CN100540468C - A kind of method for preparing expanded graphite - Google Patents
A kind of method for preparing expanded graphite Download PDFInfo
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- CN100540468C CN100540468C CNB2007100726193A CN200710072619A CN100540468C CN 100540468 C CN100540468 C CN 100540468C CN B2007100726193 A CNB2007100726193 A CN B2007100726193A CN 200710072619 A CN200710072619 A CN 200710072619A CN 100540468 C CN100540468 C CN 100540468C
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Abstract
The present invention is to provide kind of a method for preparing expanded graphite.With natural flake graphite and inorganic intercalated dose, organic intercalation agent and oxygenant according to crystalline flake graphite: inorganic intercalated dose: organic intercalation agent: the ratio uniform mixing of the weight ratio of oxygenant=1: 0.5～10: 0～10: 0.01～5; It is that the microwave heating equipment of 500～6000W expands that said mixture is directly put into power, and the microwave expansion time is 20s～30min, promptly gets expanded graphite.Advantage applies of the present invention exists: simple to operate, with short production cycle, reactant mixes back even just can expanded preparation expanded graphite in 1 minute.Do not washed, avoided the generation of a large amount of acid-bearing wastewaters in the production process with water.Owing to use microwave to make thermal source, avoided traditional high temperature service, therefore significantly reduced energy consumption.
Description
(1) technical field
What the present invention relates to is a kind of method of expanded graphite.
(2) background technology
Expanded graphite is because its excellent physics and chemical property can be widely used in industrial sectors such as iron and steel, metallurgy, oil, chemical machinery, aerospace.For example the flexible graphite article made of expanded graphite is described as the world " king of sealing " and has extremely important status in the mechanical seal field; Expanded graphite can be used as the microbe carrier that oil absorption material is used for waste oil recovery and waste water treatment in the environmental protection field; Become the heat radiating material of a new generation of traditional metal materials such as replacing copper, aluminium by the graphite radiating plate of expanded graphite preparation.Expanded graphite also can be used as medical dressing, catalyzer, fixation support and solid electrolyte etc. in addition.
At present, expanded graphite mainly is to be prepared by chemical oxidization method.Natural flake graphite makes the vermiform expanded graphite via oxidation, acidifying intercalation, washing, drying, high temperature puffing.For example number of patent application is 03122338.9, name is called technical scheme of record in " a kind of no sulphur hang down grey high-purity Preparation of Expanded Graphite method ", be with high-carbon natural flake graphite, nitric acid, diacetyl oxide, perchloric acid be blended in 30～50 ℃ of reactions preparation in 30～120 minutes acidifying graphite, then through the dipping of washing, dry and hydrochloric acid and hydrofluoric acid mixing acid, depickling, again after the drying 900～1000 ℃ expandedly make the expanded graphite that expansion multiplying power is 200～400mL/g.The whole technological operation cycle is long, and needs 900～1000 ℃ of high temperature, energy consumption big, and produce large quantity of exhaust gas in process of production, waste water causes environmental pollution.Therefore improve technology, make expanded graphite more environmental protection of production, efficient, energy-conservation be problem anxious to be solved at present.
(3) summary of the invention
At the bottom of the object of the present invention is to provide a kind of with short production cycle, energy consumption, do not produce a kind of method for preparing expanded graphite of waste water in the production process.
The object of the present invention is achieved like this:
(1) with natural flake graphite and inorganic intercalated dose, organic intercalation agent and oxygenant according to crystalline flake graphite: inorganic intercalated dose: organic intercalation agent: the ratio uniform mixing of the weight ratio of oxygenant=1: 0.5～5: 0～1: 0.01～1.
(2) said mixture directly being put into power is that the microwave heating equipment of 500～6000W expands, and the microwave expansion time is 20s～30min, promptly gets expanded graphite.
The present invention can also comprise:
1, described inorganic intercalated dose is the mixture of one or more any ratios in sulfuric acid, phosphoric acid, the nitric acid.
2, described organic intercalation agent is the mixture of one or more any ratios in aliphatic carboxylic acid, acid anhydrides or the alkyl ester.
3, described aliphatic carboxylic acid is a kind of in formic acid, acetate, propionic acid, butyric acid, caproic acid, oxalic acid, fumaric acid, toxilic acid, propanedioic acid or the Succinic Acid, is preferably formic acid, acetate, propionic acid or oxalic acid.
4, described acid anhydrides is diacetyl oxide or propionic anhydride.
5, described alkyl ester is ethyl formate, methyl-formiate, methyl acetate, dimethyl oxalate or oxalic acid diethyl ester.
6, described oxygenant is the mixture of one or more any ratios in nitric acid, Potcrate, chromic acid, potassium permanganate, potassiumchromate, potassium bichromate or the perchloric acid.
7, described microwave heating equipment power is 700～3000W, and the microwave expansion time is 20s～2min.
Compared with prior art, the present invention has following advantage:
(1) intercalation and expansion reaction are carried out in an operating unit, and be simple to operate, with short production cycle, and reactant mixes back even just can expanded preparation expanded graphite in 1 minute.
(2) do not wash, avoided the generation of a large amount of acid-bearing wastewaters in the production process with water
(3) owing to use microwave to make thermal source, avoid traditional high temperature service, therefore significantly reduced energy consumption.
(4) description of drawings
Accompanying drawing is that the expanding volume that adopts method of the present invention to obtain is the micro-structure diagram of the expanded graphite of 240mL/g.
(5) embodiment
For example the present invention is done in more detail below and describes:
Embodiment 1
With crystalline flake graphite, nitric acid, potassium bichromate by weight 1: 5: 0.3 mixed evenly after, put into microwave oven the power heating while puffing of 800W 2 minutes, obtaining expanding volume is the expanded graphite of 240mL/g.
Embodiment 2
With crystalline flake graphite, sulfuric acid, oxalic acid, perchloric acid by weight 1: 0.5: 0.2: 0.5 mixed evenly after, put into microwave oven the power heating while puffing of 700W 1 minute, obtaining expanding volume is the expanded graphite of 200mL/g.
Embodiment 3
With crystalline flake graphite, phosphoric acid, diacetyl oxide, perchloric acid by weight 1: 2: 1: 1 mixed evenly after, put into microwave oven the power heating while puffing of 2000W 1 minute, obtaining expanding volume is the expanded graphite of 235mL/g.
Embodiment 4
With crystalline flake graphite, nitric acid, formic acid, potassium permanganate by weight 1: 5: 0.3: 0.4 mixed evenly after, put into microwave oven the power heating while puffing of 3000W 20 seconds, obtaining expanding volume is the expanded graphite of 335mL/g.
Embodiment 5
With crystalline flake graphite, nitric acid, methyl-formiate, potassium permanganate by weight 1: 1: 0.5: 0.6 mixed evenly after, put into microwave oven the power heating while puffing of 1000W 40 seconds, obtaining expanding volume is the expanded graphite of 310mL/g.
Embodiment 6
With crystalline flake graphite, nitric acid, diacetyl oxide, potassium permanganate by weight 1: 2: 0.3: 0.4 mixed evenly after, put into microwave oven the power heating while puffing of 1000W 1 minute, obtaining expanding volume is the expanded graphite of 350mL/g.
Claims (9)
1, a kind of method for preparing expanded graphite is characterized in that:
(1) with natural flake graphite and inorganic intercalated dose, organic intercalation agent and oxygenant according to crystalline flake graphite: inorganic intercalated dose: organic intercalation agent: the ratio uniform mixing of the weight ratio of oxygenant=1: 0.5～5: 0～1: 0.01～1;
(2) said mixture directly being put into power is that the microwave heating equipment of 500～6000W expands, and the microwave expansion time is 20s～30min, promptly gets expanded graphite.
2, a kind of method for preparing expanded graphite according to claim 1 is characterized in that: the described inorganic intercalated dose of mixture for one or more any ratios in sulfuric acid, phosphoric acid, the nitric acid.
3, a kind of method for preparing expanded graphite according to claim 1, it is characterized in that: described organic intercalation agent is the mixture of one or more any ratios in aliphatic carboxylic acid, acid anhydrides or the alkyl ester.
4, a kind of method for preparing expanded graphite according to claim 3 is characterized in that: described aliphatic carboxylic acid is a kind of in formic acid, acetate, propionic acid, butyric acid, caproic acid, oxalic acid, fumaric acid, toxilic acid, propanedioic acid or the Succinic Acid.
5, a kind of method for preparing expanded graphite according to claim 3, it is characterized in that: described acid anhydrides is diacetyl oxide or propionic anhydride.
6, a kind of method for preparing expanded graphite according to claim 3, it is characterized in that: described alkyl ester is ethyl formate, methyl-formiate, methyl acetate, dimethyl oxalate or oxalic acid diethyl ester.
7, a kind of method for preparing expanded graphite according to claim 4, it is characterized in that: described aliphatic carboxylic acid is formic acid, acetate, propionic acid or oxalic acid.
8, a kind of method for preparing expanded graphite according to claim 1, it is characterized in that: described oxygenant is the mixture of one or more any ratios in nitric acid, Potcrate, chromic acid, potassium permanganate, potassiumchromate, potassium bichromate or the perchloric acid.
9, a kind of method for preparing expanded graphite according to claim 1, it is characterized in that: described microwave heating equipment power is 700～3000W, the microwave expansion time is 20s～2min.
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| CNB2007100726193A CN100540468C (en) | 2007-08-07 | 2007-08-07 | A kind of method for preparing expanded graphite |
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| CNB2007100726193A CN100540468C (en) | 2007-08-07 | 2007-08-07 | A kind of method for preparing expanded graphite |
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| CN100540468C true CN100540468C (en) | 2009-09-16 |
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| US8691174B2 (en) * | 2009-01-26 | 2014-04-08 | Dow Global Technologies Llc | Nitrate salt-based process for manufacture of graphite oxide |
| CN101570483A (en) * | 2009-03-27 | 2009-11-04 | 攀枝花学院 | Method for catalyzing and synthesizing ester |
| CN101891186B (en) * | 2010-06-11 | 2012-01-18 | 北京工业大学 | Method for preparing expanded graphite by adopting microwave puffing method |
| US9187612B2 (en) | 2010-08-11 | 2015-11-17 | Imerys Graphite & Carbon Switzerland Sa | Ground expanded graphite agglomerates, methods of making, and applications of the same |
| CN102476797B (en) * | 2010-11-29 | 2013-10-02 | 海洋王照明科技股份有限公司 | Preparation method for expansible graphite |
| CN102320600A (en) * | 2011-08-17 | 2012-01-18 | 山东东昀石墨科技有限公司 | Preparation method of low-sulfur expandable graphite (graphite intercalation compound) |
| RU2524933C1 (en) * | 2012-12-26 | 2014-08-10 | Андрей Павлович Захаров | Method and apparatus for producing thermally expanded graphite |
| EP2939979B1 (en) * | 2012-12-28 | 2021-10-27 | Posco | Graphene-polymer coated steel sheet |
| CN103476226B (en) * | 2013-08-27 | 2016-07-27 | 深圳市鸿富诚屏蔽材料有限公司 | A kind of preparation method of high thermal conductivity graphite radiating fins |
| CN105016332A (en) * | 2015-08-11 | 2015-11-04 | 无锡桥阳机械制造有限公司 | Preparation technology of expandable graphite |
| CN106698417A (en) * | 2015-11-17 | 2017-05-24 | 上海驭扬投资有限公司 | Method for preparing sulfur-free expansible graphite |
| CN106348653B (en) * | 2016-08-30 | 2018-12-14 | 丰县建鑫泡沫制品有限公司 | A kind of sound-insulating inner lining material and preparation method thereof that sandwich room plate uses |
| CN107840321B (en) * | 2016-09-21 | 2019-11-22 | 北京化工大学 | A kind of graphene oxide with fold, preparation method and the usage |
| CN106430178B (en) * | 2016-11-04 | 2019-04-30 | 辽宁省地质矿产研究院有限责任公司 | A kind of microwave chemical preparation method of fine scale sulphur-free expanded graphite |
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| CN107500286A (en) * | 2017-09-30 | 2017-12-22 | 湖南国盛石墨科技有限公司 | Micro crystal graphite bulking process |
| CN107445158A (en) * | 2017-09-30 | 2017-12-08 | 湖南国盛石墨科技有限公司 | The swollen expansion process of micro crystal graphite |
| CN107572515A (en) * | 2017-09-30 | 2018-01-12 | 湖南国盛石墨科技有限公司 | The preparation method of inflatable micro crystal graphite |
| CN108689403A (en) * | 2018-08-30 | 2018-10-23 | 多凌新材料科技股份有限公司 | The method that supercritical fluid auxiliary prepares expansible graphite |
| CN109467658A (en) * | 2018-11-13 | 2019-03-15 | 大同新成新材料股份有限公司 | A kind of preparation method and preparation facilities of modified graphene slurry |
| CN109467790A (en) * | 2018-12-27 | 2019-03-15 | 镇江市宜扬密封制品有限公司 | A kind of ultra-high molecular weight polyethylene product |
| CN110510608B (en) * | 2019-09-12 | 2021-12-17 | 广州机械科学研究院有限公司 | Antioxidant for improving oxidation resistance of flake graphite and application thereof |
| CN112723354B (en) * | 2020-12-24 | 2021-07-30 | 鸡西市海盛新能源材料有限公司 | Production process for preparing expandable graphite with high initial temperature |
| CN112645321B (en) * | 2020-12-24 | 2021-11-23 | 王海鹏 | Production process for preparing expandable graphite by electrolytic method |
| CN112662381A (en) * | 2020-12-26 | 2021-04-16 | 国网甘肃省电力公司经济技术研究院 | Preparation method and application of framework material for adsorbing heat storage material |
| CN115504466A (en) * | 2022-09-26 | 2022-12-23 | 鸡西环宇新能源材料有限公司 | Method and device for preparing expanded graphite |
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