CN114351488B - Composite morphology nano cellulose transparent film based on waste paper and preparation method thereof - Google Patents
Composite morphology nano cellulose transparent film based on waste paper and preparation method thereof Download PDFInfo
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- CN114351488B CN114351488B CN202111508483.2A CN202111508483A CN114351488B CN 114351488 B CN114351488 B CN 114351488B CN 202111508483 A CN202111508483 A CN 202111508483A CN 114351488 B CN114351488 B CN 114351488B
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- 239000010893 paper waste Substances 0.000 title claims abstract description 225
- 229920001046 Nanocellulose Polymers 0.000 title claims abstract description 205
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000008367 deionised water Substances 0.000 claims abstract description 26
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 26
- 239000002761 deinking Substances 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 239000000725 suspension Substances 0.000 claims description 97
- 239000000835 fiber Substances 0.000 claims description 46
- 230000007935 neutral effect Effects 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 31
- 239000012528 membrane Substances 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 29
- 238000010009 beating Methods 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 24
- 229920001131 Pulp (paper) Polymers 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 18
- 238000007664 blowing Methods 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- 238000000967 suction filtration Methods 0.000 claims description 14
- 238000007865 diluting Methods 0.000 claims description 13
- 238000004108 freeze drying Methods 0.000 claims description 13
- 238000007689 inspection Methods 0.000 claims description 11
- 238000002791 soaking Methods 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 11
- 239000002033 PVDF binder Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000007667 floating Methods 0.000 claims description 9
- 239000006260 foam Substances 0.000 claims description 9
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 7
- 239000012634 fragment Substances 0.000 claims description 5
- 238000000502 dialysis Methods 0.000 claims description 2
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000004537 pulping Methods 0.000 claims description 2
- 238000003828 vacuum filtration Methods 0.000 claims description 2
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 16
- 239000001301 oxygen Substances 0.000 abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 abstract description 16
- 230000004888 barrier function Effects 0.000 abstract description 9
- 238000004806 packaging method and process Methods 0.000 abstract description 5
- 229920002678 cellulose Polymers 0.000 description 23
- 239000001913 cellulose Substances 0.000 description 23
- 239000002699 waste material Substances 0.000 description 14
- 239000000123 paper Substances 0.000 description 13
- 238000001914 filtration Methods 0.000 description 12
- 238000001000 micrograph Methods 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 7
- 238000010298 pulverizing process Methods 0.000 description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 6
- 238000004064 recycling Methods 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/64—Paper recycling
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- Polysaccharides And Polysaccharide Derivatives (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention discloses a composite morphology nanocellulose transparent film based on waste paper, which comprises the following components in percentage by weight: 1.59 to 1.97 percent of waste paper, 31.86 to 39.29 percent of deionized water, 0 to 0.38 percent of deinking agent, 58.52 to 66.14 percent of concentrated sulfuric acid with the mass percent of 98 percent, and the sum of the weight percent of the components is 100 percent. The transparent film has higher crystallinity, good thermal performance and oxygen barrier property, and has wide application prospect in the fields of packaging and the like. Also discloses a preparation method of the composite morphology nano cellulose transparent film based on waste paper.
Description
Technical Field
The invention belongs to the fields of recycling of waste materials and extraction and preparation of nano materials, and particularly relates to a composite-morphology nano cellulose transparent film based on waste paper and a preparation method of the composite-morphology nano cellulose transparent film based on waste paper.
Background
The waste paper is produced in excess of four hundred million tons each year worldwide, the waste paper is large in quantity but low in recovery rate, a considerable part of the waste paper is still treated through landfill or incineration, huge pressure is brought to the environment, only about 50% -65% of the waste paper is recovered, the recovery and utilization way is single, most of the waste paper is used for producing recycled paper, the added value of the product is low, and the waste of resources is intangibly caused. Therefore, a new way for realizing the high-quality recycling of waste paper is sought, and the method has important practical significance and social benefit.
The waste paper contains a large amount of cellulose, has the characteristics of rich sources, low price and the like, and is an excellent cellulose resource. Based on the new concept of green development, the waste paper is utilized to produce the nanocellulose with wide application, so that the waste of paper resources can be reduced, the environment is protected, the rationalization and utilization of the resources are realized, and the recycling way of the waste paper is further developed. The film material becomes a hot spot of current research, and the preparation of the film material by taking cellulose as a raw material has good application prospect in the packaging field, plays an important role in production and life, and has important significance for developing green chemistry and promoting sustainable development of human beings.
Disclosure of Invention
The invention aims to provide a composite morphology nanocellulose transparent film based on waste paper, which has higher crystallinity, good thermal performance and oxygen barrier property and has wide application prospect in the fields of packaging and the like.
The second aim of the invention is to provide a preparation method of the nano cellulose transparent film with the composite morphology based on waste paper.
The first technical proposal adopted by the invention is that the composite morphology nano cellulose transparent film based on waste paper,
the coating comprises the following components in percentage by weight: 1.59 to 1.97 percent of waste paper, 31.86 to 39.29 percent of deionized water, 0 to 0.38 percent of deinking agent, 58.52 to 66.14 percent of concentrated sulfuric acid with the mass percent of 98 percent, and the sum of the weight percent of the components is 100 percent.
The second technical scheme adopted by the invention is that the preparation method of the composite morphology nano cellulose transparent film based on waste paper comprises the following steps:
step 1, respectively weighing the following components in parts by weight: 1.59 to 1.97 percent of waste paper, 31.86 to 39.29 percent of deionized water, 0 to 0.38 percent of deinking agent, 58.52 to 66.14 percent of concentrated sulfuric acid with the mass percent of 98 percent, and the sum of the weight percentages of the components is 100 percent;
step 2, preparing waste paper fiber, wherein the specific operation steps are as follows:
step 2.1, crushing waste paper, and adding deionized water and a deinking agent for soaking to obtain waste paper liquid;
step 2.2, pouring the waste paper liquid obtained in the step 2.1 into a beating machine for beating, pouring the waste paper liquid into a standard inspection sieve after beating is finished, flushing the waste paper liquid with water for multiple times, removing floating foam, and draining water to obtain waste paper pulp;
step 2.3, placing the waste paper pulp into a culture dish, and placing the culture dish into an electrothermal blowing drying oven for drying to obtain waste paper cakes;
step 2.4, breaking the dried waste paper cake, and putting the broken waste paper cake into a pulverizer to be broken to obtain waste paper fibers;
step 3, preparing waste paper base nano cellulose, which comprises the following specific operation steps:
step 3.1, diluting 98% by mass of concentrated sulfuric acid to 59% by mass of sulfuric acid;
step 3.2, weighing waste paper fibers, adding diluted sulfuric acid, stirring until the diluted sulfuric acid is dissolved, and stirring the waste paper fibers under the water bath condition to obtain an acidified suspension A;
step 3.3, diluting the suspension A by 10 times, cooling and standing to obtain a suspension B;
step 3.4, carrying out suction filtration and washing on the suspension B, and dialyzing to obtain a neutral nano cellulose suspension;
step 3.5, after ultrasonic dispersion of the neutral nanocellulose suspension, pouring the neutral nanocellulose suspension into a culture dish, and freeze-drying to obtain waste paper-based nanocellulose;
and 4, preparing a waste paper-based nano cellulose transparent film, wherein the specific operation steps are as follows:
step 4.1, adding deionized water into the nanocellulose prepared in the step 3.5 to prepare a nanocellulose suspension, and performing ultrasonic dispersion on the nanocellulose suspension;
step 4.2, carrying out vacuum suction filtration on the nano cellulose suspension by using a sand core filter device to obtain a wet nano cellulose film;
and 4.3, taking down the wet nano cellulose film and the microporous filter membrane together, and drying the wet nano cellulose film and the microporous filter membrane by using an air gun to obtain the nano cellulose transparent film based on the composite morphology of waste paper.
The present invention is also characterized in that,
the deinking agent comprises the following components in percentage by mass: h 2 O 2 ：NaOH：Na 2 SiO 3 ：SDBS：OP-10＝2.8～3.2：0.4～0.5：1.3～1.6：0.35～0.45：0.45～0.55。
In the step 2.1, the waste paper is crushed into fragments with the length of 15mm multiplied by 4mm to 20mm multiplied by 10mm, and the soaking time in deionized water is 20min to 40min; in the step 2.2, the pulping time of the waste paper liquid is 20-40 min, and the standard inspection sieve is 300-350 meshes.
And 2.3, drying the waste paper pulp at 80-90 ℃ for 20-24 hours.
In the step 2.4, the crushing power of the waste paper cake is 1000-1400 w, the crushing times are 2 times, the single crushing time is 20-40 s, and the interval time is 10-15 s.
Step 3.2, the water bath temperature is 40-50 ℃, the stirring rotation speed is 250-290 r/min, and the stirring time is 1h; the standing time in the step 3.3 is 1h; the suction filtration time in the step 3.4 is 1 h-2 h, and the dialysis time is 3 d-4 d.
In the step 3.5, the ultrasonic time is 20-40 min, the freeze drying temperature is-65 ℃ to-55 ℃, and the freeze drying time is 2-3 d.
In the step 4.1, the ultrasonic time is 20-40 min.
In the step 4.2, the vacuum filtration time is 1.5 to 2.5 hours, the filter membrane is made of polyvinylidene fluoride, and the aperture of the filter membrane is 0.22 mu m; and the air gun blow-drying time in the step 4.3 is 20-40 min.
The beneficial effects of the invention are as follows:
the nano cellulose film prepared by the invention has regular composite morphology in microcosmic, namely nano-sized fibers are arranged in an orientation way at the middle part of the film and are randomly arranged along the edge; nanocellulose has a high crystallinity. Macroscopically, the nanocellulose film presents certain transparency, and does not depend on the paper type and whether deinking is performed; in addition, the nano cellulose film has good heat stability and oxygen barrier property. In conclusion, the invention takes waste paper as a raw material, adopts a simple preparation process and lower preparation cost, prepares the nano cellulose transparent film with composite morphology, has higher crystallinity, good thermal performance and oxygen barrier performance, has wide application prospect in the fields of packaging and the like, realizes the recycling of waste paper, obtains a new product with higher added value, and creates economic benefit and environmental benefit.
Drawings
FIG. 1 is a schematic view of a nanocellulose film prepared in example 1 of the present invention;
FIG. 2 is a schematic view of a nanocellulose film prepared in example 2 of the present invention;
FIG. 3 is a schematic view of a nanocellulose film prepared in example 3 of the present invention;
FIG. 4 is a schematic view of a nanocellulose film prepared in example 4 of the present invention;
FIG. 5 is a schematic view of a nanocellulose film prepared in example 5 of the present invention;
FIG. 6 is a schematic view of a nanocellulose film prepared in example 6 of the present invention;
FIG. 7 is a scanning electron microscope image of the center of the nanocellulose transparent film prepared in example 1 of the present invention;
FIG. 8 is a scanning electron microscope image of the edge of the nanocellulose transparent film prepared in example 1 of the present invention;
FIG. 9 is a scanning electron microscope image of the center of the nanocellulose transparent film prepared in example 2 of the present invention;
FIG. 10 is a scanning electron microscope image of the edge of the nanocellulose transparent film prepared in example 2 of the present invention;
FIG. 11 is a scanning electron microscope image of the center of the nanocellulose transparent film prepared in example 3 of the present invention;
FIG. 12 is a scanning electron microscope image of the edge of the nanocellulose transparent film prepared in example 3 of the present invention.
FIG. 13 is a scanning electron microscope image of the center of the nanocellulose transparent film prepared in example 4 of the present invention;
FIG. 14 is a scanning electron microscope image of the edge of the nanocellulose transparent film prepared in example 4 of the present invention;
FIG. 15 is a scanning electron microscope image of the center of the nanocellulose transparent film prepared in example 5 of the present invention;
FIG. 16 is a scanning electron microscope image of the edge of the nanocellulose transparent film prepared in example 5 of the present invention;
FIG. 17 is a scanning electron microscope image of the center of the nanocellulose transparent film prepared in example 6 of the present invention;
FIG. 18 is a scanning electron microscope image of the edge of the nanocellulose transparent film prepared in example 6 of the present invention.
FIG. 19 is a graph showing the transmittance of the nanocellulose films prepared in examples 1, 2, and 3 of the present invention, showing that the nanocellulose films prepared have certain transparency;
FIG. 20 is a TG pattern of nanocellulose films prepared in examples 3, 4, and 5 of the present invention;
FIG. 21 is a graph showing the oxygen transmission rate of nanocellulose films prepared in examples 1, 2, and 3 of the present invention.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
The invention provides a composite morphology nanocellulose transparent film based on waste paper, which comprises the following raw material components in percentage by weight: 1.59 to 1.97 percent of waste paper, 31.86 to 39.29 percent of deionized water, 0 to 0.38 percent of deinking agent, 58.52 to 66.14 percent of concentrated sulfuric acid with the mass percent of 98 percent, and the sum of the weight percent of the components is 100 percent.
The invention also provides a preparation method of the composite morphology nanocellulose transparent film based on waste paper, which comprises the following steps:
step 1, respectively weighing the following components in parts by weight: 1.59 to 1.97 percent of office waste paper, 31.86 to 39.29 percent of deionized water, 0 to 0.38 percent of deinking agent, 58.52 to 66.14 percent of concentrated sulfuric acid with the mass percent of 98 percent, and the sum of the weight percentages of the components is 100 percent;
the deinking agent in the step 1 comprises the following components in percentage by mass: h 2 O 2 ：NaOH：Na 2 SiO 3 ：SDBS：OP-10＝2.8～3.2：0.4～0.5：1.3～1.6：0.35～0.45：0.45～0.55。
Step 2, preparing waste paper fiber, wherein the specific operation steps are as follows:
step 2.1, crushing waste paper into fragments of 15mm multiplied by 4mm multiplied by 20mm multiplied by 10mm, adding deionized water and a deinking agent, and soaking for 20min to 40min to obtain waste paper liquid;
2.2, pouring the waste paper liquid obtained in the step 2.1 into a beating machine for beating for 20-40 min, pouring the waste paper liquid into a standard inspection sieve with 300-350 meshes after beating, washing with water for multiple times to remove floating foam, and draining water to obtain waste paper pulp;
step 2.3, placing the waste paper pulp into a culture dish, placing the culture dish into an electrothermal blowing drying box, and drying the waste paper pulp at 80-90 ℃ for 20-24 hours to obtain waste paper cakes;
step 2.4, breaking the dried waste paper cake, putting the broken waste paper cake into a pulverizer, pulverizing the waste paper cake for 2 times at 1000-1400 w, and breaking the waste paper cake at intervals of 10-15 s for 20-40 s each time to obtain waste paper fibers;
step 3, preparing waste paper base nano cellulose, which comprises the following specific operation steps:
step 3.1, diluting 98% concentrated sulfuric acid to 59% concentration sulfuric acid by mass fraction;
step 3.2, adding diluted sulfuric acid into the waste paper fiber obtained in the step 2, stirring until the diluted sulfuric acid is dissolved, heating the waste paper fiber in a water bath, and stirring the waste paper fiber for 1h to obtain an acidified suspension A; wherein the water bath temperature is 40-50 ℃, and the stirring rotation speed is 250-290 r/min;
3.3, diluting the suspension A by 10 times, cooling and standing for 1h to obtain a suspension B;
step 3.4, carrying out suction filtration and washing on the suspension B for 1-2 h, and dialyzing for 3-4 d to obtain neutral nanocellulose suspension;
3.5, after ultrasonic dispersion of the neutral nanocellulose suspension for 20-40 min, pouring the neutral nanocellulose suspension into a culture dish, and freeze-drying the neutral nanocellulose suspension for 2-3 d at the temperature of-65 ℃ to-55 ℃ to obtain waste paper-based nanocellulose;
and 4, preparing a waste paper-based nano cellulose transparent film, wherein the specific operation steps are as follows:
step 4.1, preparing nano cellulose prepared in the step 3.5 into nano cellulose suspension, and performing ultrasonic dispersion on the nano cellulose suspension for 20-40 min;
step 4.2, vacuum filtering the nano cellulose suspension for 1.5-2.5 hours by using a sand core filtering device and a polyvinylidene fluoride filter membrane with the pore diameter of 0.22 mu m to obtain a wet nano cellulose film;
and 4.3, taking down the wet nano cellulose film and the microporous filter membrane together, blowing for 20-40 min by using an air gun, and separating the nano cellulose film from the microporous filter membrane to finally obtain the composite-morphology nano cellulose transparent film based on waste paper.
Wherein: waste paper, collected waste A4 paper (no ink, ink), waste corrugated paper (no ink, ink), waste white cardboard (no ink, ink); 98% sulfuric acid (H) 2 SO 4 ) Analytically pure, tianjin, tianli chemical reagent Co., ltd; deionized water, analytically pure, dongguan, a water treatment facility, inc.; the deinking agent comprises the following components: hydrogen peroxide (H) 2 O 2 ) Analytically pure, rich and refined chemical industry Co., tianjin; sodium hydroxide (NaOH), analytically pure, tianjin chemical reagent limited; sodium silicate (Na) 2 SiO 3 ) Analytically pure, tianjin, tianli chemical reagent Co., ltd; sodium Dodecyl Benzene Sulfonate (SDBS), analytically pure, tianjin, astrochemical agents limited; OP-10, analytically pure, sangjingsheng, inc.
Example 1
The preparation method of the composite morphology nano cellulose transparent film based on the waste paper comprises the following steps:
step 1, respectively weighing the following components in parts by weight: 1.59% of waste inkless A4 paper, 32.27% of deionized water, 0% of deinking agent and 66.14% of 98% of concentrated sulfuric acid, wherein the sum of the weight percentages of the components is 100%;
step 2, preparing waste paper fiber, wherein the specific operation steps are as follows:
step 2.1, crushing waste paper into pieces of 20mm multiplied by 10mm, adding deionized water, and soaking for 40min to obtain waste paper liquid;
step 2.2, pouring the waste paper liquid obtained in the step 2.1 into a beating machine for beating for 40min, pouring the waste paper liquid into a 325-mesh standard inspection sieve after beating, washing with water for multiple times to remove floating foam, and draining water to obtain waste paper pulp;
step 2.3, placing the waste paper pulp into a culture dish, placing the culture dish into an electrothermal blowing drying box, and drying the culture dish at 80 ℃ for 24 hours to obtain waste paper cakes;
step 2.4, breaking the dried waste paper cake, putting the broken waste paper cake into a pulverizer, pulverizing the waste paper cake for 2 times at 1000w for 40s each time, and breaking the waste paper cake at intervals of 10s to obtain waste paper fibers;
step 3, preparing waste paper base nano cellulose, which comprises the following specific operation steps:
step 3.1, diluting 98% concentrated sulfuric acid to 59% concentration sulfuric acid by mass fraction;
step 3.2, adding diluted sulfuric acid into the waste paper fiber obtained in the step 2, stirring until the diluted sulfuric acid is dissolved, heating the waste paper fiber in a water bath, and stirring the waste paper fiber for 1h to obtain an acidified suspension A; wherein the water bath temperature is 40 ℃, and the stirring rotation speed is 290r/min;
3.3, diluting the suspension A by 10 times, cooling and standing for 1h to obtain a suspension B;
step 3.4, carrying out suction filtration and washing on the suspension B for 2 hours, and dialyzing for 3 days to obtain a neutral nanocellulose suspension;
step 3.5, after ultrasonic dispersion of the neutral nanocellulose suspension for 20min, pouring the neutral nanocellulose suspension into a culture dish, and freeze-drying the neutral nanocellulose suspension for 3d at the temperature of minus 60 ℃ to obtain waste paper-based nanocellulose;
and 4, preparing a waste paper-based nano cellulose transparent film, wherein the specific operation steps are as follows:
step 4.1, preparing nano-cellulose prepared in the step 3.5 into nano-cellulose suspension, and performing ultrasonic dispersion on the nano-cellulose suspension for 20min;
step 4.2, using a sand core filter device, and using a polyvinylidene fluoride filter membrane with the aperture of 0.22 mu m in the sand core filter device to carry out vacuum suction filtration on the nano cellulose suspension for 2 hours to obtain a wet nano cellulose film;
and 4.3, taking down the wet nano cellulose film and the microporous filter membrane together, blowing for 30min by using an air gun, and separating the nano cellulose film from the microporous filter membrane to finally obtain the nano cellulose transparent film with the composite morphology based on waste paper.
From fig. 1 and 19, it can be seen that the nanocellulose film has a certain transparency; as can be seen from fig. 7 and 8, the middle part and the edge of the nanocellulose film have different microscopic morphologies, the middle part is arranged in a certain orientation, and the edges are randomly arranged, namely the composite morphology with regularity; from FIG. 21, it can be seen that the nanocellulose film has an oxygen transmission of 1.54.10 -3 /cm 3 ·mm/m 2 D KPa has high oxygen barrier property.
Example 2
A preparation method of a composite morphology nano cellulose transparent film based on waste paper comprises the following steps:
step 1, respectively weighing the following components in parts by weight: 1.63% of waste ink A4 paper, 32.66% of deionized water, 0.38% of deinking agent and 65.33% of 98% of concentrated sulfuric acid, wherein the sum of the weight percentages of the components is 100%; wherein the deinking agent comprises the following components in percentage by mass: h 2 O 2 ：NaOH：Na 2 SiO 3 ：SDBS：OP-10＝2.8：0.4：1.3：0.35：0.45。
Step 2, preparing waste paper fiber, wherein the specific operation steps are as follows:
step 2.1, crushing waste paper into pieces with the size of 18mm multiplied by 8mm, adding deionized water and a deinking agent, and soaking for 30min to obtain waste paper liquid;
step 2.2, pouring the waste paper liquid obtained in the step 2.1 into a beating machine for beating for 30min, pouring the waste paper liquid into a 325-mesh standard inspection sieve after beating, washing with water for multiple times to remove floating foam, and draining water to obtain waste paper pulp;
step 2.3, placing the waste paper pulp into a culture dish, placing the culture dish into an electrothermal blowing drying box, and drying the culture dish at 80 ℃ for 24 hours to obtain waste paper cakes;
step 2.4, breaking the dried waste paper cake, putting the broken waste paper cake into a pulverizer, pulverizing the waste paper cake for 2 times under 1200w for 30s each time, and breaking the waste paper cake at intervals of 10s to obtain waste paper fibers;
step 3, preparing waste paper base nano cellulose, which comprises the following specific operation steps:
step 3.1, 98% concentrated sulfuric acid is diluted to 59% concentration;
step 3.2, adding diluted sulfuric acid into the waste paper fiber obtained in the step 2, stirring until the diluted sulfuric acid is dissolved, heating the waste paper fiber in a water bath, and stirring the waste paper fiber for 1h to obtain an acidified suspension A; wherein the water bath temperature is 45 ℃, and the stirring rotation speed is 270r/min;
3.3, diluting the suspension A by 10 times, cooling and standing for 1h to obtain a suspension B;
step 3.4, carrying out suction filtration and washing on the suspension B for 2 hours, and dialyzing for 3 days to obtain a neutral nanocellulose suspension;
step 3.5, after ultrasonic dispersion of the neutral nanocellulose suspension for 30min, pouring the neutral nanocellulose suspension into a culture dish, and freeze-drying the neutral nanocellulose suspension for 3d at the temperature of minus 60 ℃ to obtain waste paper-based nanocellulose;
and 4, preparing a waste paper-based nano cellulose transparent film, wherein the specific operation steps are as follows:
step 4.1, preparing nano-cellulose prepared in the step 3.5 into nano-cellulose suspension, and performing ultrasonic dispersion on the nano-cellulose suspension for 30min;
step 4.2, vacuum filtering the nano cellulose suspension for 2 hours by using a sand core filtering device and a polyvinylidene fluoride filter membrane with the pore diameter of 0.22 mu m to obtain a wet nano cellulose film;
and 4.3, taking down the wet nano cellulose film and the microporous filter membrane together, blowing for 30min by using an air gun, and separating the nano cellulose film from the microporous filter membrane to finally obtain the nano cellulose transparent film with the composite morphology based on waste paper.
From fig. 2 and 19, it can be seen that the nanocellulose film has a certain transparency; from fig. 9 and 10, it is possible toThe micro-morphology of the middle part and the edge of the nano cellulose film are different, the middle part is arranged in a certain orientation, and the edges are randomly arranged, namely the regular composite morphology is realized; from FIG. 21, it can be seen that the nanocellulose film has an oxygen transmission of 5.608.10 -3 /cm 3 ·mm/m 2 D KPa has high oxygen barrier property.
Example 3
A preparation method of a composite morphology nano cellulose transparent film based on waste paper comprises the following steps:
step 1, respectively weighing the following components in parts by weight: 1.79% of waste ink A4 paper, 35.41% of deionized water, 0% of deinking agent and 62.80% of 98% of concentrated sulfuric acid by mass percent, wherein the sum of the weight percentages of the components is 100%;
step 2, preparing waste paper fiber, wherein the specific operation steps are as follows:
step 2.1, crushing waste paper into fragments of 15mm multiplied by 4mm, adding deionized water, and soaking for 20min to obtain waste paper liquid;
step 2.2, pouring the waste paper liquid obtained in the step 2.1 into a beating machine for beating for 20min, pouring the waste paper liquid into a 325-mesh standard inspection sieve after beating, washing with water for multiple times to remove floating foam, and draining water to obtain waste paper pulp;
step 2.3, placing the waste paper pulp into a culture dish, placing the culture dish into an electrothermal blowing drying box, and drying the culture dish at 80 ℃ for 24 hours to obtain waste paper cakes;
step 2.4, breaking the dried waste paper cake, putting the broken waste paper cake into a pulverizer, pulverizing the waste paper cake for 2 times at 1400w for 20s each time at intervals of 10s, and breaking the waste paper cake to obtain waste paper fibers;
step 3, preparing waste paper base nano cellulose, which comprises the following specific operation steps:
step 3.1, 98% concentrated sulfuric acid is diluted to 59% concentration;
step 3.2, adding diluted sulfuric acid into the waste paper fiber obtained in the step 2, stirring until the diluted sulfuric acid is dissolved, heating the waste paper fiber in a water bath, and stirring the waste paper fiber for 1h to obtain an acidified suspension A; wherein the water bath temperature is 50 ℃, and the stirring rotation speed is 250r/min;
3.3, diluting the suspension A by 10 times, cooling and standing for 1h to obtain a suspension B;
step 3.4, carrying out suction filtration and washing on the suspension B for 2 hours, and dialyzing 3 to obtain a neutral nano cellulose suspension;
step 3.5, after ultrasonic dispersion of the neutral nanocellulose suspension for 40min, pouring the neutral nanocellulose suspension into a culture dish, and freeze-drying the neutral nanocellulose suspension for 3d at the temperature of minus 60 ℃ to obtain waste paper-based nanocellulose;
and 4, preparing a waste paper-based nano cellulose transparent film, wherein the specific operation steps are as follows:
step 4.1, preparing nano-cellulose prepared in the step 3.5 into nano-cellulose suspension, and performing ultrasonic dispersion on the nano-cellulose suspension for 40min;
step 4.2, vacuum filtering the nano cellulose suspension for 2 hours by using a sand core filtering device and a polyvinylidene fluoride filter membrane with the pore diameter of 0.22 mu m to obtain a wet nano cellulose film;
and 4.3, taking down the wet nano cellulose film and the microporous filter membrane together, blowing for 30min by using an air gun, and separating the nano cellulose film from the microporous filter membrane to finally obtain the nano cellulose transparent film with the composite morphology based on waste paper.
It can be seen from fig. 3 and 19 that the nanocellulose film has a certain transparency; as can be seen from fig. 11 and fig. 12, the middle part and the edge of the nanocellulose film have different microscopic morphologies, the middle part is arranged in a certain orientation, and the edges are randomly arranged, namely, the nanocellulose film has a regular composite morphology; the calculation shows that the nano cellulose has higher crystallinity of 43%; from fig. 20, it can be seen that the nanocellulose film has better thermal stability, and the nanocellulose begins to thermally decompose from 143 ℃; from FIG. 21, it can be seen that the nanocellulose film has an oxygen transmission of 40.448.10 -3 /cm 3 ·mm/m 2 d.KPa, has higher oxygen barrier property.
Example 4
A preparation method of a composite morphology nano cellulose transparent film based on waste paper comprises the following steps:
step 1, respectively weighing the following components in parts by weight: 1.86% of waste black white cardboard, 37.25% of deionized water, 0% of deinking agent and 60.89% of 98% of concentrated sulfuric acid, wherein the sum of the weight percentages of the components is 100%;
step 2, preparing waste paper fiber, wherein the specific operation steps are as follows:
step 2.1, crushing waste paper into pieces of 20mm multiplied by 10mm, adding deionized water, and soaking for 40min to obtain waste paper liquid;
step 2.2, pouring the waste paper liquid obtained in the step 2.1 into a beating machine for beating for 40min, pouring the waste paper liquid into a 325-mesh standard inspection sieve after beating, washing with water for multiple times to remove floating foam, and draining water to obtain waste paper pulp;
step 2.3, placing the waste paper pulp into a culture dish, placing the culture dish into an electrothermal blowing drying box, and drying the culture dish at 80 ℃ for 24 hours to obtain waste paper cakes;
step 2.4, breaking the dried waste paper cake, putting the broken waste paper cake into a multi-functional pulverizer, pulverizing the waste paper cake for 2 times at 1000w for 40s each time at intervals of 10s, and breaking the waste paper cake to obtain waste paper fibers;
step 3, preparing waste paper base nano cellulose, which comprises the following specific operation steps:
step 3.1, 98% concentrated sulfuric acid is diluted to 59% concentration;
step 3.2, adding diluted sulfuric acid into the waste paper fiber obtained in the step 2, stirring until the diluted sulfuric acid is dissolved, heating the waste paper fiber in a water bath, and stirring the waste paper fiber for 1h to obtain an acidified suspension A; wherein the water bath temperature is 40 ℃, and the stirring rotation speed is 290r/min;
3.3, diluting the suspension A by 10 times, cooling and standing for 1h to obtain a suspension B;
step 3.4, carrying out suction filtration and washing on the suspension B for 2 hours, and dialyzing for 3 days to obtain a neutral nanocellulose suspension;
step 3.5, after ultrasonic dispersion of the neutral nanocellulose suspension for 20min, pouring the neutral nanocellulose suspension into a culture dish, and freeze-drying the neutral nanocellulose suspension for 3d at the temperature of minus 60 ℃ to obtain waste paper-based nanocellulose;
and 4, preparing a waste paper-based nano cellulose transparent film, wherein the specific operation steps are as follows:
step 4.1, preparing nano-cellulose prepared in the step 3.5 into nano-cellulose suspension, and performing ultrasonic dispersion on the nano-cellulose suspension for 20min;
step 4.2, vacuum filtering the nano cellulose suspension for 2 hours by using a sand core filtering device and a polyvinylidene fluoride filter membrane with the pore diameter of 0.22 mu m to obtain a wet nano cellulose film;
and 4.3, taking down the wet nano cellulose film and the microporous filter membrane together, blowing for 30min by using an air gun, and separating the nano cellulose film from the microporous filter membrane to finally obtain the nano cellulose transparent film with the composite morphology based on waste paper. It can be seen from fig. 4 and 19 that the nanocellulose film has a certain transparency; as can be seen from fig. 13 and 14, the middle part and the edge of the nanocellulose film have different microscopic morphologies, the middle part is arranged in a certain orientation, and the edges are randomly arranged, namely the composite morphology with regularity; the calculation shows that the nano cellulose has higher crystallinity of 35 percent; from fig. 20, it can be seen that the nanocellulose film has better thermal stability, and the nanocellulose starts to thermally decompose from 207 ℃.
Example 5
A preparation method of a composite morphology nano cellulose transparent film based on waste paper comprises the following steps:
step 1, respectively weighing the following components in parts by weight: 1.91% of waste ink corrugated paper, 38.73% of deionized water, 0% of deinking agent, 59.36% of 98% of concentrated sulfuric acid, wherein the sum of the weight percentages of the components is 100%;
step 2, preparing waste paper fiber, wherein the specific operation steps are as follows:
step 2.1, crushing waste paper into pieces with the size of 18mm multiplied by 8mm, adding deionized water, and soaking for 30min to obtain waste paper liquid;
step 2.2, pouring the waste paper liquid obtained in the step 2.1 into a beating machine for beating for 30min, pouring the waste paper liquid into a 325-mesh standard inspection sieve after beating, washing with water for multiple times to remove floating foam, and draining water to obtain waste paper pulp;
step 2.3, placing the waste paper pulp into a culture dish, placing the culture dish into an electrothermal blowing drying box, and drying the culture dish at 80 ℃ for 24 hours to obtain waste paper cakes;
step 2.4, breaking the dried waste paper cake, putting the broken waste paper cake into a pulverizer, pulverizing the waste paper cake for 2 times under 1200w for 30s each time, and breaking the waste paper cake at intervals of 10s to obtain waste paper fibers;
step 3, preparing waste paper base nano cellulose, which comprises the following specific operation steps:
step 3.1, 98% concentrated sulfuric acid is diluted to 59% concentration;
step 3.2, adding diluted sulfuric acid into the waste paper fiber obtained in the step 2, stirring until the diluted sulfuric acid is dissolved, heating the waste paper fiber in a water bath, and stirring the waste paper fiber for 1h to obtain an acidified suspension A; wherein the water bath temperature is 45 ℃, and the stirring rotation speed is 270r/min;
3.3, diluting the suspension A by 10 times, cooling and standing for 1h to obtain a suspension B;
step 3.4, carrying out suction filtration and washing on the suspension B for 2 hours, and dialyzing for 3 days to obtain a neutral nanocellulose suspension;
step 3.5, after ultrasonic dispersion of the neutral nanocellulose suspension for 30min, pouring the neutral nanocellulose suspension into a culture dish, and freeze-drying the neutral nanocellulose suspension for 3d at the temperature of minus 60 ℃ to obtain waste paper-based nanocellulose;
and 4, preparing a waste paper-based nano cellulose transparent film, wherein the specific operation steps are as follows:
step 4.1, preparing nano-cellulose prepared in the step 3.5 into nano-cellulose suspension, and performing ultrasonic dispersion on the nano-cellulose suspension for 30min;
step 4.2, vacuum filtering the nano cellulose suspension for 2 hours by using a sand core filtering device and a polyvinylidene fluoride filter membrane with the pore diameter of 0.22 mu m to obtain a wet nano cellulose film;
and 4.3, taking down the wet nano cellulose film and the microporous filter membrane together, blowing for 30min by using an air gun, and separating the nano cellulose film from the microporous filter membrane to finally obtain the nano cellulose transparent film with the composite morphology based on waste paper.
It can be seen from fig. 5 and 19 that the nanocellulose film has a certain transparency; as can be seen from fig. 15 and fig. 16, the middle part and the edge of the nanocellulose film have different microscopic morphologies, the middle part is arranged in a certain orientation, and the edges are randomly arranged, namely, the nanocellulose film has a regular composite morphology; as can be seen from fig. 20, the nanocellulose film has better thermal stability, and nanocellulose starts to thermally decompose from 174 ℃.
Example 6
A preparation method of a composite morphology nano cellulose transparent film based on waste paper comprises the following steps:
step 1, respectively weighing the following components in parts by weight: 1.88% of waste ink corrugated paper, 39.29% of deionized water, 0.31% of deinking agent and 58.52% of 98% of concentrated sulfuric acid, wherein the sum of the weight percentages of the components is 100%; wherein the mass ratio of each component in the deinking agent is as follows: h 2 O 2 ：NaOH：Na 2 SiO 3 ：SDBS：OP-10＝3.2：0.5：1.6：0.45：0.55。
Step 2, preparing waste paper fiber, wherein the specific operation steps are as follows:
step 2.1, crushing waste paper into fragments of 15mm multiplied by 4mm, adding deionized water and a deinking agent, and soaking for 20min to obtain waste paper liquid;
step 2.2, pouring the waste paper liquid obtained in the step 2.1 into a beating machine for beating for 20min, pouring the waste paper liquid into a 325-mesh standard inspection sieve after beating, washing with water for multiple times to remove floating foam, and draining water to obtain waste paper pulp;
step 2.3, placing the waste paper pulp into a culture dish, placing the culture dish into an electrothermal blowing drying box, and drying the culture dish at 80 ℃ for 24 hours to obtain waste paper cakes;
step 2.4, breaking the dried waste paper cake, putting the broken waste paper cake into a pulverizer, pulverizing the waste paper cake for 2 times at 1400w for 20s each time at intervals of 10s, and breaking the waste paper cake to obtain waste paper fibers;
step 3, preparing waste paper base nano cellulose, which comprises the following specific operation steps:
step 3.1, 98% concentrated sulfuric acid is diluted to 59% concentration;
step 3.2, adding diluted sulfuric acid into the waste paper fiber obtained in the step 2, stirring until the diluted sulfuric acid is dissolved, heating the waste paper fiber in a water bath, and stirring the waste paper fiber for 1h to obtain an acidified suspension A; wherein the water bath temperature is 50 ℃, and the stirring rotation speed is 250r/min;
3.3, diluting the suspension A by 10 times, cooling and standing for 1h to obtain a suspension B;
step 3.4, carrying out suction filtration and washing on the suspension B for 2 hours, and dialyzing for 3 days to obtain a neutral nanocellulose suspension;
step 3.5, after ultrasonic dispersion of the neutral nanocellulose suspension for 40min, pouring the neutral nanocellulose suspension into a culture dish, and freeze-drying the neutral nanocellulose suspension for 3d at the temperature of minus 60 ℃ to obtain waste paper-based nanocellulose;
and 4, preparing a waste paper-based nano cellulose transparent film, wherein the specific operation steps are as follows:
step 4.1, preparing nano-cellulose prepared in the step 3.5 into nano-cellulose suspension, and performing ultrasonic dispersion on the nano-cellulose suspension for 40min;
step 4.2, vacuum filtering the nano cellulose suspension for 2 hours by using a sand core filtering device and a polyvinylidene fluoride filter membrane with the pore diameter of 0.22 mu m to obtain a wet nano cellulose film;
and 4.3, taking down the wet nano cellulose film and the microporous filter membrane together, blowing for 30min by using an air gun, and separating the nano cellulose film from the microporous filter membrane to finally obtain the nano cellulose transparent film with the composite morphology based on waste paper. It can be seen from fig. 6 and 19 that the nanocellulose film has a certain transparency; as can be seen from fig. 17 and fig. 18, the middle part and the edge of the nanocellulose film have different microscopic morphologies, the middle part is arranged in a certain orientation, and the edges are randomly arranged, namely, the nanocellulose film has a regular composite morphology; the calculation shows that the nano cellulose has higher crystallinity of 61 percent.
It was found that the nanocellulose transparent films can be prepared in examples 1 to 6. In order to further understand the morphology structure, microscopic observation is carried out on the films prepared in the examples 1 to 6 by using a field emission scanning electron microscope, and the obtained cellulose is in a short rod structure, the diameter is 20nm to 50nm, the length is 100nm to 400nm, the nano-size is in nano-size, the orientation of the nano-size cellulose is strong in the middle part of the film, and the edge parts are randomly arranged;the crystallinity of the nanocellulose film is calculated, so that the nanocellulose can be obtained to have higher crystallinity, wherein the crystallinity of the nanocellulose prepared by using waste corrugated paper can reach 61%; the thermal gravimetric analysis is carried out on the nano cellulose film, and according to a TG graph, the thermal stability of the nano cellulose film is good, wherein the thermal decomposition temperature of the nano cellulose prepared from the waste white cardboard is up to 207 ℃; the oxygen transmittance of the nano cellulose film is detected, and according to the oxygen transmittance graph, the nano cellulose film has higher oxygen barrier property, wherein the minimum oxygen transmittance of the nano cellulose film prepared by discarding A4 paper is 1.548.10 -3 /cm 3 ·mm/m 2 ·d·KPa。
The nanocellulose film based on the waste paper prepared by the invention has the following characteristics: microcosmically, the nano cellulose film has regular composite morphology, namely the nano-scale fibers are arranged in an orientation way at the middle part of the film, and the edges of the nano-scale fibers are randomly arranged; nanocellulose has a high crystallinity. Macroscopic, the nano cellulose film has certain transparency without depending on paper types and deinking or not, so that the process flow can be simplified and the production cost can be reduced; in addition, the nano cellulose film has good thermal stability and oxygen barrier property, and has wide application prospect in the fields of packaging and the like. In summary, the invention provides the preparation method of the nanocellulose transparent film based on the composite morphology of the waste paper, which not only realizes the recycling of the waste paper, but also obtains products with higher added value through a simple preparation process and lower preparation cost, and creates economic benefit and environmental benefit.
Claims (1)
1. The preparation method of the composite morphology nano cellulose transparent film based on the waste paper is characterized by comprising the following steps of:
step 1, respectively weighing the following components in parts by weight: 1.59 to 1.97 percent of waste paper, 31.86 to 39.29 percent of deionized water, 0 to 0.38 percent of deinking agent, 58.52 to 66.14 percent of concentrated sulfuric acid with the mass percent of 98 percent, and the sum of the weight percentages of the components is 100 percent;
each group of deinking agent in the step 1The mass ratio of the components is as follows: h 2 O 2 ：NaOH：Na 2 SiO 3 ：SDBS：OP-10=2.8～3.2：0.4～0.5：1.3～1.6：0.35～0.45：0.45～0.55；
Step 2, preparing waste paper fiber, wherein the specific operation steps are as follows:
step 2.1, crushing waste paper, and adding deionized water and a deinking agent for soaking to obtain waste paper liquid;
the waste paper in the step 2.1 is crushed into fragments with the length of 15mm multiplied by 4mm multiplied by 20mm multiplied by 10mm, and the soaking time in deionized water is 20min to 40min;
step 2.2, pouring the waste paper liquid obtained in the step 2.1 into a beating machine for beating, pouring the waste paper liquid into a standard inspection sieve after beating is finished, flushing the waste paper liquid with water for multiple times, removing floating foam, and draining water to obtain waste paper pulp;
in the step 2.2, the pulping time of the waste paper liquid is 20-40 min, and the standard inspection sieve is 300-350 meshes;
step 2.3, placing the waste paper pulp into a culture dish, and placing the culture dish into an electrothermal blowing drying oven for drying to obtain waste paper cakes;
the drying temperature of the waste paper pulp in the step 2.3 is 80-90 ℃ and the drying time is 20-24 hours;
step 2.4, breaking the dried waste paper cake, and putting the broken waste paper cake into a pulverizer to be broken to obtain waste paper fibers;
in the step 2.4, the crushing power of the waste paper cake is 1000 w-1400 w, the crushing times are 2 times, the single crushing time is 20 s-40 s, and the interval time is 10 s-15 s;
step 3, preparing waste paper base nano cellulose, which comprises the following specific operation steps:
step 3.1, diluting 98% by mass of concentrated sulfuric acid to 59% by mass of sulfuric acid;
step 3.2, weighing waste paper fibers, adding diluted sulfuric acid, stirring until the diluted sulfuric acid is dissolved, and stirring the waste paper fibers under the water bath condition to obtain an acidified suspension A;
the water bath temperature in the step 3.2 is 40-50 ℃, the stirring rotation speed is 250-290 r/min, and the stirring time is 1h;
step 3.3, diluting the suspension A by 10 times, cooling and standing to obtain a suspension B;
the standing time in the step 3.3 is 1h;
step 3.4, carrying out suction filtration and washing on the suspension B, and dialyzing to obtain a neutral nano cellulose suspension;
the suction filtration time in the step 3.4 is 1 h-2 h, and the dialysis time is 3 d-4 d;
step 3.5, after ultrasonic dispersion of the neutral nanocellulose suspension, pouring the neutral nanocellulose suspension into a culture dish, and freeze-drying to obtain waste paper-based nanocellulose;
the ultrasonic time in the step 3.5 is 20-40 min, the freeze-drying temperature is-65-55 ℃, and the freeze-drying time is 2-3 d;
and 4, preparing a waste paper-based nano cellulose transparent film, wherein the specific operation steps are as follows:
step 4.1, adding deionized water into the nanocellulose prepared in the step 3.5 to prepare a nanocellulose suspension, and performing ultrasonic dispersion on the nanocellulose suspension;
the ultrasonic time in the step 4.1 is 20-40 min;
step 4.2, carrying out vacuum suction filtration on the nano cellulose suspension by using a sand core filter device to obtain a wet nano cellulose film;
the vacuum filtration time in the step 4.2 is 1.5-2.5 hours, the filter membrane is made of polyvinylidene fluoride, and the pore diameter of the filter membrane is 0.22 mu m;
and 4.3, taking down the wet nano cellulose film and the microporous filter membrane, drying the wet nano cellulose film and the microporous filter membrane by using an air gun, wherein the drying time of the air gun is 20-40 min, and finally obtaining the composite morphology nano cellulose transparent film based on waste paper.
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