WO2019047164A1 - 一种氧化石墨烯的制备方法 - Google Patents

一种氧化石墨烯的制备方法 Download PDF

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WO2019047164A1
WO2019047164A1 PCT/CN2017/101055 CN2017101055W WO2019047164A1 WO 2019047164 A1 WO2019047164 A1 WO 2019047164A1 CN 2017101055 W CN2017101055 W CN 2017101055W WO 2019047164 A1 WO2019047164 A1 WO 2019047164A1
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graphene oxide
anode
cathode
solution
water
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PCT/CN2017/101055
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English (en)
French (fr)
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孙红芳
邢锋
李大望
刘剑
丁铸
董必钦
范冰
蔡泽荣
任志丽
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深圳大学
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Priority to PCT/CN2017/101055 priority Critical patent/WO2019047164A1/zh
Publication of WO2019047164A1 publication Critical patent/WO2019047164A1/zh
Priority to ZA201907480A priority patent/ZA201907480B/en

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/182—Graphene
    • C01B32/198—Graphene oxide
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals

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  • the invention belongs to the technical field of material preparation, and in particular relates to a method for preparing graphene oxide.
  • Graphene is a two-dimensional carbon material with a hexagonal honeycomb structure. It has excellent conductivity of 106 ⁇ -1 cm -1 (per ohm per centimeter) and high carrier velocity of 2.0 ⁇ 10 5 cm 2 V -1 s - 1 (square centimeter per volt per second), high theoretical specific surface area 2630 m 2 g -1 (square meter per gram), excellent mechanical properties (Young's modulus 1TPa (Tepa) and high thermal conductivity of approximately 5000 Wm - Excellent properties such as 1 K -1 (watts per meter per degree). Due to the above properties, graphene has attracted extensive attention in the fields of electronics, optical transparent electrodes, chemical catalysis, fuel cells, gas storage, construction, and metal corrosion protection.
  • the commonly used preparation methods of GO include two kinds, one is to form a first-order graphite intercalation compound under the action of strong acid and strong oxidant (such as concentrated nitric acid, aqua regia, concentrated sulfuric acid, etc.), and then the interlayer is The compound continues to undergo deep liquid phase oxidation reaction under the action of excess strong oxidant (such as potassium perchlorate, potassium permanganate, hydrogen peroxide), obtains graphite oxide after hydrolysis, and removes impurities of acid or salt by filtration washing, ultrasonic or
  • the GO material can be obtained by stirring a mixture of graphite oxide and water for a long time.
  • the other is an electrochemical method, that is, graphite as an anode, with strong acid (perchloric acid, sulfuric acid or nitric acid), strong alkali (NaOH) or sulfate (Na 2 SO 4 , K 2 SO 4 , (NH 4 ) 2 SO 4 )
  • the inorganic salt is an electrolyte solution, and after a certain period of time, a suspension solution of GO is obtained.
  • the chemical preparation method of GO may have problems such as generation of harmful gases, more process factors, and complicated process of the preparation process in the preparation process.
  • the GO material prepared by the electrochemical method strong acid or sulfate is generally left. If it is applied to the concrete field, it will cause corrosion to the concrete or the steel bar, thereby affecting the safety and durability of the concrete. Therefore, electrochemically prepared GO materials require rinsing and purification. The purification process of GO is very complicated and takes the most time and cost in the entire production process.
  • the invention provides a preparation method of graphene oxide, which aims to solve the problems of generating harmful gases, having many process factors, complicated process of preparation process, and existing electrochemical preparation in the existing chemical preparation method. In the process, residual strong acid or sulfate causes complications in the corrosion and purification process.
  • the invention provides a method for preparing graphene oxide, comprising:
  • a carbon-containing carbon source is used as an anode, and a conductive material is used as a cathode in the electrolyte water;
  • the solution of the graphene oxide is dried to obtain the graphene oxide.
  • the invention provides a method for preparing graphene oxide.
  • the method for preparing graphene oxide uses water as an electrolyte, and has no pollution, and the graphene oxide has a good dispersion in a solution, and the impurities are less and need no purification, and the preparation process simple.
  • FIG. 1 is a schematic view of an apparatus for preparing graphene oxide provided by the present invention
  • FIG. 2 is a schematic view of a solution of graphene oxide obtained after completion of preparation according to Embodiment 1 of the present invention
  • Example 3 is a scanning electron micrograph of graphene oxide provided in Example 1 of the present invention.
  • Example 4 is a transmission electron micrograph of graphene oxide provided in Example 1 of the present invention.
  • Example 6 is a UV spectrum test chart of graphene oxide provided in Example 1 of the present invention.
  • Example 7 is a Raman test chart of graphene oxide provided in Example 3 of the present invention.
  • Figure 9 is a graph showing the ultraviolet spectrum of graphene oxide prepared in Example 4 of the present invention.
  • Embodiments of the present invention provide a method for preparing graphene oxide, which mainly includes the following steps:
  • a carbon-containing carbon source is used as an anode, and a conductive material is used as a cathode in the electrolyte water;
  • a solution of graphene oxide is obtained by passing a direct current to the anode and the cathode for more than 3 minutes;
  • the solution of graphene oxide is dried to obtain graphene oxide.
  • FIG. 1 is a device for preparing graphene oxide, which uses water as an electrolyte.
  • water molecules are ionized into hydrogen ions and hydroxide ions.
  • the negatively charged hydroxide ions move toward the anode, and the hydroxide ions entering the anode will pull out the graphite layer from the anode, and obtain single or multiple layers of graphene oxide in the electrolyte.
  • Hydrogen ions that do not enter the anode lose electrons near the anode and are oxidized to produce a small amount of oxygen. As shown in Fig.
  • an electrolyte containing graphene oxide is shown.
  • the electrolyte was filtered and dried to obtain a black substance, and the black substance was subjected to scanning electron microscopy and transmission electron microscopy.
  • the substance was in the form of a sheet and the size was different.
  • the material was subjected to UV spectroscopy and Raman testing.
  • Fig. 6 and Fig. 7 in the ultraviolet spectrum test chart, there was a peak at 230 nm (nanometer), and in the Raman test chart, at 1300 cm -1 (per centimeter). Peaks appeared at 1600 cm -1 and the material was confirmed to be graphene oxide.
  • the above method for preparing graphene oxide uses water as an electrolyte, which is non-polluting, and the graphene oxide is preferably dispersed in a solution, the impurities are less, and the preparation process is simple.
  • the electrolyzed water is tap water, deionized water or distilled water.
  • the anode is a carbon fiber composite (Carbon Fiber Reinforced Polymer, CFRP) cloth / board, carbon fiber (Carbon Fiber, CF) Other carbon-containing materials such as cloth/plate or graphite.
  • CFRP Carbon Fiber Reinforced Polymer
  • CFRP Carbon Fiber Reinforced Polymer
  • CFRP Carbon Fiber Reinforced Polymer
  • CF Carbon Fiber
  • the cathode is, but not limited to, a conductive material such as platinum, titanium, iron or graphite. In practical applications, the cathode can be any electrically conductive material.
  • the current of the direct current is 0.5 ⁇ 500 mA.
  • the anode is connected to the anode of the DC power source, and the cathode is connected to the cathode of the DC power source.
  • the solution of graphene oxide may be subjected to filtration or centrifugation before being dried.
  • the distance between the anode and the cathode is from 1 to 100 cm (cm).
  • the degree of oxidation of graphene oxide can be controlled by controlling the distance between the cathode and the anode, the magnitude of the direct current, and the type of anode material.
  • the oxygen generated in the vicinity of the anode etches the anode material, a small amount of nano carbon onion is generated, and the product prepared by the method of the present invention contains graphene oxide and highly oxidized carbon onion, and does not Causes contamination of the electrolyte. It should be noted that when the prepared product is applied to a material such as concrete, the carbon onion does not adversely affect properties such as concrete, and it is not necessary to purify the graphene oxide.
  • the area of the anode is 5 to 1000 cm 2 (cm 2 )
  • the area of the cathode is 5 to 1000 cm 2
  • the distance between the anode and the cathode is 1 to 100 cm.
  • the distance between the anode and the cathode can affect the degree and oxidation of the prepared graphene oxide.
  • the distance between the anode and the cathode is also related to the area of the anode and cathode. The larger the area of the anode and cathode, the greater the distance between the anode and cathode required to produce the same percentage of graphene oxide.
  • the solution of graphene oxide is filtered and dried to obtain graphene oxide.
  • FIG. 2 is a solution of the graphene oxide prepared in the first embodiment, which is filtered and dried after the graphene oxide solution in FIG. TEM observation and UV spectroscopy, as shown in Figure 3 to Figure 6, Figure 3, Figure 4 and Figure 5 show the micro-morphology of graphene oxide, Figure 6 shows the UV spectrum test chart, Figure 6 It is known that a peak appears at 230 nm, indicating that the product is graphene oxide.
  • the solution of graphene oxide is filtered and dried to obtain graphene oxide.
  • a 150 cm 2 carbon fiber cloth was used as an anode, and a 15 cm 2 stainless steel piece was placed as a cathode in electrolyte tap water, and the distance between the CFRP cloth and the stainless steel piece was 2 cm;
  • the carbon fiber cloth is connected to the positive pole of the direct current power source, and the stainless steel piece is connected to the negative pole of the direct current power source, and the solution of graphene oxide is obtained under the conditions of direct current 4, 10, 20 and 30 mA, and the energization time is 3 days;
  • the solution of graphene oxide is filtered and dried to obtain graphene oxide.
  • a 150 cm 2 carbon fiber cloth was used as an anode, and a 15 cm 2 stainless steel piece was placed as a cathode in electrolyte tap water, and the distance between the CFRP cloth and the stainless steel piece was 5 cm;
  • the carbon fiber cloth is connected to the positive pole of the direct current power source, and the stainless steel piece is connected to the negative pole of the direct current power source, and the solution of graphene oxide is obtained under the conditions of direct current 4, 10, 20 and 30 mA, and the energization time is 3 days;
  • the solution of graphene oxide is filtered and dried to obtain graphene oxide.
  • FIGS. 8 and 9 are ultraviolet spectra of the graphene oxide prepared in Example 3 and Example 4, respectively.
  • the ultraviolet spectrum of Fig. 8 and Fig. 9 is very different.
  • the ultraviolet spectrum shown in Fig. 8 there is a small peak at 200 nm, which is a highly oxidized nano carbon onion, and a large peak at 230 nm is low.
  • a slope is formed, indicating that the degree of oxidation and the size of the formed graphene oxide are between the two.

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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Abstract

一种氧化石墨烯的制备方法，该方法包括：将含碳的碳源作为阳极，导电材料作为阴极置于电解液水中，对阳极和阴极通直流电3分钟以上得到氧化石墨烯的溶液，对所述氧化石墨烯的溶液进行干燥处理，得到所述氧化石墨烯。该制备氧化石墨烯的方法中使用水作为电解液，无污染，且氧化石墨烯在溶液中分散液较好，杂质少不需要纯化，制备过程简单。

Description

一种氧化石墨烯的制备方法 技术领域
本发明属于材料制备技术领域，尤其涉及一种氧化石墨烯的制备方法。
背景技术
石墨烯是一种六角形蜂巢结构的二维碳材料，具有优良的导电性106 Ω-1cm-1（每欧姆每厘米）、高载荷子运动速度2.0×105 cm2 V-1 s-1（平方厘米每伏每秒）、高理论比表面积2630 m2g-1（平方米每克） 、优异的力学性能（杨氏模量1TPa （特帕）以及高热导性大约为5000 Wm-1K-1（瓦每米每度）等优良性能。由于上述性能，石墨烯在电子学、光学透明电极、化学催化、燃料电池、气体储藏、建筑、金属防腐等领域引起了广泛的关注。氧化石墨烯（graphene oxide，GO）是石墨烯的衍生物之一，结构与石墨烯相似，只是在其底部平面或者边缘的碳原子链接有含氧官能团（-OH、C-O-C、C=O 以及-COOH等）。由于含氧功能团的存在，GO很容易分散在有机溶剂和水等不同的基体中。例如，GO可与聚合物或陶瓷基体结合增强机械和电性能。
目前，GO常用的制备方法包括两种，一种是将石墨在强酸和强氧化剂（比如浓硝酸、王水、浓硫酸等）的作用下形成一阶的石墨层间化合物，然后将此层间化合物在过量强氧化剂（比如高氯酸钾、高锰酸钾、双氧水）的作用下继续发生深度液相氧化反应，水解后得到氧化石墨，以及通过过滤水洗的方式去除酸或者盐的杂质之后，超声或者长时间搅拌氧化石墨和水的混合物即可获得GO材料。另外一种是电化学方法，即将石墨作为阳极，以强酸 (过氯酸、硫酸或硝酸)、强碱（NaOH）或者硫酸盐（Na2SO4、K2SO4、(NH4)2SO4）等无机盐为电解液，通电一段时间后便得到GO的悬浮溶液。
但是，GO的化学制备方法在制备过程中会存在生成有害气体、工艺因素较多、以及制备过程的工艺复杂等问题。电化学方法制备的GO材料中一般会残留强酸或硫酸盐，若应用于混凝土领域，会对混凝土或钢筋造成腐蚀，进而影响混凝土的安全性和耐久性。因此，电化学制备的GO材料需要冲洗与纯化， GO的纯化过程非常复杂，在整个生产流程中费时最多、成本最高。
 技术问题
本发明提供一种氧化石墨烯的制备方法，旨在解决现有的化学制备方法中，会出现生成有害气体，工艺因素较多，以及制备过程的工艺复杂等问题，以及现有的电化学制备方法中，残留强酸或硫酸盐造成腐蚀和纯化过程复杂的问题。
 技术解决方案
本发明提供的一种氧化石墨烯的制备方法，包括：
将含碳的碳源作为阳极，导电材料作为阴极置于电解液水中；
对所述阳极和所述阴极通直流电3分钟以上得到所述氧化石墨烯的溶液；
对所述氧化石墨烯的溶液进行干燥处理，得到所述氧化石墨烯。
 有益效果
本发明提供的一种氧化石墨烯的制备方法，该制备氧化石墨烯的方法中使用水作为电解液，无污染，且氧化石墨烯在溶液中分散液较好，杂质少不需要纯化，制备过程简单。
附图说明
为了更清楚地说明本发明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发明的一些实施例。
图1是本发明提供的一种氧化石墨烯的制备装置的示意图；
图2是本发明实施例1提供的在制备完成后得到的氧化石墨烯的溶液的示意图；
图3是本发明实施例1提供的氧化石墨烯的扫描电镜图；
图4是本发明实施例1提供的氧化石墨烯的透射电镜图；
图5是本发明实施例1提供的氧化石墨烯的另一透射电镜图；
图6是本发明实施例1提供的氧化石墨烯的紫外光谱测试图；
图7是本发明实施例3提供的氧化石墨烯的拉曼测试图；
图8为本发明实施例3制备得到的氧化石墨烯的紫外光谱图；
图9为本发明实施例4制备得到的氧化石墨烯的紫外光谱图。
 本发明的实施方式
为使得本发明的发明目的、特征、优点能够更加的明显和易懂，下面将结合本发明实施例中的附图，对本发明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发明一部分实施例，而非全部实施例。基于本发明中的实施例，本领域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，都属于本发明保护的范围。
本发明实施例提供一种氧化石墨烯的制备方法，该方法主要包括以下步骤：
将含碳的碳源作为阳极，导电材料作为阴极置于电解液水中；
对阳极和阴极通直流电3分钟以上得到氧化石墨烯的溶液；
对氧化石墨烯的溶液进行干燥处理，得到氧化石墨烯。
本发明提供一种氧化石墨烯的制备方法，如图1所示，图1为制备氧化石墨烯的装置，利用水作为电解液，通直流电时，水分子被电离为氢离子和氢氧根离子，在外加电场的作用下，带负电的氢氧根离子向阳极移动，进入阳极中的氢氧根离子将从阳极中拉出石墨层，在电解液中得到单层或多层的氧化石墨烯。没有进入阳极的氢氧根离子在阳极附近失去电子被氧化产生少量的氧气。如图2所示为包含氧化石墨烯的电解液。对电解液进行过滤和干燥，得到黑色的物质，并对黑色物质进行扫描电镜和透射电镜测试，如图3、图4和图5所示，物质呈片状，大小不同。对物质进行紫外光谱测试和拉曼测试，如图6和图7所示，在紫外光谱测试图中，在230nm（纳米）处存在峰，拉曼测试图中，在1300cm-1（每厘米）和1600cm-1处均有峰出现，证实该物质为氧化石墨烯。上述制备氧化石墨烯的方法中使用水作为电解液，无污染，且氧化石墨烯在溶液中分散液较好，杂质少不需要纯化，制备过程简单。
具体的，电解水为自来水、去离子水或蒸馏水。阳极为碳纤维复合材料（Carbon Fiber Reinforced Polymer，CFRP）布/板、碳纤维（Carbon Fiber，CF）布/板或石墨等其他含碳的材料。阴极为但不限于铂、钛、铁或石墨等导电材料。在实际应用中，阴极可以是任何导电的物质。直流电的电流为0.5~500毫安。在应用时，阳极连接直流电源的正极，阴极连接直流电源的负极。
进一步的，对氧化石墨烯的溶液进行干燥之前还可以进行过滤或离心等处理。
优选地，阳极和所述阴极的距离为1-100cm（厘米）。在实际应用中，可以通过控制阴极和阳极的距离、直流电流的大小、阳极材料的种类来控制氧化石墨烯的氧化程度。
需要说明的是，由于在阳极附近产生的氧气对阳极材料进行刻蚀，会产生少量纳米碳洋葱，本发明所采用的方法制备得到的产物包含了氧化石墨烯和高氧化的碳洋葱，不会使电解液出现污染物。需要说明的是，将制备得到的产物应用于混凝土等材料中时，碳洋葱不会对混凝土之类的性能造成不利影响，不需要对氧化石墨烯进行提纯。
优选地，阳极的面积为5~1000cm2（平方厘米），阴极的面积为5~1000cm2，阳极和阴极之间的距离为1~100cm。需要说明的是，阳极和阴极之间的距离可以影响制备得到的氧化石墨烯的氧化程度和含量，其中，对于相同面积的阳极和阴极，阳极和阴极的距离越近，氧化程度越低，氧化石墨烯的含量越高；阳极和阴极的距离越远，氧化程度越高，氧化石墨烯的含量越低。在实际应用中，阳极和阴极的距离还与阳极和阴极的面积相关，阳极和阴极的面积越大，制备相同百分比的氧化石墨烯所需的阳极和阴极的距离越大。
实施例1
将10cm2的石墨作为阳极，15cm2的不锈钢片作为阴极置于电解液自来水中，石墨和不锈钢片的距离为5cm；
将石墨连接直流电源正极，不锈钢片连接直流电源的负极，在直流电流4、20 和30毫安，通电时间为5天的条件下，得到氧化石墨烯的溶液；
对氧化石墨烯的溶液进行过滤、干燥，得到氧化石墨烯。
其中，请参照图2、图3、图4、图5和图6，图2为实施例1制备得到的氧化石墨烯的溶液，对图2中的氧化石墨烯溶液过滤、干燥后进行扫描电镜、透射电镜观察和紫外光谱测试，如图3到图6所示，图3、图4和图5显示出了氧化石墨烯的微观形貌，图6示出了紫外光谱测试图，由图6可知，在230nm处出现峰，表明产物为氧化石墨烯。
实施例2
将150cm2的CFRP布作为阳极，15cm2的不锈钢片作为阴极置于电解液自来水中，碳纤维和石墨的距离为5cm；
将CFRP布连接直流电源正极，不锈钢片连接直流电源的负极，在直流电流10毫安，通电时间为5天的条件下，得到氧化石墨烯的溶液；
对氧化石墨烯的溶液进行过滤、干燥，得到氧化石墨烯。
实施例3
将150cm2的碳纤维布作为阳极，15cm2的不锈钢片作为阴极置于电解液自来水中，CFRP布和不锈钢片的距离为2cm；
将碳纤维布连接直流电源正极，不锈钢片连接直流电源的负极，在直流电流4、10、20和30毫安，通电时间为3天的条件下，得到氧化石墨烯的溶液；
对氧化石墨烯的溶液进行过滤、干燥，得到氧化石墨烯。
实施例4
将150cm2的碳纤维布作为阳极，15cm2的不锈钢片作为阴极置于电解液自来水中，CFRP布和不锈钢片的距离为5cm；
将碳纤维布连接直流电源正极，不锈钢片连接直流电源的负极，在直流电流4、10、20和30毫安，通电时间为3天的条件下，得到氧化石墨烯的溶液；
对氧化石墨烯的溶液进行过滤、干燥，得到氧化石墨烯。
所得氧化石墨烯的拉曼谱和紫外谱如图7、图8和图9所示，图8和图9分别为实施例3和实施例4制备得到的氧化石墨烯的紫外光谱图。其中，图8和图9的紫外光谱有很大的区别，在图8所示的紫外光谱图中，在200nm处有个小峰，为高氧化的纳米碳洋葱，在230nm处有个大峰为低氧化的氧化石墨烯，但总体上产物以230nm处的氧化石墨烯为主。在图9所示的紫外光谱图中，200nm与230nm之间成了一个坡状，说明生成的氧化石墨烯的氧化程度和片层大小位于二者之间。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (7)

  1. 一种氧化石墨烯的制备方法，其特征在于，所述方法包括：
    将含碳的碳源作为阳极，导电材料作为阴极置于电解液水中；
    对所述阳极和所述阴极通直流电3分钟以上得到所述氧化石墨烯的溶液；
    对所述氧化石墨烯的溶液进行干燥处理，得到所述氧化石墨烯。
  2. 根据权利要求1所述的方法，其特征在于，所述电解水为自来水、去离子水或蒸馏水。
  3. 根据权利要求1所述的方法，其特征在于，所述阳极为碳纤维增强复合材料布/板、碳纤维布/板或石墨。
  4. 根据权利要求1所述的方法，其特征在于，所述阴极为铂、钛、铁或石墨。
  5. 根据权利要求1所述的方法，其特征在于，所述直流电的电流为0.5~500毫安。
  6. 根据权利要求1所述的方法，其特征在于，所述阳极的面积为5~1000平方厘米，所述阴极的面积为5~1000平方厘米。
  7. 根据权利要求6所述的方法，其特征在于，所述阳极和所述阴极的距离为1~100厘米。
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