CN111607223A - Anti-static packaging film and preparation method thereof - Google Patents
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
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- C08J2429/00—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
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- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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Abstract
The invention belongs to the field of packaging films, and particularly relates to an anti-static packaging film and a preparation method thereof, wherein the preparation method comprises the following steps: s1, preparing GO; s2, obtaining a polyvinyl alcohol solution with the solid content of 20-25%; s3, preparing GO/Fe3O4ECIP-PVA; s4, adding aniline according to the molar weight which is 3-8 times that of the polyvinyl alcohol after the reaction of the step S3, and obtaining the product through the oxidation-reduction reaction of the anilineTo RGO/Fe3O4ECIP-PVA/PANI dispersions; s5, the RGO/Fe obtained in the step S43O4the/ECIP-PVA/PANI dispersion was processed to form a film. The square packaging film obtained by the method has good thermal stability, tensile property and antistatic property.
Description
Technical Field
The invention belongs to the field of packaging films, and particularly relates to an anti-static packaging film and a preparation method thereof.
Technical Field
With the rapid development of modern science and technology and electronic industry, electronic products are becoming more miniaturized and integrated, and sensitivity is increasing. When the electrostatic charge accumulated on the object reaches a certain degree, electrostatic sparks are generated, and the generated electromagnetic pulse and discharge current can cause great damage to products. The electrostatic phenomenon generally exists in the industries of aerospace, petrochemical industry, pharmacy, mining, food and the like, and if the industries are not paid attention, huge loss can be brought. Worldwide annual losses due to discharge hazards in the microelectronics art are reported to be more than billions of dollars. With the development of polymer materials and material composite technologies, antistatic technologies and antistatic packaging materials are increasingly gaining attention and are rapidly developing. The increase of the demand of antistatic packaging materials and the attention of the society to green packaging both put forward higher requirements on the problem of electrostatic protection, and the development of composite functional materials with good stability, economy, environmental protection, energy conservation and high efficiency becomes a trend.
The antistatic packaging material can be classified into antistatic agent treatment type, conductive material filling type, plating type, coating type, surface modification type, composite type and structure conductive polymer according to different technological methods for obtaining the antistatic function of the material. The most widely used at present are filled antistatic materials.
Graphene has been widely used as a novel inorganic material for antistatic materials due to its good conductivity. In addition, the nano Fe with good conductivity and macroscopic quantum tunneling effect3O4Also find application in antistatic materials. But whether graphene or nano-Fe3O4In the antistatic material, the filler exists in a form of filling material, so that the filler may be lost in the using process, so that the antistatic effect is reduced, and on the other hand, the graphene only used as the filler cannot increase the electron conduction among polymer chains, so that the antistatic effect is influenced.
Disclosure of Invention
The invention aims to overcome the defects of graphene and nano Fe in the prior art3O4The material is unevenly distributed and easily lost to causeThe antistatic material has poor antistatic effect, and provides a preparation method of an antistatic packaging film and the antistatic material prepared by the preparation method.
The purpose of the invention is realized by the following technical scheme:
a preparation method of an anti-static packaging film comprises the following steps:
s1, preparing GO;
s2, dissolving polyvinyl alcohol in hot water at the temperature of 90-95 ℃, stirring until colorless transparent liquid is obtained, and then heating and evaporating to obtain a polyvinyl alcohol solution with the solid content of 20-25%;
s3, mixing GO and nano Fe3O4Mixing the modifier with ECIP according to a molar ratio of 1 (2-5) to (1-5) to obtain a mixed modifier, dissolving the mixed modifier into the polyvinyl alcohol solution obtained in the step S2 according to a mass ratio of 1 (20-60), adjusting the pH of the solution to 9-12, reacting for 3-7 h at 80-90 ℃, adjusting the pH of the solution to be neutral to obtain GO/Fe3O4/ECIP-PVA；
S4, adding aniline according to the molar weight which is 3-8 times of that of polyvinyl alcohol after the reaction of the step S3, and obtaining RGO/Fe through oxidation-reduction reaction of aniline3O4ECIP-PVA/PANI dispersions;
s5, the RGO/Fe obtained in the step S43O4the/ECIP-PVA/PANI dispersion was processed to form a film.
In the preparation method, GO represents graphene oxide, ECIP is epichlorohydrin, PVA is polyvinyl alcohol, RGO is reduced graphene oxide, and PANI is polyaniline.
The preparation method of GO in step S1 adopts a classical Hummer method. Step S2, polyvinyl alcohol is dissolved, and then GO and nano Fe are added in step S33O4And ECIP, wherein-Cl on the added ECIP reacts with-OH on the polyvinyl alcohol to graft a plurality of epoxy groups on the polyvinyl alcohol. Meanwhile, a large number of-COOH exist on the edge of GO and react with-OH on the polyvinyl alcohol, and a plurality of-COOH exist on the surface of GO, so that a plurality of polyvinyl alcohol molecular chains can be crosslinked under long-time reaction. Thus, graphene and macromolecules can be connected through covalent bondsThen, the nano Fe is generated through strong surface acting force between the graphene and the nano particles3O4Is adsorbed on the surface of the graphene, thereby ensuring the graphene and the nano Fe3O4Loss during long-term use. In addition, epoxy groups on the polyvinyl alcohol react with aniline to be grafted into aniline rings, and then polyaniline is formed through polymerization. Due to the conjugated relation between the polyaniline molecules and the graphene forming molecular chains, electrons can be transferred in the polyaniline molecular chains and can be transferred among the copolymer molecular chains through the graphene molecules, so that the transfer of the electrons is facilitated, and the antistatic effect is improved. In addition, nano Fe is also added into a polymer reaction system3O4Due to nano Fe3O4Has larger specific surface area and can generate strong physical adsorption with the graphene material. Graphene molecules cross-linked with different molecular chains, nano-Fe3O4And the graphene is adsorbed on the surface of the graphene, so that the graphene can be uniformly filled between molecular chains.
Preferably, GO and nano Fe in the step S33O4The molar ratio of ECIP to ECIP is 1 (2-3) to (1-3).
Preferably, GO and nano Fe in the step S33O4And ECIP in a molar ratio of 1:2: 3.
Preferably, the reaction temperature in the step S3 is 82-85 ℃.
Preferably, the reaction time in the step S3 is 4-6 h.
Preferably, the oxygen reduction reaction of aniline in step S4 includes the following steps:
s41, adding aniline in the step S3, keeping the temperature at 80-85 ℃, reacting for 1-3 h, and then adjusting the pH to 1-2;
s42, adding excessive ammonium sulfate in the step S41 to react for 20-30 h at the temperature of 80-85 ℃;
s43, filling the mixed solution after the reaction in the step S42 into a dialysis bag with the molecular weight of 1000-1500, and dialyzing for 20-25 h with distilled water to obtain the product.
Preferably, the molecular weight of the dialysis bag in the step S43 is 1200.
The dialysis bag with proper molecular weight is selected to ensure that the polymer obtained by dialysis is the target copolymer and improve the target polymer (RGO/Fe)3O4ECIP-PVA/PANI) purity, thereby improving the antistatic effect of the material.
The packaging film obtained by the preparation method of the anti-static packaging film.
Compared with the prior art, the invention has the following technical effects:
the invention discloses a preparation method of an antistatic packaging film, which is prepared by GO and nano Fe3O4The antistatic packaging film is obtained by modifying polyaniline graft copolymerization polyvinyl alcohol. Graphene is connected with a polymer through a covalent bond, and then nano Fe is subjected to strong surface acting force between the graphene and nano particles3O4The composite material is adsorbed on the surface of graphene, so that on one hand, the acting force between the filler and the polymer can be increased, the loss of the filler in the use process is prevented, on the other hand, different molecular chains are crosslinked through the graphene, the transmission of electrons between the different molecular chains is increased, and the antistatic capacity of the composite material is further improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below with reference to specific examples and comparative examples. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Unless otherwise specified, the devices used in the present examples, comparative examples and experimental examples were all conventional experimental devices, the materials and reagents used were commercially available without specific reference, and the experimental methods without specific reference were also conventional experimental methods.
Example 1
A preparation method of an anti-static packaging film comprises the following steps:
s1, preparing GO by adopting a Hummer method;
s2, dissolving polyvinyl alcohol in hot water at the temperature of 90-95 ℃, stirring until colorless transparent liquid is obtained, and then heating and evaporating to obtain a polyvinyl alcohol solution with the solid content of 25%;
s3, mixing GO and nano Fe3O4Mixing the modified solution and ECIP according to a molar ratio of 1:2:5 to obtain a mixed modifier, dissolving the mixed modifier into the polyvinyl alcohol solution obtained in the step S2 according to a mass ratio of 1:20, adjusting the pH of the solution to 9, reacting for 7 hours at 80 ℃, adjusting the pH of the solution to be neutral, and obtaining GO/Fe3O4/ECIP-PVA；
S4, adding aniline according to 3 times of the molar weight of polyvinyl alcohol after the reaction of the step S3, and performing oxidation-reduction reaction on the aniline to obtain an RGO/Fe3O4/ECIP-PVA/PANI dispersoid;
s5, processing the RGO/Fe3O4/ECIP-PVA/PANI dispersion obtained in the step S4 to form a film.
The oxygen reduction reaction of aniline in the step S4 includes the steps of:
s41, adding aniline in the step S3, keeping the temperature at 80 ℃, reacting for 3 hours, and then adjusting the pH value to 1;
s42, adding excessive ammonium sulfate in the step S41 to react for 20 hours at 80 ℃;
s43, filling the mixed solution after the reaction in the step S42 into a dialysis bag with the molecular weight of 1000, and dialyzing for 25 hours by using distilled water to obtain the product.
The antistatic packaging film obtained according to the method.
Example 2
A preparation method of an anti-static packaging film comprises the following steps:
s1, preparing GO by adopting a Hummer method;
s2, dissolving polyvinyl alcohol in hot water at the temperature of 90-95 ℃, stirring until colorless transparent liquid is obtained, and then heating and evaporating to obtain a polyvinyl alcohol solution with the solid content of 20%;
s3, mixing GO and nano Fe3O4Mixing with ECIP according to the molar ratio of 1:5:1 to obtain a mixed modifier, and dissolving the mixed modifier into the polyethylene obtained in the step S2 according to the mass ratio of 1:60In enol solution, adjusting the pH of the solution to be 12, reacting for 3 hours at the temperature of 90 ℃, adjusting the pH of the solution to be neutral, and obtaining GO/Fe3O4/ECIP-PVA；
S4, adding aniline according to 8 times of the molar weight of polyvinyl alcohol after the reaction of the step S3, and performing oxidation-reduction reaction on the aniline to obtain an RGO/Fe3O4/ECIP-PVA/PANI dispersoid;
s5, processing the RGO/Fe3O4/ECIP-PVA/PANI dispersion obtained in the step S4 to form a film.
The oxygen reduction reaction of aniline in the step S4 includes the steps of:
s41, adding aniline in the step S3, keeping the temperature at 85 ℃ for reaction for 1h, and then adjusting the pH to 2;
s42, adding excessive ammonium sulfate in the step S41 to react for 30h at 85 ℃;
s43, filling the mixed solution after the reaction in the step S42 into a dialysis bag with the molecular weight of 1500, and dialyzing for 20 hours by using distilled water to obtain the product.
The antistatic packaging film obtained according to the method.
Example 3
A preparation method of an anti-static packaging film comprises the following steps:
s1, preparing GO by adopting a Hummer method;
s2, dissolving polyvinyl alcohol in hot water at the temperature of 90-95 ℃, stirring until colorless transparent liquid is obtained, and then heating and evaporating to obtain a polyvinyl alcohol solution with the solid content of 23%;
s3, mixing GO and nano Fe3O4Mixing the modified solution and ECIP according to a molar ratio of 1:3:4 to obtain a mixed modifier, dissolving the mixed modifier into the polyvinyl alcohol solution obtained in the step S2 according to a mass ratio of 1:40, adjusting the pH of the solution to 10, reacting for 5 hours at 85 ℃, adjusting the pH of the solution to be neutral, and obtaining GO/Fe3O4/ECIP-PVA；
S4, adding aniline according to 5 times of the molar weight of polyvinyl alcohol after the reaction of the step S3, and performing oxidation-reduction reaction on the aniline to obtain an RGO/Fe3O4/ECIP-PVA/PANI dispersoid;
s5, processing the RGO/Fe3O4/ECIP-PVA/PANI dispersion obtained in the step S4 to form a film.
The oxygen reduction reaction of aniline in the step S4 includes the steps of:
s41, adding aniline in the step S3, keeping the temperature at 82 ℃ for reaction for 2 hours, and then adjusting the pH value to 1.5;
s42, adding excessive ammonium sulfate in the step S41 to react for 24 hours at 82 ℃;
s43, filling the mixed solution after the reaction in the step S42 into a dialysis bag with the molecular weight of 1200, and dialyzing for 22 hours by using distilled water to obtain the product.
The antistatic packaging film obtained according to the method.
Comparative example 1
Compared with the example 3, the step S3 of the comparative example does not add nano Fe3O4Otherwise, the same as in example 3.
Comparative example 2
Compared with example 3, the step S3 of the comparative example is not added with GO, and the rest is the same as example 3.
Comparative example 3
Compared with example 3, GO and nano Fe are not added in step S3 in the comparative example3O4Otherwise, the same as in example 3.
Experimental example 1
After the seeding mills obtained in the examples and comparative examples were vacuum dried, they were tested using a thermogravimetric analyzer. The test conditions were N2Under the atmosphere, the temperature range is 25-650 ℃, and the heating rate is 10 ℃/min. The test results are shown in table 1.
TABLE 1 film thermal stability test results
| Group of | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| 50～150℃ | 3.5％ | 3.5％ | 2.9％ | 3.5％ | 3.3％ | 3.1％ |
| 290～410℃ | 25.3％ | 27.8％ | 24.7％ | 35.2％ | 38.4％ | 35.2％ |
| 410～500℃ | 75.2％ | 79.3％ | 71.4％ | 83.4％ | 85.2％ | 87.2％ |
From the above table, it can be seen that the composite film undergoes three stages of thermal degradation at 50-500 ℃. First temperature of 50 to 150 ℃The thermal degradation of the individual stages is mainly due to the evaporation of water molecules. The second stage is mainly a thermal decomposition stage of polyvinyl alcohol at 290-410 ℃. From the above table, it can be seen that the thermal degradation rate of the example group is obviously lower than that of the comparative example group, mainly because the polyvinyl alcohol molecular chain of the example group is crosslinked by the graphene oxide to form a whole, thereby increasing the stability of the whole molecule. Comparative example 2 lack of cross-linking between GO molecular chains and therefore the thermal stability is reduced, comparative example 1 does not have nano Fe3O4Due to nano Fe3O4Can be combined with GO to increase the thermal stability of the composite. Comparative example 3 without GO and nano-Fe3O4The decomposition degree is more severe. A large amount of aniline starts to decompose in the 410-500 ℃ stage, but as can be seen from the table above, the example group still shows better thermal stability than the comparative example. Explanation, GO and nano Fe3O4Has synergistic effect in enhancing the thermal stability of the composite film.
Comparative example 2
The tensile strength of the composite film was analyzed using a TS2000-S universal tester. The dehumidified specimen has a width of 25mm and a length of 180mm, and is repeated at least five times for each sample. The test results are shown in Table 2.
TABLE 2 tensile Strength test results of composite films
It can be seen from the above table that the tensile strength of the example group is significantly stronger than that of the comparative example group. The main reason is that the overall mechanical properties are stronger after GO crosslinks multiple molecular chains. Comparative example 1 due to the lack of nano-Fe3O4The tensile property of the alloy is reduced, and the tensile property of the alloy is obviously reduced due to the fact that GO is absent in comparative example 2, mainly because GO can be crosslinked with different molecular chains to form stable structured molecules, and nano Fe3O4Further enhanced with GO structure as a filler layerThe tensile property of the composite film is improved. Comparative example 3 lack GO and Nano Fe3O4Comparative example 3, which is much poorer in tensile properties than comparative examples 1 and 2, illustrates GO and nano Fe3O4Has synergistic effect on improving the tensile property of the composite film.
Experimental example 3
And testing the conductivity of the composite film by adopting a four-probe resistivity tester. The sheet resistance of each group was calculated and the test results are shown in table 3.
TABLE 3 composite surface resistance test
From the above table, it can be seen that the surface resistance of the composite surface of the embodiment group reaches 106 orders of magnitude, and the composite surface has good conductivity and can effectively eliminate the generated static charge. GO crosslinks the two molecular weights by reaction of-COOH at the edges with-OH on the polyvinyl alcohol. The formation of RGO during the reduction of GO increases its ability to transport electrons. Meanwhile, the polyaniline molecular chain can transfer electrons on the molecular chain, and the RGO can transfer electrons between the molecular chains, so that the antistatic capacity of the material is improved.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. The preparation method of the anti-static packaging film is characterized by comprising the following steps:
s1, preparing GO;
s2, dissolving polyvinyl alcohol in hot water at the temperature of 90-95 ℃, stirring until colorless transparent liquid is obtained, and then heating and evaporating to obtain a polyvinyl alcohol solution with the solid content of 20-25%;
s3, mixing GO and nano Fe3O4Mixing the modifier with ECIP according to a molar ratio of 1 (2-5) to (1-5) to obtain a mixed modifier, dissolving the mixed modifier into the polyvinyl alcohol solution obtained in the step S2 according to a mass ratio of 1 (20-60), adjusting the pH of the solution to 9-12, reacting for 3-7 h at 80-90 ℃, adjusting the pH of the solution to be neutral to obtain GO/Fe3O4/ECIP-PVA；
S4, adding aniline according to the molar weight which is 3-8 times of that of polyvinyl alcohol after the reaction of the step S3, and obtaining RGO/Fe through oxidation-reduction reaction of aniline3O4ECIP-PVA/PANI dispersions;
s5, the RGO/Fe obtained in the step S43O4the/ECIP-PVA/PANI dispersion was processed to form a film.
2. The method for preparing the antistatic packaging film as claimed in claim 1, wherein GO and nano Fe in the step S33O4The molar ratio of ECIP to ECIP is 1 (2-3) to (1-3).
3. The preparation method of the antistatic packaging film as claimed in claim 2, wherein GO and nano Fe in the step S33O4And ECIP in a molar ratio of 1:2: 3.
4. The method for preparing the antistatic packaging film according to claim 1, wherein the reaction temperature in the step S3 is 82-85 ℃.
5. The method for preparing the antistatic packaging film according to claim 1, wherein the reaction time in the step S3 is 4-6 h.
6. The method for preparing the antistatic packaging film according to claim 1, wherein the step S4 of performing the oxygen reduction reaction on the aniline comprises the following steps:
s41, adding aniline in the step S3, keeping the temperature at 80-85 ℃, reacting for 1-3 h, and then adjusting the pH to 1-2;
s42, adding excessive ammonium sulfate in the step S41 to react for 20-30 h at the temperature of 80-85 ℃;
s43, filling the mixed solution after the reaction in the step S42 into a dialysis bag with the molecular weight of 1000-1500, and dialyzing for 20-25 h with distilled water to obtain the product.
7. The method for preparing an antistatic packaging film as claimed in claim 6, wherein the molecular weight of the dialysis bag in the step S43 is 1200.
8. The packaging film obtained by the method for producing an antistatic packaging film as claimed in any one of claims 1 to 7.
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