CN114539800B - Preparation method and application of high-toughness high-transparency heat-sealable cellulose film - Google Patents
Preparation method and application of high-toughness high-transparency heat-sealable cellulose film Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J5/18—Manufacture of films or sheets
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- C08J2397/00—Characterised by the use of lignin-containing materials
- C08J2397/02—Lignocellulosic material, e.g. wood, straw or bagasse
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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 field of preparation of heat-sealable packaging materials, and particularly relates to a preparation method of a high-toughness high-transparency heat-sealable cellulose film, which comprises the following steps: (1) dissolution of cellulose: preparing a chloride salt solution, adding plant fibers and dissolving the plant fibers after the chloride salt solution reaches a transparent solution state at a proper temperature; (2) blending: adding a plasticizer after the dissolution of the plant fiber is completed to fully blend the plant fiber; (3) coating film; (4) solvent replacement: immersing the coated film into a coagulating bath for organic solvent replacement so that the residual salt content is kept in a fixed concentration range; and (5) air-drying. The cellulose membrane prepared by the method can be completely degraded, has good biocompatibility, shows the characteristics of high transparency and high toughness, can be thermally bonded at a relatively low temperature, and expands the application scenes of the cellulose membrane in different industries such as food, cosmetics and the like.
Description
Technical Field
The invention belongs to the field of preparation of heat-sealable packaging materials, and particularly relates to a preparation method of a high-toughness high-transparency heat-sealable cellulose film.
Background
Under the background of national plastic inhibition and carbon reduction action acceleration, packaging materials such as plastics and the like are gradually forbidden due to gradual depletion of petroleum resources, serious environmental pollution and undegradable reasons, and various countries in the world are actively searching for degradable materials capable of replacing plastics. Cellulose is used as a natural polymer material which has wide sources, good biocompatibility and degradability, plays a very important role in a plurality of green renewable energy sources, and the annual global natural yield can reach 1500 hundred million tons, however, because the tight combination of hydrogen bonds among macromolecular chains of cellulose leads to the fact that the cellulose is not easy to dissolve and has no fatal defect of melting point, the two fatal defects directly limit the acceleration process of the industrialization of cellulose products, and more seriously limit the substitution of cellulose films as packaging materials for heat-sealable plastics, so the heat-sealing modification of the cellulose films is always a hot spot work of the packaging industry.
Currently, a coating process is commonly used to prepare a heat sealable cellulosic film. Xue Mengqing et al, of the university of east China, immerse Lyocell cellulose membranes prepared from waste cotton in solutions of silane coupling agents, methylene dichloride and the like to modify the same, and although the heat-sealable cellulose membranes are obtained, the immersion process is equivalent to adding a layer of coating on the surface of the cellulose membranes, the coating plays a role in enabling the Lyocell cellulose membranes to have heat-sealable characteristics, and the cellulose membranes do not obtain heat-sealable properties. Thus, the coating process for preparing a heat sealable cellulose film has the disadvantage that the process flow is more cumbersome than direct blending, and in order to make the surface coating heat sealable, materials such as polyester which are harmful to the environment are often used. The residue of materials such as polyester on the surface of packaging materials limits their use in the industries of foods, cosmetics, commodities, etc. Thus, the heat-sealable modification of cellulose films can be achieved with real value by direct blending of the cellulose films with environmentally benign substances.
The patent document of application number 202110402446.7 discloses a method for producing heat-sealable food packaging paper, wherein a surface sizing agent with water-proof, oil-proof and heat-sealing properties is coated on the surface of paper by adopting a film transfer sizing mode to produce the heat-sealable food packaging paper, and the heat-sealing mode of a heat sealing machine is used for realizing bag making or box making of the product, but the steps are complicated, not completely degradable and still need to be further improved.
Disclosure of Invention
Based on the above-mentioned drawbacks and deficiencies of the prior art, it is an object of the present invention to at least solve one or more of the above-mentioned problems of the prior art, in other words, to provide a method for preparing a high-toughness high-transparency heat-sealable cellulose film satisfying one or more of the aforementioned needs.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
a method for preparing a high-toughness high-transparency heat-sealable cellulose film, comprising the steps of:
(1) Placing plant cellulose into salt solution, stirring and dissolving;
(2) Preparing a plasticizer, and blending the plasticizer with a cellulose solution to obtain a mixed solution;
(3) Pouring the mixed solution into a film making device, and scraping and coating a film on a glass plate;
(4) After blade coating, placing the film into a coagulating bath, carrying out organic solvent replacement, and controlling the mass ratio of residual salt of the cellulose film;
(5) And (3) air-drying the cellulose membrane replaced in the step (4) to form a membrane.
Preferably, the mass ratio of the residual salt is 20-30%, and the mass ratio of the residual salt refers to the ratio of the mass of the final salt to the mass of the original added salt.
Preferably, the plant fiber comprises one or more of cotton, flax, wood pulp and bagasse.
Preferably, the salt solution is a chloride salt solution.
Preferably, the chloride salt solution is a chloride salt solution capable of dissolving cellulose, including zinc chloride solution or ferric chloride solution.
Preferably, the mass of the cellulose in the step (1) is 1-2.5% of the mass ratio of the relative solvent, preferably the mass of the cellulose is 0.4-1.0g, the mass fraction of the salt solution is 70% -80%, and the temperature is 70-90 ℃.
Preferably, the plasticizer in the step (2) includes an alcohol having a water-retaining effect and also includes an alcohol having a water-absorbing effect.
Preferably, the alcohol with water retention effect comprises glycerin, the alcohol with water absorption effect comprises any one of sorbitol, pentaerythritol and xylitol, the mass ratio of the glycerin to any one of sorbitol, pentaerythritol and xylitol is 1 (0.5-1), and the mass ratio of the sum of the glycerin and the sorbitol to the xylitol is 10-20% relative to the cellulose solution.
Preferably, the thickness of the film forming device in the step (3) is 250-750 μm, preferably 250 μm, 500 μm and 750 μm; the coagulating bath in the step (4) adopts any one of ethanol, methanol and acetone, the volume is 500-900 mL, and the time is 35-40 min;
preferably, the air-drying film forming environment temperature in the step (5) is 15-20 ℃ and the humidity is 40-60%.
Compared with the prior art, the invention has the beneficial effects that:
(1) The high-toughness high-transparency heat-sealable cellulose film prepared by the invention is completely degradable.
(2) The plasticizer is biologically friendly, nontoxic and harmless.
(3) Compared with a coating method, the preparation process of the cellulose film is simpler and more convenient, and the prepared heat-sealable cellulose film has high toughness and high transparency, can be heat-sealed at about 100 ℃, realizes the direct heat sealing property of the cellulose film, and is beneficial to expanding the application market of the cellulose film in the fields of foods, cosmetics and packaging.
Drawings
FIG. 1 is a scanning electron microscope image of a cross section of a junction of two cellulose films according to example 1 of the present invention;
FIG. 2 is a physical comparison of the heat-sealable cellulose film of example 1 of the present invention with the non-heat-sealable cellulose film of comparative example 1 after hot pressing.
Detailed Description
In the following description, some embodiments of the invention are described in order to more clearly illustrate the embodiments of the invention. It will be obvious to those having ordinary skill in the art that many other embodiments may be substituted for those illustrated and described without undue burden.
The inventor of the heat-sealable cellulose film prepared by the invention happens to find that the solution after dissolution of cellulose cannot be completely removed after film formation, and the salt solution which cannot be completely removed is skillfully converted into an inducer for realizing heat sealing under the action of heat. When the cellulose is dissolved into a film by using a chloride salt solution and a plasticizer, for example, a zinc chloride solution, although a certain zinc ion remains in the cellulose film, the zinc ion reaches a certain concentration value and a part of water is not separated, the plasticizer has the functions of water retention and water absorption, and the concentration of the remaining zinc ion reaches a certain value only by the presence of the plasticizer. Therefore, even if the cellulose film that has been formed is returned to the sol state again by heat when the concentration of the residual zinc ions reaches a certain value under the synergistic effect of the plasticizer and the residual salt solution, so that it is bonded together by external pressure.
The preparation method of the high-toughness high-transparency heat-sealable cellulose film comprises the following specific steps:
(1) Dissolving plant fiber with certain mass in chloride solution with certain concentration, stirring at constant speed at certain temperature for dissolving until transparent yellowish viscous state is shown;
(2) Preparing a mixed plasticizer with a certain proportion, stirring and mixing the mixed plasticizer to a flowing state at a certain temperature, and blending the mixed plasticizer with a cellulose solution in a proper proportion to obtain a mixed solution;
(3) Pouring the mixed solution into a film making device for film coating, wherein the film making device selects proper thickness, and knifing and film making are carried out on a glass plate;
(4) After the scraping, the mixture is placed into a coagulation bath with a certain volume for proper time of organic solvent replacement;
(5) Replacing the organic solvent of the step (4) and continuing the replacement of the organic solvent for a proper time in a certain volume so that the residual salt amount of the cellulose membrane is within a certain range;
(6) And (3) placing the cellulose membrane subjected to the organic solvent replacement in the steps (4) and (5) in a proper environment, and performing air drying to form the membrane.
In the invention, the steps (4) and (5) can be carried out for a proper time by replacing the organic solvent once, so that the residual salt amount of the cellulose membrane is within a certain range;
salt solution action: cellulose cannot be dissolved in water or organic solvent, and the high-concentration chloride salt solution can break a large number of hydrogen bonds between cellulose molecules and between cellulose molecules, so that cellulose is dissolved.
Organic solvents such as ethanol, methanol, acetone are used in the coagulation bath to displace the zinc chloride from the film, and these organic solvents are volatile and after air drying only the fibres and part of the residual salts remain in the cellulose film.
The plasticizer comprises alcohol with water-retaining effect such as glycerol, and also comprises any one of alcohol with water-absorbing effect such as sorbitol, pentaerythritol, and xylitol.
Example 1:
the preparation method of the high-toughness high-transparency heat-sealable cellulose film comprises the following steps:
(1) 0.8g of cotton fiber is dissolved in a zinc chloride solution with the mass fraction of 70 percent, and is stirred at a constant speed at 90 ℃ for dissolution until the cotton fiber is in a transparent light yellow sticky state;
(2) The mass ratio of the prepared glycerin to the sorbitol is 2:1, mixing glycerol and sorbitol in a mass ratio of 15% relative to a cellulose membrane solution system at 90 ℃ under stirring until the mixture is in a flowing state, and blending the mixture with a cellulose solution to obtain a mixed solution;
(3) Pouring the mixed solution into a film making device for film coating, wherein the film making device is used for film coating on a glass plate in a blade mode, and the thickness of the film making device is 750 mu m;
(4) After the scraping, the mixture is placed into ethanol of 500 mL for 30min for organic solvent replacement;
(5) Changing the organic solvent in the step (4), and continuing to replace the organic solvent in the ethanol of 250mL for 8 minutes so that the mass ratio of the residual salt of the cellulose membrane is 24%;
(6) And (3) placing the cellulose film subjected to the organic solvent replacement in the steps (4) and (5) in an environment with the temperature of 15 ℃ and the humidity of 40% for air drying to form the film.
Example 2:
(1) Dissolving 0.8g flax fiber in 70% zinc chloride solution by mass fraction, stirring at a constant speed at 70 ℃ for dissolving until the flax fiber presents a transparent light yellow viscous state;
(2) The mass ratio of the prepared glycerin to the sorbitol is 2:1, mixing glycerol and sorbitol in a mass ratio of 10% relative to a cellulose membrane solution system at 80 ℃ under stirring until the mixture is in a flowing state, and blending the mixture with a cellulose solution to obtain a mixed solution;
(3) Pouring the mixed solution into a film making device for film coating, wherein the film making device is used for film coating on a glass plate in a blade mode, and the thickness of the film making device is 250 mu m;
(4) After the scraping, the mixture is placed into 500 mL organic ethanol for 30min of organic solvent replacement;
(5) Changing the organic solvent in the step (4), and continuing to replace the organic solvent in the ethanol of 250mL for 5 minutes so that the mass ratio of the residual salt of the cellulose membrane is 30%;
(6) And (3) placing the cellulose film subjected to the organic solvent replacement in the steps (4) and (5) in an environment with the temperature of 15 ℃ and the humidity of 40% for air drying to form the film.
Example 3:
(1) Dissolving 0.8g of wood pulp fiber in a ferric chloride solution with the mass fraction of 90%, and uniformly stirring at 90 ℃ to dissolve until the wood pulp fiber is in a transparent light yellow viscous state;
(2) The mass ratio of the prepared glycerin to the sorbitol is 1:1, mixing glycerol and sorbitol in a mass ratio of 15% relative to a cellulose membrane solution system at 90 ℃ under stirring until the mixture is in a flowing state, and blending the mixture with a cellulose solution to obtain a mixed solution;
(3) Pouring the mixed solution into a film making device for film coating, wherein the film making device is used for film coating on a glass plate in a blade mode, and the thickness of the film making device is 500 mu m;
(4) After being scraped, the mixture is placed into 800 and mL ethanol for 40 minutes of organic solvent replacement; so that the mass ratio of the residual salt of the cellulose film is 28%;
(5) And (3) placing the cellulose film subjected to the organic solvent replacement in the step (4) in an environment with the temperature of 20 ℃ and the humidity of 50% for air drying to form a film.
Example 4:
(1) 0.4g of bagasse fiber is dissolved in 70% ferric chloride solution by mass fraction, and is stirred at a constant speed at 70 ℃ for dissolution until the bagasse fiber is in a transparent light yellow viscous state;
(2) The mass ratio of the prepared glycerin to the sorbitol is 2:1, mixing glycerin and sorbitol with a mass ratio of 20% relative to a cellulose film solution system at 70 ℃ under stirring until the mixture is in a flowing state, and blending the mixture with a cellulose solution to obtain a mixed solution;
(3) Pouring the mixed solution into a film making device for film coating, wherein the film making device is used for film coating on a glass plate in a blade mode, and the thickness of the film making device is 200 mu m;
(4) After the scraping, the mixture is placed into ethanol of 500 mL for 30min for organic solvent replacement;
(5) Changing the organic solvent in the step (4), and continuously replacing the organic solvent in 300 mL ethanol for 10min so that the mass ratio of the residual salt of the cellulose membrane is 20%;
(6) And (3) placing the cellulose film subjected to the organic solvent replacement in the steps (4) and (5) in an environment with the temperature of 20 ℃ and the humidity of 40% for air drying to form the film.
Example 5:
(1) 0.6g of cotton fiber is dissolved in a zinc chloride solution with the mass fraction of 90 percent, and is stirred at a constant speed at 90 ℃ to be dissolved until the cotton fiber presents a transparent light yellow sticky state;
(2) The mass ratio of the prepared glycerin to the sorbitol is 2:1, mixing glycerol and sorbitol in a mass ratio of 15% relative to a cellulose membrane solution system at 90 ℃ under stirring until the mixture is in a flowing state, and blending the mixture with a cellulose solution to obtain a mixed solution;
(3) Pouring the mixed solution into a film making device for film coating, wherein the film making device is used for film coating on a glass plate in a blade mode, and the thickness of the film making device is 750 mu m;
(4) After the scraping, the mixture is placed into ethanol of 500 mL for 30min for organic solvent replacement;
(5) Changing the organic solvent in the step (4), and continuing to replace the organic solvent in 400mL ethanol for 5min so that the mass ratio of the residual salt of the cellulose membrane is 20%;
(6) And (3) placing the cellulose film subjected to the organic solvent replacement in the steps (4) and (5) in an environment with the temperature of 15 ℃ and the humidity of 60%, and performing air drying to form the film.
Comparative example 1:
the cellulose membrane of comparative example 1 differs from example 1 in that:
in the step (5), the organic solvent in the step (4) is replaced, and the organic solvent is replaced in 1000 mL ethanol for 30min, namely, the residual salt in the membrane is removed as far as possible, so that the mass ratio of the residual salt in the cellulose membrane is 5%;
other steps and process parameters were the same as in example 1.
Comparative example 2:
the cellulose membrane of comparative example 2 differs from example 1 in that:
in the step (5), the organic solvent in the step (4) is replaced, and the organic solvent is replaced in 800mL ethanol for 30min, namely, the residual salt in the membrane is removed as far as possible, so that the mass ratio of the residual salt in the cellulose membrane is 10%;
other steps and process parameters were the same as in example 1.
Comparative example 3:
the cellulose membrane of comparative example 3 differs from example 1 in that:
in the step (5), the organic solvent in the step (4) is replaced, and the organic solvent is replaced in 500 mL ethanol for 30min, namely, the residual salt in the membrane is removed as far as possible, so that the mass ratio of the residual salt in the cellulose membrane is 15%;
other steps and process parameters were the same as in example 1.
Comparative example 4:
the cellulose membrane of comparative example 4 differs from example 1 in that:
in the step (5), the organic solvent in the step (4) is replaced, and the organic solvent is replaced in 100 mL ethanol for 5min, so that the mass ratio of the residual salt of the cellulose membrane is 40%;
other steps and process parameters were the same as in example 1.
Comparative example 5:
the cellulose membrane of comparative example 4 differs from example 1 in that:
in step (5), the organic solvent of step (4) is not replaced so that the residual salt mass ratio of the cellulose membrane is 45%;
other steps and process parameters were the same as in example 1.
The cellulose films prepared in examples 1 to 5 and comparative examples 1 to 5 are summarized in table 1 below.
TABLE 1
In the above examples, the residual salt is solely referred to as chloride salt, and the residual amount is determined according to the mass loss in thermogravimetric analysis (TGA) by the following calculation method: the difference in the ordinate corresponding to the range of 480-550 degrees celsius of the TGA profile.
The residual salt mass ratio refers to the ratio of the final salt mass to the original added salt mass.
The following sections of the high-toughness, high-transparency heat-sealable cellulose films of this example after bonding were observed using a field emission scanning electron microscope (FE-SEM) and the mechanical properties, transparency, and melting point of the cellulose films were characterized by a universal tester (ASTM), ultraviolet-visible spectrophotometry (UV-vis), and Differential Scanning Calorimeter (DSC) as shown in table 2.
TABLE 2
In Table 1, the volume of the second solvent replacement was within 250mL-400mL and the time was within 5-10min when the replacement solvent continued from examples 1-5; correspondingly, if only one solvent replacement is used, the volume is within 500-800mL, and the time is within 35-40min, so that the residual salt mass ratio of the cellulose film is within 20-30%, and conditions are created for returning the cellulose film to the viscous state of the sol under the heating state to realize thermal bonding. As shown in fig. 1, the layers in the cross-sectional SEM images exhibited compactness from layer to layer, no obvious cracks were seen, indicating excellent adhesion from film to film.
In contrast, comparative examples 1 to 5 showed that the heat-sealable cellulose film of comparative example 1 had a heat-sealable property, as shown in FIG. 2, in which the cellulose film at the hot press was broken by the hot press, and no adhesive mark was found; when the amount of the solvent is controlled so that the residual salt mass ratio is 20% or less (as in comparative examples 1,2 and 3), the effect as a solvent cannot be achieved at a certain temperature due to the low concentration of the residual zinc ions, and when the residual salt mass ratio is 30% or more (as in comparative examples 4 and 5), the film cannot be formed due to excessive residual zinc ions, which cannot be air-dried due to excessive moisture.
As can be seen from Table 2, the test results of the universal tester of examples 1-5 show that the tensile elongation of the cellulose film can reach 50%;
the ultraviolet-visible spectrophotometry test result shows that the transparency of the cellulose film can reach 90%; differential scanning calorimeter test results show that the melting point of cellulose can be reduced to 90 ℃ at the lowest. As shown in fig. 2, the heat-sealable cellulose film of the present embodiment can be bonded and subjected to a certain external force after hot pressing. In comparative examples 1 to 5, however, the tensile elongation was relatively low, and the melting point was not measured, so that the cellulose film at the hot press was broken under the action of the hot press, and no bonding trace was found.
In conclusion, the residual salt-induced high-toughness high-transparency heat-sealable cellulose film provided by the embodiment of the invention not only has the function of realizing heat bonding at relatively low temperature, but also is in a high-toughness high-transparency state, is completely degradable in the environment, is nontoxic and harmless, increases the substitution of the cellulose film to plastics, and also expands the application scenes of the cellulose film in the fields of foods, cosmetics, packaging and the like.
Because of the numerous embodiments of the present invention, the experimental data of each embodiment is huge and not suitable for the one-by-one listing of the descriptions herein, but the content of the verification needed by each embodiment and the final conclusion obtained are close. Therefore, the verification contents of each example are not described one by one, and only examples 1 to 5 are used as representatives to describe the superiority of the present invention.
The foregoing is only illustrative of the preferred embodiments and principles of the present invention, and modifications in specific embodiments will occur to those skilled in the art upon reading the teachings herein, and such modifications are intended to be included within the scope of the invention.
Claims (5)
1. A method for preparing a high-toughness high-transparency heat-sealable cellulose film, comprising the steps of:
(1) Placing plant cellulose into salt solution, stirring and dissolving;
(2) Preparing a plasticizer, and blending the plasticizer with a cellulose solution to obtain a mixed solution;
(3) Pouring the mixed solution into a film making device, and scraping and coating a film on a glass plate;
(4) After blade coating, placing the film into a coagulating bath, carrying out organic solvent replacement, and controlling the mass ratio of residual salt of the cellulose film;
(5) Air-drying the cellulose membrane replaced in the step (4) to form a membrane;
in the step (1), the salt solution is a zinc chloride solution with the mass fraction of 70% -80%;
in the step (2), the plasticizer comprises alcohol with water-retaining effect and alcohol with water-absorbing effect; the alcohol with the water retention effect comprises glycerin, the alcohol with the water absorption effect comprises any one of sorbitol, pentaerythritol and xylitol, the mass ratio of the glycerin to any one of the sorbitol, the pentaerythritol and the xylitol is 1 (0.5-1), and the mass ratio of the sum of the glycerin and the sorbitol to the xylitol is 10-20% relative to the mass ratio of the cellulose solution;
in the step (4), the mass ratio of the residual salt is 20-30%, and the mass ratio of the residual salt refers to the ratio of the mass of the final salt to the mass of the original added salt.
2. The method of making a high tenacity, high transparency, heat sealable cellulosic film according to claim 1, wherein said plant fibers comprise one or more of cotton, flax, wood pulp, bagasse.
3. The method for producing a high-toughness high-transparency heat-sealable cellulose film according to claim 1, wherein the mass ratio of cellulose to solvent in the step (1) is 1 to 2.5% and the temperature is 70 to 90 ℃.
4. The method for producing a high-toughness high-transparency heat-sealable cellulose film according to claim 1, wherein the thickness of the film forming machine in the step (3) is 250 to 750 μm; the coagulating bath in the step (4) adopts any one of ethanol, methanol and acetone, the volume is 500-900 mL, and the time is 35-40 min.
5. The method for producing a high-toughness high-transparency heat-sealable cellulose film according to claim 1, wherein the air-dried film in step (5) has an ambient temperature of 15 to 20 ℃ and a humidity of 40 to 60%.
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