WO2018187921A1 - Improved preparation method for graphene oxide - Google Patents
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- WO2018187921A1 WO2018187921A1 PCT/CN2017/079980 CN2017079980W WO2018187921A1 WO 2018187921 A1 WO2018187921 A1 WO 2018187921A1 CN 2017079980 W CN2017079980 W CN 2017079980W WO 2018187921 A1 WO2018187921 A1 WO 2018187921A1
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- C01B32/198—Graphene oxide
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- the present invention relates to an improved method for preparing graphene oxide, which belongs to the field of preparation of high dielectric materials.
- High dielectric materials are a widely used insulating material, and because of its excellent electrical storage and uniform electric field properties, it has very important applications in the electronics, motor and cable industries. With the development of high performance and size miniaturization of many important electronic devices such as capacitors, resonators, filters, and memories, high dielectric materials are receiving more and more attention. At present, high dielectric materials are widely used. Traditional ceramic materials have high brittleness, high processing temperature and high loss; polymer materials have excellent processing properties, but usually have a low dielectric constant.
- the object of the present invention is to provide an improved method for preparing graphene oxide in order to overcome the deficiencies of materials prepared by conventional preparation methods.
- the present invention adopts the following technical solutions: [0006]
- the present invention provides an improved method for preparing graphene oxide, comprising the following steps:
- Step 1 Pre-oxidation, heating concentrated sulfuric acid, adding potassium persulfate and phosphorus pentoxide, controlling the temperature and stirring until the reactants are all dissolved. After the temperature of the reaction system is lowered, graphite powder is added, and the reactant is added. The mixture was heated with stirring under a water bath, then cooled to room temperature, and the resulting product was stirred at room temperature overnight after dilution;
- Step two washing and drying, suction filtration of the product, and washing, until the solution obtained by the last suction filtration is neutral, and then evaporate the solid on the core funnel into a semi-dry state;
- Step three oxidation, the concentrated sulfuric acid is poured into, and cooled with an ice water bath, and then the above product and potassium permanganate are slowly added without stirring, maintaining the temperature of the reaction system until the reactants are completely dissolved;
- Step 4 terminate the reaction, add deionized water to the reaction system, control the temperature of the reaction system, remove the reactants, add deionized water and stir the reaction;
- Step 5 remove potassium permanganate, add hydrogen peroxide to the reaction system, continue to stir and then stand overnight;
- Step 6 wash and concentrate, remove the supernatant, rinse with HC1 solution, and then reuse Rinse with deionized water until the solution is neutral, and then centrifuge the product to obtain a high concentration of graphite oxide.
- Step 7 Ultrasonic dialysis, the obtained graphite oxide is diluted with water, then subjected to ultrasonic treatment, and dialyzed for one to two weeks to obtain a yellow-brown uniformly dispersed single-layer graphite oxide dilute solution.
- the concentrated sulfuric acid in the above step 1 is 25 mL, and the potassium persulfate and the phosphorus pentoxide are each 5
- the temperature of the reaction system is lowered to 80 ° C, and 6 g of graphite powder is added to form a foam, and the foam gradually subsides within 30 min.
- the reactant is heated under stirring in a water bath at 80 ° C for 4.5 h, then cooled to room temperature, diluted with 1 L of deionized water, and the obtained product is stirred at room temperature overnight.
- the water bath is heated to 35. C, the reaction system continues to react at this temperature for 2 h
- step four as the water is continuously added, the activity of the reactants is continuously lowered until the finally added deionized water no longer causes a significant temperature change.
- the system first changes from dark brown to brown, then to earthy yellow, and finally to orange yellow.
- the hydrogen peroxide in the above step 5 is 25 mL and 30%, and the stirring is continued for 30 minutes.
- the HCl solution in the above step 6 is 5%.
- the improved method for preparing graphene oxide provided by the invention, the prepared graphene oxide comprehensively has the advantages of high conductivity, large specific surface area and good mechanical properties of CEC and CEHEC. Brief description of the diagram
- FIG. 1 is a schematic diagram of a UV-vis spectrum of graphene oxide prepared by the present invention.
- the present invention provides an improved method for preparing graphene oxide.
- the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It is understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention
- the improved method for preparing graphene oxide provided by the embodiment specifically includes the following steps:
- the graphene oxide has two absorption peaks in the test range, which are located near 230 nm and 300 nm, respectively.
- the n electrons on the bond orbit absorb the energy and then transition to the ⁇ * anti-bond orbit.
- the method for preparing the improved graphene oxide provided by the invention has the advantages that the graphene oxide has a high electrical conductivity, a large specific surface area, and good mechanical properties of CEC and CEHEC.
Abstract
Provided is an improved preparation method for graphene oxide. The method comprises pre-oxidation, washing and drying, oxidization, termination reaction, removal of potassium permanganate, washing and concentration, and ultrasonic dialysis, thereby obtaining a graphene oxide solution. The graphene oxide prepared using the method combines the advantages of relatively high electrical conductivity and a relatively large specific surface area of graphene as well as good mechanical properties of cellulose such as CEC and CEHEC.
Description
改进的氧化石墨烯的制备方法 Improved method for preparing graphene oxide
技术领域 Technical field
[0001] 本发明涉及一种改进的氧化石墨烯的制备方法， 属于高介电材料制备领域。 [0001] The present invention relates to an improved method for preparing graphene oxide, which belongs to the field of preparation of high dielectric materials.
背景技术 Background technique
[0002] 高介电材料是一种应用前景非常广泛的绝缘材料， 由于它有着很好的储存电能 和均匀电场的性能， 因而在电子、 电机和电缆行业中都有非常重要的应用。 随 着电容器、 谐振器、 滤波器、 存储器等众多重要电子器件向高性能化和尺寸微 型化方向的发展， 高介电材料受到越来越多的关注。 目前， 高介电材料广泛应 用， 传统的陶瓷材料脆性大、 加工温度高、 损耗大； 聚合物材料具有优良的加 工性能， 但是通常介电常数又较低。 [0002] High dielectric materials are a widely used insulating material, and because of its excellent electrical storage and uniform electric field properties, it has very important applications in the electronics, motor and cable industries. With the development of high performance and size miniaturization of many important electronic devices such as capacitors, resonators, filters, and memories, high dielectric materials are receiving more and more attention. At present, high dielectric materials are widely used. Traditional ceramic materials have high brittleness, high processing temperature and high loss; polymer materials have excellent processing properties, but usually have a low dielectric constant.
技术问题 technical problem
[0003] 目前大部分高介电材料都有各自的局限， 聚合物质轻、 易加工、 具有多尺度结 构和特殊柔韧性等特性， 使得聚合物基复合材料作为新型的高介电材料被广泛 研究。 为改善聚合物基复合材料的综合介电性能， 包括最大限度地提高材料介 电常数、 降低介电损耗以及保证材料的介电强度等， 我们采用聚合物与石墨烯 复合的方法。 石墨烯是由碳原子以 sp 2杂化连接的单原子层构成的新型二维原子 晶体， 其以其优良的力学、 电学、 光学等性能成为纳米材料研究的热点。 [0003] At present, most of the high dielectric materials have their own limitations, the polymer is light, easy to process, has multi-scale structure and special flexibility, so that polymer-based composite materials are widely studied as a new type of high dielectric materials. . In order to improve the comprehensive dielectric properties of polymer-based composites, including maximizing the dielectric constant of materials, reducing dielectric loss, and ensuring the dielectric strength of materials, we use a combination of polymers and graphene. Graphene is a novel two-dimensional atomic crystal composed of a single atomic layer of carbon atoms connected by sp 2 hybridization. It has become a hot spot in nanomaterials research with its excellent mechanical, electrical and optical properties.
问题的解决方案 Problem solution
技术解决方案 Technical solution
[0004] 鉴于上述现有技术的不足之处， 本发明的目的在于提供一种改进的氧化石墨烯 的制备方法。 In view of the above deficiencies of the prior art, it is an object of the present invention to provide an improved method for preparing graphene oxide.
[0005] 本发明的目的是为了克服传统制备方法制备的材料的不足， 提供了一种改进的 氧化石墨烯的制备方法。 为了达到上述目的， 本发明采取了以下技术方案： [0006] 本发明提供了一种改进的氧化石墨烯的制备方法， 包括以下步骤： [0005] The object of the present invention is to provide an improved method for preparing graphene oxide in order to overcome the deficiencies of materials prepared by conventional preparation methods. In order to achieve the above object, the present invention adopts the following technical solutions: [0006] The present invention provides an improved method for preparing graphene oxide, comprising the following steps:
[0007] 步骤一、 预氧化， 对浓硫酸加热， 加入过硫酸钾和五氧化二磷， 控制温度并进 行搅拌直至反应物全部溶解。 将反应体系的温度降低后加入石墨粉， 将反应物
在水浴下搅拌加热， 然后将其冷却至室温， 稀释后将所得的产物在室温下搅拌 过夜； [0007] Step 1. Pre-oxidation, heating concentrated sulfuric acid, adding potassium persulfate and phosphorus pentoxide, controlling the temperature and stirring until the reactants are all dissolved. After the temperature of the reaction system is lowered, graphite powder is added, and the reactant is added. The mixture was heated with stirring under a water bath, then cooled to room temperature, and the resulting product was stirred at room temperature overnight after dilution;
[0008] 步骤二、 洗涤干燥， 抽滤所得产物， 并进行洗涤， 直至最后一次抽滤所得的溶 液为中性， 然后将砂芯漏斗上的固体蒸发为半干状态； [0008] Step two, washing and drying, suction filtration of the product, and washing, until the solution obtained by the last suction filtration is neutral, and then evaporate the solid on the core funnel into a semi-dry state;
[0009] 步骤三、 氧化， 将浓硫酸倒入， 并用冰水浴冷却， 然后依次将上述产物和高锰 酸钾缓慢地加入并不停搅拌， 保持反应体系的温度， 直至反应物完全溶解； [0010] 步骤四、 终止反应， 向反应体系中加入去离子水， 控制反应体系的温度， 将反 应物移出， 再加入去离子水并进行搅拌反应； [0009] Step three, oxidation, the concentrated sulfuric acid is poured into, and cooled with an ice water bath, and then the above product and potassium permanganate are slowly added without stirring, maintaining the temperature of the reaction system until the reactants are completely dissolved; 0010] Step 4, terminate the reaction, add deionized water to the reaction system, control the temperature of the reaction system, remove the reactants, add deionized water and stir the reaction;
[0011] 步骤五、 去除高锰酸钾， 向反应体系中加入过氧化氢， 继续搅拌后静置过夜； [0012] 步骤六、 洗涤浓缩， 除去上清液， 用 HC1溶液冲洗， 然后再用去离子水冲洗， 直至所得的溶液为中性， 再将所得的产物用离心机离心， 得到高浓度的氧化石 墨. [0011] Step 5, remove potassium permanganate, add hydrogen peroxide to the reaction system, continue to stir and then stand overnight; [0012] Step 6, wash and concentrate, remove the supernatant, rinse with HC1 solution, and then reuse Rinse with deionized water until the solution is neutral, and then centrifuge the product to obtain a high concentration of graphite oxide.
[0013] 步骤七、 超声透析， 将所得的氧化石墨加水稀释， 然后进行超声处理， 并透析 一到两周， 即得到黄褐色的均一分散的单层氧化石墨稀溶液。 [0013] Step 7. Ultrasonic dialysis, the obtained graphite oxide is diluted with water, then subjected to ultrasonic treatment, and dialyzed for one to two weeks to obtain a yellow-brown uniformly dispersed single-layer graphite oxide dilute solution.
[0014] 优选的， 上述步骤一中所述浓硫酸为 25 mL， 所述过硫酸钾和五氧化二磷各为 5 [0014] Preferably, the concentrated sulfuric acid in the above step 1 is 25 mL, and the potassium persulfate and the phosphorus pentoxide are each 5
[0015] 优选的， 上述步骤一中将反应体系的温度降低到 80°C， 再加入 6 g石墨粉， 出现 泡沫， 泡沫在 30 min内逐渐消退。 [0015] Preferably, in the above step 1, the temperature of the reaction system is lowered to 80 ° C, and 6 g of graphite powder is added to form a foam, and the foam gradually subsides within 30 min.
[0016] 优选的， 上述步骤一中将反应物在 80°C水浴下搅拌加热 4.5 h， 然后将其冷却至 室温， 用 1 L去离子水稀释， 将所得的产物在室温下搅拌过夜。 [0016] Preferably, in the above step 1, the reactant is heated under stirring in a water bath at 80 ° C for 4.5 h, then cooled to room temperature, diluted with 1 L of deionized water, and the obtained product is stirred at room temperature overnight.
[0017] 优选的， 上述步骤三后将水浴升温至 35。C， 使反应体系在此温度下继续反应 2 h [0017] Preferably, after the above step three, the water bath is heated to 35. C, the reaction system continues to react at this temperature for 2 h
[0018] 优选的， 上述步骤四随着水的不断加入， 反应物的活性不断降低， 直至最后加 入的去离子水不再引起明显的温度变化。 [0018] Preferably, in the above step four, as the water is continuously added, the activity of the reactants is continuously lowered until the finally added deionized water no longer causes a significant temperature change.
[0019] 优选的， 上述步骤五加入过氧化氢的过程中， 体系先由黑褐色变为咖啡色， 再 变为土黄色， 最后变为橙黄色。 [0019] Preferably, in the process of adding hydrogen peroxide in the above step 5, the system first changes from dark brown to brown, then to earthy yellow, and finally to orange yellow.
[0020] 优选的， 上述步骤五中的过氧化氢为 25 mL30%， 继续搅拌吋间为 30min。 [0020] Preferably, the hydrogen peroxide in the above step 5 is 25 mL and 30%, and the stirring is continued for 30 minutes.
[0021] 优选的， 上述步骤六中的 HC1溶液为 5%。
发明的有益效果 [0021] Preferably, the HCl solution in the above step 6 is 5%. Advantageous effects of the invention
有益效果 Beneficial effect
[0022] 本发明提供的改进的氧化石墨烯的制备方法， 制备出的氧化石墨烯综合了石墨 烯具有较高的导电率、 较大的比表面积和 CEC、 CEHEC良好的机械性能等优点 对附图的简要说明 [0022] The improved method for preparing graphene oxide provided by the invention, the prepared graphene oxide comprehensively has the advantages of high conductivity, large specific surface area and good mechanical properties of CEC and CEHEC. Brief description of the diagram
附图说明 DRAWINGS
[0023] 图 1为本发明制备的氧化石墨烯的 UV-vis图谱示意图。 1 is a schematic diagram of a UV-vis spectrum of graphene oxide prepared by the present invention.
本发明的实施方式 Embodiments of the invention
[0024] 本发明提供一种改进的氧化石墨烯的制备方法， 为使本发明的目的、 技术方案 及效果更加清楚、 明确， 以下参照附图并举实施例对本发明进一步详细说明。 应当理解， 此处所描述的具体实施例仅用以解释本发明， 并不用于限定本发明 [0024] The present invention provides an improved method for preparing graphene oxide. The present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It is understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention
[0025] 本实施例提供的改进的氧化石墨烯的制备方法， 具体包括以下步骤： [0025] The improved method for preparing graphene oxide provided by the embodiment specifically includes the following steps:
[0026] 1) 预氧化： 在 100 mL锥形瓶中加入 25 mL浓硫酸， 将温度加热到 90°C， 然后加 入 5 g过硫酸钾和 5 g五氧化二磷， 控制温度在 80~100°C， 搅拌 20 min， 直至反应 物全部溶解。 然后， 将反应体系的温度降低到 80°C， 再加入 6 g石墨粉， 出现泡 沫， 泡沫在 30 min内逐渐消退， 将反应物在 80°C水浴下搅拌加热 4.5 h， 然后将其 冷却至室温， 用 1 L去离子水稀释， 将所得的产物在室温下搅拌过夜。 [0026] 1) Pre-oxidation: Add 25 mL of concentrated sulfuric acid to a 100 mL Erlenmeyer flask, heat the temperature to 90 ° C, then add 5 g of potassium persulfate and 5 g of phosphorus pentoxide to control the temperature at 80-100 Stir at °C for 20 min until the reaction was completely dissolved. Then, the temperature of the reaction system was lowered to 80 ° C, 6 g of graphite powder was added, foam appeared, and the foam gradually subsided within 30 min. The reaction was heated in a water bath at 80 ° C for 4.5 h, and then cooled to It was diluted with 1 L of deionized water at room temperature and the obtained product was stirred at room temperature overnight.
[0027] 2) 洗涤干燥： 抽滤所得产物， 并用大量去离子水洗涤， 直至最后一次抽滤所 得的溶液为中性， 然后将砂芯漏斗上的固体蒸发为半干状态。 2) Washing and drying: The obtained product was suction filtered, and washed with a large amount of deionized water until the solution obtained by the last suction filtration was neutral, and then the solid on the core funnel was evaporated to a semi-dry state.
[0028] 3) 氧化： 将 230 mL浓硫酸倒入 1 L的锥形瓶中， 并用冰水浴冷却到 0°C， 然后 依次将上述产物 （预氧化石墨） 和 30 g高锰酸钾缓慢地加入到锥形瓶中， 其间不 停地搅拌， 并保持反应体系的温度不高于 10°C， 直至反应物完全溶解。 将水浴升 温至 35°C， 使反应体系在此温度下继续反应 2 h。 [0028] 3) Oxidation: Pour 230 mL of concentrated sulfuric acid into a 1 L Erlenmeyer flask and cool to 0 ° C with an ice water bath, then slowly add the above product (pre-oxidized graphite) and 30 g of potassium permanganate in sequence. Add to the Erlenmeyer flask, stirring constantly, and keep the temperature of the reaction system not higher than 10 ° C until the reactants are completely dissolved. The water bath was warmed to 35 ° C, and the reaction system was allowed to continue to react at this temperature for 2 h.
[0029] 4) 终止反应： 向反应体系中加入 460 mL去离子水 （起初去离子水要缓慢地加
入） ， 控制反应体系的温度低于 50°C。 随着水的不断加入， 反应物的活性不断降 低， 直至最后加入的去离子水不再引起明显的温度变化。 将反应物移入 2 L的烧 杯中， 再加入 1.4 L的去离子水， 搅拌反应 2 h。 [0029] 4) Stop the reaction: Add 460 mL of deionized water to the reaction system (initially deionized water should be slowly added) In), the temperature of the reaction system is controlled to be lower than 50 °C. As water continues to be added, the activity of the reactants continues to decrease until the last added deionized water no longer causes significant temperature changes. The reaction was transferred to a 2 L beaker, then 1.4 L of deionized water was added and the reaction was stirred for 2 h.
[0030] 5) 去除高锰酸钾： 向反应体系中加入 25 mL30%的过氧化氢， 在此过程中， 体 系先由黑褐色变为咖啡色， 再变为土黄色， 最后变为橙黄色， 继续搅拌 30 min后 静置过夜。 [0030] 5) Removal of potassium permanganate: 25 mL of 30% hydrogen peroxide was added to the reaction system. In the process, the system first changed from dark brown to brown, then to earthy yellow, and finally to orange-yellow. Stirring was continued for 30 min and allowed to stand overnight.
[0031] 6) 洗涤浓缩： 除去上清液， 用大量的 5%的 HC1溶液冲洗， 然后再用大量的去 离子水冲洗， 直至所得的溶液为中性。 最后将所得的产物用离心机离心， 得到 高浓度的氧化石墨。 6) Washing and concentrating: The supernatant was removed, rinsed with a large amount of 5% HCl solution, and then rinsed with a large amount of deionized water until the resulting solution was neutral. Finally, the obtained product was centrifuged to obtain a high concentration of graphite oxide.
[0032] 7) 超声透析： 将所得的氧化石墨加水稀释， 然后进行超声处理， 并透析一到 两周， 即得到黄褐色的均一分散的单层氧化石墨稀溶液。 7) Ultrasonic dialysis: The obtained graphite oxide was diluted with water, then ultrasonicated, and dialyzed for one to two weeks to obtain a yellow-brown uniformly dispersed single-layer graphite oxide dilute solution.
[0033] 从图 1中可以看出， 氧化石墨烯在测试范围内有两个吸收峰， 分别位于 230 nm 和 300 nm附近。 处于 230 nm处的吸收峰是由于芳香族的 C=C键的 π电子吸收光波 能量后跃迁到 π*反键轨道， 而 300 nm处的较弱的肩峰是由于 C=0键的处于非键 轨道上的 n电子吸收能量后向 π*反键轨道的跃迁。 [0033] As can be seen from FIG. 1, the graphene oxide has two absorption peaks in the test range, which are located near 230 nm and 300 nm, respectively. The absorption peak at 230 nm is due to the π electron absorption of the aromatic C=C bond, which shifts to the π* anti-bond orbital, while the weaker shoulder at 300 nm is due to the C=0 bond. The n electrons on the bond orbit absorb the energy and then transition to the π* anti-bond orbit.
[0034] 本发明提供的改进的氧化石墨烯的制备方法， 制备出的氧化石墨烯综合了石墨 烯具有较高的导电率、 较大的比表面积和 CEC、 CEHEC良好的机械性能等优点 The method for preparing the improved graphene oxide provided by the invention has the advantages that the graphene oxide has a high electrical conductivity, a large specific surface area, and good mechanical properties of CEC and CEHEC.
[0035] [0035]
[0036] 可以理解的是， 对本领域普通技术人员来说， 可以根据本发明的技术方案及其 发明构思加以等同替换或改变， 而所有这些改变或替换都应属于本发明所附的 权利要求的保护范围。
[0036] It is to be understood that those skilled in the art can make equivalent substitutions or changes in accordance with the technical solutions of the present invention and the inventive concepts thereof, and all such changes or substitutions should belong to the appended claims. protected range.
Claims
[权利要求 1] 一种改进的氧化石墨烯的制备方法， 其特征在于： 所述制备方法包括 以下步骤： [Claim 1] An improved method for preparing graphene oxide, characterized in that: the preparation method comprises the following steps:
步骤一、 预氧化， 对浓硫酸加热， 加入过硫酸钾和五氧化二磷， 控制 温度并进行搅拌直至反应物全部溶解； Step one, pre-oxidation, heating concentrated sulfuric acid, adding potassium persulfate and phosphorus pentoxide, controlling the temperature and stirring until the reactants are all dissolved;
将反应体系的温度降低后加入石墨粉， 将反应物在水浴下搅拌加热， 然后将其冷却至室温， 稀释后将所得的产物在室温下搅拌过夜； 步骤二、 洗涤干燥， 抽滤所得产物， 并进行洗涤， 直至最后一次抽滤 所得的溶液为中性， 然后将砂芯漏斗上的固体蒸发为半干状态； 步骤三、 氧化， 将浓硫酸倒入， 并用冰水浴冷却， 然后依次将上述产 物和高锰酸钾缓慢地加入并不停搅拌， 保持反应体系的温度， 直至反 应物完全溶解； After the temperature of the reaction system is lowered, graphite powder is added, and the reactant is heated under stirring in a water bath, and then cooled to room temperature. After dilution, the obtained product is stirred at room temperature overnight; Step 2, washing and drying, and suction-filtering the obtained product, And washing, until the solution obtained by the last suction filtration is neutral, and then evaporating the solid on the core funnel into a semi-dry state; Step 3, oxidizing, pouring concentrated sulfuric acid, and cooling with an ice water bath, and then sequentially The product and potassium permanganate are slowly added without stirring, maintaining the temperature of the reaction system until the reactants are completely dissolved;
步骤四、 终止反应， 向反应体系中加入去离子水， 控制反应体系的温 度， 将反应物移出， 再加入去离子水并进行搅拌反应； Step 4, the reaction is terminated, deionized water is added to the reaction system, the temperature of the reaction system is controlled, the reactant is removed, and deionized water is added and stirred;
步骤五、 去除高锰酸钾， 向反应体系中加入过氧化氢， 继续搅拌后静 置过夜； Step 5, removing potassium permanganate, adding hydrogen peroxide to the reaction system, continuing to stir and then standing overnight;
步骤六、 洗涤浓缩， 除去上清液， 用 HC1溶液冲洗， 然后再用去离子 水冲洗， 直至所得的溶液为中性， 再将所得的产物用离心机离心， 得 到高浓度的氧化石墨； Step 6. Wash and concentrate, remove the supernatant, rinse with HC1 solution, and then rinse with deionized water until the solution is neutral, and then centrifuge the obtained product to obtain high concentration of graphite oxide;
步骤七、 超声透析， 将所得的氧化石墨加水稀释， 然后进行超声处理 ， 并透析一到两周， 即得到黄褐色的均一分散的单层氧化石墨稀溶液 Step 7. Ultrasonic dialysis, the obtained graphite oxide is diluted with water, then subjected to ultrasonic treatment, and dialyzed for one to two weeks to obtain a yellow-brown uniformly dispersed single-layer graphite oxide dilute solution.
[权利要求 2] 如权利要求 1所述的改进的氧化石墨烯的制备方法， 其特征在于： 所 述步骤一中所述浓硫酸为 25 mL， 所述过硫酸钾和五氧化二磷各为 5 g [Claim 2] The method for preparing improved graphene oxide according to claim 1, wherein: in the first step, the concentrated sulfuric acid is 25 mL, and the potassium persulfate and the phosphorus pentoxide are each 5 g
[权利要求 3] 如权利要求 1或 2所述的改进的氧化石墨烯的制备方法， 其特征在于： 所述步骤一中将反应体系的温度降低到 80°C， 再加入 6 g石墨粉， 出 现泡沫， 泡沫在 30 min内逐渐消退。
[Claim 3] The method for preparing improved graphene oxide according to claim 1 or 2, wherein: in the first step, the temperature of the reaction system is lowered to 80 ° C, and then 6 g of graphite powder is added. Foam appeared and the foam gradually subsided within 30 minutes.
[权利要求 4] 如权利要求 1或 2所述的改进的氧化石墨烯的制备方法， 其特征在于： 所述步骤一中将反应物在 80°C水浴下搅拌加热 4.5 h， 然后将其冷却至 室温， 用 1 L去离子水稀释， 将所得的产物在室温下搅拌过夜。 [Claim 4] The method for preparing improved graphene oxide according to claim 1 or 2, wherein: in the step 1, the reactant is heated and heated in a water bath at 80 ° C for 4.5 h, and then cooled. To room temperature, it was diluted with 1 L of deionized water and the obtained product was stirred at room temperature overnight.
[权利要求 5] 如权利要求 1所述的改进的氧化石墨烯的制备方法， 其特征在于： 所 述步骤三后将水浴升温至 35°C， 使反应体系在此温度下继续反应 2 h [Claim 5] The method for preparing improved graphene oxide according to claim 1, wherein: after the third step, the water bath is heated to 35 ° C, and the reaction system is further reacted at the temperature for 2 h.
[权利要求 6] 如权利要求 1所述的改进的氧化石墨烯的制备方法， 其特征在于： 所 述步骤四随着水的不断加入， 反应物的活性不断降低， 直至最后加入 的去离子水不再引起明显的温度变化。 [Claim 6] The method for preparing improved graphene oxide according to claim 1, wherein: in the fourth step, as the water is continuously added, the activity of the reactant is continuously decreased until the last added deionized water. No longer causes significant temperature changes.
[权利要求 7] 如权利要求 1所述的改进的氧化石墨烯的制备方法， 其特征在于： 所 述步骤五加入过氧化氢的过程中， 体系先由黑褐色变为咖啡色， 再变 为土黄色， 最后变为橙黄色。 [Claim 7] The method for preparing improved graphene oxide according to claim 1, wherein: in the process of adding hydrogen peroxide in the step five, the system first changes from dark brown to brown, and then to soil. Yellow, and finally turns orange.
[权利要求 8] 如权利要求 1或 7所述的改进的氧化石墨烯的制备方法， 其特征在于： 所述步骤五中的过氧化氢为 25 mL30% , 继续搅拌吋间为 30min。 [Claim 8] The method for preparing improved graphene oxide according to claim 1 or 7, wherein: the hydrogen peroxide in the step 5 is 25 mL and 30%, and the stirring is continued for 30 minutes.
[权利要求 9] 如权利要求 1所述的改进的氧化石墨烯的制备方法， 其特征在于： 所 述步骤六中的 HC1溶液为 5%。
[Claim 9] The method for producing improved graphene oxide according to claim 1, wherein the HCl solution in the step 6 is 5%.
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