dissolving L-aspartic acid in an acid solution, centrifugally stirring for a plurality of hours, adding a polyvinyl alcohol aqueous solution, centrifugally stirring, and casting to form the transparent flame-retardant film. The polyvinyl alcohol film prepared by the invention has excellent flame retardant property and good transparency, and the flame retardant can be stably combined with the polyvinyl alcohol to form a high-transparency flame retardant polyvinyl alcohol film with good mechanical property. The method for preparing the flame-retardant film has the advantages of simple process, low cost and easy mass production.
Description
Technical Field
The invention relates to the technical field of polymer chemistry, in particular to a preparation method of a high-transparency flame-retardant polyvinyl alcohol film.
Background
Polyvinyl alcohol (PVA) is a water-soluble polymer that is hydrolyzed from polyvinyl acetate and has extremely wide applications. The performance is unique, the repeated units contain hydroxyl groups, the polarity is strong, and hydrogen bonds are easy to form between the repeated units, so that the polyvinyl alcohol has the properties of excellent water solubility, film forming property, oil resistance and the like. The film material prepared from the polyvinyl alcohol has the characteristics of excellent biocompatibility, excellent mechanical property, excellent barrier property and the like, and is widely used in the fields of antibiosis and bacteriostasis, flexible photoelectric devices, gas barrier and the like. However, as a film product with smaller thickness, the flammability is far higher than that of a product with larger wall thickness, and the film product can release harmful substances such as unsaturated aldehyde, ketone and the like when burning, so that huge hidden danger is caused in the use process, and the application of the polyvinyl alcohol film is hindered. When the flame retardant modification of the polyvinyl alcohol film is carried out, the problems that the transparency or mechanical property of the polyvinyl alcohol film is deteriorated due to the flame retardant are always encountered. It is therefore necessary to make transparent flame retardant modifications.
Flame retardation studies of polyvinyl alcohol films are classified into additive type and reactive type. The reactive flame retardant is that the flame retardant and the polyvinyl alcohol are subjected to chemical reaction to form covalent bonds, so that the flame retardant effect is achieved. The added flame retardant means that the flame retardant is dispersed in the polyvinyl alcohol matrix by a physical mixing mode, and does not react with the matrix. The added flame retardant has great negative influence on the transparency and the like of the film, and the reactive flame retardant has the problems of high cost, low grafting rate of polyvinyl alcohol and the like, so the reactive flame retardant has the problems of comprehensive flame retardance, transparency, mechanical property and the like.
In summary, a method for preparing a highly transparent flame retardant polyvinyl alcohol film is provided in the present application.
Disclosure of Invention
Object of the invention
In order to solve the technical problems in the background technology, the invention provides a preparation method of a high-transparency flame-retardant polyvinyl alcohol film.
(II) technical scheme
In order to solve the problems, the invention provides a preparation method of a high-transparency flame-retardant polyvinyl alcohol film, which comprises the following method steps:
s1, adding L-aspartic acid into an acid solution under a heating condition, centrifugally stirring, and forming an L-aspartate solution from the L-aspartic acid and the acid solution;
s2, adding a polyvinyl alcohol solution into the L-aspartate solution obtained in the step S1, and stirring for reaction to obtain a mixed solution;
s3, pouring the mixed solution obtained in the step S2 into a mold, standing at normal temperature to volatilize part of the solvent, and drying in an oven to form a film to obtain the transparent flame-retardant polyvinyl alcohol film.
Preferably, in the step S1, the heating temperature is 50-80 ℃, the centrifugal stirring time is 1-3 hours, the acid solution is any one of sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid and oxalic acid, and the concentration of the acid solution is 0.5-2mol/L.
Preferably, in step S2, the concentration of the polyvinyl alcohol solution is 5% -20%.
Preferably, in step S2, the stirring reaction temperature is 70-100 ℃, and the stirring reaction time is 1-4 hours.
Preferably, in the step S2, the mixed solution is based on the total mass of the polyvinyl alcohol and the L-aspartic acid, the mass content of the solvent acid solution is 5% -50%, and the mass content of the L-aspartic acid is 5% -35%;
preferably, in step S3, the normal temperature is set for 8-12 hours, and the drying temperature is 40-80 ℃.
Preferably, in step S3, the transparent flame retardant polyvinyl alcohol film has a thickness of 50 to 500 μm after being dried.
A highly transparent flame retardant polyvinyl alcohol film prepared according to the above-described method for preparing a highly transparent flame retardant polyvinyl alcohol film.
The technical scheme of the invention has the following beneficial technical effects:
1. the polyvinyl alcohol flame-retardant film with excellent performance is prepared by a simple one-pot method technology, the polyvinyl alcohol film has excellent flame-retardant performance, the flame retardant can be stably combined with the polyvinyl alcohol, and the flame-retardant polyvinyl alcohol film has high transparency.
2. The L-aspartic acid in the flame-retardant film of the present invention is used as a flame retardant, and the L-aspartic acid content may be added to a high level.
3. The preparation method of the flame-retardant transparent film provided by the invention has the advantages of simple implementation process, high efficiency, rapidness, low cost and easiness in realizing mass production.
Drawings
FIG. 1 is a photograph of the transparency of the flame retardant transparent films prepared in comparative example one and examples one, three, five, seven, eight.
FIG. 2 is an infrared spectrum of a flame retardant transparent film prepared in comparative example one and examples one, three, five, seven.
Fig. 3 is a drawing of tensile data of the flame retardant transparent films prepared in comparative example one and examples one, three, five, and seven.
Fig. 4 is an SEM photograph and EDS data plot of example eight.
FIG. 5 is a photograph of the combustion of comparative example one, comparative example two and examples one, three, five and seven.
Fig. 6 is a flow chart of the present invention.
Detailed Description
The present invention will be further described in detail with reference to the following embodiments, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the description is only illustrative and is not intended to limit the scope of the invention. In addition, in the following description, descriptions of well-known structures and techniques are omitted so as not to unnecessarily obscure the present invention.
Example 1
As shown in FIG. 6, the invention provides a preparation method of a high-transparency flame-retardant polyvinyl alcohol film, which comprises the steps of stirring and heating 0.105g of L-aspartic acid at 70 ℃ for 1 hour, dissolving in 10g of 1mol/L sulfuric acid solution, adding 10g of 20% polyvinyl alcohol solution, placing in an oil bath pot at 90 ℃ for stirring and reacting for 2 hours to obtain a mixed solution, pouring the mixed solution into an acrylic mold plate, placing at room temperature for 12 hours, volatilizing part of the solvent, and drying at 55 ℃ to obtain the transparent flame-retardant film.
Example two
As shown in FIG. 6, the invention provides a preparation method of a high-transparency flame-retardant polyvinyl alcohol film, which comprises the steps of stirring and heating 0.22g of L-aspartic acid at 70 ℃ for 1 hour, dissolving in 10g of 1mol/L sulfuric acid solution, adding 10g of 20% polyvinyl alcohol solution, placing in an oil bath pot, stirring and reacting for 2 hours to obtain a mixed solution, pouring the mixed solution into an acrylic mold plate, placing at room temperature for 12 hours, volatilizing part of the solvent, and drying at 55 ℃ to obtain the transparent flame-retardant film.
Example III
As shown in FIG. 6, the invention provides a preparation method of a high-transparency flame-retardant polyvinyl alcohol film, which comprises the steps of stirring and heating 0.35g of L-aspartic acid at 70 ℃ for 1 hour, dissolving in 10g of 1mol/L sulfuric acid solution, adding 10g of 20% polyvinyl alcohol solution, placing in an oil bath pot, stirring and reacting for 2 hours to obtain a mixed solution, pouring the mixed solution into an acrylic mold plate, placing at room temperature for 12 hours, volatilizing part of the solvent, and drying at 55 ℃ to obtain the transparent flame-retardant film.
Example IV
As shown in FIG. 6, the invention provides a preparation method of a high-transparency flame-retardant polyvinyl alcohol film, which comprises the steps of stirring and heating 0.50g of L-aspartic acid at 70 ℃ for 1 hour, dissolving in 10g of 1mol/L sulfuric acid solution, adding 10g of 20% polyvinyl alcohol solution, placing in an oil bath pot, stirring and reacting for 2 hours to obtain a mixed solution, pouring the mixed solution into an acrylic mold plate, placing at room temperature for 12 hours, volatilizing part of the solvent, and drying at 55 ℃ to obtain the transparent flame-retardant film.
Example five
As shown in FIG. 6, the invention provides a preparation method of a high-transparency flame-retardant polyvinyl alcohol film, which comprises the steps of stirring and heating 0.67g of L-aspartic acid at 70 ℃ for 1 hour, dissolving in 10g of 1mol/L sulfuric acid solution, adding 10g of 20% polyvinyl alcohol solution, placing in an oil bath pot, stirring and reacting for 2 hours to obtain a mixed solution, pouring the mixed solution into an acrylic mold plate, placing at room temperature for 12 hours, volatilizing part of the solvent, and drying at 55 ℃ to obtain the transparent flame-retardant film.
Example six
As shown in FIG. 6, the invention provides a preparation method of a high-transparency flame-retardant polyvinyl alcohol film, which comprises the steps of stirring and heating 0.86g of L-aspartic acid at 70 ℃ for 1 hour, dissolving in 10g of 1mol/L sulfuric acid solution, adding 10g of 20% polyvinyl alcohol solution, placing in an oil bath pot, stirring and reacting for 2 hours to obtain a mixed solution, pouring the mixed solution into an acrylic mold plate, placing at room temperature for 12 hours, volatilizing part of the solvent, and drying at 55 ℃ to obtain the transparent flame-retardant film.
Example seven
As shown in FIG. 6, the invention provides a preparation method of a high-transparency flame-retardant polyvinyl alcohol film, which comprises the steps of stirring and heating 1.08g of L-aspartic acid at 70 ℃ for 1 hour, dissolving in 10g of 1mol/L sulfuric acid solution, adding 10g of 20% polyvinyl alcohol solution, placing in an oil bath pot, stirring and reacting for 2 hours to obtain a mixed solution, pouring the mixed solution into an acrylic mold plate, placing at room temperature for 12 hours, volatilizing part of the solvent, and drying at 55 ℃ to obtain the transparent flame-retardant film.
Example eight
As shown in FIG. 6, the invention provides a preparation method of a high-transparency flame-retardant polyvinyl alcohol film, which comprises the steps of stirring and heating 0.67g of L-aspartic acid at 70 ℃ for 1 hour, dissolving in 10g of 1mol/L hydrochloric acid solution, adding 10g of 20% polyvinyl alcohol solution, placing in an oil bath pot, stirring and reacting for 2 hours to obtain a mixed solution, pouring the mixed solution into an acrylic mold plate, placing at room temperature for 12 hours, volatilizing part of the solvent, and drying at 55 ℃ to obtain the transparent flame-retardant film.
To verify the preferences of the present invention, the products obtained in the above examples were tested, a comparative example was set, comparative example one: a pure polyvinyl alcohol film; comparative example two: films prepared according to example four without L-aspartic acid.
In the above embodiment, the test apparatus and method are as follows:
vertical Combustion Performance (UL 94) test was performed using a horizontal vertical Combustion instrument FTT0082, from FTT company, UK, according to GB/T2408-2008.
Infrared spectroscopy FTIR test: a Fourier transform infrared spectrometer (Prrestige-21, shimadzu International trade Co., ltd.) was used. ATR module, 25 ℃ test.
Mechanical property test: a computer single column tensile tester (HF-6008, jinan Mitsui Chang tester manufacturing Co., ltd.) was used for the test method according to ASTM-D368-14.
Microcosmic morphology testing: an electron scanning electron microscope (Flex SEM1000, hitachi, japan) was used. Tested under 3.0KV accelerating voltage.
The test results are shown in FIGS. 1-5 and Table one, which is UL-94 vertical burning data for examples one through seven.
TABLE 1 vertical Combustion data
FIG. 1 is a photograph showing transparency of comparative example one and examples one, three, five, seven and eight, and it can be seen from the figure that when the acid solvent is sulfuric acid and hydrochloric acid solutions, the films are transparent, and the films prepared by examples with different contents are high in transparency.
FIG. 2 is an infrared spectrum of 3500cm of films obtained in comparative example one and examples one, three, five, and seven -1 -3000cm -1 The hydroxyl peak red shifted, indicating the hydrogen bonding between the flame retardant and the polyvinyl alcohol film.
FIG. 3 shows the mechanical properties of the films prepared in comparative example one and examples one, three, five and seven, and it can be seen from the graph that the films prepared in examples have good tensile properties.
FIG. 4 is an SEM microtopography of the film obtained in example eight and an EDS of the nitrogen distribution. Crystals or other solid blocks of flame retardant were not seen from SEM pictures, and the surface of the film was also smooth, and it was seen from DES that nitrogen was uniformly distributed in the film, and thus that flame retardant was uniformly distributed in the film prepared in the examples.
Fig. 5 is a photograph of the combustion of comparative example one, comparative example two and examples one, three, five and seven, and it can be seen from the figure that the flame retardant effect of the transparent flame retardant film prepared by the examples is obvious.
Table 1 shows the vertical burning data for comparative example one and examples one to seven, from which it can be seen that the L-aspartic acid content was ten percent, and the grade had reached the V-0 grade.
According to the analysis, the polyvinyl alcohol flame-retardant film with excellent performance is prepared by a simple one-pot method technology, the flame-retardant performance of the polyvinyl alcohol film is excellent, the flame retardant can be stably combined with the polyvinyl alcohol, and the flame-retardant polyvinyl alcohol film has high transparency. The L-aspartic acid in the flame-retardant film of the present invention can be added to a high content as a flame retardant. The flame-retardant transparent film and the preparation method thereof provided by the invention have the advantages of simple implementation process, high efficiency, rapidness, low cost and easiness in realizing mass production.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the above-described embodiments, and that the above-described embodiments and descriptions are only preferred embodiments of the present invention, and are not intended to limit the invention, and that various changes and modifications may be made therein without departing from the spirit and scope of the invention as claimed.
Claims (7)
1. The preparation method of the high-transparency flame-retardant polyvinyl alcohol film is characterized by comprising the following method steps:
s1, adding L-aspartic acid into an acid solution under a heating condition, centrifugally stirring, forming an L-aspartate solution from the L-aspartic acid and the acid solution, wherein the heating temperature is 50-80 ℃, the centrifugal stirring time is 1-3 hours, the acid solution is any one of sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid and oxalic acid, and the concentration of the acid solution is 0.5-2mol/L;
s2, adding a polyvinyl alcohol solution into the L-aspartate solution obtained in the step S1, and stirring for reaction to obtain a mixed solution;
s3, pouring the mixed solution obtained in the step S2 into a mold, standing at normal temperature to volatilize part of the solvent, and then drying in an oven to form a film to obtain the transparent flame-retardant polyvinyl alcohol film.
2. The method for preparing a highly transparent flame retardant polyvinyl alcohol film according to claim 1, wherein the concentration of the polyvinyl alcohol solution in step S2 is 5% -20%.
3. The method for producing a highly transparent flame retardant polyvinyl alcohol film according to claim 1, wherein in step S2, the stirring reaction temperature is 70 to 100 ℃ and the stirring reaction time is 1 to 4 hours.
4. The method for producing a highly transparent flame retardant polyvinyl alcohol film according to claim 1, wherein in step S2, the mixed solution has a solvent acid solvent mass content of 5% to 50% and the L-aspartic acid mass content of 5% to 35% based on the total mass of polyvinyl alcohol and the L-aspartic acid.
5. The method for producing a highly transparent flame retardant polyvinyl alcohol film according to claim 1, wherein in step S3, the normal temperature holding time is 8 to 12 hours and the drying temperature is 40 to 80 ℃.
6. The method for preparing a highly transparent flame retardant polyvinyl alcohol film according to claim 1, wherein in step S3, the thickness of the transparent flame retardant polyvinyl alcohol film after drying is 50-500 μm.
7. A highly transparent flame retardant polyvinyl alcohol film, characterized by being produced according to the production method of a highly transparent flame retardant polyvinyl alcohol film as claimed in any one of claims 1 to 6.
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