WO2022095100A1 - Preparation method for multi-scale nanocellulose film based on flax fibers - Google Patents

Preparation method for multi-scale nanocellulose film based on flax fibers Download PDF

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WO2022095100A1
WO2022095100A1 PCT/CN2020/128895 CN2020128895W WO2022095100A1 WO 2022095100 A1 WO2022095100 A1 WO 2022095100A1 CN 2020128895 W CN2020128895 W CN 2020128895W WO 2022095100 A1 WO2022095100 A1 WO 2022095100A1
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nanocellulose
flax
suspension
scale
preparing
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马翔
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苏州纳昇源新材料科技有限公司
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
    • D—TEXTILES; PAPER
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with hydrogen peroxide or peroxides of metals; with persulfuric, permanganic, pernitric, percarbonic acids or their salts
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    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
    • D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
    • D06M13/2246—Esters of unsaturated carboxylic acids
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    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/402—Amides imides, sulfamic acids
    • D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic

Definitions

  • the present application relates to a method for preparing a multi-scale nanocellulose film based on flax fiber, in particular to a method for preparing a multi-scale nanocellulose film based on flax fiber.
  • Nanocellulose has a wide range of sources, high strength, and its It is degradable by itself. Nanocellulose obtained from natural cellulose has some excellent strength and physical and chemical properties that cellulose does not have. It has become a research hotspot at home and abroad. Nanocellulose, as a natural renewable biomass polymer functional material, It has broad application prospects in the fields of biology, medicine, papermaking and food.
  • Nanocellulose materials derived from it are favored by researchers due to their huge specific surface area, excellent mechanical properties, high crystallinity, high hydrophilicity, and ultra-fine structure. Films prepared from nanocellulose have good biodegradable properties, gas barrier properties, mechanical properties and light transmittance, and have great potential to replace plastic films, and nanocellulose films also have great potential in developing new materials.
  • traditional methods for preparing nanocellulose include chemical method and mechanical method, acid hydrolysis method is commonly used in chemical method, and sulfuric acid is the most commonly used inorganic acid in acid hydrolysis.
  • nanocellulose is obtained by hydrolysis with 64% sulfuric acid at 45 °C for about 30 min.
  • This method usually takes a long time and has a low yield (about 30%).
  • the mechanical method mainly adopts fine grinding treatment, which consumes more energy. Therefore, a method for preparing a multi-scale nanocellulose membrane based on flax fiber is proposed to solve the above problems.
  • a method for preparing a multi-scale nanocellulose membrane based on flax fiber comprises the following steps:
  • step (2) centrifuging and washing the fiber suspension obtained in step (1), and collecting the liquid obtained by centrifugation as a pretreatment solution; adjusting the solid residue obtained by centrifugation with an alkaline solution to neutrality, and then centrifuging and washing to remove inorganic salts to obtain activated flax plant fibers ;
  • step (2) diluting the activated flax plant fiber obtained in step (2) and grinding to obtain an activated flax plant fiber suspension
  • step (4) high-pressure homogenizing the flax activated plant fiber suspension obtained in step (4) to obtain a nano flax cellulose suspension
  • the moisture content of the nanocellulose film wet paper sheet is reduced to 10-20% after vacuum pressing, and the moisture content of the nanocellulose film wet paper sheet is reduced to 2.5-6% after drying in an oven to obtain a flax fiber-based multiscale nanocellulose films.
  • the mass concentration of the sulfuric acid in the step (1) is 35%-40%; the mass-volume ratio of the flax plant fiber to the sulfuric acid is 1 g: (6-10) ml.
  • the temperature of the hydrolysis in the step (1) is 32°C to 45°C, and the time is 10min-30min.
  • the alkali solution in the step (2) is sodium hydroxide solution, potassium hydroxide solution or ammonia water.
  • the residual sulfuric acid recovered in the step (2) can be continuously added to the pretreatment reaction process.
  • an aqueous solution of nanocellulose and deionized water can also be used and mixed to obtain a suspension, the suspension is stirred in a water bath at 85-95°C for 2-3 hours, and then ultrasonically treated for 5-15 minutes, Then vacuum defoaming for 5-20min to obtain nano flax cellulose suspension.
  • the stirring speed in the step (6) is 500-700 r/min.
  • the forming plate in the step (8) is a polytetrafluoroethylene plate.
  • infrared heating or electromagnetic heating is used to preheat the forming plate.
  • the thickness of the pure nanocellulose film prepared in the step (9) is 10 ⁇ m ⁇ 60 ⁇ m.
  • the present application provides a method for preparing a multi-scale nanocellulose film based on flax fibers.
  • Fig. 1 is the flow chart of the preparation method of the present application.
  • the terms “installed”, “set up”, “provided with”, “connected”, “connected”, “socketed” should be construed broadly. For example, it may be a fixed connection, a detachable connection, or a unitary structure; it may be a mechanical connection, or an electrical connection; it may be directly connected, or indirectly connected through an intermediary, or between two devices, elements, or components. internal communication.
  • installed may be a fixed connection, a detachable connection, or a unitary structure; it may be a mechanical connection, or an electrical connection; it may be directly connected, or indirectly connected through an intermediary, or between two devices, elements, or components. internal communication.
  • a method for preparing a multi-scale nanocellulose film based on flax fiber comprising the following steps:
  • step (2) centrifuging and washing the fiber suspension obtained in step (1), and collecting the liquid obtained by centrifugation as a pretreatment solution; adjusting the solid residue obtained by centrifugation with an alkaline solution to neutrality, and then centrifuging and washing to remove inorganic salts to obtain activated flax plant fibers ;
  • step (2) diluting the activated flax plant fiber obtained in step (2) and grinding to obtain an activated flax plant fiber suspension
  • step (4) high-pressure homogenizing the flax activated plant fiber suspension obtained in step (4) to obtain a nano flax cellulose suspension
  • the moisture content of the nanocellulose film wet paper sheet is reduced to 10-20% after vacuum pressing, and the moisture content of the nanocellulose film wet paper sheet is reduced to 2.5-6% after drying in an oven to obtain a flax fiber-based multiscale nanocellulose films.
  • the mass concentration of the sulfuric acid in the step (1) is 35%-40%; the mass-volume ratio of the flax plant fiber to the sulfuric acid is 1 g: (6-10) ml.
  • the temperature of the hydrolysis in the step (1) is 45° C. and the time is 30 min.
  • the alkali solution in the step (2) is sodium hydroxide solution, potassium hydroxide solution or ammonia water.
  • the residual sulfuric acid recovered in the step (2) can be continuously added to the pretreatment reaction process.
  • an aqueous nanocellulose solution and deionized water can also be used and mixed to obtain a suspension, the suspension is stirred in a water bath at 95°C for 2 to 3 hours, and then ultrasonically treated for 15 minutes, and then vacuum defoamed 20min to obtain nano flax cellulose suspension.
  • the stirring speed in the step (6) is 700r/min.
  • the forming plate in the step (8) is a polytetrafluoroethylene plate.
  • infrared heating or electromagnetic heating is used to preheat the forming plate.
  • the thickness of the pure nanocellulose film prepared in the step (9) is 60 ⁇ m.
  • the above method is applicable to the preparation method of multi-scale nanocellulose film based on flax fiber.
  • Embodiment 2 is a diagrammatic representation of Embodiment 1:
  • a method for preparing a multi-scale nanocellulose film based on flax fiber comprising the following steps:
  • step (2) centrifuging and washing the fiber suspension obtained in step (1), and collecting the liquid obtained by centrifugation as a pretreatment solution; adjusting the solid residue obtained by centrifugation with an alkaline solution to neutrality, and then centrifuging and washing to remove inorganic salts to obtain activated flax plant fibers ;
  • step (2) diluting the activated flax plant fiber obtained in step (2) and grinding to obtain an activated flax plant fiber suspension
  • step (4) high-pressure homogenizing the flax activated plant fiber suspension obtained in step (4) to obtain a nano flax cellulose suspension
  • the moisture content of the nanocellulose film wet paper sheet is reduced to 10-20% after vacuum pressing, and the moisture content of the nanocellulose film wet paper sheet is reduced to 2.5-6% after drying in an oven to obtain a flax fiber-based multiscale nanocellulose films.
  • the mass concentration of the sulfuric acid in the step (1) is 35%; the mass-volume ratio of the flax plant fiber to the sulfuric acid is 1 g: (6-10) ml.
  • the temperature of the hydrolysis in the step (1) was 32° C. and the time was 10 min.
  • the alkali solution in the step (2) is sodium hydroxide solution, potassium hydroxide solution or ammonia water.
  • the residual sulfuric acid recovered in the step (2) can be continuously added to the pretreatment reaction process.
  • an aqueous solution of nanocellulose and deionized water can also be used and mixed to obtain a suspension, the suspension is stirred in a water bath at 85°C for 2-3 hours, and then ultrasonically treated for 5 minutes, and then vacuum defoamed 5min to obtain nano flax cellulose suspension.
  • the stirring speed in the step (6) is 500r/min.
  • the forming plate in the step (8) is a polytetrafluoroethylene plate.
  • infrared heating or electromagnetic heating is used to preheat the forming plate.
  • the thickness of the pure nanocellulose film prepared in the step (9) is 10 ⁇ m.
  • the above method is applicable to the preparation method of multi-scale nanocellulose film based on flax fiber.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)

Abstract

A preparation method for a multi-scale nanocellulose film based on flax fibers, comprising: weighing flax plant fibers, then adding sulfuric acid for hydrolysis to perform pretreatment, after the hydrolysis is completed, adding water to terminate the reaction, and obtaining a fiber suspension; performing centrifugal washing on the obtained fiber suspension, and collecting a liquid obtained by centrifuging and using the liquid as a pretreatment liquid; adjusting, by using an alkaline solution, solid residues obtained by centrifuging to be neutral, then performing centrifugal washing, and removing an inorganic salt to obtain activated flax plant fibers; separately recovering, by using a membrane separation method, a carbohydrate component and residual sulfuric acid in the collected pretreatment liquid; diluting the obtained activated flax plant fibers, and performing disc milling to obtain an activated flax plant fiber suspension; performing high-pressure homogenization on the obtained activated flax plant fiber suspension to obtain a flax nanocellulose suspension; and uniformly spraying the flax nanocellulose suspension, which is uniformly dispersed, onto a forming plate, reducing a moisture content, and then obtaining a multi-scale nanocellulose film based on flax fibers.

Description

一种基于亚麻纤维的多尺度纳米纤维素膜制备方法A kind of preparation method of multi-scale nanocellulose membrane based on flax fiber 技术领域technical field
本申请涉及一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，具体是一种基于亚麻纤维的多尺度纳米纤维素膜制备方法。The present application relates to a method for preparing a multi-scale nanocellulose film based on flax fiber, in particular to a method for preparing a multi-scale nanocellulose film based on flax fiber.
背景技术Background technique
近年来，难降解的塑料垃圾已经成为世界公认的治理难题，我国为限制和减少塑料的使用，规定从2008年6月1日起全国范围内禁止生产、销售、使用厚度小于0.025mm的塑料购物袋，所用的超市、商场、集贸市场等商品零售场所实行塑料购物袋有偿使用制度，一律不得免费提供塑料购物袋，2018年起我国全面禁止废塑料的进口，近年来，随着仿生学的发展和人们环保意识的增强，通过仿生方法生产一种可降解的环境友好型薄膜以用于食品包装及材料表面功能修饰的想法受到社会普遍关注，纳米纤维素来源广泛，强度较高，且其本身可降解，由天然纤维素得到的纳米纤维素，具有纤维素不具备的一些优异强度和物理化学性能，成为了国内外研究的热点，纳米纤维素作为天然可再生生物质高分子功能材料，在生物、医药、造纸和食品等领域具有广阔的应用前景。In recent years, refractory plastic waste has become a recognized problem in the world. In order to limit and reduce the use of plastics, my country has banned the production, sale and use of plastics with a thickness of less than 0.025mm from June 1, 2008. Bags, supermarkets, shopping malls, bazaars and other commodity retail places implement the system of paid use of plastic shopping bags, and plastic shopping bags shall not be provided free of charge. Since 2018, my country has completely banned the import of waste plastics. In recent years, with the development of bionics With the development and the enhancement of people's awareness of environmental protection, the idea of producing a degradable and environmentally friendly film for food packaging and material surface functional modification through biomimetic methods has received widespread attention from the society. Nanocellulose has a wide range of sources, high strength, and its It is degradable by itself. Nanocellulose obtained from natural cellulose has some excellent strength and physical and chemical properties that cellulose does not have. It has become a research hotspot at home and abroad. Nanocellulose, as a natural renewable biomass polymer functional material, It has broad application prospects in the fields of biology, medicine, papermaking and food.
纤维素作为自然界广泛存在的生物可降解材料，受到了各界广泛的关注。由其衍生出的纳米纤维素材料，凭借其巨大的比表面积、优良的力学性、高结晶度、高亲水性、超精细结构等性能受到了研究者的青睐。利用纳米纤维素制备的薄膜，具有良好的生物可降解性能，气体阻隔性能，力学性能和透光性，在替代塑料薄膜方面具有巨大的潜力，同时纳米纤维素薄膜在开发新材料方面也具有很大潜力，传统制备纳米纤维素的方法有化学法和机械法，化学法中常用的是酸水解法，酸水解中硫酸是最常用的无机酸。通常用64%硫酸在45℃下水解30min左右得到纳米纤维素，这种方法通常耗时长且得率较低(约30%)。机械法主要采用精磨处理，耗能较高。因此，针对上述问题提出一种基于亚麻纤维的多尺度纳米纤维素膜制备方法。As a biodegradable material that exists widely in nature, cellulose has received extensive attention from all walks of life. Nanocellulose materials derived from it are favored by researchers due to their huge specific surface area, excellent mechanical properties, high crystallinity, high hydrophilicity, and ultra-fine structure. Films prepared from nanocellulose have good biodegradable properties, gas barrier properties, mechanical properties and light transmittance, and have great potential to replace plastic films, and nanocellulose films also have great potential in developing new materials. Great potential, traditional methods for preparing nanocellulose include chemical method and mechanical method, acid hydrolysis method is commonly used in chemical method, and sulfuric acid is the most commonly used inorganic acid in acid hydrolysis. Usually, nanocellulose is obtained by hydrolysis with 64% sulfuric acid at 45 °C for about 30 min. This method usually takes a long time and has a low yield (about 30%). The mechanical method mainly adopts fine grinding treatment, which consumes more energy. Therefore, a method for preparing a multi-scale nanocellulose membrane based on flax fiber is proposed to solve the above problems.
技术解决方案technical solutions
一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，所述电网规划的综合评价方法包括如下步骤：A method for preparing a multi-scale nanocellulose membrane based on flax fiber, the comprehensive evaluation method for power grid planning comprises the following steps:
（1）称取亚麻植物纤维，再加入硫酸水解进行预处理，水解结束后，加入水终止反应，得纤维悬浮液；(1) Weigh flax plant fiber, add sulfuric acid for hydrolysis for pretreatment, and after the hydrolysis is completed, add water to terminate the reaction to obtain a fiber suspension;
（2）将步骤（1）得到的纤维悬浮液离心洗涤，收集离心所得液体为预处理液；用碱溶液调节离心所得固体残渣至中性，再离心洗涤，除去无机盐，得活化亚麻植物纤维；(2) centrifuging and washing the fiber suspension obtained in step (1), and collecting the liquid obtained by centrifugation as a pretreatment solution; adjusting the solid residue obtained by centrifugation with an alkaline solution to neutrality, and then centrifuging and washing to remove inorganic salts to obtain activated flax plant fibers ;
（3）采用膜分离的方法分别回收步骤（2）收集到的预处理液中的碳水化合物组分和残余硫酸；(3) Recover carbohydrate components and residual sulfuric acid in the pretreatment solution collected in step (2) by means of membrane separation;
（4）将步骤（2）得到的亚麻活化植物纤维稀释，盘磨，得活化亚麻植物纤维悬浮液；(4) diluting the activated flax plant fiber obtained in step (2) and grinding to obtain an activated flax plant fiber suspension;
（5）将步骤（4）得到的亚麻活化植物纤维悬浮液高压均质，得到纳米亚麻纤维素悬浮液；(5) high-pressure homogenizing the flax activated plant fiber suspension obtained in step (4) to obtain a nano flax cellulose suspension;
（6）将纳米纤维素悬浮液加热至80～90℃，配成0.5‰～0.9‰,、1‰～1.99%以及2%～3%的三份悬浮液，并搅拌均匀；(6) Heat the nanocellulose suspension to 80～90℃, prepare three suspensions of 0.5‰～0.9‰, 1‰～1.99% and 2%～3%, and stir evenly;
（7）将上述分散均匀的纳米纤维素悬浮液通过流浆箱布浆后均匀地喷涂于成型板上，成型板加热至110～125℃；(7) The above-mentioned uniformly dispersed nanocellulose suspension is sprayed evenly on the forming plate through the headbox, and the forming plate is heated to 110～125℃;
（8）控制成型板的加热长度及纸机车速，使纳米纤维素悬浮液中水分含量降至20～30%，得到纳米纤维素薄膜湿纸页；(8) Control the heating length of the forming plate and the speed of the paper machine, so that the moisture content in the nanocellulose suspension is reduced to 20-30%, and the nanocellulose film wet paper sheet is obtained;
（9） 将纳米纤维素薄膜湿纸页经真空压榨后水分含量降至10～20%，继续将纳米纤维素薄膜湿纸页经烘箱干燥后水分含量降至2.5～6%，得到基于亚麻纤维的多尺度的纳米纤维素薄膜。(9) The moisture content of the nanocellulose film wet paper sheet is reduced to 10-20% after vacuum pressing, and the moisture content of the nanocellulose film wet paper sheet is reduced to 2.5-6% after drying in an oven to obtain a flax fiber-based multiscale nanocellulose films.
进一步地，所述步骤（1）中所述硫酸的质量浓度为35%-40%；所述亚麻植物纤维与硫酸的质量体积比为1g：（6~10）ml。Further, the mass concentration of the sulfuric acid in the step (1) is 35%-40%; the mass-volume ratio of the flax plant fiber to the sulfuric acid is 1 g: (6-10) ml.
进一步地，所述步骤（1）中的水解的温度为32℃~45℃，时间为10min-30min。Further, the temperature of the hydrolysis in the step (1) is 32°C to 45°C, and the time is 10min-30min.
进一步地，所述步骤（2）中的碱溶液为氢氧化钠溶液、氢氧化钾溶液或者氨水。Further, the alkali solution in the step (2) is sodium hydroxide solution, potassium hydroxide solution or ammonia water.
进一步地，所述步骤（2）中回收的残余硫酸可继续添加到预处理反应过程中。Further, the residual sulfuric acid recovered in the step (2) can be continuously added to the pretreatment reaction process.
进一步地，所述步骤（5）中也可采用纳米纤维素水溶液以及去离子水并混合得悬浮液，将悬浮液在85～95℃的水浴中搅拌2～3h， 再超声处理5～15min，然后真空脱泡5～20min，得到纳米亚麻纤维素悬浮液。Further, in the step (5), an aqueous solution of nanocellulose and deionized water can also be used and mixed to obtain a suspension, the suspension is stirred in a water bath at 85-95°C for 2-3 hours, and then ultrasonically treated for 5-15 minutes, Then vacuum defoaming for 5-20min to obtain nano flax cellulose suspension.
进一步地，所述步骤（6）中的搅拌速度为500～700r/min。Further, the stirring speed in the step (6) is 500-700 r/min.
进一步地，所述步骤（8）中的成型板为聚四氟乙烯板。Further, the forming plate in the step (8) is a polytetrafluoroethylene plate.
进一步地，所述步骤（7）中采用红外加热或者电磁加热预先对成型板进行加热。Further, in the step (7), infrared heating or electromagnetic heating is used to preheat the forming plate.
进一步地，所述步骤（9）中制得的纯纳米纤维素薄膜厚度为10μm～60μm。Further, the thickness of the pure nanocellulose film prepared in the step (9) is 10 μm˜60 μm.
有益效果beneficial effect
本申请的有益效果是：本申请提供了一种基于亚麻纤维的多尺度纳米纤维素膜制备方法。The beneficial effects of the present application are as follows: the present application provides a method for preparing a multi-scale nanocellulose film based on flax fibers.
附图说明Description of drawings
为了更清楚地说明本申请实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本申请的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性的前提下，还可以根据这些附图获得其它的附图。In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the following briefly introduces the accompanying drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are only These are some embodiments of the present application, and for those of ordinary skill in the art, other drawings can also be obtained from these drawings without any creative effort.
图1为本申请制备方法流程图。Fig. 1 is the flow chart of the preparation method of the present application.
本发明的实施方式Embodiments of the present invention
为了使本技术领域的人员更好地理解本申请方案，下面将结合本申请实施例中的附图，对本申请实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本申请一部分的实施例，而不是全部的实施例。基于本申请中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都应当属于本申请保护的范围。In order to make those skilled in the art better understand the solutions of the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are only The embodiments are part of the present application, but not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work shall fall within the scope of protection of the present application.
需要说明的是，本申请的说明书和权利要求书及上述附图中的术语“第一”、“第二”等是用于区别类似的对象，而不必用于描述特定的顺序或先后次序。应该理解这样使用的数据在适当情况下可以互换，以便这里描述的本申请的实施例。此外，术语“包括”和“具有”以及他们的任何变形，意图在于覆盖不排他的包含，例如，包含了一系列步骤或单元的过程、方法、系统、产品或设备不必限于清楚地列出的那些步骤或单元，而是可包括没有清楚地列出的或对于这些过程、方法、产品或设备固有的其它步骤或单元。It should be noted that the terms "first", "second", etc. in the description and claims of the present application and the above drawings are used to distinguish similar objects, and are not necessarily used to describe a specific sequence or sequence. It is to be understood that the data so used are interchangeable under appropriate circumstances for the embodiments of the application described herein. Furthermore, the terms "comprising" and "having" and any variations thereof, are intended to cover non-exclusive inclusion, for example, a process, method, system, product or device comprising a series of steps or units is not necessarily limited to those expressly listed Rather, those steps or units may include other steps or units not expressly listed or inherent to these processes, methods, products or devices.
在本申请中，术语“上”、“下”、“左”、“右”、“前”、“后”、“顶”、“底”、“内”、“外”、“中”、“竖直”、“水平”、“横向”、“纵向”等指示的方位或位置关系为基于附图所示的方位或位置关系。这些术语主要是为了更好地描述本申请及其实施例，并非用于限定所指示的装置、元件或组成部分必须具有特定方位，或以特定方位进行构造和操作。In this application, the terms "upper", "lower", "left", "right", "front", "rear", "top", "bottom", "inner", "outer", "middle", The orientation or positional relationship indicated by "vertical", "horizontal", "horizontal", "longitudinal", etc. is based on the orientation or positional relationship shown in the drawings. These terms are primarily used to better describe the present application and its embodiments, and are not intended to limit the fact that the indicated device, element, or component must have a particular orientation, or be constructed and operated in a particular orientation.
并且，上述部分术语除了可以用于表示方位或位置关系以外，还可能用于表示其他含义，例如术语“上”在某些情况下也可能用于表示某种依附关系或连接关系。对于本领域普通技术人员而言，可以根据具体情况理解这些术语在本申请中的具体含义。In addition, some of the above-mentioned terms may be used to express other meanings besides orientation or positional relationship. For example, the term "on" may also be used to express a certain attachment or connection relationship in some cases. For those of ordinary skill in the art, the specific meanings of these terms in the present application can be understood according to specific situations.
此外，术语“安装”、“设置”、“设有”、“连接”、“相连”、“套接”应做广义理解。例如，可以是固定连接，可拆卸连接，或整体式构造；可以是机械连接，或电连接；可以是直接相连，或者是通过中间媒介间接相连，又或者是两个装置、元件或组成部分之间内部的连通。对于本领域普通技术人员而言，可以根据具体情况理解上述术语在本申请中的具体含义。Furthermore, the terms "installed", "set up", "provided with", "connected", "connected", "socketed" should be construed broadly. For example, it may be a fixed connection, a detachable connection, or a unitary structure; it may be a mechanical connection, or an electrical connection; it may be directly connected, or indirectly connected through an intermediary, or between two devices, elements, or components. internal communication. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood according to specific situations.
需要说明的是，在不冲突的情况下，本申请中的实施例及实施例中的特征可以相互组合。下面将参考附图并结合实施例来详细说明本申请。It should be noted that the embodiments in the present application and the features of the embodiments may be combined with each other in the case of no conflict. The present application will be described in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
实施例一：Example 1:
一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，所述基于亚麻纤维的多尺度纳米纤维素膜制备方法包括如下步骤：A method for preparing a multi-scale nanocellulose film based on flax fiber, comprising the following steps:
（1）称取亚麻植物纤维，再加入硫酸水解进行预处理，水解结束后，加入水终止反应，得纤维悬浮液；(1) Weigh flax plant fiber, add sulfuric acid for hydrolysis for pretreatment, and after the hydrolysis is completed, add water to terminate the reaction to obtain a fiber suspension;
（2）将步骤（1）得到的纤维悬浮液离心洗涤，收集离心所得液体为预处理液；用碱溶液调节离心所得固体残渣至中性，再离心洗涤，除去无机盐，得活化亚麻植物纤维；(2) centrifuging and washing the fiber suspension obtained in step (1), and collecting the liquid obtained by centrifugation as a pretreatment solution; adjusting the solid residue obtained by centrifugation with an alkaline solution to neutrality, and then centrifuging and washing to remove inorganic salts to obtain activated flax plant fibers ;
（3）采用膜分离的方法分别回收步骤（2）收集到的预处理液中的碳水化合物组分和残余硫酸；(3) Recover carbohydrate components and residual sulfuric acid in the pretreatment solution collected in step (2) by means of membrane separation;
（4）将步骤（2）得到的亚麻活化植物纤维稀释，盘磨，得活化亚麻植物纤维悬浮液；(4) diluting the activated flax plant fiber obtained in step (2) and grinding to obtain an activated flax plant fiber suspension;
（5）将步骤（4）得到的亚麻活化植物纤维悬浮液高压均质，得到纳米亚麻纤维素悬浮液；(5) high-pressure homogenizing the flax activated plant fiber suspension obtained in step (4) to obtain a nano flax cellulose suspension;
（6）将纳米纤维素悬浮液加热至80～90℃，配成0.5‰～0.9‰,、1‰～1.99%以及2%～3%的三份悬浮液，并搅拌均匀；(6) Heat the nanocellulose suspension to 80～90℃, prepare three suspensions of 0.5‰～0.9‰, 1‰～1.99% and 2%～3%, and stir evenly;
（7）将上述分散均匀的纳米纤维素悬浮液通过流浆箱布浆后均匀地喷涂于成型板上，成型板加热至110～125℃；(7) The above-mentioned uniformly dispersed nanocellulose suspension is sprayed evenly on the forming plate through the headbox, and the forming plate is heated to 110～125℃;
（8）控制成型板的加热长度及纸机车速，使纳米纤维素悬浮液中水分含量降至20～30%，得到纳米纤维素薄膜湿纸页；(8) Control the heating length of the forming plate and the speed of the paper machine, so that the moisture content in the nanocellulose suspension is reduced to 20-30%, and the nanocellulose film wet paper sheet is obtained;
（9） 将纳米纤维素薄膜湿纸页经真空压榨后水分含量降至10～20%，继续将纳米纤维素薄膜湿纸页经烘箱干燥后水分含量降至2.5～6%，得到基于亚麻纤维的多尺度的纳米纤维素薄膜。(9) The moisture content of the nanocellulose film wet paper sheet is reduced to 10-20% after vacuum pressing, and the moisture content of the nanocellulose film wet paper sheet is reduced to 2.5-6% after drying in an oven to obtain a flax fiber-based multiscale nanocellulose films.
进一步地，所述步骤（1）中所述硫酸的质量浓度为35%-40%；所述亚麻植物纤维与硫酸的质量体积比为1g：（6~10）ml。Further, the mass concentration of the sulfuric acid in the step (1) is 35%-40%; the mass-volume ratio of the flax plant fiber to the sulfuric acid is 1 g: (6-10) ml.
进一步地，所述步骤（1）中的水解的温度为45℃，时间为30min。Further, the temperature of the hydrolysis in the step (1) is 45° C. and the time is 30 min.
进一步地，所述步骤（2）中的碱溶液为氢氧化钠溶液、氢氧化钾溶液或者氨水。Further, the alkali solution in the step (2) is sodium hydroxide solution, potassium hydroxide solution or ammonia water.
进一步地，所述步骤（2）中回收的残余硫酸可继续添加到预处理反应过程中。Further, the residual sulfuric acid recovered in the step (2) can be continuously added to the pretreatment reaction process.
进一步地，所述步骤（5）中也可采用纳米纤维素水溶液以及去离子水并混合得悬浮液，将悬浮液在95℃的水浴中搅拌2～3h， 再超声处理15min，然后真空脱泡20min，得到纳米亚麻纤维素悬浮液。Further, in the step (5), an aqueous nanocellulose solution and deionized water can also be used and mixed to obtain a suspension, the suspension is stirred in a water bath at 95°C for 2 to 3 hours, and then ultrasonically treated for 15 minutes, and then vacuum defoamed 20min to obtain nano flax cellulose suspension.
进一步地，所述步骤（6）中的搅拌速度为700r/min。Further, the stirring speed in the step (6) is 700r/min.
进一步地，所述步骤（8）中的成型板为聚四氟乙烯板。Further, the forming plate in the step (8) is a polytetrafluoroethylene plate.
进一步地，所述步骤（7）中采用红外加热或者电磁加热预先对成型板进行加热。Further, in the step (7), infrared heating or electromagnetic heating is used to preheat the forming plate.
进一步地，所述步骤（9）中制得的纯纳米纤维素薄膜厚度为60μm。Further, the thickness of the pure nanocellulose film prepared in the step (9) is 60 μm.
上述方法适用于基于亚麻纤维的多尺度纳米纤维素膜制备方法。The above method is applicable to the preparation method of multi-scale nanocellulose film based on flax fiber.
实施例二：Embodiment 2:
一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，所述基于亚麻纤维的多尺度纳米纤维素膜制备方法包括如下步骤：A method for preparing a multi-scale nanocellulose film based on flax fiber, comprising the following steps:
（1）称取亚麻植物纤维，再加入硫酸水解进行预处理，水解结束后，加入水终止反应，得纤维悬浮液；(1) Weigh flax plant fiber, add sulfuric acid for hydrolysis for pretreatment, and after the hydrolysis is completed, add water to terminate the reaction to obtain a fiber suspension;
（2）将步骤（1）得到的纤维悬浮液离心洗涤，收集离心所得液体为预处理液；用碱溶液调节离心所得固体残渣至中性，再离心洗涤，除去无机盐，得活化亚麻植物纤维；(2) centrifuging and washing the fiber suspension obtained in step (1), and collecting the liquid obtained by centrifugation as a pretreatment solution; adjusting the solid residue obtained by centrifugation with an alkaline solution to neutrality, and then centrifuging and washing to remove inorganic salts to obtain activated flax plant fibers ;
（3）采用膜分离的方法分别回收步骤（2）收集到的预处理液中的碳水化合物组分和残余硫酸；(3) Recover carbohydrate components and residual sulfuric acid in the pretreatment solution collected in step (2) by means of membrane separation;
（4）将步骤（2）得到的亚麻活化植物纤维稀释，盘磨，得活化亚麻植物纤维悬浮液；(4) diluting the activated flax plant fiber obtained in step (2) and grinding to obtain an activated flax plant fiber suspension;
（5）将步骤（4）得到的亚麻活化植物纤维悬浮液高压均质，得到纳米亚麻纤维素悬浮液；(5) high-pressure homogenizing the flax activated plant fiber suspension obtained in step (4) to obtain a nano flax cellulose suspension;
（6）将纳米纤维素悬浮液加热至80～90℃，配成0.5‰～0.9‰,、1‰～1.99%以及2%～3%的三份悬浮液，并搅拌均匀；(6) Heat the nanocellulose suspension to 80～90℃, prepare three suspensions of 0.5‰～0.9‰, 1‰～1.99% and 2%～3%, and stir evenly;
（7）将上述分散均匀的纳米纤维素悬浮液通过流浆箱布浆后均匀地喷涂于成型板上，成型板加热至110～125℃；(7) The above-mentioned uniformly dispersed nanocellulose suspension is sprayed evenly on the forming plate through the headbox, and the forming plate is heated to 110～125℃;
（8）控制成型板的加热长度及纸机车速，使纳米纤维素悬浮液中水分含量降至20～30%，得到纳米纤维素薄膜湿纸页；(8) Control the heating length of the forming plate and the speed of the paper machine, so that the moisture content in the nanocellulose suspension is reduced to 20-30%, and the nanocellulose film wet paper sheet is obtained;
（9） 将纳米纤维素薄膜湿纸页经真空压榨后水分含量降至10～20%，继续将纳米纤维素薄膜湿纸页经烘箱干燥后水分含量降至2.5～6%，得到基于亚麻纤维的多尺度的纳米纤维素薄膜。(9) The moisture content of the nanocellulose film wet paper sheet is reduced to 10-20% after vacuum pressing, and the moisture content of the nanocellulose film wet paper sheet is reduced to 2.5-6% after drying in an oven to obtain a flax fiber-based multiscale nanocellulose films.
进一步地，所述步骤（1）中所述硫酸的质量浓度为35%；所述亚麻植物纤维与硫酸的质量体积比为1g：（6~10）ml。Further, the mass concentration of the sulfuric acid in the step (1) is 35%; the mass-volume ratio of the flax plant fiber to the sulfuric acid is 1 g: (6-10) ml.
进一步地，所述步骤（1）中的水解的温度为32℃，时间为10min。Further, the temperature of the hydrolysis in the step (1) was 32° C. and the time was 10 min.
进一步地，所述步骤（2）中的碱溶液为氢氧化钠溶液、氢氧化钾溶液或者氨水。Further, the alkali solution in the step (2) is sodium hydroxide solution, potassium hydroxide solution or ammonia water.
进一步地，所述步骤（2）中回收的残余硫酸可继续添加到预处理反应过程中。Further, the residual sulfuric acid recovered in the step (2) can be continuously added to the pretreatment reaction process.
进一步地，所述步骤（5）中也可采用纳米纤维素水溶液以及去离子水并混合得悬浮液，将悬浮液在85℃的水浴中搅拌2～3h， 再超声处理5min，然后真空脱泡5min，得到纳米亚麻纤维素悬浮液。Further, in the step (5), an aqueous solution of nanocellulose and deionized water can also be used and mixed to obtain a suspension, the suspension is stirred in a water bath at 85°C for 2-3 hours, and then ultrasonically treated for 5 minutes, and then vacuum defoamed 5min to obtain nano flax cellulose suspension.
进一步地，所述步骤（6）中的搅拌速度为500r/min。Further, the stirring speed in the step (6) is 500r/min.
进一步地，所述步骤（8）中的成型板为聚四氟乙烯板。Further, the forming plate in the step (8) is a polytetrafluoroethylene plate.
进一步地，所述步骤（7）中采用红外加热或者电磁加热预先对成型板进行加热。Further, in the step (7), infrared heating or electromagnetic heating is used to preheat the forming plate.
进一步地，所述步骤（9）中制得的纯纳米纤维素薄膜厚度为10μm。Further, the thickness of the pure nanocellulose film prepared in the step (9) is 10 μm.
上述方法适用于基于亚麻纤维的多尺度纳米纤维素膜制备方法。The above method is applicable to the preparation method of multi-scale nanocellulose film based on flax fiber.
以上所述仅为本申请的优选实施例而已，并不用于限制本申请，对于本领域的技术人员来说，本申请可以有各种更改和变化。凡在本申请的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本申请的保护范围之内。The above descriptions are only preferred embodiments of the present application, and are not intended to limit the present application. For those skilled in the art, the present application may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of this application shall be included within the protection scope of this application.

Claims (10)

  1. 一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，其特征在于：所述基于亚麻纤维的多尺度纳米纤维素膜制备方法包括如下步骤：（1）称取亚麻植物纤维，再加入硫酸水解进行预处理，水解结束后，加入水终止反应，得纤维悬浮液；（2）将步骤（1）得到的纤维悬浮液离心洗涤，收集离心所得液体为预处理液；用碱溶液调节离心所得固体残渣至中性，再离心洗涤，除去无机盐，得活化亚麻植物纤维；（3）采用膜分离的方法分别回收步骤（2）收集到的预处理液中的碳水化合物组分和残余硫酸；（4）将步骤（2）得到的亚麻活化植物纤维稀释，盘磨，得活化亚麻植物纤维悬浮液；（5）将步骤（4）得到的亚麻活化植物纤维悬浮液高压均质，得到纳米亚麻纤维素悬浮液；（6）将纳米纤维素悬浮液加热至80～90℃，配成0.5‰～0.9‰,、1‰～1.99%以及2%～3%的三份悬浮液，并搅拌均匀；A method for preparing a multi-scale nanocellulose film based on flax fiber, characterized in that: the method for preparing a multi-scale nanocellulose film based on flax fiber comprises the following steps: (1) Weighing flax plant fiber, adding sulfuric acid to hydrolyze Pretreatment is carried out, after the hydrolysis is completed, water is added to terminate the reaction to obtain a fiber suspension; (2) the fiber suspension obtained in step (1) is centrifuged and washed, and the liquid obtained by centrifugation is collected as a pretreatment liquid; the solid obtained by centrifugation is adjusted with an alkaline solution The residue is neutralized, and then centrifuged and washed to remove inorganic salts to obtain activated flax plant fibers; (3) The carbohydrate components and residual sulfuric acid in the pretreatment solution collected in step (2) are recovered respectively by membrane separation; ( 4) diluting the activated flax plant fiber obtained in step (2) and grinding to obtain an activated flax plant fiber suspension; (5) homogenizing the activated flax plant fiber suspension obtained in step (4) under high pressure to obtain nano flax fiber (6) Heat the nanocellulose suspension to 80～90℃, prepare three suspensions of 0.5‰～0.9‰, 1‰～1.99% and 2%～3%, and stir evenly;
    （7）将上述分散均匀的纳米纤维素悬浮液通过流浆箱布浆后均匀地喷涂于成型板上，成型板加热至110～125℃；（8）控制成型板的加热长度及纸机车速，使纳米纤维素悬浮液中水分含量降至20～30%，得到纳米纤维素薄膜湿纸页；（9） 将纳米纤维素薄膜湿纸页经真空压榨后水分含量降至10～20%，继续将纳米纤维素薄膜湿纸页经烘箱干燥后水分含量降至2.5～6%，得到纯纳米纤维素薄膜。(7) The uniformly dispersed nanocellulose suspension is sprayed evenly on the forming plate through the headbox, and the forming plate is heated to 110-125°C; (8) The heating length of the forming plate and the speed of the paper machine are controlled. , the moisture content in the nanocellulose suspension is reduced to 20-30%, and the nanocellulose film wet paper sheet is obtained; (9) the moisture content of the nanocellulose film wet paper sheet is reduced to 10-20% after vacuum pressing, The moisture content of the wet paper sheet of the nanocellulose film is further reduced to 2.5-6% after drying in an oven to obtain a pure nanocellulose film.
  2. 根据权利要求1所述的一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，其特征在于：所述步骤（1）中所述硫酸的质量浓度为35%-40%；所述亚麻植物纤维与硫酸的质量体积比为1g：（6~10）ml。The method for preparing a multi-scale nanocellulose film based on flax fiber according to claim 1, wherein the mass concentration of the sulfuric acid in the step (1) is 35%-40%; The mass-volume ratio of fiber to sulfuric acid is 1g:(6~10)ml.
  3. 根据权利要求1所述的一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，其特征在于：所述步骤（1）中的水解的温度为32℃~45℃，时间为10min-30min。The method for preparing a multi-scale nanocellulose film based on flax fiber according to claim 1, wherein the temperature of the hydrolysis in the step (1) is 32°C to 45°C, and the time is 10min-30min.
  4. 根据权利要求1所述的一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，其特征在于：所述步骤（2）中的碱溶液为氢氧化钠溶液、氢氧化钾溶液或者氨水。The method for preparing a multi-scale nanocellulose membrane based on flax fiber according to claim 1, wherein the alkaline solution in the step (2) is sodium hydroxide solution, potassium hydroxide solution or ammonia water.
  5. 根据权利要求1所述的一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，其特征在于：所述步骤（2）中回收的残余硫酸可继续添加到预处理反应过程中。 The method for preparing a multi-scale nanocellulose membrane based on flax fiber according to claim 1, wherein the residual sulfuric acid recovered in the step (2) can be continuously added to the pretreatment reaction process.
  6. 根据权利要求1所述的一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，其特征在于：所述步骤（5）中也可采用纳米纤维素水溶液以及去离子水并混合得悬浮液，将悬浮液在85～95℃的水浴中搅拌2～3h， 再超声处理5～15min，然后真空脱泡5～20min，得到纳米亚麻纤维素悬浮液。The method for preparing a multi-scale nanocellulose membrane based on flax fiber according to claim 1, characterized in that: in the step (5), an aqueous solution of nanocellulose and deionized water can also be used and mixed to obtain a suspension, The suspension is stirred in a water bath at 85 to 95° C. for 2 to 3 hours, and then subjected to ultrasonic treatment for 5 to 15 minutes, and then vacuum defoamed for 5 to 20 minutes to obtain a nano flax cellulose suspension.
  7. 根据权利要求1所述的一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，其特征在于：所述步骤（6）中的搅拌速度为500～700r/min。The method for preparing a multi-scale nanocellulose film based on flax fiber according to claim 1, wherein the stirring speed in the step (6) is 500-700 r/min.
  8. 根据权利要求1所述的一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，其特征在于：所述步骤（8）中的成型板为聚四氟乙烯板。The method for preparing a multi-scale nanocellulose film based on flax fiber according to claim 1, wherein the forming plate in the step (8) is a polytetrafluoroethylene plate.
  9. 根据权利要求1所述的一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，其特征在于：所述步骤（7）中采用红外加热或者电磁加热预先对成型板进行加热。The method for preparing a multi-scale nanocellulose film based on flax fiber according to claim 1, characterized in that: in the step (7), infrared heating or electromagnetic heating is used to preheat the forming plate.
  10. 根据权利要求1所述的一种基于亚麻纤维的多尺度纳米纤维素膜制备方法，其特征在于：所述步骤（9）中制得的纯纳米纤维素薄膜厚度为10μm～60μm。The method for preparing a multi-scale nanocellulose film based on flax fiber according to claim 1, wherein the thickness of the pure nanocellulose film obtained in the step (9) is 10 μm to 60 μm.
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