CN102936353B - Method for preparing high air tightness antibacterial reinforced membrane by using straws - Google Patents
Method for preparing high air tightness antibacterial reinforced membrane by using straws Download PDFInfo
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- CN102936353B CN102936353B CN201210388060.6A CN201210388060A CN102936353B CN 102936353 B CN102936353 B CN 102936353B CN 201210388060 A CN201210388060 A CN 201210388060A CN 102936353 B CN102936353 B CN 102936353B
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Abstract
The present invention relates to a method for preparing a high air tightness antibacterial reinforced membrane by using straws. The method is characterized by comprising the following steps: (1) preparing a straw solution: carrying out a steam decrepitation treatment on straws to obtain a decrepitation product, carrying out hydrogen peroxide rinsing and drying to obtain straw powder, taking an ion liquid and heating until the ion liquid is completely molten, adding the straw powder to mix to obtain a straw liquid, and adding inorganic silver nanometer silver antibacterial powder to the prepared straw liquid to obtain the straw solution; and (2) preparing a high air tightness antibacterial reinforced membrane: taking a cellulose product and flatly fixing on a glass plate, tanking the cellulose product from an oven, uniformly coating the straw solution obtained from the step (1) on the cellulose product, soaking for 2-3 hours by using water after cooling, washing until the ion liquid is completely precipitated, and carrying out open-air drying to obtain the high air tightness antibacterial reinforced membrane. According to the present invention, the method has characteristics of simple process, green property, and no pollution, and the prepared membrane has characteristics of high air tightness, high moisture permeability, and good mechanical property.
Description
Technical field
The present invention relates to a kind of straw of using for the method for the antibiotic reinforcing membrane of high-air-tightness.
Background technology
Approach and the method for China's straw circulating recycling are the large technical tasks receiving much concern for many years.According to incompletely statistics, the whole world can produce the stalk of nearly 2,000,000,000 t every year, various agricultural crop straw annual production approximately 6.4 hundred million t of China, and along with the raising of crop yield prediction, stalk output also improves thereupon.Except minority stalk is used as animal feed, farm manure and rural area fuel, most of stalks are stacked even directly to be burned, and has not only wasted large number of biological resource, also severe contamination environment.
Summary of the invention
The object of the present invention is to provide a kind of straw of using for the method for the antibiotic reinforcing membrane of high-air-tightness, the antibiotic reinforcing membrane of high-air-tightness prepared by the method has the feature of high strength, high-air-tightness, high water vapour permeability.
For achieving the above object, the technical solution adopted in the present invention is that the method with straw for the antibiotic reinforcing membrane of high-air-tightness, is characterized in that it comprises the steps:
(1) prepare stalk solution:
Stalk is cleaned and is chopped into the long short stem of 4~6 mm, at the pressure of 1.2-1.5MPa, under 60-90s condition, by steam explosion (adopt steam explosion device, or claim steam explosion equipment), process, obtain quick-fried broken product;
By above-mentioned quick-fried broken product hydrogen peroxide rinsing, make its color and luster consistent after again ovendry power be broken to can be sub by 60 mesh sieves, obtain straw powder, stand-by;
Get ionic liquid and be heated to it and melt completely, add stalk powder to mix, 100 ℃ of constant temperature stir 2-3 hour, until solution becomes transparence, obtain stalk liquid; In described stalk liquid (or claiming ionic liquid stalk solution), the mass percentage concentration of stalk powder is 3%-10%;
In the stalk liquid making, add inorganic silver nano-silver antibacterial powder [as inorganic silver nano-silver antibacterial powder JDGKP-003, Jinda Nanotechnology (Xiamen) Co., Ltd.], disperse to stir, obtain stalk solution; Wherein the addition of inorganic silver nano-silver antibacterial powder is 1% of stalk liquid quality;
(2) preparation of the antibiotic reinforcing membrane of high-air-tightness:
Extracting cellulose goods are entirely fixed on sheet glass and (guarantee that it has some tension), heat and within 1-2 hour, remove moisture in 100 ℃ of baking ovens;
From baking oven, take out rapidly cellulosics, by the stalk solution obtaining in step (1) be evenly coated in cellulosics above, the painting amount of stalk solution is 200-300g/mm
2; The 2-3 hour that is soaked in water after cooling, and repetitive scrubbing to ionic liquid separates out completely, takes out film and cellulosics matrix material, dries, and obtains the antibiotic reinforcing membrane of high-air-tightness.
Described stalk can be the stem stalk (being that stalk is the above mixing of any one or two kinds in rice straw, wheat straw waste, maize straw, broomcorn straw, is any proportioning during two kinds of above mixing) of the farm crop such as paddy and wheat, corn or Chinese sorghum.
Described hydrogen peroxide rinsing, H in rinsing hydrogen peroxide used
2o
2massfraction be 1%-2%.
Described ionic liquid is chlorination 1-butyl-3-Methylimidazole ([bmim] Cl).
Described cellulosics is the cellulosicss such as absorbent cotton, gunny products or viscose fiber fabric.
Described inorganic silver nano-silver antibacterial powder refers to and can carry out the inhibition of high-efficiency broad spectrum and kill ultramicro powder various pathogenic bacterium such as Klebsiella pneumonia, intestinal bacteria, Staphylococcus aureus bacillus, Candida albicanss.
For strengthening effect of the present invention, in the stalk solution making, can add glycerine, improve the flexibility of reinforcing membrane, the add-on of glycerine is the 1%-3% of stalk solution quality.
The invention has the beneficial effects as follows:
(1) adopt stalk masking, raw material is cheap and easy to get, and production technology optimization has not only been avoided waste and its pollution to environment of waste resource, has also met production and living needs.
(2) adopt solion (ionic liquid) to cook solvating agent, technical process is simple, and dissolution time is short, and does not need extra catalyst, and solvent recuperation recycling, does not almost have contaminative to environment and biology.
(3) reinforcing membrane that the present invention makes, has high-air-tightness, strong water vapour permeability, and after compound with cellulose fiber fiber products, obtain compared with hard intensity, cracky, does not have good mechanical property, can be used as the upper isolation of medical treatment anti-biotic material.
Accompanying drawing explanation
Fig. 1 is the quick-fried figure after broken of the rice straw of the embodiment of the present invention 1.
Fig. 2 is the straw powder figure of the embodiment of the present invention 1.
Fig. 3 is the rice straw solution figure of the embodiment of the present invention 1.
Fig. 4 is air-tight membrane figure prepared by the rice straw liquid of the embodiment of the present invention 1.
Fig. 5 is the antibiotic reinforcing membrane figure of the high-air-tightness of the embodiment of the present invention 1.
Fig. 6 is that the reinforcing membrane under the Electronic Speculum of the embodiment of the present invention 1 is amplified the figure of 45 times.
Fig. 7 is that the reinforcing membrane under the Electronic Speculum of the embodiment of the present invention 1 is amplified the figure of 100 times.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention, should be understood that these examples are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that after having read the content of the present invention's instruction, those skilled in the art can do work to the present invention and change or revise, and these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1:
Method with straw for the antibiotic reinforcing membrane of high-air-tightness, it comprises the steps:
(1) prepare stalk solution:
Stalk (stalk is rice straw) is cleaned and is chopped into the long short stem of 4~6 mm, at the pressure of 1.3MPa, under 80s condition, by steam explosion (adopt steam explosion device, or claim steam explosion equipment), process, obtain quick-fried broken product;
By above-mentioned quick-fried broken product hydrogen peroxide rinsing, make its color and luster consistent after again ovendry power be broken to can be sub by 60 mesh sieves, obtain straw powder, stand-by;
Get ionic liquid and be heated to it and melt completely, add stalk powder to mix, 100 ℃ of constant temperature stir 2-3 hour, until solution becomes transparence, obtain stalk liquid; In described stalk liquid (ionic liquid stalk solution), the mass percentage concentration of stalk powder is 10%.
In the stalk liquid making, add inorganic silver nano-silver antibacterial powder [as inorganic silver nano-silver antibacterial powder JDGKP-003, Jinda Nanotechnology (Xiamen) Co., Ltd.], disperse to stir, obtain stalk solution; Wherein the addition of inorganic silver nano-silver antibacterial powder is 1% of stalk liquid quality;
In the stalk solution making, add glycerine, the add-on of glycerine is 1% of stalk solution quality.
Described hydrogen peroxide rinsing, rinsing oxydol H used
2o
2massfraction be 1%-2%.
Described ionic liquid is chlorination 1-butyl-3-Methylimidazole ([bmim] Cl).
(2) preparation of the antibiotic reinforcing membrane of high-air-tightness:
The cotton gauze (being absorbent cotton, cellulosics) of making even after whole degreasing is entirely fixed on sheet glass and (guarantees that it has some tension), heats and within 1 hour, remove moisture in 100 ℃ of baking ovens;
From baking oven, take out rapidly cellulosics, by the stalk solution obtaining in step (1) be evenly coated in cellulosics above, the painting amount of stalk solution is 255g/mm
2; The 2-3 hour that is soaked in water after cooling, and repetitive scrubbing to ionic liquid separates out completely, takes out film and cellulosics matrix material, dries, and obtains the antibiotic reinforcing membrane of high-air-tightness.
Fig. 1 is the quick-fried figure after broken of rice straw.Steam explosion is processed the hemicellulose in good degradation of rice straw, reduces its degree of crystallinity, is convenient to stalk and dissolves, and shows the quick-fried form of straw and the plesiomorphism of former straw after broken in figure, is thread, and color burn, is brown color.
Fig. 2 is the straw powder figure of the embodiment of the present invention 1.
Fig. 3 is rice straw solution figure, shows that straw is well dissolved in ionic liquid in figure, and solution is faint yellow transparence, compared with thickness.
Fig. 4 is air-tight membrane (being the antibiotic reinforcing membrane of high-air-tightness) figure prepared by rice straw liquid.In figure, show this air-tight membrane water white transparency, for without interfacial film, embody its high-air-tightness.
Fig. 5, Fig. 6, Fig. 7 are that the high-air-tightness reinforcing membrane making is amplified different multiples figure.Three figure from macroscopic view to microcosmic angle, demonstrate this reinforcing membrane for without interfacial film respectively, completely compound with cellulosics.
Recording this film air penetrability is 8.65L/m
2s, water vapour permeability is 1240g/m
224h, tensile strength is 569MPa.Illustrate that the antibiotic reinforcing membrane of high-air-tightness prepared by the method has the feature of high strength, high-air-tightness, high water vapour permeability.
Embodiment 2:
Method with straw for the antibiotic reinforcing membrane of high-air-tightness, it comprises the steps:
(1) prepare stalk solution:
Wheat straw waste is cleaned and is chopped into the long short stem of 4~6 mm, at the pressure of 1.2MPa, under 60s condition, by steam explosion (adopt steam explosion device, or claim steam explosion equipment), process, obtain quick-fried broken product;
By above-mentioned quick-fried broken product hydrogen peroxide rinsing, make its color and luster consistent after again ovendry power be broken to can be sub by 60 mesh sieves, obtain straw powder, stand-by;
Get ionic liquid [chlorination 1-butyl-3-Methylimidazole ([bmim] Cl)] and be heated to it and melt completely, add stalk powder to mix, 100 ℃ of constant temperature stir 2-3 hour, until solution becomes transparence, obtain stalk liquid; In described stalk liquid (ionic liquid stalk solution), the mass percentage concentration of stalk powder is 8%.
In the stalk liquid making, add inorganic silver nano-silver antibacterial powder (as inorganic silver nano-silver antibacterial powder JDGKP-003, Jinda Nanotechnology (Xiamen) Co., Ltd.), disperse to stir, obtain stalk solution; Wherein the addition of inorganic silver nano-silver antibacterial powder is 1% of stalk liquid quality;
(2) preparation of the antibiotic reinforcing membrane of high-air-tightness:
The cotton gauze (cellulosics) of making even after whole degreasing is entirely fixed on sheet glass and (guarantees that it has some tension), heats and within 1-2 hour, remove moisture in 100 ℃ of baking ovens;
From baking oven, take out rapidly cellulosics, with glass stick by the stalk solution obtaining in step (1) be evenly coated in cellulosics above, be coated with 2 times, the painting amount of stalk solution is 254g/mm
2; The 2-3 hour that is soaked in water after cooling, and repetitive scrubbing to ionic liquid separates out completely, takes out film and cellulosics matrix material, dries, and obtains the antibiotic reinforcing membrane of high-air-tightness.
The air penetrability that records the antibiotic reinforcing membrane of this high-air-tightness is 8.35L/m
2s, water vapour permeability is 1470g/m
224h, tensile strength is 554MPa.Illustrate that the antibiotic reinforcing membrane of high-air-tightness prepared by the method has the feature of high strength, high-air-tightness, high water vapour permeability.
Embodiment 3:
Method with straw for the antibiotic reinforcing membrane of high-air-tightness, it comprises the steps:
(1) prepare stalk solution:
Maize straw is cleaned and is chopped into the long short stem of 4~6 mm, at the pressure of 1.5MPa, under 90s condition, by steam explosion (adopt steam explosion device, or claim steam explosion equipment), process, obtain quick-fried broken product;
By above-mentioned quick-fried broken product hydrogen peroxide rinsing, make its color and luster consistent after again ovendry power be broken to can be sub by 60 mesh sieves, obtain straw powder, stand-by;
Get ionic liquid and be heated to it and melt completely, add stalk powder to mix, 100 ℃ of constant temperature stir 2-3 hour, until solution becomes transparence, obtain stalk liquid; In described stalk liquid (ionic liquid stalk solution), the mass percentage concentration of stalk powder is 6%.
In the stalk liquid making, add inorganic silver nano-silver antibacterial powder (as inorganic silver nano-silver antibacterial powder JDGKP-003, Jinda Nanotechnology (Xiamen) Co., Ltd.), disperse to stir, obtain stalk solution; Wherein the addition of inorganic silver nano-silver antibacterial powder is 1% of stalk liquid quality;
Described ionic liquid is chlorination 1-butyl-3-Methylimidazole ([bmim] Cl).
(2) preparation of the antibiotic reinforcing membrane of high-air-tightness:
The textile hydro-entangled non-woven fabric (cellulosics) of making even after whole degreasing is entirely fixed on sheet glass, heats and within 1-2 hour, remove moisture in 100 ℃ of baking ovens;
From baking oven, take out rapidly cellulosics, with glass stick the stalk solution obtaining in step (1) be evenly coated in cellulosics above, the painting amount of stalk solution is 276g/mm
2; The 2-3 hour that is soaked in water after cooling, and repetitive scrubbing to ionic liquid separates out completely, takes out film and cellulosics matrix material, dries, and obtains the antibiotic reinforcing membrane of high-air-tightness.
Recording this film air penetrability is 9.43L/m
2s, water vapour permeability is 1560g/m
224h, tensile strength is 464MPa.Illustrate that the antibiotic reinforcing membrane of high-air-tightness prepared by the method has the feature of high strength, high-air-tightness, high water vapour permeability.
Embodiment 4:
Method with straw for the antibiotic reinforcing membrane of high-air-tightness, it comprises the steps:
(1) prepare stalk solution:
Wheat straw waste is cleaned and is chopped into the long short stem of 4~6 mm, at the pressure of 1.5MPa, under 90s condition, by steam explosion (adopt steam explosion device, or claim steam explosion equipment), process, obtain quick-fried broken product;
By above-mentioned quick-fried broken product hydrogen peroxide rinsing, make its color and luster consistent after again ovendry power be broken to can be sub by 60 mesh sieves, obtain straw powder, stand-by;
Get ionic liquid and be heated to it and melt completely, add stalk powder to mix, 100 ℃ of constant temperature stir 2-3 hour, until solution becomes transparence, obtain stalk liquid; In described stalk liquid (ionic liquid stalk solution), the mass percentage concentration of stalk powder is 10%.
In the stalk liquid making, add inorganic silver nano-silver antibacterial powder (as inorganic silver nano-silver antibacterial powder JDGKP-003, Jinda Nanotechnology (Xiamen) Co., Ltd.), disperse to stir, obtain stalk solution; Wherein the addition of inorganic silver nano-silver antibacterial powder is 1% of stalk liquid quality;
Described ionic liquid is chlorination 1-butyl-3-Methylimidazole ([bmim] Cl).
(2) preparation of the antibiotic reinforcing membrane of high-air-tightness:
The viscose fiber fabric (being cellulosics) of making even after whole degreasing is entirely fixed on sheet glass, heats and within 1-2 hour, remove moisture in 100 ℃ of baking ovens;
From baking oven, take out rapidly cellulosics, by the stalk solution obtaining in step (1) be evenly coated in cellulosics above, the painting amount of stalk solution is 255g/mm
2; The 2-3 hour that is soaked in water after cooling, and repetitive scrubbing to ionic liquid separates out completely, takes out film and cellulosics matrix material, dries, and obtains the antibiotic reinforcing membrane of high-air-tightness.
Recording this film air penetrability is 8.95L/m
2s, water vapour permeability is 1870g/m
224h, tensile strength is 311MPa.Illustrate that the antibiotic reinforcing membrane of high-air-tightness prepared by the method has the feature of high strength, high-air-tightness, high water vapour permeability.
Embodiment 5:
Method with straw for the antibiotic reinforcing membrane of high-air-tightness, it comprises the steps:
(1) prepare stalk solution:
Broomcorn straw is cleaned and is chopped into the long short stem of 4~6 mm, at the pressure of 1.2MPa, under 90s condition, by steam explosion (adopt steam explosion device, or claim steam explosion equipment), process, obtain quick-fried broken product;
By above-mentioned quick-fried broken product hydrogen peroxide rinsing, make its color and luster consistent after again ovendry power be broken to can be sub by 60 mesh sieves, obtain straw powder, stand-by;
Get ionic liquid [chlorination 1-butyl-3-Methylimidazole ([bmim] Cl)] and be heated to it and melt completely, add stalk powder to mix, 100 ℃ of constant temperature stir 2-3 hour, until solution becomes transparence, obtain stalk liquid; In described stalk liquid (ionic liquid stalk solution), the mass percentage concentration of stalk powder is 10%.
In the stalk liquid making, add inorganic silver nano-silver antibacterial powder (as inorganic silver nano-silver antibacterial powder JDGKP-003, Jinda Nanotechnology (Xiamen) Co., Ltd.), disperse to stir, obtain stalk solution; Wherein the addition of inorganic silver nano-silver antibacterial powder is 1% of stalk liquid quality;
(2) preparation of the antibiotic reinforcing membrane of high-air-tightness:
Get gunny products (cellulosics) and be entirely fixed on sheet glass, guarantee that it has some tension, in 100 ℃ of baking ovens, heat and within 1-2 hour, remove moisture;
From baking oven, take out rapidly cellulosics, by the stalk solution obtaining in step (1) be evenly coated in cellulosics above, the painting amount of stalk solution is 256g/mm
2; The 2-3 hour that is soaked in water after cooling, and repetitive scrubbing to ionic liquid separates out completely, takes out film and cellulosics matrix material, dries, and obtains the antibiotic reinforcing membrane of high-air-tightness.
Recording this film air penetrability is 9.65L/m
2s, water vapour permeability is 1740g/m
224h, tensile strength is 364MPa.Illustrate that the antibiotic reinforcing membrane of high-air-tightness prepared by the method has the feature of high strength, high-air-tightness, high water vapour permeability.
Embodiment 6:
Substantially the same manner as Example 1, difference is: stalk is rice straw and wheat straw waste, and the quality of the two respectively accounts for 1/2.
Recording this film air penetrability is 8.62L/m
2s, water vapour permeability is 1130g/m
224h, tensile strength is 432MPa.Illustrate that the antibiotic reinforcing membrane of high-air-tightness prepared by the method has the feature of high strength, high-air-tightness, high water vapour permeability.
Embodiment 7:
Substantially the same manner as Example 1, difference is: stalk is rice straw, wheat straw waste, maize straw and broomcorn straw, and four quality respectively accounts for 1/4.
Recording this film air penetrability is 8.11L/m
2s, water vapour permeability is 1240g/m
224h, tensile strength is 423MPa.Illustrate that the antibiotic reinforcing membrane of high-air-tightness prepared by the method has the feature of high strength, high-air-tightness, high water vapour permeability.
Embodiment 8:
Substantially the same manner as Example 1, difference is: in the stalk solution making, can add glycerine, the add-on of glycerine is 3% of stalk solution quality.
Recording this film air penetrability is 8.61L/m
2s, water vapour permeability is 1540g/m
224h, tensile strength is 349MPa.Illustrate that the antibiotic reinforcing membrane of high-air-tightness prepared by the method has the feature of high strength, high-air-tightness, high water vapour permeability.
Embodiment 9:
Substantially the same manner as Example 1, difference is: in described stalk liquid (ionic liquid stalk solution), the mass percentage concentration of stalk powder is 3%.
Recording this film air penetrability is 8.44L/m
2s, water vapour permeability is 1132g/m
224h, tensile strength is 321MPa.Illustrate that the antibiotic reinforcing membrane of high-air-tightness prepared by the method has the feature of high strength, high-air-tightness, high water vapour permeability.
Embodiment 10:
Substantially the same manner as Example 1, difference is: described stalk liquid painting amount is 200g/mm
2, recording this film air penetrability is 7.95L/m
2s, water vapour permeability is 1142g/m
224h, tensile strength is 439MPa.Illustrate that the antibiotic reinforcing membrane of high-air-tightness prepared by the method has the feature of high strength, high-air-tightness, high water vapour permeability.
Embodiment 11:
Substantially the same manner as Example 1, difference is: described stalk liquid painting amount is 300g/mm
2, recording this film air penetrability is 9.35L/m
2s, water vapour permeability is 1540g/m
224h, tensile strength is 598MPa.Illustrate that the antibiotic reinforcing membrane of high-air-tightness prepared by the method has the feature of high strength, high-air-tightness, high water vapour permeability.
Claims (5)
1. the method for the antibiotic reinforcing membrane of high-air-tightness with straw, is characterized in that it comprises the steps:
(1) prepare stalk solution:
Stalk is cleaned and is chopped into the long short stem of 4~6 mm, at the pressure of 1.2-1.5MPa, under 60-90s condition, by steam explosion, process, obtain quick-fried broken product;
By above-mentioned quick-fried broken product hydrogen peroxide rinsing, make its color and luster consistent after again ovendry power be broken to can be sub by 60 mesh sieves, obtain straw powder, stand-by;
Get ionic liquid and be heated to it and melt completely, add stalk powder to mix, 100 ℃ of constant temperature stir 2-3 hour, until solution becomes transparence, obtain stalk liquid; In described stalk liquid, the mass percentage concentration of stalk powder is 3%-10%;
In the stalk liquid making, add inorganic silver nano-silver antibacterial powder, disperse to stir, obtain stalk solution; Wherein the addition of inorganic silver nano-silver antibacterial powder is 1% of stalk liquid quality;
(2) preparation of the antibiotic reinforcing membrane of high-air-tightness:
Extracting cellulose goods are entirely fixed on sheet glass, heat and within 1-2 hour, remove moisture in 100 ℃ of baking ovens;
From baking oven, take out cellulosics, by the stalk solution obtaining in step (1) be evenly coated in cellulosics above; The 2-3 hour that is soaked in water after cooling, and wash to ionic liquid and separate out completely, dry, obtain the antibiotic reinforcing membrane of high-air-tightness.
2. the straw of using according to claim 1 is for the method for the antibiotic reinforcing membrane of high-air-tightness, it is characterized in that: described stalk is the above mixing of any one or two kinds in rice straw, wheat straw waste, maize straw, broomcorn straw, during two kinds of above mixing, is any proportioning.
3. the straw of using according to claim 1, for the method for the antibiotic reinforcing membrane of high-air-tightness, is characterized in that: described ionic liquid is chlorination 1-butyl-3-Methylimidazole.
4. the straw of using according to claim 1, for the method for the antibiotic reinforcing membrane of high-air-tightness, is characterized in that: described cellulosics is absorbent cotton, gunny products or viscose fiber fabric.
5. the straw of using according to claim 1, for the method for the antibiotic reinforcing membrane of high-air-tightness, is characterized in that: in the stalk solution making, can add glycerine, the add-on of glycerine is the 1%-3% of stalk solution quality.
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CN108360299A (en) * | 2018-03-01 | 2018-08-03 | 宁波纳新生物科技有限公司 | A kind of onionskin of silver nanoparticles loaded and preparation method thereof |
CN108395724A (en) * | 2018-03-12 | 2018-08-14 | 安徽农业大学 | A kind of preparation method of tea grounds/cellulose preservative film |
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CN111635640B (en) * | 2019-03-01 | 2021-06-22 | 中国科学院化学研究所 | Composite material based on agricultural wastes and preparation method and application thereof |
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