CN111249757A - Carbon fiber photothermal conversion material and its use in purification and recovery of multi-media solvent - Google Patents
Carbon fiber photothermal conversion material and its use in purification and recovery of multi-media solvent Download PDFInfo
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Abstract
Description
技术领域technical field
本发明涉及一种多介质溶剂纯化回收方法,具体涉及一种采用高效碳纤维作为光热转换材料,通过太阳能溶剂蒸发纯化回收溶剂的方法,属于材料化学和太阳能转换技术领域。The invention relates to a method for purifying and recovering a multi-media solvent, in particular to a method for using high-efficiency carbon fiber as a photothermal conversion material, and purifying and recovering a solvent through solar solvent evaporation, belonging to the technical fields of material chemistry and solar energy conversion.
背景技术Background technique
太阳能作为一种清洁的可再生绿色能源成为近年来能源利用的焦点,太阳能光热转换膜蒸馏技术被认为是一种经济和有效的解决方案。而目前以蒸馏法为主的太阳能溶剂纯化技术普遍存在光热转换效率低和稳定性差,即盐分析出导致蒸发装置老化、耐有机溶剂差等问题,因此对光热转换技术的研究大多数集中在海水淡化、污水处理等方面。As a clean and renewable green energy, solar energy has become the focus of energy utilization in recent years, and solar thermal conversion membrane distillation technology is considered as an economical and effective solution. At present, the solar solvent purification technology mainly based on the distillation method generally has problems such as low photothermal conversion efficiency and poor stability, that is, the salt analysis leads to the aging of the evaporation device and the poor resistance to organic solvents. Therefore, most of the research on photothermal conversion technology focuses on In seawater desalination, sewage treatment and so on.
有机溶剂在生活和生产中广泛应用的有机化合物,分子量不大,它存在于涂料、粘合剂、漆和清洁剂中。有机溶剂种类繁多,使用广泛且用量巨大,有机溶剂不经处理就排入环境,不但有毒副作用,还会在大气的对流层产生酸烟雾、光化学烟雾等,在大气的平流层消耗臭氧,最终会危害人类和动植物的生命安全。现有的有机溶剂纯化回收处理方法无法精处理或精处理效率非常低,没有经济效益,不符合低碳的发展趋势。Organic solvent is an organic compound widely used in life and production, with a small molecular weight, which exists in coatings, adhesives, lacquers and cleaners. There are many kinds of organic solvents, which are widely used and used in huge amounts. Organic solvents are discharged into the environment without treatment, which not only has toxic and side effects, but also produces acid smog and photochemical smog in the troposphere of the atmosphere. The safety of human and animal life. The existing organic solvent purification and recovery treatment methods cannot be refined or have very low refining efficiency, have no economic benefits, and are not in line with the development trend of low carbon.
研发耐有机溶剂、耐高浓度盐腐蚀、高效光热转换材料及光热转换装置,并广泛应用于多种溶剂介质的纯化回收,打破本领域技术壁垒,将切实有力地推动国家绿色、可持续发展进程,具有深远的战略意义和良好的社会效益。Research and develop organic solvent-resistant, high-concentration salt corrosion-resistant, high-efficiency photothermal conversion materials and photothermal conversion devices, which are widely used in the purification and recovery of various solvent media, breaking the technical barriers in this field, and will effectively promote the country's green and sustainable development. The development process has far-reaching strategic significance and good social benefits.
发明内容SUMMARY OF THE INVENTION
本发明的主要目的在于提供一种碳纤维光热转换材料及其制备方法,从而克服现有技术的不足。The main purpose of the present invention is to provide a carbon fiber photothermal conversion material and a preparation method thereof, so as to overcome the deficiencies of the prior art.
本发明的另一目的在于提供所述碳纤维光热转换材料于纯化回收多介质溶剂体系中的用途。Another object of the present invention is to provide the use of the carbon fiber photothermal conversion material in the purification and recovery of a multi-media solvent system.
本发明的又一目的在于提供一种碳纤维光热转换装置。Another object of the present invention is to provide a carbon fiber photothermal conversion device.
为实现前述发明目的,本发明采用的技术方案包括:In order to realize the foregoing invention purpose, the technical scheme adopted in the present invention includes:
本发明实施例提供了一种碳纤维光热转换材料的制备方法,其包括:使包含有碳纤维和0.01~10wt%碳源的水热反应液于温度为150~300℃、压力为0.6~5MPa的条件下水热反应1~24h,从而在碳纤维表面原位生成连续的水热碳层。The embodiment of the present invention provides a preparation method of a carbon fiber photothermal conversion material, which includes: making a hydrothermal reaction solution containing carbon fiber and 0.01-10wt% carbon source at a temperature of 150-300°C and a pressure of 0.6-5MPa Under the condition of hydrothermal reaction for 1-24h, a continuous hydrothermal carbon layer is formed in situ on the surface of carbon fiber.
进一步地,所述碳源包括水溶性糖类物质、水溶性多糖类物质和易水解多糖类物质中的任意一种或两种以上的组合。Further, the carbon source includes any one or a combination of two or more of water-soluble saccharides, water-soluble polysaccharides, and easily hydrolyzed polysaccharides.
本发明实施例还提供了一种碳纤维光热转换材料,其包括碳纤维,所述碳纤维表面原位生长有连续的水热碳层。Embodiments of the present invention also provide a carbon fiber photothermal conversion material, which includes carbon fibers, and a continuous hydrothermal carbon layer is grown on the surface of the carbon fibers in situ.
本发明实施例还提供了由前述方法制备的碳纤维光热转换材料或前述的碳纤维光热转换材料于纯化回收多介质溶剂体系中的用途。The embodiments of the present invention also provide the carbon fiber photothermal conversion material prepared by the foregoing method or the use of the foregoing carbon fiber photothermal conversion material in purifying and recovering a multi-media solvent system.
在一些优选实施例中,所述的用途包括:将多介质溶剂体系与碳纤维光热转换材料接触,并以设定的光线照射碳纤维光热转换材料,使碳纤维光热转换材料进行光热转换并产生热能,从而促使多介质溶剂体系中的至少部分溶剂受热蒸发,实现多介质溶剂体系的纯化回收。In some preferred embodiments, the use includes: contacting the multi-medium solvent system with the carbon fiber photothermal conversion material, and irradiating the carbon fiber photothermal conversion material with a set light, so that the carbon fiber photothermal conversion material performs photothermal conversion and Heat energy is generated, so that at least part of the solvent in the multi-media solvent system is heated and evaporated, so as to realize the purification and recovery of the multi-media solvent system.
本发明实施例还提供了一种碳纤维光热转换装置,其包括由前述方法制备的碳纤维光热转换材料或前述的碳纤维光热转换材料。An embodiment of the present invention also provides a carbon fiber photothermal conversion device, which includes the carbon fiber photothermal conversion material prepared by the foregoing method or the foregoing carbon fiber photothermal conversion material.
在一些优选实施例中,所述的碳纤维光热转换装置包括光热转换膜、液体容器以及冷凝回收单元,所述光热转换膜由所述碳纤维光热转换材料编制形成,当所述液体容器盛装有多介质溶剂体系时,至少是所述光热转换膜的局部区域浮于所述多介质溶剂体系的液面上,且在以设定的光线照射碳纤维光热转换材料时,所述碳纤维光热转换材料能进行光热转换而促使多介质溶剂体系中的至少部分溶剂受热蒸发,所述冷凝回收单元用于将该被蒸发的至少部分溶剂冷凝回收。In some preferred embodiments, the carbon fiber light-to-heat conversion device includes a light-to-heat conversion film, a liquid container, and a condensation recovery unit, and the light-to-heat conversion film is woven from the carbon fiber light-to-heat conversion material. When the multi-media solvent system is contained, at least a local area of the photothermal conversion film floats on the liquid surface of the multi-media solvent system, and when the carbon fiber photothermal conversion material is irradiated with a set light, the carbon fiber The photothermal conversion material can perform photothermal conversion to promote at least part of the solvent in the multi-media solvent system to be heated and evaporated, and the condensation recovery unit is used for condensation recovery of the evaporated at least part of the solvent.
与现有技术相比,本发明的有益效果至少在于:Compared with the prior art, the beneficial effects of the present invention are at least as follows:
本发明提供的高效碳纤维光热转换材料具有高比表面积、高粗糙度和大量的官能团,其在光热转换应用中,具有高效的太阳能转化效率,不仅可用于太阳能高效脱盐、快速水蒸发,而且因高效碳纤维光热转换材料的具有高强度、高化学和结构稳定性、耐有机溶剂等优点,在污水介质、海水、有机溶剂纯化、油水分离等多介质溶剂体系中仍具有高效、稳定的分离性能。同时,本发明提供的多介质溶剂纯化回收方法简单,蒸发效率高,绿色无污染;原材料易得,非常适合工业化生产;碳纤维光热转换装置简单,易于放大。The high-efficiency carbon fiber photothermal conversion material provided by the present invention has high specific surface area, high roughness and a large number of functional groups, and in the application of photothermal conversion, it has high solar energy conversion efficiency, not only can be used for efficient solar energy desalination, fast water evaporation, but also Due to the high strength, high chemical and structural stability, and resistance to organic solvents of high-efficiency carbon fiber photothermal conversion materials, it still has efficient and stable separation in multi-media solvent systems such as sewage media, seawater, organic solvent purification, and oil-water separation. performance. At the same time, the multi-medium solvent purification and recovery method provided by the invention is simple, has high evaporation efficiency, and is green and pollution-free; raw materials are readily available, which is very suitable for industrial production; and the carbon fiber photothermal conversion device is simple and easy to enlarge.
附图说明Description of drawings
图1是本发明一典型实施方案之中高效碳纤维光热转换装置的结构示意图。FIG. 1 is a schematic structural diagram of a high-efficiency carbon fiber photothermal conversion device in a typical embodiment of the present invention.
图2a是本发明实施例1中的碳纤维的扫描电镜图。Figure 2a is a scanning electron microscope image of the carbon fiber in Example 1 of the present invention.
图2b是本发明实施例1中覆盖水热碳层的碳纤维的扫描电镜图。2b is a scanning electron microscope image of the carbon fiber covered with the hydrothermal carbon layer in Example 1 of the present invention.
图3是本发明实施例1中高效碳纤维光热转换装置中染色溶剂蒸发前后染料的紫外吸收谱图。3 is the ultraviolet absorption spectrum of the dye before and after the evaporation of the dyeing solvent in the high-efficiency carbon fiber photothermal conversion device in Example 1 of the present invention.
图4是本发明实施例2中高效碳纤维光热转换装置的实物图。FIG. 4 is a physical diagram of the high-efficiency carbon fiber photothermal conversion device in Example 2 of the present invention.
附图标记说明:1-光热转换膜,2-PS泡沫,3-混合溶液容器,4-倾斜冷凝面板,5-冷凝箱体,6-冷凝液出口。Explanation of reference numerals: 1-light-to-heat conversion film, 2-PS foam, 3-mixed solution container, 4-inclined condensation panel, 5-condensation box, 6-condensate outlet.
具体实施方式Detailed ways
如前所述,鉴于现有技术的不足,本案发明人经长期研究和大量实践,提出了本发明的技术方案,其主要是提供一种高效碳纤维光热转换材料及光热转换装置,以及一种多介质纯化回收方法,此方法为采用高效碳纤维光热转换材料及光热转换装置对包括污水介质、海水、油水乳液体系、印染废溶剂、混合溶剂体系等多介质溶剂体系进行纯化回收。As mentioned above, in view of the deficiencies of the prior art, the inventor of the present invention has proposed the technical solution of the present invention after long-term research and extensive practice, which mainly provides a high-efficiency carbon fiber light-to-heat conversion material and a light-to-heat conversion device, and a A multi-medium purification and recovery method, the method uses high-efficiency carbon fiber photothermal conversion materials and photothermal conversion devices to purify and recover multi-media solvent systems including sewage media, seawater, oil-water emulsion systems, printing and dyeing waste solvents, mixed solvent systems, and the like.
如下将对该技术方案、其实施过程及原理等作进一步的解释说明。The technical solution, its implementation process and principle will be further explained as follows.
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合附图及实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。此外,下面所描述的本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention, but not to limit the present invention. In addition, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.
本发明实施例的一个方面提供了一种碳纤维光热转换材料的制备方法,其包括:使包含有碳纤维和0.01~10wt%碳源的水热反应液于温度为150~300℃、压力为0.6~5MPa的条件下水热反应1~24h,从而在碳纤维表面原位生成连续的水热碳层。One aspect of the embodiments of the present invention provides a method for preparing a carbon fiber photothermal conversion material, comprising: making a hydrothermal reaction solution containing carbon fibers and 0.01-10wt% carbon source at a temperature of 150-300°C and a pressure of 0.6 Under the condition of ~5MPa, the hydrothermal reaction is carried out for 1 ~ 24h, so that a continuous hydrothermal carbon layer is formed in situ on the surface of the carbon fiber.
其中,反应釜压力为0.6~5MPa、温度为150~300℃。Wherein, the pressure of the reactor is 0.6~5MPa, and the temperature is 150~300℃.
进一步地,所述碳源包括天然物质碳源:如水溶性糖类物质、水溶性多糖类物质和易水解多糖类物质等中的任意一种或两种以上的组合,例如,可以优选为葡萄糖、蔗糖、羧甲基纤维素、果糖、麦芽糖等,但不限于此。Further, the carbon source includes a natural material carbon source: such as any one or a combination of two or more in water-soluble carbohydrates, water-soluble polysaccharides, and easily hydrolyzed polysaccharides, for example, can be preferably Glucose, sucrose, carboxymethyl cellulose, fructose, maltose, etc., but not limited thereto.
本发明实施例的另一个方面还提供了一种碳纤维光热转换材料,其包括碳纤维,所述碳纤维表面原位生长有连续的水热碳层。Another aspect of the embodiments of the present invention also provides a carbon fiber photothermal conversion material, which includes carbon fibers, and a continuous hydrothermal carbon layer is grown in-situ on the surfaces of the carbon fibers.
进一步地,所述水热碳层表面具有羰基、醌基和羟基中的任意一种或两种以上的组合的官能团,所述水热碳层的表面粗糙度为5~100nm,所述水热碳层的比表面积为1~5m2/g。Further, the surface of the hydrothermal carbon layer has any one or a combination of functional groups of carbonyl, quinone and hydroxyl groups, the surface roughness of the hydrothermal carbon layer is 5-100 nm, and the hydrothermal carbon layer has a surface roughness of 5-100 nm. The specific surface area of the carbon layer is 1 to 5 m 2 /g.
其中,所述水热碳层具有高比表面积、高粗糙度和大量的官能团,在光热转换应用中,具有高效的太阳能转化效率,不仅可用于太阳能高效脱盐、快速水蒸发,而且因高效碳纤维的高强度、高化学和结构稳定性、耐有机溶剂等优点,在污水介质、海水、有机溶剂纯化、油水分离等多介质溶剂体系中仍具有高效、稳定的分离性能。Among them, the hydrothermal carbon layer has high specific surface area, high roughness and a large number of functional groups, and has high solar energy conversion efficiency in photothermal conversion applications. It has the advantages of high strength, high chemical and structural stability, and resistance to organic solvents, and still has efficient and stable separation performance in multi-media solvent systems such as sewage media, seawater, organic solvent purification, and oil-water separation.
本发明实施例的另一个方面还提供了由前述方法制备的碳纤维光热转换材料或前述的碳纤维光热转换材料于纯化回收多介质溶剂体系中的用途。Another aspect of the embodiments of the present invention also provides the carbon fiber photothermal conversion material prepared by the foregoing method or the use of the foregoing carbon fiber photothermal conversion material in purifying and recovering a multi-media solvent system.
在一些优选实施例中,所述的用途,即一种多介质溶剂纯化回收的方法包括:将多介质溶剂体系与碳纤维光热转换材料接触,并以设定的光线照射碳纤维光热转换材料,使碳纤维光热转换材料进行光热转换并产生热能,从而促使多介质溶剂体系中的至少部分溶剂受热蒸发,实现多介质溶剂体系的纯化回收。In some preferred embodiments, the use, that is, a method for purifying and recovering a multi-media solvent comprises: contacting the multi-media solvent system with the carbon fiber photothermal conversion material, and irradiating the carbon fiber photothermal conversion material with a set light, The carbon fiber photothermal conversion material is made to perform photothermal conversion and generate thermal energy, thereby promoting at least part of the solvent in the multi-media solvent system to be heated and evaporated, and realizing the purification and recovery of the multi-media solvent system.
进一步地,所述设定的光线为太阳光,但不限于此。Further, the set light is sunlight, but not limited thereto.
进一步地,所述多介质溶剂体系包含至少一种挥发性溶剂与至少一种非挥发或难挥发性物质溶质的组合或两种以上挥发性不同的溶剂的组合,例如,可以优选为污水介质、海水、盐水、油水乳液体系、印染废有机溶剂、混合溶剂体系等,但不限于此。Further, the multi-media solvent system comprises a combination of at least one volatile solvent and at least one non-volatile or less volatile material solute or a combination of two or more solvents with different volatility, for example, it may preferably be a sewage medium, Seawater, brine, oil-water emulsion system, printing and dyeing waste organic solvent, mixed solvent system, etc., but not limited to this.
进一步地,所述多介质溶剂体系中的溶剂可以是水、有机溶剂等。Further, the solvent in the multi-media solvent system can be water, organic solvent and the like.
进一步地,所述碳纤维光热转换材料被编织为膜状。Further, the carbon fiber light-to-heat conversion material is woven into a film shape.
综上,本发明提供的多介质溶剂纯化回收方法简单,蒸发效率高,绿色无污染;原材料易得,非常适合工业化生产。In conclusion, the method for purifying and recovering the multi-medium solvent provided by the present invention is simple, has high evaporation efficiency, is green and pollution-free; the raw materials are readily available, and is very suitable for industrial production.
本发明实施例的另一个方面还提供了一种碳纤维光热转换装置,其包括由前述方法制备的碳纤维光热转换材料或前述的碳纤维光热转换材料。Another aspect of the embodiments of the present invention also provides a carbon fiber photothermal conversion device, which includes the carbon fiber photothermal conversion material prepared by the foregoing method or the foregoing carbon fiber photothermal conversion material.
在一些优选实施例中,所述的碳纤维光热转换装置包括光热转换膜、液体容器以及冷凝回收单元,所述光热转换膜由所述碳纤维光热转换材料编制形成,当所述液体容器盛装有多介质溶剂体系时,至少是所述光热转换膜的局部区域浮于所述多介质溶剂体系的液面上,且在以设定的光线照射碳纤维光热转换材料时,所述碳纤维光热转换材料能进行光热转换而促使多介质溶剂体系中的至少部分溶剂受热蒸发,所述冷凝回收单元用于将该被蒸发的至少部分溶剂冷凝回收。In some preferred embodiments, the carbon fiber light-to-heat conversion device includes a light-to-heat conversion film, a liquid container, and a condensation recovery unit, and the light-to-heat conversion film is woven from the carbon fiber light-to-heat conversion material. When the multi-media solvent system is contained, at least a local area of the photothermal conversion film floats on the liquid surface of the multi-media solvent system, and when the carbon fiber photothermal conversion material is irradiated with a set light, the carbon fiber The photothermal conversion material can perform photothermal conversion to promote at least part of the solvent in the multi-media solvent system to be heated and evaporated, and the condensation recovery unit is used for condensation recovery of the evaporated at least part of the solvent.
进一步地,当所述液体容器盛装有多介质溶剂体系时,所述光热转换膜的局部区域浮于所述多介质溶剂体系的液面上,其余区域位于所述多介质溶剂体系的液面下方。Further, when the liquid container contains a multi-media solvent system, a local area of the light-to-heat conversion film floats on the liquid surface of the multi-media solvent system, and the rest of the area is located on the liquid surface of the multi-media solvent system. below.
在一些优选实施例中,所述冷凝回收单元包括冷凝箱体和倾斜设置的冷凝面板,所述冷凝面板扣合在冷凝箱体上部的敞口端处,所述液体容器置于所述冷凝箱体内,且所述冷凝箱体上还设置有冷凝液出口。In some preferred embodiments, the condensation recovery unit includes a condensation tank and a condensing panel arranged obliquely, the condensation panel is fastened at the open end of the upper part of the condensation tank, and the liquid container is placed in the condensation tank Inside the body, and the condensate box is also provided with a condensate outlet.
进一步地,所述冷凝面板的倾斜角度为20-80°。Further, the inclination angle of the condensation panel is 20-80°.
进一步地,所述光热转换膜的至少局部区域结合在浮体材料上部形成双层结构,所述浮体材料的密度小于多介质溶剂体系。Further, at least a partial area of the light-to-heat conversion film is combined on the upper part of the floating body material to form a double-layer structure, and the density of the floating body material is lower than that of the multi-media solvent system.
其中,所述浮体材料的密度低、热导率低隔热性能好、可漂浮于多介质溶剂体系表面,优选可以是PS泡沫,但不限于此,PS泡沫周围的碳纤维光热转换材料伸入多介质溶剂体系内。Wherein, the floating body material has low density, low thermal conductivity, good heat insulation performance, and can float on the surface of the multi-media solvent system, preferably PS foam, but not limited to this, the carbon fiber photothermal conversion material around the PS foam extends into the in a multi-media solvent system.
具体的,请参阅图1所示,为本发明一典型实施例中一种碳纤维光热转换装置的结构示意图。所述碳纤维光热转换装置包括高效碳纤维光热转换材料编制而成的光热转换膜1、PS泡沫2、混合溶液容器3、倾斜冷凝面板4、冷凝箱体5和冷凝液出口6。Specifically, please refer to FIG. 1 , which is a schematic structural diagram of a carbon fiber light-to-heat conversion device in a typical embodiment of the present invention. The carbon fiber photothermal conversion device includes a
所述混合溶液容器3置于冷凝箱体5内,所述倾斜冷凝面板4扣合在冷凝箱体5上部的敞口端处,在冷凝箱体5与混合溶液容器3之间的底部设置有一冷凝液出口6,所述由碳纤维光热转换材料编制而成的光热转换膜1紧密贴合在PS泡沫2的上部构成双层结构,双层结构的光热转换膜1和PS泡沫2漂浮在混合溶液容器3内的混合溶液液面上,PS泡沫周围的碳纤维光热转换材料伸入所述混合溶液内。The
进一步地,所述的PS泡沫密度低、热导率低隔热性能好、可漂浮于混合溶液表面。所述倾斜冷凝面板4的倾斜角度α为20-80°。Further, the PS foam has low density, low thermal conductivity and good thermal insulation performance, and can float on the surface of the mixed solution. The inclination angle α of the
综上所述,本发明提供的碳纤维光热转换装置简单,易于放大。To sum up, the carbon fiber photothermal conversion device provided by the present invention is simple and easy to enlarge.
以下结合若干较佳实施例及附图对本发明的技术方案作进一步的解释说明,但其中的实验条件和设定参数不应视为对本发明基本技术方案的局限。并且本发明的保护范围不限于下述的实施例。The technical solution of the present invention will be further explained below with reference to some preferred embodiments and accompanying drawings, but the experimental conditions and setting parameters therein should not be regarded as limitations to the basic technical solution of the present invention. And the protection scope of the present invention is not limited to the following embodiments.
实施例1Example 1
将葡萄糖配制成3wt%的水溶液,作为水热反应液。将碳纤维100g加入0.5升不锈钢高压反应釜中,加入水热反应液将碳纤维淹没。密封反应釜,压力为0.6MPa,升温至180℃,保温6小时。降温至室温,大量的去离子水清洗五次。将水热碳纤维放入托盘,放进真空烘箱,50℃真空干燥12小时,得到水热碳层覆盖的高效碳纤维光热转换材料。其中,碳纤维的扫描电镜图如图2a所示,覆盖水热碳层的碳纤维的扫描电镜图如图2b所示,水热碳层的表面粗糙度为40nm,比表面积为5m2/g。Glucose was prepared into a 3 wt % aqueous solution as a hydrothermal reaction solution. 100 g of carbon fibers were added to a 0.5-liter stainless steel autoclave, and a hydrothermal reaction solution was added to submerge the carbon fibers. The reaction kettle was sealed, the pressure was 0.6MPa, the temperature was raised to 180°C, and the temperature was kept for 6 hours. Cool to room temperature and wash five times with plenty of deionized water. Put the hydrothermal carbon fiber into a tray, put it into a vacuum oven, and vacuum dry it at 50°C for 12 hours to obtain a high-efficiency carbon fiber photothermal conversion material covered with a hydrothermal carbon layer. The SEM image of the carbon fiber is shown in Figure 2a, and the SEM image of the carbon fiber covered with the hydrothermal carbon layer is shown in Figure 2b. The surface roughness of the hydrothermal carbon layer is 40 nm and the specific surface area is 5 m 2 /g.
将制备的高效碳纤维光热转换材料编制而成光热转换膜,组装到光热转换装置中,并纯化回收含有1000ppm苏丹Ⅲ的二甲基乙酰胺(DMAc)溶液,对高沸点(165.1℃)DMAc溶剂的蒸发速率高达0.98Kg m-2h-1,回收的DMAc含量高达99.99%,光热转换效率高达93%。图3是本实施例中高效碳纤维光热转换装置中染色溶剂蒸发前后染料浓度(紫外吸收谱图)。将制备的水热碳层覆盖的高效碳纤维光热转换材料在DMAc溶剂中长期浸泡,碳纤维无变化,保持强的机械性能及高效光热转换效率。The prepared high-efficiency carbon fiber photothermal conversion material was prepared into a photothermal conversion film, which was assembled into a photothermal conversion device, and a dimethylacetamide (DMAc) solution containing 1000 ppm Sudan III was purified and recovered. The evaporation rate of DMAc solvent is as high as 0.98Kg m -2 h -1 , the recovered DMAc content is as high as 99.99%, and the photothermal conversion efficiency is as high as 93%. Fig. 3 is the dye concentration (ultraviolet absorption spectrum) before and after evaporation of the dyeing solvent in the high-efficiency carbon fiber photothermal conversion device in this embodiment. When the prepared high-efficiency carbon fiber photothermal conversion material covered with a hydrothermal carbon layer is immersed in a DMAc solvent for a long time, the carbon fiber remains unchanged and maintains strong mechanical properties and high photothermal conversion efficiency.
实施例2Example 2
按照实施例1的方法制备水热碳层覆盖的高效碳纤维光热转换材料,然后将制备的高效碳纤维光热转换材料编制而成光热转换膜,组装到光热转换装置(如图4所示)中,并纯化回收油含量10000ppm的油水乳液。经测试,溶剂蒸发速率高达1.25Kg m-2h-1,是自然蒸发速率(0.2Kg m-2h-1)的6倍,纯化回收的水中含油量降低至11.9ppm,光热转换效率高达94%。A high-efficiency carbon fiber photothermal conversion material covered with a hydrothermal carbon layer was prepared according to the method of Example 1, and then the prepared high-efficiency carbon fiber photothermal conversion material was prepared into a photothermal conversion film, which was assembled into a photothermal conversion device (as shown in Figure 4). ), and purified and recovered the oil-water emulsion with an oil content of 10,000 ppm. After testing, the evaporation rate of the solvent is as high as 1.25Kg m -2 h -1 , which is 6 times the natural evaporation rate (0.2Kg m -2 h -1 ), the oil content in the purified and recovered water is reduced to 11.9ppm, and the photothermal conversion efficiency is as high as 94%.
实施例3Example 3
将蔗糖配制成2wt%的水溶液,作为水热反应。将碳纤维100g加入0.5升不锈钢高压反应釜中,加入水热反应液将碳纤维淹没。密封反应釜,压力为0.8MPa,升温至150℃,保温10小时。降温至室温,大量的去离子水清洗五次。将水热碳纤维放入托盘,放进真空烘箱,50℃真空干燥12小时,得到水热碳层覆盖的高效碳纤维光热转换材料,水热碳层的表面粗糙度为35nm,比表面积为4m2/g。Sucrose was formulated into a 2 wt% aqueous solution as a hydrothermal reaction. 100 g of carbon fibers were added to a 0.5-liter stainless steel autoclave, and a hydrothermal reaction solution was added to submerge the carbon fibers. The reaction kettle was sealed, the pressure was 0.8 MPa, the temperature was raised to 150 °C, and the temperature was maintained for 10 hours. Cool to room temperature and wash five times with plenty of deionized water. Put the hydrothermal carbon fiber into the tray, put it in a vacuum oven, and vacuum dry it at 50 °C for 12 hours to obtain a high-efficiency carbon fiber photothermal conversion material covered by a hydrothermal carbon layer. The surface roughness of the hydrothermal carbon layer is 35nm and the specific surface area is 4m2 /g.
将制备的高效碳纤维光热转换材料编制而成光热转换膜,组装到光热转换装置中,并用于浓度为3.5wt%的海水淡化。经测试,水的蒸发速率高达1.47Kg m-2h-1,光热转换效率高达92.5%。The prepared high-efficiency carbon fiber photothermal conversion material is prepared into a photothermal conversion film, which is assembled into a photothermal conversion device and used for seawater desalination with a concentration of 3.5 wt%. After testing, the evaporation rate of water is as high as 1.47Kg m -2 h -1 , and the photothermal conversion efficiency is as high as 92.5%.
实施例4Example 4
将羧甲基纤维素配制成0.01wt%的水溶液,作为水热反应液。将碳纤维100g加入0.5升不锈钢高压反应釜中,加入水热反应液将碳纤维淹没。密封反应釜,压力为5MPa,升温至300℃,保温20小时。降温至室温,大量的去离子水清洗五次。将水热碳纤维放入托盘,放进真空烘箱,50℃真空干燥12小时,得到水热碳层覆盖的高效碳纤维光热转换材料,水热碳层的表面粗糙度为80nm,比表面积为5m2/g。The carboxymethyl cellulose was prepared into a 0.01 wt % aqueous solution as a hydrothermal reaction solution. 100 g of carbon fibers were added to a 0.5-liter stainless steel autoclave, and a hydrothermal reaction solution was added to submerge the carbon fibers. The reaction kettle was sealed, the pressure was 5MPa, the temperature was raised to 300°C, and the temperature was kept for 20 hours. Cool to room temperature and wash five times with plenty of deionized water. Put the hydrothermal carbon fiber into the tray, put it in a vacuum oven, and vacuum dry it at 50 °C for 12 hours to obtain a high-efficiency carbon fiber photothermal conversion material covered by a hydrothermal carbon layer. The surface roughness of the hydrothermal carbon layer is 80nm, and the specific surface area is 5m 2 /g.
将制备的高效碳纤维光热转换材料编制而成光热转换膜,组装到光热转换装置中,处理高浓度死海水体系,其中Na+、K+、Mg2+、Ca2+浓度分别为29198、936、2520、898mg/L,蒸发后Na+、K+、Mg2+、Ca2+浓度分别为9、0.56、0.26、2.03mg/L,达到直饮水标准,室外产水率高达5.4Lm-2day-1,光热转换效率高达93%。The prepared high-efficiency carbon fiber photothermal conversion material is prepared into a photothermal conversion film, which is assembled into a photothermal conversion device to process a high-concentration Dead Sea water system, where the concentrations of Na + , K + , Mg 2+ , and Ca 2+ are 29198 , 936, 2520, 898mg/L, Na + , K + , Mg 2+ , Ca 2+ concentrations were 9, 0.56, 0.26, 2.03mg/L after evaporation, reaching the standard of direct drinking water, and the outdoor water production rate was as high as 5.4Lm -2 day -1 , the photothermal conversion efficiency is as high as 93%.
实施例5Example 5
将果糖配制成10wt%的水溶液,作为水热反应液。将碳纤维100g加入0.5升不锈钢高压反应釜中,加入水热反应液将碳纤维淹没。密封反应釜,压力为1.5MPa,升温至200℃,保温24小时。降温至室温,大量的去离子水清洗五次。将水热碳纤维放入托盘,放进真空烘箱,50℃真空干燥12小时,得到水热碳层覆盖的高效碳纤维光热转换材料,水热碳层的表面粗糙度为100nm,比表面积为5m2/g。The fructose was prepared into a 10wt% aqueous solution as a hydrothermal reaction solution. 100 g of carbon fibers were added to a 0.5-liter stainless steel autoclave, and a hydrothermal reaction solution was added to submerge the carbon fibers. The reaction kettle was sealed, the pressure was 1.5MPa, the temperature was raised to 200°C, and the temperature was kept for 24 hours. Cool to room temperature and wash five times with plenty of deionized water. Put the hydrothermal carbon fiber into the tray, put it in a vacuum oven, and vacuum dry it at 50 °C for 12 hours to obtain a high-efficiency carbon fiber photothermal conversion material covered by a hydrothermal carbon layer. The surface roughness of the hydrothermal carbon layer is 100nm, and the specific surface area is 5m 2 /g.
将制备的高效碳纤维光热转换材料编制而成光热转换膜,组装到光热转换装置中,并纯化回收含有1000ppm苏丹Ⅲ的二甲基甲酰胺DMF溶液,对高沸点(152.8℃)DMF溶剂的蒸发速率高达0.99Kg m-2h-1,回收的DMF含量高达99.99%,光热转换效率高达94%。将制备的水热碳层覆盖的高效碳纤维在DMF溶剂中长期浸泡,碳纤维无变化,保持强的机械性能及高效光热转换效率。The prepared high-efficiency carbon fiber photothermal conversion material was prepared into a photothermal conversion film, which was assembled into a photothermal conversion device, and the dimethylformamide DMF solution containing 1000 ppm Sudan III was purified and recovered. The evaporation rate is as high as 0.99Kg m -2 h -1 , the recovered DMF content is as high as 99.99%, and the photothermal conversion efficiency is as high as 94%. When the prepared high-efficiency carbon fiber covered by the hydrothermal carbon layer is soaked in DMF solvent for a long time, the carbon fiber remains unchanged and maintains strong mechanical properties and high photothermal conversion efficiency.
实施例6Example 6
将麦芽糖配制成3wt%的水溶液,作为水热反应液。将碳纤维100g加入0.5升不锈钢高压反应釜中,加入水热反应液将碳纤维淹没。密封反应釜,压力为2MPa,升温至250℃,保温1小时。降温至室温,大量的去离子水清洗五次。将水热碳纤维放入托盘,放进真空烘箱,50℃真空干燥12小时,得到水热碳层覆盖的高效碳纤维光热转换材料,水热碳层的表面粗糙度为30nm,比表面积为1m2/g。The maltose was prepared into a 3 wt % aqueous solution as a hydrothermal reaction solution. 100 g of carbon fibers were added to a 0.5-liter stainless steel autoclave, and a hydrothermal reaction solution was added to submerge the carbon fibers. The reaction kettle was sealed, the pressure was 2MPa, the temperature was raised to 250°C, and the temperature was kept for 1 hour. Cool to room temperature and wash five times with plenty of deionized water. Put the hydrothermal carbon fiber into the tray, put it in a vacuum oven, and vacuum dry it at 50°C for 12 hours to obtain a high-efficiency carbon fiber photothermal conversion material covered by a hydrothermal carbon layer. The surface roughness of the hydrothermal carbon layer is 30nm and the specific surface area is 1m 2 /g.
制备的高效碳纤维光热转换材料编制而成光热转换膜,组装到光热转换装置中,并纯化回收油含量10000ppm的油水乳液。经测试,溶剂蒸发速率高达1.26Kg m-2h-1,是自然蒸发速率(0.2Kg m-2h-1)的6倍,纯化回收的水中含油量降低至10ppm,光热转换效率高达93%。The prepared high-efficiency carbon fiber photothermal conversion material is prepared into a photothermal conversion film, which is assembled into a photothermal conversion device, and an oil-water emulsion with an oil content of 10,000 ppm is purified and recovered. After testing, the evaporation rate of the solvent is as high as 1.26Kg m -2 h -1 , which is 6 times the natural evaporation rate (0.2Kg m -2 h -1 ), the oil content in the purified and recovered water is reduced to 10ppm, and the photothermal conversion efficiency is as high as 93 %.
此外,本案发明人还利用前文所列出的其它原料以及其它工艺条件等替代实施例1-6中的各种原料及相应工艺条件进行了相应试验,所获高效碳纤维光热转换材料及碳纤维光热转换装置对多介质溶剂的纯化回收效果亦较为理想,基本与实施例1-6产品相似。In addition, the inventors of the present application also carried out corresponding experiments by using other raw materials and other process conditions listed above to replace the various raw materials and corresponding process conditions in Examples 1-6. The obtained high-efficiency carbon fiber photothermal conversion materials and carbon fiber light The purification and recovery effect of the thermal conversion device on the multi-media solvent is also ideal, which is basically similar to that of the products in Examples 1-6.
应当指出,以上所述本发明的具体实施方式,并不构成对本发明保护范围的限定。任何根据本发明的技术构思所作出的各种其他相应的改变与变形,均应包含在本发明权利要求的保护范围内。It should be noted that the specific embodiments of the present invention described above do not limit the protection scope of the present invention. Any other corresponding changes and modifications made according to the technical concept of the present invention shall be included in the protection scope of the claims of the present invention.
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