CN110790265A - Inlaying method of potassium ion graphene - Google Patents
Inlaying method of potassium ion graphene Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 229910001414 potassium ion Inorganic materials 0.000 title claims abstract description 90
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 27
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000011591 potassium Substances 0.000 claims abstract description 22
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 7
- 239000011733 molybdenum Substances 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 34
- 230000032798 delamination Effects 0.000 claims description 28
- 239000000203 mixture Substances 0.000 claims description 14
- 239000012071 phase Substances 0.000 claims description 13
- 239000008346 aqueous phase Substances 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 239000000376 reactant Substances 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- -1 ammonium peroxide Chemical class 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 229930006000 Sucrose Natural products 0.000 claims description 6
- XXQBEVHPUKOQEO-UHFFFAOYSA-N potassium superoxide Chemical compound [K+].[K+].[O-][O-] XXQBEVHPUKOQEO-UHFFFAOYSA-N 0.000 claims description 6
- 239000005720 sucrose Substances 0.000 claims description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 5
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 5
- 239000011736 potassium bicarbonate Substances 0.000 claims description 5
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 5
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 5
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 5
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 claims description 3
- XNCSCQSQSGDGES-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]propyl-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)C(C)CN(CC(O)=O)CC(O)=O XNCSCQSQSGDGES-UHFFFAOYSA-N 0.000 claims description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- 125000000185 sucrose group Chemical group 0.000 claims description 3
- 235000015320 potassium carbonate Nutrition 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 230000008595 infiltration Effects 0.000 abstract description 2
- 238000001764 infiltration Methods 0.000 abstract description 2
- 239000003921 oil Substances 0.000 abstract 4
- 239000002199 base oil Substances 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 230000001050 lubricating effect Effects 0.000 abstract 1
- 239000010705 motor oil Substances 0.000 abstract 1
- 229910001415 sodium ion Inorganic materials 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 6
- 238000009736 wetting Methods 0.000 description 6
- 230000007613 environmental effect Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 238000012827 research and development Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
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- 238000005516 engineering process Methods 0.000 description 2
- 238000004299 exfoliation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 description 2
- 235000011181 potassium carbonates Nutrition 0.000 description 2
- 235000002639 sodium chloride Nutrition 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000000859 sublimation Methods 0.000 description 2
- 230000008022 sublimation Effects 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
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- 210000003608 fece Anatomy 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 150000004804 polysaccharides Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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Abstract
Description
技术领域technical field
本发明涉及石墨烯的技术领域，尤其涉及一种钾离子石墨烯的镶嵌方法。The invention relates to the technical field of graphene, in particular to a method for inlaying potassium ion graphene.
背景技术Background technique
钾离子石墨烯镶嵌法，主要是本研发组成员也从事在离子镶嵌质做出的功能性石墨烯上，找寻更多功能特性的应用对接未来石墨烯产业发展科技研究。例如在电池的阴极应用，或阳极应用上等等。据了解也可在不同特性的石墨烯上的功能性方向…为催化反应等等作对应性材料用途目的。钾离子石墨烯镶嵌法也是未来在石墨烯应用科技上一个重要环节之一，当然本文以电池应用上作为基础考虑，以环保和无污染的角度去研发这功能性应用配合。The potassium ion graphene mosaic method is mainly because the members of the R&D team are also engaged in the research on the functional graphene made by the ion mosaic material to find the application of more functional properties to connect the future development of the graphene industry. For example, in cathode applications of batteries, or anode applications, etc. It is understood that the functional direction on graphene with different characteristics can also be used for the purpose of catalyzing reactions and so on for corresponding material purposes. Potassium ion graphene mosaic method is also one of the important links in graphene application technology in the future. Of course, this paper takes battery application as a basic consideration, and develops this functional application from the perspective of environmental protection and pollution-free.
发明内容SUMMARY OF THE INVENTION
针对上述技术中存在的不足之处，本发明提供一种降低成本、操作方便的钾离子石墨烯的镶嵌方法。Aiming at the deficiencies existing in the above-mentioned technologies, the present invention provides a method for inlaying potassium ion graphene with reduced cost and convenient operation.
为了达到上述目的，本发明一种钾离子石墨烯的镶嵌方法，包括如下步骤：In order to achieve the above object, a kind of mosaic method of potassium ion graphene of the present invention, comprises the steps:
将天然鳞片石墨粉以及钾材料分别放入两个不同的钼船器皿中，并放入真空反应釜中抽真空；Put the natural flake graphite powder and potassium material into two different molybdenum vessels respectively, and put them into the vacuum reactor for vacuuming;
采用高周波加热法加热真空反应釜中温度，使所述钾材料中的钾离子升华到所述天然鳞片石墨粉上形成钾离子石墨粉；Adopt high-frequency heating method to heat the temperature in the vacuum reactor, so that potassium ions in the potassium material are sublimated to the natural flake graphite powder to form potassium ion graphite powder;
待所述钾离子石墨粉冷却后，将所述钾离子石墨粉进行水相石墨烯剥离，得到钾离子石墨烯。After the potassium ion graphite powder is cooled, the potassium ion graphite powder is subjected to water-phase graphene peeling to obtain potassium ion graphene.
其中，所述将所述钾离子石墨粉进行水相石墨烯剥离的方法，包括如下步骤：Wherein, the described potassium ion graphite powder is carried out the method for water phase graphene peeling, comprises the following steps:
将所述钾离子石墨粉、拆层剂以及食糖进行混合；Mixing described potassium ion graphite powder, delamination agent and sugar;
搅拌3h-5h，使所述拆层剂充分混合于所述钾离子石墨粉的石墨层之间形成水相混合物；Stir for 3h-5h, so that the delamination agent is fully mixed between the graphite layers of the potassium ion graphite powder to form an aqueous mixture;
将螯合撞击剂加入所述水相混合物中搅拌均匀形成水相反应物；adding the chelating impactor to the aqueous phase mixture and stirring to form an aqueous phase reactant;
所述水相反应物静置反应1-1.5h，形成所述钾离子石墨烯。The aqueous phase reactant is allowed to stand for 1-1.5 hours to form the potassium ion graphene.
其中，所述真空反应釜抽真空为负二至负五个大气压，钾材料与鳞片石墨烯的混合质量比为钾材料：鳞片石墨烯＝1:10-3:10。Wherein, the vacuuming of the vacuum reactor is negative two to negative five atmospheres, and the mixing mass ratio of potassium material and flake graphene is potassium material: flake graphene=1:10-3:10.
其中，所述天然鳞片石墨粉的尺寸为200目-3000目，所述钾材料为碳酸钾以及氢氧化钾中的一种或多种。Wherein, the size of the natural flake graphite powder is 200 mesh-3000 mesh, and the potassium material is one or more of potassium carbonate and potassium hydroxide.
其中，所述食糖为蔗糖，所述蔗糖的加入量按质量分数计算，占所述钾离子石墨粉的0.1％～10％。Wherein, the sugar is sucrose, and the added amount of the sucrose accounts for 0.1% to 10% of the potassium ion graphite powder calculated by mass fraction.
其中，所述拆层剂为碳酸氢钾、碳酸氢铵、过氧化钾以及过氧化铵中的一种或多种，所述拆层剂的加入量按质量分数计算，占所述钾离子石墨粉的10％～20％。Wherein, the delamination agent is one or more of potassium bicarbonate, ammonium bicarbonate, potassium peroxide and ammonium peroxide, and the addition of the delamination agent is calculated by mass fraction, accounting for the potassium ion graphite 10% to 20% of the powder.
其中，所述螯合撞击剂为EDTA、PTDA、PDTA以及HEDTA中的一种或多种，所述螯合撞击剂的加入量按质量分数计算，占所述钾离子石墨粉的10％～20％。Wherein, the chelating impactor is one or more of EDTA, PTDA, PDTA and HEDTA, and the added amount of the chelating impactor is calculated by mass fraction, accounting for 10% to 20% of the potassium ion graphite powder. %.
本发明一种根据权利要求1-7所述的钾离子石墨烯镶嵌方法的应用，将该方法生产的钾离子石墨烯应用于化学电池，作为铝氧电池的阳极使用。A kind of application of the potassium ion graphene mosaic method according to claims 1-7 of the present invention, the potassium ion graphene produced by the method is applied to a chemical battery, and used as an anode of an aluminum-oxygen battery.
本发明的有益效果是：The beneficial effects of the present invention are:
与现有技术相比，本方案通过将钾离子通过升华到天然鳞片石墨粉上，如同镀膜渗入。渗入完成后，再进入水相石墨烯剥离过程，从而得到镶嵌有钾离子的石墨烯。钾离子石墨烯作为功能性石墨烯可以作为化学电池的阳极片，在正负极反应中起到催化作用，可以减少溶液型导电液体的使用，增强化学电池的安全性与实用性。Compared with the prior art, this solution penetrates through the sublimation of potassium ions onto the natural flake graphite powder like a coating film. After the infiltration is completed, the water-phase graphene exfoliation process is performed to obtain graphene embedded with potassium ions. As functional graphene, potassium ion graphene can be used as the anode sheet of chemical battery, which plays a catalytic role in positive and negative reactions, which can reduce the use of solution-type conductive liquid and enhance the safety and practicability of chemical battery.
附图说明Description of drawings
图1为本发明钾离子石墨烯的镶嵌方法的流程示意图；Fig. 1 is the schematic flow sheet of the mosaic method of potassium ion graphene of the present invention;
图2为本发明钾离子石墨粉进行水相剥离的方法流程示意图。Fig. 2 is the schematic flow chart of the method for the potassium ion graphite powder of the present invention to carry out water phase exfoliation.
具体实施方式Detailed ways
为了更清楚地表述本发明，下面结合附图对本发明作进一步地描述。In order to express the present invention more clearly, the present invention will be further described below with reference to the accompanying drawings.
参阅图1，本发明一种钾离子石墨烯的镶嵌方法，包括如下步骤：Referring to Fig. 1, a kind of mosaic method of potassium ion graphene of the present invention, comprises the steps:
步骤S100，原材料准备：Step S100, raw material preparation:
将天然鳞片石墨粉以及钾材料分别放入两个不同的钼船器皿中，并放入真空反应釜中抽真空；真空反应釜抽真空为负二至负五个大气压，钾材料与鳞片石墨烯的混合质量比为钾材料：鳞片石墨烯＝1:10-3:10；所述天然鳞片石墨粉的尺寸为200目-3000目，所述钾材料为碳酸钾以及氢氧化钾中的一种或多种。Put natural flake graphite powder and potassium material into two different molybdenum vessels respectively, and put into vacuum reactor for vacuuming; vacuum reactor vacuuming is negative two to negative five atmospheres, potassium material and scale graphene The mixing mass ratio is potassium material: flake graphene=1:10-3:10; the size of described natural flake graphite powder is 200 orders-3000 orders, and described potassium material is a kind of in potassium carbonate and potassium hydroxide or more.
步骤S200，钾离子高温升华：Step S200, high temperature sublimation of potassium ions:
采用高周波加热法加热真空反应釜中温度，使所述钾材料中的钾离子升华到所述天然鳞片石墨粉上形成钾离子石墨粉；Adopt high-frequency heating method to heat the temperature in the vacuum reactor, so that potassium ions in the potassium material are sublimated to the natural flake graphite powder to form potassium ion graphite powder;
步骤S300，石墨烯水相剥离：Step S300, the graphene water phase is peeled off:
待所述钾离子石墨粉冷却后，将所述钾离子石墨粉进行水相石墨烯剥离，得到钾离子石墨烯。After the potassium ion graphite powder is cooled, the potassium ion graphite powder is subjected to water-phase graphene peeling to obtain potassium ion graphene.
在天然鳞片石墨粉上加工，先把钾离子用真空加温升华钾离子进入到石鳞片石墨上。仿用真空镀膜原理，把钾离子镀入鳞片石墨上，再通过水体石墨烯浆料生产法生产出带钾离子特性的功能石墨烯出来。可方便为日后电池应用上发挥效果，包括一些催化应用上。To process on the natural flake graphite powder, the potassium ions are first sublimated by vacuum heating to enter the flake graphite. By imitating the principle of vacuum coating, potassium ions are plated on flake graphite, and then functional graphene with potassium ion characteristics is produced by the water body graphene slurry production method. It can be convenient for future battery applications, including some catalytic applications.
请进一步参阅图2，将所述钾离子石墨粉进行水相石墨烯剥离的方法，包括如下步骤：Please further refer to Fig. 2, the method that described potassium ion graphite powder is carried out water phase graphene peeling, comprises the following steps:
S310、将所述钾离子石墨粉、拆层剂以及食糖进行混合；所述食糖为蔗糖，所述蔗糖的加入量按质量分数计算，占所述钾离子石墨粉的0.1％～10％。所述拆层剂为碳酸氢钾、碳酸氢铵、过氧化钾以及过氧化铵中的一种或多种，所述拆层剂的加入量按质量分数计算，占所述钾离子石墨粉的10％～20％。S310, mixing the potassium ion graphite powder, the delamination agent and the sugar; the sugar is sucrose, and the added amount of the sucrose is calculated by mass fraction, accounting for 0.1%-10% of the potassium ion graphite powder. Described delamination agent is one or more in potassium bicarbonate, ammonium bicarbonate, potassium peroxide and ammonium peroxide, and the add-on of described delamination agent is calculated by mass fraction, accounting for the potassium ion graphite powder. 10% to 20%.
S320、搅拌3h-5h，使所述拆层剂充分混合于所述钾离子石墨粉的石墨层之间形成水相混合物；S320, stirring for 3h-5h, so that the delamination agent is fully mixed between the graphite layers of the potassium ion graphite powder to form an aqueous phase mixture;
拆层剂是必要的，然而拆层剂在现在应用上都是两大类。就是酸性和碱性方面，但是我们发展的方向在石墨烯研发领域上。我们都是以环保方向，达到零排放的目的进发。于是我们研发拆层剂方面都用食品级和环保上的基础入手，这是我们从事石墨烯工业化和量产化的技术定位。Delamination agents are necessary, but delamination agents are currently used in two categories. It is acidity and alkalinity, but the direction of our development is in the field of graphene research and development. We are all in the direction of environmental protection, to achieve the goal of zero emissions. Therefore, we start with the basis of food grade and environmental protection in the research and development of delamination agents, which is our technical positioning for the industrialization and mass production of graphene.
首先我们应用拆层剂的配方方面，不用任何强酸和强碱方面的材料为主。业界很多时用了强酸和强碱后…又要在环保处理上花一翻工夫，也最怕带来污染的后遗症。而我们开发鳞片石墨应用的拆层剂，所做出来的石墨烯是严格的环保和零排放要求。所以多年来，我们都以食品级的材料去研发拆层剂。First of all, we use the formulation of the delamination agent, and do not use any strong acid and strong alkali materials. The industry has used strong acids and alkalis for a lot of time...and they have to spend a lot of time on environmental protection treatment, and they are most afraid of the sequelae of pollution. And we develop a layer-removing agent for flake graphite application, and the graphene produced is strictly environmental protection and zero-emission requirements. Therefore, over the years, we have used food-grade materials to develop delamination agents.
在食品级的拆层剂上，我们都被免应用钠离子化合物材料。当然，如氯化钠是食盐，但是我们都不应用带有钠离子的化合物。原因，制造石墨烯过程中，尤其是在水相中处理时。用了钠离子就不能排走了，原因在内陆上带有钠离子的化合物是不能应用于植物灌溉上。因钠离子是逆制植物生长的，甚至谁多科学指出，人畜粪便都不可以做肥料…原因是与钠离子有关。所以我们应用的拆层上是没有钠离子的化合物基础上的食品级材料，一般以钾基底和胺基底的化合物为主。We are free from the use of sodium ion compound materials on food-grade delamination agents. Of course, as sodium chloride is table salt, but we don't use compounds with sodium ions. The reason, during the manufacturing of graphene, especially when it is processed in the aqueous phase. When sodium ions are used, they cannot be removed, because compounds with sodium ions in the inland cannot be used for plant irrigation. Because sodium ions are counterproductive to plant growth, no one even scientifically pointed out that human and animal manures cannot be used as fertilizers... The reason is that it is related to sodium ions. Therefore, the demolition layer we apply is food-grade materials based on compounds without sodium ions, generally based on potassium-based and amine-based compounds.
S330、将螯合撞击剂加入所述水相混合物中搅拌均匀形成水相反应物；所述螯合撞击剂为EDTA、PTDA、PDTA以及HEDTA中的一种或多种，所述螯合撞击剂的加入量按质量分数计算，占所述钾离子石墨粉的10％～20％。S330, adding a chelating impactor to the aqueous phase mixture and stirring to form an aqueous reactant; the chelating impactor is one or more of EDTA, PTDA, PDTA and HEDTA, and the chelating impactor is The added amount of potassium ion is calculated by mass fraction, accounting for 10% to 20% of the potassium ion graphite powder.
S340、所述水相反应物静置反应1-1.5h，形成所述钾离子石墨烯。S340, the aqueous phase reactant is allowed to stand and react for 1-1.5 hours to form the potassium ion graphene.
本发明一种根据权利要求1-7所述的钾离子石墨烯镶嵌方法的应用，将该方法生产的钾离子石墨烯应用于化学电池，作为铝氧电池的阳极使用。A kind of application of the potassium ion graphene mosaic method according to claims 1-7 of the present invention, the potassium ion graphene produced by the method is applied to a chemical battery, and used as an anode of an aluminum-oxygen battery.
加上配比的糖后，润湿速度和渗透上，比原来的速度会快上七到八倍。一般都可有三小时内完成拆层剂的渗透和润湿能力，而且省电和时间…是供大形量产应用上的一个有效方法。糖这种物质由于是分子结构是多聚和多糖链，对天然鳞片石墨粉的水溶润湿中非常有效，加上配合我们的多种复方式拆层剂，如多聚碳酸螯合物和过氧化合物等配合，甚至在拆层剂中带镶嵌离子金属等，都可作很好的润湿配合。在实验中，我们发现，天然鳞片石墨粉很容易和拆层剂在水中结合。而且没有从前处理润湿中上所需要的长时间搅拌，进行石墨粉润湿制备剂。从前做反应制备剂所需的时间一般是24小时后最好，也视乎气候而定。原因混合拆层剂在鳞片石墨上，由于鳞片石墨之间有空气存在，在混合时要加上负压抽出空气让拆层剂渗入。本文应用崭新拆层剂配方和糖的结合，可在非常短的时间生产石墨烯。在实验过程中，由鳞片石墨粉开始、加入拆层剂和水溶混合上做好制备液、最后加上撞击剂所需时间是平均五小时内便生产出石墨烯了。根据石墨烯层数所需要，可把制造时间缩短，添加了食糖在拆层剂上，可加快渗透作用而无需抽真空处理，让石墨渗入拆层剂，不受空气影响进行制备剂去进行撞击而生产出石墨烯了。After adding the proportion of sugar, the wetting speed and penetration will be seven to eight times faster than the original speed. Generally, the penetration and wetting ability of the delamination agent can be completed within three hours, and it saves electricity and time... It is an effective method for mass production applications. Because of the molecular structure of sugar is a poly and polysaccharide chain, it is very effective for the water solubility and wetting of natural flake graphite powder. In addition, it cooperates with our various delamination agents, such as polycarbonate chelate and percolate. Oxygen compounds, etc., and even inlaid ionic metals in the delamination agent, can be used for good wetting. In the experiment, we found that the natural flake graphite powder is easy to combine with the delaminating agent in water. Moreover, the preparation agent for graphite powder wetting is performed without the long-time stirring required for the pretreatment wetting. In the past, the time required for the preparation of the reaction preparation was generally best after 24 hours, also depending on the weather. The reason is that the mixed delamination agent is on the flake graphite. Since there is air between the flake graphite, a negative pressure should be added to draw out the air during mixing to allow the delamination agent to penetrate. In this paper, a combination of a novel delaminating agent formulation and sugar can be used to produce graphene in a very short time. During the experiment, starting from the flake graphite powder, adding the delamination agent and water-soluble mixing to make the preparation solution, and finally adding the impact agent, the time required to produce graphene is an average of five hours. According to the needs of the number of graphene layers, the manufacturing time can be shortened, and sugar can be added to the delamination agent, which can speed up the penetration without vacuum treatment, so that the graphite can penetrate into the delamination agent, and the preparation agent is not affected by the air. And produced graphene.
实施例一Example 1
本发明一种钾离子石墨烯的镶嵌方法，包括如下步骤：A kind of mosaic method of potassium ion graphene of the present invention, comprises the steps:
1)将100g天然鳞片石墨粉以及10g钾材料分别放入两个不同的钼船器皿中，并放入真空反应釜中抽真空，达到负两个大气压到负五个大气压；1) 100g natural flake graphite powder and 10g potassium material are put into two different molybdenum vessels respectively, and put into vacuum reactor and vacuumize, reach negative two atmospheres to negative five atmospheres;
2)采用高周波加热法加热真空反应釜中温度至900摄氏度-1100摄氏度，使所述钾材料中的钾离子升华到所述天然鳞片石墨粉上形成钾离子石墨粉；2) adopt high-frequency heating method to heat the temperature in the vacuum reactor to 900 degrees Celsius-1100 degrees Celsius, so that potassium ions in the potassium material are sublimated on the natural flake graphite powder to form potassium ion graphite powder;
3)待所述钾离子石墨粉冷却后，将所述钾离子石墨粉、11g碳酸氢钾以及0.11g食糖进行混合；3) after the potassium ion graphite powder is cooled, the potassium ion graphite powder, 11g potassium bicarbonate and 0.11g sugar are mixed;
4)搅拌3h-5h，使所述拆层剂充分混合于所述钾离子石墨粉的石墨层之间形成水相混合物；4) stirring for 3h-5h to fully mix the delamination agent between the graphite layers of the potassium ion graphite powder to form an aqueous mixture;
5)将11g为EDTA以及PTDA加入所述水相混合物中搅拌均匀形成水相反应物；5) 11g is that EDTA and PTDA are added in the water phase mixture and stir to form water phase reactant;
6)所述水相反应物静置反应1-1.5h，形成所述钾离子石墨烯。6) The aqueous phase reactant is allowed to stand for 1-1.5 hours to form the potassium ion graphene.
钾离子石墨烯作为功能性石墨烯可以作为化学电池的正负极反应催化剂，可以减少溶液型导电液体的使用，增强化学电池的安全性与实用性。As functional graphene, potassium ion graphene can be used as a catalyst for positive and negative reactions in chemical batteries, which can reduce the use of solution-based conductive liquids and enhance the safety and practicability of chemical batteries.
实施例二Embodiment 2
本发明一种钾离子石墨烯的镶嵌方法，包括如下步骤：A kind of mosaic method of potassium ion graphene of the present invention, comprises the steps:
1)将100g天然鳞片石墨粉以及30g钾材料分别放入两个不同的钼船器皿中，并放入真空反应釜中抽真空，达到负两个大气压到负五个大气压；1) 100g natural flake graphite powder and 30g potassium material are put into two different molybdenum vessels respectively, and put into vacuum reactor and vacuumize, reach negative two atmospheres to negative five atmospheres;
2)采用高周波加热法加热真空反应釜中温度至900摄氏度-1100摄氏度，使所述钾材料中的钾离子升华到所述天然鳞片石墨粉上形成钾离子石墨粉；2) adopt high-frequency heating method to heat the temperature in the vacuum reactor to 900 degrees Celsius-1100 degrees Celsius, so that potassium ions in the potassium material are sublimated on the natural flake graphite powder to form potassium ion graphite powder;
3)待所述钾离子石墨粉冷却后，将所述钾离子石墨粉、26g碳酸氢钾以及13g食糖进行混合；3) after the potassium ion graphite powder is cooled, the potassium ion graphite powder, 26g potassium bicarbonate and 13g sugar are mixed;
4)搅拌3h-5h，使所述拆层剂充分混合于所述钾离子石墨粉的石墨层之间形成水相混合物；4) stirring for 3h-5h to fully mix the delamination agent between the graphite layers of the potassium ion graphite powder to form an aqueous mixture;
5)将26g为EDTA以及PTDA加入所述水相混合物中搅拌均匀形成水相反应物；5) 26g is that EDTA and PTDA are added in the water phase mixture and stir to form water phase reactant;
6)所述水相反应物静置反应1-1.5h，形成所述钾离子石墨烯。6) The aqueous phase reactant is allowed to stand for 1-1.5 hours to form the potassium ion graphene.
以上公开的仅为本发明的几个具体实施例，但是本发明并非局限于此，任何本领域的技术人员能思之的变化都应落入本发明的保护范围。The above disclosures are only a few specific embodiments of the present invention, but the present invention is not limited thereto, and any changes that can be conceived by those skilled in the art should fall within the protection scope of the present invention.
Claims (8)
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