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CN108752644A - A kind of the cation modifying nano-cellulose/composite membrane of polyvinyl alcohol and preparation method of high intensity - Google Patents

A kind of the cation modifying nano-cellulose/composite membrane of polyvinyl alcohol and preparation method of high intensity Download PDF

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CN108752644A
CN108752644A CN201810447182.5A CN201810447182A CN108752644A CN 108752644 A CN108752644 A CN 108752644A CN 201810447182 A CN201810447182 A CN 201810447182A CN 108752644 A CN108752644 A CN 108752644A
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polyvinyl alcohol
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modified nanocellulose
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李群
邹杨
段林娟
王新鸽
李颖
张世超
邹竹帆
史亚鹏
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Tianjin University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/08—Cellulose derivatives
    • C08L1/26—Cellulose ethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
    • C08L29/02—Homopolymers or copolymers of unsaturated alcohols
    • C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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    • C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
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    • C08J2301/26—Cellulose ethers
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
    • C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2401/08—Cellulose derivatives
    • C08J2401/26—Cellulose ethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
    • C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/06—Biodegradable

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Abstract

The invention discloses a kind of cation modifying of high intensity nano-cellulose/composite membrane of polyvinyl alcohol and preparation methods, belong to nanocomposite preparation field.Its basic characteristics is, using modified nanometer cellulose as reinforcing agent, to be added in poly-vinyl alcohol solution after carrying out cation modifying processing to nano-cellulose, composite membrane is prepared by the tape casting technique.Cation modifying nano-cellulose/composite membrane of polyvinyl alcohol mechanical property prepared by the present invention is relatively strong and excellent optical performance, biocompatibility, the degradability for retaining composite membrane of polyvinyl alcohol simultaneously have applications well foreground in high-strength degradable packaging material.

Description

一种高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜及 制备方法A high-strength cationized modified nanocellulose/polyvinyl alcohol composite film and Preparation

技术领域technical field

本发明属于纳米复合材料制备领域，具体涉及一种高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜及制备方法。The invention belongs to the field of nanocomposite material preparation, and in particular relates to a high-strength cationized modified nanocellulose/polyvinyl alcohol composite film and a preparation method.

背景技术Background technique

聚乙烯醇(PVA)是一种无毒、可降解的水溶性的线性多羟基聚合物，具有良好的成膜性、阻隔性、生物相容性。近年来，聚乙烯醇在包装领域应用十分广泛，但由于其成膜强度性能的缺陷限制其发展。Polyvinyl alcohol (PVA) is a non-toxic, degradable, water-soluble linear polyhydroxy polymer with good film-forming properties, barrier properties, and biocompatibility. In recent years, polyvinyl alcohol has been widely used in the packaging field, but its development is limited due to the defects of its film-forming strength properties.

纳米纤维素(cellulose nanofibers，CNF)由于其纳米尺度，具有高强度、轻质的特点，同时可再生、可生物降解，被广泛应用于增强复合材料、过滤材料、吸附材料、生物医药材料等领域。纳米纤维素的制备方法包括TEMPO催化氧化法，酶处理，以及高压均质，超声处理等机械处理方法。将纳米纤维素作为增强剂加入聚乙烯醇溶液中，可制备出高强度复合膜，但与聚乙烯醇混合过程中，由于电性相斥，纳米纤维素难以与聚乙烯醇混合均匀，从而影响成膜质量。Due to its nanoscale, cellulose nanofibers (CNF) have the characteristics of high strength, light weight, renewable and biodegradable, and are widely used in reinforced composite materials, filter materials, adsorption materials, biomedical materials and other fields. . The preparation method of nanocellulose includes TEMPO catalytic oxidation method, enzyme treatment, and mechanical treatment methods such as high-pressure homogenization and ultrasonic treatment. Adding nanocellulose as a reinforcing agent to polyvinyl alcohol solution can prepare a high-strength composite film, but in the process of mixing with polyvinyl alcohol, due to electrical repulsion, it is difficult to mix nanocellulose with polyvinyl alcohol evenly, thus affecting Film quality.

而对纳米纤维素进行阳离子化改性能够很好地解决这个问题。阳离子纤维素作为纤维素的衍生物之一，主要通过酯化、醚化或者加成试剂对纳米纤维素的处理，在纤维素链中引入含有叔胺、季铵盐和季磷盐等结构所制备而成，稳定纳米颗粒的同时也附以纳米纤维素新的特性，在纺织印染、环境防护等领域均有应用。阳离子化改性纳米纤维素和PVA极性相近，界面相容性好，都有着良好的可生物降解性，是环境友好型材料。阳离子有着高刚性和高强度，而PVA的刚性和强度相对较弱，制备阳离子化改性纳米纤维素 /PVA复合材料可大大拓宽阳离子化改性纳米纤维素和聚乙烯醇的应用，尤其在高强度可溶性包装材料领域具有广阔应用前景。Cationic modification of nanocellulose can solve this problem well. As one of the derivatives of cellulose, cationic cellulose mainly treats nanocellulose through esterification, etherification or addition reagents, and introduces structures containing tertiary amines, quaternary ammonium salts and quaternary phosphonium salts into the cellulose chain. Prepared, stable nano-particles are also attached with new properties of nano-cellulose, and have applications in textile printing and dyeing, environmental protection and other fields. Cationic modified nanocellulose and PVA have similar polarity, good interfacial compatibility, good biodegradability, and are environmentally friendly materials. The cation has high rigidity and high strength, while the rigidity and strength of PVA are relatively weak. The preparation of cationized modified nanocellulose/PVA composite materials can greatly broaden the application of cationized modified nanocellulose and polyvinyl alcohol, especially in high The field of strength soluble packaging materials has broad application prospects.

发明内容Contents of the invention

本发明主要解决的技术问题是：针对聚乙烯醇复合膜力学性能的不足，从而限制其在包装等领域的应用的问题，提供一种高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜及制各方法。其基本特点是以阳离子化改性纳米纤维素作为增强剂，加入聚乙烯醇溶液中，通过流延法工艺制备出力学性能较强且光学性能优良的高强度复合膜。The main technical problem to be solved by the present invention is to provide a high-strength cationic modified nano-cellulose/polyvinyl alcohol composite film for the lack of mechanical properties of polyvinyl alcohol composite film, which limits its application in packaging and other fields. Membranes and methods of making them. Its basic feature is to use cationized modified nano-cellulose as a reinforcing agent, add it to polyvinyl alcohol solution, and prepare a high-strength composite film with strong mechanical properties and excellent optical properties by casting method.

本发明通过以下技术方案实施：The present invention is implemented through the following technical solutions:

(1)制备阳离子化改性纳米纤维素/聚乙烯醇复合膜成膜液：称取聚乙烯醇和去离子水，水浴下混合得到聚乙烯醇水溶液，将阳离子化改性纳米纤维素以及丙三醇分别加入到聚乙烯醇水溶液中，室温搅拌5～ 10min后水浴超声2h；然后水浴静置消泡5～10min，得到阳离子化改性纳米纤维素/聚乙烯醇复合膜成膜液。(1) Preparation of cationized modified nanocellulose/polyvinyl alcohol composite film film-forming solution: weigh polyvinyl alcohol and deionized water, mix them in a water bath to obtain an aqueous polyvinyl alcohol solution, and mix cationized modified nanocellulose and glycerin Alcohols were added to the polyvinyl alcohol aqueous solution, stirred at room temperature for 5-10 minutes, and then ultrasonicated in a water bath for 2 hours; then the water bath was left to defoam for 5-10 minutes to obtain a cationized modified nanocellulose/polyvinyl alcohol composite film film-forming solution.

(2)制备高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜：将上述成膜液静置冷却后，采用流延法均匀倾倒在玻璃板上，在室温下风干24h，得到高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜。(2) Preparation of high-strength cationized modified nanocellulose/polyvinyl alcohol composite film: After the above-mentioned film-forming liquid is left to cool, it is evenly poured on a glass plate by casting method, and air-dried for 24 hours at room temperature to obtain a high-strength film-forming solution. Strong cationized modified nanocellulose/polyvinyl alcohol composite membrane.

所述阳离子化改性纳米纤维素为醚化改性纳米纤维素。The cationized modified nanocellulose is etherified modified nanocellulose.

所述水浴温度、水浴静置消泡均为70℃。The temperature of the water bath and the static defoaming in the water bath are both 70°C.

所述搅拌为机械搅拌，转速为500r/min～600r/min。The stirring is mechanical stirring, and the rotating speed is 500r/min-600r/min.

所述一种高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜及制备方法中，阳离子化改性纳米纤维素∶聚乙烯醇∶去离子水∶丙三醇重量比为(2～30)∶(4～5)∶(70～100)∶(2～3)。In the described high-strength cationized modified nanocellulose/polyvinyl alcohol composite film and its preparation method, the weight ratio of cationized modified nanocellulose: polyvinyl alcohol: deionized water: glycerol is (2～ 30): (4-5): (70-100): (2-3).

所述一种高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜及制备方法中，膜厚度为18～19μm。In the high-strength cationized modified nano-cellulose/polyvinyl alcohol composite film and its preparation method, the film thickness is 18-19 μm.

与现有技术相比，本发明具有以下优点：Compared with the prior art, the present invention has the following advantages:

(1)本发明采用流延法制备复合膜，工艺流程简单，相比于吹塑法、挤出法等制膜方法，更易操作，大大降低了制膜成本。(1) The present invention adopts the tape-casting method to prepare the composite film, and the process flow is simple. Compared with film-making methods such as blow molding method and extrusion method, it is easier to operate and greatly reduces the film-making cost.

(2)本发明制备的复合膜将阳离子化改性纳米纤维素作为增强剂加入聚乙烯醇膜中，其中对纳米纤维素的阳离子化改性处理，有效地解决了纳米纤维素在聚乙烯醇溶液中易团聚的问题，从而促进其在聚乙烯醇溶液中的均匀分散，使得复合膜力学性能大大提高。(2) The composite film prepared by the present invention adds cationized modified nanocellulose in the polyvinyl alcohol film as a reinforcing agent, wherein the cationic modification of nanocellulose effectively solves the problem of nanocellulose in polyvinyl alcohol The problem of easy agglomeration in the solution, thereby promoting its uniform dispersion in the polyvinyl alcohol solution, greatly improves the mechanical properties of the composite film.

(3)本发明制备的高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜具备优良的光学、力学性能，同时可生物降解，可以扩大聚乙烯醇膜材料在包装、医药等领域的应用。(3) The high-strength cationized modified nanocellulose/polyvinyl alcohol composite film prepared by the present invention has excellent optical and mechanical properties, and is biodegradable at the same time, which can expand the application of polyvinyl alcohol film materials in the fields of packaging, medicine, etc. application.

具体实施方式Detailed ways

下面通过具体实施实例对本发明的最佳实施方案进一步详述。The best embodiment of the present invention will be further described in detail below through specific implementation examples.

1.制备阳离子化改性纳米纤维素/聚乙烯醇复合膜成膜液：称取4g聚乙烯醇，在70℃恒温水浴下加入盛有88ml去离子水的烧杯中，混合搅拌15min后在70℃水浴中消泡5min，制得聚乙烯醇溶液，在聚乙烯醇溶液中依次加入浓度1.0％的阳离子化改性纳米纤维素溶胶、1g丙三醇，室温搅拌10min，将混合液水浴超声2h，置于70℃水浴中消泡5min，制得阳离子化改性纳米纤维素/聚乙烯醇复合膜成膜液；1. Preparation of cationized modified nanocellulose/polyvinyl alcohol composite film film-forming liquid: weigh 4g of polyvinyl alcohol, add it to a beaker containing 88ml of deionized water in a constant temperature water bath at 70°C, mix and stir for 15 minutes, and then set at 70 Defoaming in a water bath at ℃ for 5 minutes to prepare a polyvinyl alcohol solution, sequentially add cationized modified nano-cellulose sol with a concentration of 1.0% and 1 g of glycerol to the polyvinyl alcohol solution, stir at room temperature for 10 minutes, and ultrasonicate the mixed solution in a water bath for 2 hours , placed in a 70°C water bath for defoaming for 5 minutes to prepare a cationized modified nanocellulose/polyvinyl alcohol composite film-forming solution;

2.制备高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜：将阳离子化改性纳米纤维素/聚乙烯醇复合膜成膜液冷却，通过流延法均匀倾倒在玻璃板上，在室温下风干24h后得到高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜。2. Preparation of high-strength cationized modified nanocellulose/polyvinyl alcohol composite film: cooling the cationized modified nanocellulose/polyvinyl alcohol composite film film-forming solution, pouring it evenly on a glass plate by casting method, After air-drying at room temperature for 24 hours, a high-strength cationized modified nanocellulose/polyvinyl alcohol composite film was obtained.

Claims (5)

1.一种高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜及制备方法，其特征在于如下制备步骤：1. A high-strength cationic modified nano-cellulose/polyvinyl alcohol composite film and preparation method, is characterized in that following preparation steps: (1)制备阳离子化改性纳米纤维素/聚乙烯醇复合膜成膜液：称取聚乙烯醇和去离子水，水浴下混合得到聚乙烯醇水溶液，将阳离子化改性纳米纤维素以及丙三醇分别加入到聚乙烯醇水溶液中，室温搅拌后水浴超声2h；然后水浴静置消泡，得到阳离子化改性纳米纤维素/聚乙烯醇复合膜成膜液。(1) Preparation of cationized modified nanocellulose/polyvinyl alcohol composite film film-forming solution: weigh polyvinyl alcohol and deionized water, mix them in a water bath to obtain an aqueous polyvinyl alcohol solution, and mix cationized modified nanocellulose and glycerin Alcohols were respectively added to the polyvinyl alcohol aqueous solution, stirred at room temperature and then ultrasonicated in a water bath for 2 hours; then defoamed in a water bath to obtain a cationized modified nanocellulose/polyvinyl alcohol composite film film-forming liquid. (2)制备高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜：将上述成膜液静置冷却后，采用流延法均匀倾倒在玻璃板上，在室温下风干24h，得到高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜。(2) Preparation of high-strength cationized modified nanocellulose/polyvinyl alcohol composite film: After the above-mentioned film-forming liquid is left to cool, it is evenly poured on a glass plate by casting method, and air-dried for 24 hours at room temperature to obtain a high-strength film-forming solution. Strong cationized modified nanocellulose/polyvinyl alcohol composite membrane. 2.根据权利要求1所述一种高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜及制备方法，其特征在于：所述阳离子化改性纳米纤维素为醚化改性纳米纤维素。2. A high-strength cationized modified nanocellulose/polyvinyl alcohol composite film and its preparation method according to claim 1, characterized in that: said cationized modified nanocellulose is etherified modified nanofiber white. 3.根据权利要求1所述一种高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜及制备方法，其特征在于：步骤(1)所述水浴静置消泡温度为70℃水浴。3. A high-strength cationized modified nanocellulose/polyvinyl alcohol composite film and its preparation method according to claim 1, characterized in that: the defoaming temperature of the water bath in step (1) is 70°C in a water bath . 4.根据权利要求1所述一种高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜及制备方法，其特征在于：复合膜中阳离子化改性纳米纤维素∶聚乙烯醇∶去离子水∶丙三醇重量比为(2～30)∶(4～5)∶(70～100)∶(2～3)。4. a kind of high-strength cationic modified nanocellulose/polyvinyl alcohol composite membrane and preparation method according to claim 1, is characterized in that: cationic modified nanocellulose in the composite membrane: polyvinyl alcohol: remove Ionized water: glycerol weight ratio is (2-30): (4-5): (70-100): (2-3). 5.根据权利要求1所述一种高强度的阳离子化改性纳米纤维素/聚乙烯醇复合膜及制备方法，其特征在于：步骤(2)所述阳离子化改性纳米纤维素/聚乙烯醇复合膜厚度为18～19μm。5. A kind of high-strength cationized modified nanocellulose/polyvinyl alcohol composite film and preparation method according to claim 1, characterized in that: step (2) described cationized modified nanocellulose/polyethylene The thickness of the alcohol composite film is 18-19 μm.
CN201810447182.5A 2018-05-11 2018-05-11 A kind of the cation modifying nano-cellulose/composite membrane of polyvinyl alcohol and preparation method of high intensity Pending CN108752644A (en)

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CN113042112A (en) * 2021-03-16 2021-06-29 福建师范大学 Preparation method of functionalized cation exchange membrane
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