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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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000010439 graphite Substances 0.000 title claims abstract description 52
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000009830 intercalation Methods 0.000 claims abstract description 15
- 230000002687 intercalation Effects 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical group CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 12
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 6
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 5
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 claims description 5
- 235000019253 formic acid Nutrition 0.000 claims description 5
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- 239000012286 potassium permanganate Substances 0.000 claims description 5
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 4
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical group CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 4
- 235000011054 acetic acid Nutrition 0.000 claims description 4
- 150000008065 acid anhydrides Chemical class 0.000 claims description 4
- 125000005907 alkyl ester group Chemical group 0.000 claims description 4
- 235000019260 propionic acid Nutrition 0.000 claims description 4
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 3
- QLOKJRIVRGCVIM-UHFFFAOYSA-N 1-[(4-methylsulfanylphenyl)methyl]piperazine Chemical compound C1=CC(SC)=CC=C1CN1CCNCC1 QLOKJRIVRGCVIM-UHFFFAOYSA-N 0.000 claims description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N Caprylic acid Natural products CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 2
- LOMVENUNSWAXEN-UHFFFAOYSA-N Methyl oxalate Chemical compound COC(=O)C(=O)OC LOMVENUNSWAXEN-UHFFFAOYSA-N 0.000 claims description 2
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 2
- GONOPSZTUGRENK-UHFFFAOYSA-N benzyl(trichloro)silane Chemical compound Cl[Si](Cl)(Cl)CC1=CC=CC=C1 GONOPSZTUGRENK-UHFFFAOYSA-N 0.000 claims description 2
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 claims description 2
- WYACBZDAHNBPPB-UHFFFAOYSA-N diethyl oxalate Chemical compound CCOC(=O)C(=O)OCC WYACBZDAHNBPPB-UHFFFAOYSA-N 0.000 claims description 2
- WBJINCZRORDGAQ-UHFFFAOYSA-N formic acid ethyl ester Natural products CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000001530 fumaric acid Substances 0.000 claims description 2
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 239000011976 maleic acid Substances 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N n-hexanoic acid Natural products CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 claims description 2
- WYVAMUWZEOHJOQ-UHFFFAOYSA-N propionic anhydride Chemical compound CCC(=O)OC(=O)CC WYVAMUWZEOHJOQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000001384 succinic acid Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 239000002351 wastewater Substances 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000000376 reactant Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- -1 metallurgy Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Abstract
Description
(一)技术领域 (1) Technical field
本发明涉及的是一种膨胀石墨的方法。The invention relates to a method for expanding graphite.
(二)背景技术 (2) Background technology
膨胀石墨由于其优异的物理和化学性能，可广泛用于钢铁、冶金、石油、化工机械、宇航等工业部门。例如膨胀石墨制成的柔性石墨制品被誉为世界“密封之王”在机械密封领域具有极其重要的地位；膨胀石墨在环保领域可作为吸油材料用于废油回收以及废水治理中的微生物载体；由膨胀石墨制备的石墨散热板成为取代铜、铝等传统金属材料的新一代的散热基材。此外膨胀石墨还可用作医用敷料、催化剂、固定化载体及固体电解液等。Due to its excellent physical and chemical properties, expanded graphite can be widely used in steel, metallurgy, petroleum, chemical machinery, aerospace and other industrial sectors. For example, flexible graphite products made of expanded graphite are known as the "king of seals" in the world and have an extremely important position in the field of mechanical seals; expanded graphite can be used as an oil-absorbing material in the field of environmental protection for waste oil recovery and microbial carriers in wastewater treatment; Graphite heat sinks made of expanded graphite have become a new generation of heat dissipation substrates that replace traditional metal materials such as copper and aluminum. In addition, expanded graphite can also be used as medical dressings, catalysts, immobilized carriers and solid electrolytes.
目前，膨胀石墨主要是由化学氧化法制备。天然鳞片石墨经由氧化、酸化插层、水洗、干燥、高温膨化制得蠕虫状膨胀石墨。例如专利申请号为03122338.9，名称为“一种无硫低灰高纯膨胀石墨的制备方法”中记载的技术方案，是将高碳天然鳞片石墨、硝酸、乙酸酐、高氯酸混合在30～50℃反应30～120分钟制备酸化石墨、然后经水洗、干燥、以及盐酸和氢氟酸混合酸的浸渍、脱酸、再干燥后900～1000℃膨化制得膨胀倍率为200～400mL/g的膨胀石墨。整个工艺操作周期长，而且需要900～1000℃高温、能耗大，而且在生产过程中产生大量废气、废水造成环境污染。因此改进工艺、使膨胀石墨的生产更环保、高效、节能是目前急待解决的问题。At present, expanded graphite is mainly prepared by chemical oxidation. Vermicular expanded graphite is obtained from natural flake graphite through oxidation, acidification intercalation, water washing, drying and high temperature expansion. For example, the patent application number is 03122338.9, and the title is "a preparation method of sulfur-free low-ash high-purity expanded graphite". React at 50°C for 30-120 minutes to prepare acidified graphite, then wash with water, dry, impregnate with mixed acid of hydrochloric acid and hydrofluoric acid, deacidify, and then dry at 900-1000°C to obtain graphite with an expansion ratio of 200-400mL/g expanded graphite. The whole process has a long operation cycle, and requires high temperature of 900-1000°C, high energy consumption, and produces a large amount of waste gas and waste water during the production process, causing environmental pollution. Therefore, improving the process and making the production of expanded graphite more environmentally friendly, efficient and energy-saving is an urgent problem to be solved at present.
(三)发明内容 (3) Contents of the invention
本发明的目的在于提供一种生产周期短、能耗底、生产过程中不产生废水的一种制备膨胀石墨的方法。The object of the present invention is to provide a method for preparing expanded graphite with short production cycle, low energy consumption and no waste water during the production process.
本发明的目的是这样实现的：The purpose of the present invention is achieved like this:
(1)将天然鳞片石墨与无机插层剂、有机插层剂以及氧化剂按照鳞片石墨∶无机插层剂∶有机插层剂∶氧化剂的重量比＝1∶0.5～5∶0～1∶0.01～1的比例均匀混合。(1) natural flake graphite and inorganic intercalation agent, organic intercalation agent and oxidizing agent are according to flake graphite: inorganic intercalation agent: organic intercalation agent: the weight ratio=1: 0.5～5: 0～1: 0.01～of oxidant 1 ratio to mix evenly.
(2)将上述混合物直接放入功率为500～6000W的微波加热设备中进行膨胀，微波膨胀时间为20s～30min，即得膨胀石墨。(2) The above mixture is directly put into a microwave heating device with a power of 500-6000W for expansion, and the microwave expansion time is 20s-30min, and the expanded graphite is obtained.
本发明还可以包括：The present invention may also include:
1、所述的无机插层剂为硫酸、磷酸、硝酸中的一种或两种以上任何比例的混合物。1. The inorganic intercalation agent is one of sulfuric acid, phosphoric acid and nitric acid or a mixture of two or more in any proportion.
2、所述的有机插层剂为脂肪族羧酸、酸酐或烷基酯中的一种或两种以上任何比例的混合物。2. The organic intercalation agent is one or a mixture of two or more of aliphatic carboxylic acids, acid anhydrides or alkyl esters in any proportion.
3、所述的脂肪族羧酸是甲酸、乙酸、丙酸、丁酸、己酸、草酸、富马酸、马来酸、丙二酸或丁二酸中的一种，优选为甲酸、乙酸、丙酸或草酸。3. The aliphatic carboxylic acid is one of formic acid, acetic acid, propionic acid, butyric acid, hexanoic acid, oxalic acid, fumaric acid, maleic acid, malonic acid or succinic acid, preferably formic acid and acetic acid , propionic acid or oxalic acid.
4、所述的酸酐是乙酸酐或丙酸酐。4. The acid anhydride is acetic anhydride or propionic anhydride.
5、所述的烷基酯是甲酸乙酯、甲酸甲酯、乙酸甲酯、草酸二甲酯或草酸二乙酯。5. The alkyl ester is ethyl formate, methyl formate, methyl acetate, dimethyl oxalate or diethyl oxalate.
6、所述的氧化剂为硝酸、氯酸钾、铬酸、高锰酸钾、铬酸钾、重铬酸钾或高氯酸中的一种或两种以上任何比例的混合物。6. The oxidizing agent is one of nitric acid, potassium chlorate, chromic acid, potassium permanganate, potassium chromate, potassium dichromate or perchloric acid or a mixture of two or more in any proportion.
7、所述的微波加热设备功率为700～3000W，微波膨胀时间为20s～2min。7. The power of the microwave heating equipment is 700-3000W, and the microwave expansion time is 20s-2min.
与现有技术相比，本发明具有如下优点：Compared with prior art, the present invention has following advantage:
(1)插层反应与膨胀反应在一个操作单元中进行，操作简单、生产周期短，反应物混合后甚至在1分钟内就可以膨化制备膨胀石墨。(1) The intercalation reaction and the expansion reaction are carried out in one operation unit, which is simple in operation and short in production cycle, and the expanded graphite can be prepared even within 1 minute after the reactants are mixed.
(2)生产过程中不用水洗、避免了大量含酸废水的生成(2) There is no need for washing in the production process, avoiding the generation of a large amount of acid-containing wastewater
(3)由于使用微波作热源，避免了传统的高温设备，因此显著降低了能耗。(3) Due to the use of microwaves as a heat source, traditional high-temperature equipment is avoided, thereby significantly reducing energy consumption.
(四)附图说明 (4) Description of drawings
附图是采用本发明的方法获得的膨胀体积为240mL/g的膨胀石墨的微观结构图。Accompanying drawing is the microstructure figure that adopts the expansion volume that the method of the present invention obtains is the expanded graphite of 240mL/g.
(五)具体实施方式 (5) Specific implementation methods
下面举例对本发明做更详细地描述：The following examples describe the present invention in more detail:
实施例1Example 1
将鳞片石墨、硝酸、重铬酸钾按重量比1∶5∶0.3的比例混合均匀后，放入微波炉中在800W的功率加热膨化2分钟，获得膨胀体积为240mL/g的膨胀石墨。Flake graphite, nitric acid, and potassium dichromate were mixed evenly in a weight ratio of 1:5:0.3, and then heated and expanded in a microwave oven at a power of 800W for 2 minutes to obtain expanded graphite with an expanded volume of 240mL/g.
实施例2Example 2
将鳞片石墨、硫酸、草酸、高氯酸按重量比1∶0.5∶0.2∶0.5的比例混合均匀后，放入微波炉中在700W的功率加热膨化1分钟，获得膨胀体积为200mL/g的膨胀石墨。After mixing flake graphite, sulfuric acid, oxalic acid, and perchloric acid in a weight ratio of 1:0.5:0.2:0.5, put it in a microwave oven and heat it at 700W for 1 minute to obtain expanded graphite with an expansion volume of 200mL/g. .
实施例3Example 3
将鳞片石墨、磷酸、乙酸酐、高氯酸按重量比1∶2∶1∶1的比例混合均匀后，放入微波炉中在2000W的功率加热膨化1分钟，获得膨胀体积为235mL/g的膨胀石墨。After mixing flake graphite, phosphoric acid, acetic anhydride, and perchloric acid in a weight ratio of 1:2:1:1, put it in a microwave oven and heat it at 2000W for 1 minute to obtain an expanded volume of 235mL/g. graphite.
实施例4Example 4
将鳞片石墨、硝酸、甲酸、高锰酸钾按重量比1∶5∶0.3∶0.4的比例混合均匀后，放入微波炉中在3000W的功率加热膨化20秒，获得膨胀体积为335mL/g的膨胀石墨。After mixing flake graphite, nitric acid, formic acid, and potassium permanganate in a weight ratio of 1:5:0.3:0.4, put it in a microwave oven and heat it at 3000W for 20 seconds to obtain an expanded volume of 335mL/g. graphite.
实施例5Example 5
将鳞片石墨、硝酸、甲酸甲酯、高锰酸钾按重量比1∶1∶0.5∶0.6的比例混合均匀后，放入微波炉中在1000W的功率加热膨化40秒，获得膨胀体积为310mL/g的膨胀石墨。After mixing flake graphite, nitric acid, methyl formate, and potassium permanganate in a weight ratio of 1:1:0.5:0.6, put it in a microwave oven and heat it at 1000W for 40 seconds to obtain an expanded volume of 310mL/g of expanded graphite.
实施例6Example 6
将鳞片石墨、硝酸、乙酸酐、高锰酸钾按重量比1∶2∶0.3∶0.4的比例混合均匀后，放入微波炉中在1000W的功率加热膨化1分钟，获得膨胀体积为350mL/g的膨胀石墨。After mixing flake graphite, nitric acid, acetic anhydride, and potassium permanganate in a weight ratio of 1:2:0.3:0.4, put it in a microwave oven and heat it at 1000W for 1 minute to obtain an expanded volume of 350mL/g. expanded graphite.
Claims (9)
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| WO2010085443A1 (en) * | 2009-01-26 | 2010-07-29 | Dow Global Technologies Inc. | 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 |
| WO2012020099A1 (en) | 2010-08-11 | 2012-02-16 | Timcal S.A. | 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 |
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