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CN102241827B - Adjusting method of natural vegetable fiber and polylactic acid interface - Google Patents

Adjusting method of natural vegetable fiber and polylactic acid interface Download PDF

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Publication number
CN102241827B
CN102241827B CN 201110123995 CN201110123995A CN102241827B CN 102241827 B CN102241827 B CN 102241827B CN 201110123995 CN201110123995 CN 201110123995 CN 201110123995 A CN201110123995 A CN 201110123995A CN 102241827 B CN102241827 B CN 102241827B
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natural plant
hexamethyldisiloxane
reaction chamber
polylactic acid
temperature plasma
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CN102241827A (en
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吴义强
李新功
郑霞
李辉
凌启飞
陈卫民
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Central South University of Forestry and Technology
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Abstract

一种天然植物纤维与聚乳酸界面调控方法,以六甲基二硅氧烷热挥发气体作为气体介质,采用低温等离子处理仪在常压下对天然植物纤维进行处理,在天然植物纤维表面沉积超薄硅—氧—碳化合物非极性层,改变天然植物纤维表面性能,从而达到调控天然植物纤维与聚乳酸界面相容性目的。本发明摆脱了组成相存在十分清晰的界面,粘结力差的缺陷,使得应力在界面能有效地传递,可以改善天然植物纤维与聚乳酸相容性,从而提高复合材料的综合性能。A method for regulating the interface between natural plant fibers and polylactic acid, using hexamethyldisiloxane hot volatile gas as the gas medium, using a low-temperature plasma processor to treat the natural plant fibers under normal pressure, and depositing ultra- The thin silicon-oxygen-carbon compound nonpolar layer changes the surface properties of natural plant fibers, thereby achieving the purpose of regulating the interfacial compatibility between natural plant fibers and polylactic acid. The invention gets rid of the defects of very clear interface and poor cohesive force in the composition phase, so that the stress can be effectively transmitted at the interface, and the compatibility between natural plant fiber and polylactic acid can be improved, thereby improving the comprehensive performance of the composite material.

Description

一种天然植物纤维与聚乳酸界面调控方法A method for regulating the interface between natural plant fiber and polylactic acid

技术领域 technical field

本发明涉及一种用于复合材料界面调控方法,属于复合材料制造领域,具体是一种天然植物纤维与聚乳酸界面调控方法。 The invention relates to a method for regulating the interface of composite materials, belonging to the field of composite material manufacturing, in particular to a method for regulating the interface between natural plant fibers and polylactic acid.

背景技术 Background technique

木纤维、竹纤维以及麻纤维等天然植物纤维具有长径比大、比强度高、比表面积大、密度低、价廉以及可再生性和可生物降解等优点,是与聚乳酸等可降解塑料复合制备可生物降解复合材料的优质原料。但是,天然植物纤维是由纤维素、半纤维素、木质素及各种抽提物组成,它是一种不均匀的各向异性材料,界面特性复杂。其主要成分纤维素、半纤维素和木质素等含有大量的极性羟基和酚羟基官能团,使得其表面表现出很强的化学极性,导致植物纤维聚乳酸等生物可降解塑料基材间界面相容性差,微观上呈非均匀体系,两相存在十分清晰的界面,粘结力差,使得应力在界面不能有效地传递,所制备的可生物降解复合材料的物理力学性能显著降低,从而影响复合材料的综合性能。 Natural plant fibers such as wood fiber, bamboo fiber and hemp fiber have the advantages of large aspect ratio, high specific strength, large specific surface area, low density, low price, renewability and biodegradability. Composite preparation of high-quality raw materials for biodegradable composite materials. However, natural plant fiber is composed of cellulose, hemicellulose, lignin and various extracts. It is an inhomogeneous anisotropic material with complex interfacial properties. Its main components, cellulose, hemicellulose, and lignin, contain a large number of polar hydroxyl and phenolic hydroxyl functional groups, making its surface exhibit strong chemical polarity, resulting in the interface between plant fibers, polylactic acid, and other biodegradable plastic substrates. Poor compatibility, microscopically inhomogeneous system, two phases have a very clear interface, poor cohesion, so that the stress cannot be effectively transmitted at the interface, the physical and mechanical properties of the prepared biodegradable composite material are significantly reduced, thus affecting Comprehensive properties of composite materials.

因此,在制备天然植物纤维增强聚乳酸可生物降解复合材料时需要对天然植物纤维与聚乳酸界面进行调控,使亲水的极性天然植物纤维表面与疏水的非极性聚乳酸界面之间具有良好的相容性,使天然植物纤维的表面层与聚乳酸表面层之间达到分子间的融合。 Therefore, when preparing natural plant fiber-reinforced polylactic acid biodegradable composites, it is necessary to regulate the interface between natural plant fibers and polylactic acid, so that there is a positive interaction between the hydrophilic polar natural plant fiber surface and the hydrophobic non-polar polylactic acid interface. Good compatibility enables intermolecular fusion between the surface layer of natural plant fibers and the surface layer of polylactic acid.

发明内容 Contents of the invention

本发明所解决的技术问题在于提供一种天然植物纤维与聚乳酸界面调控方法,改善天然植物纤维与聚乳酸界面相容性,以解决上述背景技术中的缺点。 The technical problem to be solved by the present invention is to provide a method for regulating the interface between natural plant fibers and polylactic acid to improve the interfacial compatibility between natural plant fibers and polylactic acid, so as to solve the above-mentioned shortcomings in the background technology.

本发明所解决的技术问题采用以下技术方案来实现: The technical problem solved by the present invention adopts following technical scheme to realize:

一种天然植物纤维与聚乳酸界面调控方法,区别于其他调控方法的显著特征为:以六甲基二硅氧烷热挥发气体作为改性介质,采用低温等离子处理仪在常压下对天然植物纤维表面进行改性处理,在天然植物纤维表面沉积超薄硅—氧—碳化合物非极性层,改变天然植物纤维表面性能,从而达到调控天然植物纤维与聚乳酸界面相容性目的。 A method for regulating the interface between natural plant fibers and polylactic acid, which is different from other regulating methods in that it uses hot volatile gas of hexamethyldisiloxane as a modification medium, and uses a low-temperature plasma processor to treat natural plants under normal pressure. The surface of the fiber is modified, and an ultra-thin silicon-oxygen-carbon compound non-polar layer is deposited on the surface of the natural plant fiber to change the surface properties of the natural plant fiber, so as to achieve the purpose of regulating the interfacial compatibility between the natural plant fiber and polylactic acid.

具体方法如下: The specific method is as follows:

(1)将500ml的六甲基二硅氧烷倒入容积为三倍容积的圆底烧瓶中,将烧瓶口用带有阀门、接有流量计的耐高温软管与低温等离子体处理仪反应室连接(处理前处于关闭状态)。 (1) Pour 500ml of hexamethyldisiloxane into a round-bottom flask with three times the volume, and use a high-temperature-resistant hose with a valve and a flow meter to react with the low-temperature plasma processor at the mouth of the flask Chamber connections (closed prior to processing).

(2)将装有六甲基二硅氧烷的圆底烧瓶放置在水浴锅上,并将水浴锅温度调定在100℃。 (2) Place the round bottom flask filled with hexamethyldisiloxane on a water bath, and set the temperature of the water bath at 100°C.

(3)称取一定量的天然植物纤维放入低温等离子体处理仪反应室内的载物台。 (3) Weigh a certain amount of natural plant fiber and put it into the stage in the reaction chamber of the low-temperature plasma processing apparatus.

(4)开启低温等离子体处理仪的真空泵抽去反应室内的空气,抽气的同时打开耐高温软管上阀门,将气态的六甲基二硅氧烷充入反应室,调节流量计控制进入反应室气态的六甲基二硅氧烷流量,经过一段时间后达到动态平衡,保持反应室内一个大气压。 (4) Turn on the vacuum pump of the low-temperature plasma processor to pump out the air in the reaction chamber, open the valve on the high-temperature-resistant hose while pumping air, fill the gaseous hexamethyldisiloxane into the reaction chamber, and adjust the flow meter to control the inlet The flow rate of the gaseous hexamethyldisiloxane in the reaction chamber reaches a dynamic equilibrium after a period of time, maintaining an atmospheric pressure in the reaction chamber.

(5)按下低温等离子体处理仪射频功率源开关,调节射频功率,对天然植物纤维进行等离子体处理,处理3min或4min后关闭仪射频功率源开关和耐高温软管上阀门,天然植物纤维取出后可直接用于制备可生物降解复合材料的增强材料。 (5) Press the RF power source switch of the low-temperature plasma processor, adjust the RF power, and perform plasma treatment on natural plant fibers. After 3 minutes or 4 minutes, turn off the RF power source switch of the instrument and the valve on the high-temperature-resistant hose, and the natural plant fibers After being taken out, it can be directly used to prepare reinforcement materials of biodegradable composite materials.

有益效果:利用本发明的方法处理的天然植物纤维表面会沉积一层超薄硅—氧—碳化合物非极性层,可以改善天然植物纤维与聚乳酸相容性,从而实现利用天然植物纤维与聚乳酸复合制备可生物降解复合材料的界面调控。 Beneficial effects: the surface of the natural plant fiber treated by the method of the present invention will deposit a non-polar layer of silicon-oxygen-carbon compound, which can improve the compatibility between the natural plant fiber and polylactic acid, thereby realizing the utilization of natural plant fiber and Interfacial regulation of biodegradable composites prepared by polylactic acid compounding.

具体实施方式 Detailed ways

下面举实例对本发明进行详细描述。 The present invention is described in detail with examples below.

实施例1 Example 1

1、将500ml的六甲基二硅氧烷倒入容积为1500ml的圆底烧瓶中,将烧瓶口用带有阀门、接有流量计的耐高温软管与低温等离子体处理仪反应室连接(处理前处于关闭状态)。 1. Pour 500ml of hexamethyldisiloxane into a round bottom flask with a volume of 1500ml, and connect the mouth of the flask to the reaction chamber of the low temperature plasma processor with a high temperature resistant hose with a valve and a flow meter ( closed before processing).

2、将装有六甲基二硅氧烷的圆底烧瓶放置在水浴锅上,并将水浴锅温度调定在100℃。 2. Place the round bottom flask filled with hexamethyldisiloxane on the water bath, and set the temperature of the water bath at 100°C.

3、称取一定量的天然植物纤维放入低温等离子体处理仪反应室内的载物台。 3. Weigh a certain amount of natural plant fiber and put it into the stage in the reaction chamber of the low-temperature plasma processing apparatus.

4、开启低温等离子体处理仪的真空泵抽去反应室内的空气,抽气的同时打开耐高温软管上阀门,将气态的六甲基二硅氧烷充入反应室,调节流量计控制进入反应室气态的六甲基二硅氧烷流量,经过一段时间后达到动态平衡,保持反应室内一个大气压。 4. Turn on the vacuum pump of the low-temperature plasma processor to pump out the air in the reaction chamber, open the valve on the high-temperature resistant hose while pumping air, fill the gaseous hexamethyldisiloxane into the reaction chamber, and adjust the flow meter to control the reaction. The gaseous hexamethyldisiloxane flow rate in the chamber will reach a dynamic equilibrium after a period of time to maintain an atmospheric pressure in the reaction chamber.

5、按下低温等离子体处理仪射频功率源开关,调节射频功率为30W,对天然植物纤维进行等离子体处理4min,天然植物纤维取出后可直接用于制备可生物降解复合材料的增强材料。 5. Press the RF power source switch of the low-temperature plasma processor, adjust the RF power to 30W, and conduct plasma treatment on the natural plant fibers for 4 minutes. After the natural plant fibers are taken out, they can be directly used to prepare reinforcement materials for biodegradable composite materials.

实施例1主要用于稻草和麦秸类表面含有釉质层的天然植物纤维与聚乳酸界面调控。 Example 1 is mainly used for regulating the interface between natural plant fibers with enamel layer on the surface of rice straw and wheat straw and polylactic acid.

实施例2 Example 2

1、将500ml的六甲基二硅氧烷倒入容积为1500ml的圆底烧瓶中,将烧瓶口用带有阀门、接有流量计的耐高温软管与低温等离子体处理仪反应室连接(处理前处于关闭状态)。 1. Pour 500ml of hexamethyldisiloxane into a round bottom flask with a volume of 1500ml, and connect the mouth of the flask to the reaction chamber of the low temperature plasma processor with a high temperature resistant hose with a valve and a flow meter ( closed before processing).

2、将装有六甲基二硅氧烷的圆底烧瓶放置在水浴锅上,并将水浴锅温度调定在100℃。 2. Place the round bottom flask filled with hexamethyldisiloxane on the water bath, and set the temperature of the water bath at 100°C.

3、称取一定量的天然植物纤维放入低温等离子体处理仪反应室内的载物台。 3. Weigh a certain amount of natural plant fiber and put it into the stage in the reaction chamber of the low-temperature plasma processing apparatus.

4、开启低温等离子体处理仪的真空泵抽去反应室内的空气,抽气的同时打开耐高温软管上阀门,将气态的六甲基二硅氧烷充入反应室,调节流量计控制进入反应室气态的六甲基二硅氧烷流量,经过一段时间后达到动态平衡,保持反应室内一个大气压。 4. Turn on the vacuum pump of the low-temperature plasma processor to pump out the air in the reaction chamber, open the valve on the high-temperature resistant hose while pumping air, fill the gaseous hexamethyldisiloxane into the reaction chamber, and adjust the flow meter to control the reaction. The gaseous hexamethyldisiloxane flow rate in the chamber will reach a dynamic equilibrium after a period of time to maintain an atmospheric pressure in the reaction chamber.

5、按下低温等离子体处理仪射频功率源开关,调节射频功率为20W,对天然植物纤维进行等离子体处理3min,天然植物纤维取出后可直接用于制备可生物降解复合材料的增强材料。 5. Press the RF power source switch of the low-temperature plasma processor, adjust the RF power to 20W, and conduct plasma treatment on the natural plant fibers for 3 minutes. After the natural plant fibers are taken out, they can be directly used to prepare reinforcement materials for biodegradable composite materials.

实施例2主要用于木纤维和竹纤维等表面不含有釉质层的天然植物纤维与聚乳酸界面调控。 Embodiment 2 is mainly used for regulating the interface between natural plant fibers such as wood fibers and bamboo fibers that do not contain an enamel layer and polylactic acid.

以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定                                                

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。 The basic principles and main features of the present invention and the advantages of the present invention have been shown and described above. Those skilled in the industry should understand that the present invention is not limited by the above-mentioned embodiments. What are described in the above-mentioned embodiments and the description only illustrate the principle of the present invention. Without departing from the spirit and scope of the present invention, the present invention will also have Variations and improvements all fall within the scope of the claimed invention. The protection scope of the present invention is defined by the appended claims and their equivalents
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.

Claims (1)

1. a natural plant fibre and poly(lactic acid) interface regulate and control method as gaseous media, adopt the low-temperature plasma processing instrument under normal pressure natural plant fibre to be processed with the hot volatilization gas of hexamethyldisiloxane, it is characterized in that concrete operation method is as follows:
(1) hexamethyldisiloxane of 500ml is poured in the round-bottomed flask that volume is three times of volumes, the flask mouth is used with valve, the Thermostable flexible hose that is connected under meter be connected with Low Temperature Plasma Treating instrument reaction chamber;
The round-bottomed flask that (2) hexamethyldisiloxane will be housed is placed on water-bath, and the water-bath temperature is set up at 100 ℃;
(3) take by weighing the Stage microscope that a certain amount of natural plant fibre is put into Low Temperature Plasma Treating instrument reaction chamber;
(4) vacuum pump of opening the Low Temperature Plasma Treating instrument is taken out the indoor air of dereaction, open valve on the Thermostable flexible hose when bleeding, the hexamethyldisiloxane of gaseous state is filled with reaction chamber, the control of adjust flux meter enters the hexamethyldisiloxane flow of reaction chamber gaseous state, after after a while, reach running balance, keep normal atmosphere in the reaction chamber;
(5) press Low Temperature Plasma Treating instrument radio frequency power source switch, regulate radio frequency power, natural plant fibre is carried out Cement Composite Treated by Plasma, close valve on instrument radio frequency power source switch and the Thermostable flexible hose after processing 3min or 4min, natural plant fibre takes out the strongthener that can be directly used in the preparation biodegradable composite.
CN 201110123995 2011-05-14 2011-05-14 Adjusting method of natural vegetable fiber and polylactic acid interface Expired - Fee Related CN102241827B (en)

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CN1776027A (en) * 2005-12-01 2006-05-24 苏州大学 Diamond-like biomaterial and preparation method thereof
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