CN104851614A - Doped lithium manganese iron phosphate-straw-based carbon composite electrode material and preparation method thereof - Google Patents
Doped lithium manganese iron phosphate-straw-based carbon composite electrode material and preparation method thereof Download PDFInfo
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- CN104851614A CN104851614A CN201510157770.1A CN201510157770A CN104851614A CN 104851614 A CN104851614 A CN 104851614A CN 201510157770 A CN201510157770 A CN 201510157770A CN 104851614 A CN104851614 A CN 104851614A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/42—Powders or particles, e.g. composition thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/38—Carbon pastes or blends; Binders or additives therein
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a doped lithium manganese iron phosphate straw-based carbon composite electrode material, and is characterized by being prepared from the following raw materials in parts by weight: 3-5 parts of lithium manganese iron phosphate, 1-2 parts of diethylenetriamine, 1-2 parts of tetramethoxysilane, 1-2 parts of tetrabutyl titanate, 0.2-0.4 parts of ammonium persulfate, 1-2 parts of soluble glass, 1000-1200 parts of straws, 8-12 part of zinc chloride, 4-7 parts of citric acid, 3-5 parts of modified acetylene black, and 100-150 parts of distilled water. The modified acetylene black added to the doped lithium manganese iron phosphate straw-based carbon composite electrode material has the advantages of enhancing conductivity and improving high-multiplying power charge-discharge properties, and the doped lithium manganese iron phosphate has relatively high energy density, and also has good charge and discharge cycle reversibility, thereby solving the problem that straw-based carbon is not high in energy density as an electrode material.
Description
Technical field
The present invention relates to chemical energy source Material Field, particularly a kind of doping phosphoric acid ferromanganese lithium straw base charcoal combination electrode material and preparation method thereof.
Background technology
Active carbon is a kind of porousness chemical substance of black.The outstanding advantages of active carbon is that internal pore structure is flourishing, specific area is large, has excellent absorption property and good chemical stability, physical stability and uses the performances such as rear regenerating easily that lost efficacy.It can decolour, deodorization, desulfurization, de-benzene, optionally can also remove some chemical impurity in liquid phase or gas phase.It also can adsorb Cucumber as catalyst, and chemical reaction velocity is accelerated greatly, is that body cut out by good catalyst.Why active carbon has so many function, is because there is flourishing pore structure charcoal surface.Obtain the quality raw materials with the active carbon of flourishing pore structure, bigger serface and excellent absorption property and mainly contain timber, agricultural crop straw, pitch, petroleum coke and coal-tar residue etc.Stalk it there is natural porosity structure, the active carbon specific area made is large, and cheap, phosphorus content high, electrode material for super capacitor mainly contains conducting polymer and combination electrode material, metal oxide, carbon-based material.And the attention rate of carbon-based material is the highest in these materials, study the earliest, and technology is also ripe.For the preparation of the active carbon of electrode material mainly in material with carbon element of ultracapacitor.Active carbon as the advantage of electrode material for super capacitor is: abundant raw material, cheap, and performance is good.But it is not high that unique shortcoming is exactly the energy density of material with carbon element, and the iron manganese phosphate for lithium of doping has higher energy density, also has good charging and discharging circulation reversibility energy.
Summary of the invention
The object of this invention is to provide a kind of doping phosphoric acid ferromanganese lithium straw base charcoal combination electrode material and preparation method thereof.
In order to realize object of the present invention, the present invention is by following scheme implementation:
A kind of doping phosphoric acid ferromanganese lithium straw base charcoal combination electrode material, is made up of the raw material of following weight portion: iron manganese phosphate for lithium 3-5, diethylenetriamines 1-2, methyl silicate 1-2, butyl titanate 1-2, ammonium persulfate 0.2-0.4, waterglass 1-2, stalk 1000-1200, zinc chloride 8-12, citric acid 4-7, modification acetylene black 3-5, distilled water 100-150;
Described modification acetylene black is made up of the raw material of following weight portion: barium sulfate 3-5, acetylene black 40-60, lignin 1-2, molybdenum bisuphide 4-5, silicon tetrachloride 5-7, polyvinyl alcohol 2-3, distilled water 10-20; Preparation method is: be added in the solution of silicon tetrachloride by barium sulfate, lignin, molybdenum bisuphide, ultrasonic disperse 1-2 hour, again by the material suction filtration post-drying of gained, be added in the aqueous solution of polyvinyl alcohol and form suspension-turbid liquid, again suspension-turbid liquid is coated in the acetylene black after ozone activation, under the condition of 600-700 ° of C, sinter 3-5 hour, after naturally cooling to room temperature, grind to form 200-400 order powder.
A kind of doping phosphoric acid ferromanganese lithium straw base charcoal combination electrode material of the present invention, be made up of following concrete step:
(1) powder of straw is broken into fine particle shape, clean up post-drying, moisture controls at about 20-25%, again zinc chloride and citric acid are added in distilled water, add stalk after stirring and soak 4-8 hour, be added to after drying dewaters in retort, first low-temperature carbonization 1-2 hour under 250-350 ° of C, raised temperature, to 450-550 ° of C, continues charing for subsequent use after 1-2 hour;
(2) butyl titanate, methyl silicate, waterglass are added in distilled water, be heated to 60-70 ° of C stir, add the material of iron manganese phosphate for lithium, diethylenetriamines, ammonium persulfate and step (1) again, stirring reaction 1-2 hour, to be added in microwave dryer dry 3-5 hour under 130-150 ° of C after reaction terminates;
(3) by the product of step (2) and the mixing of modification acetylene black, ball milling 2-3 hour under the atmosphere of nitrogen, then be added in calciner and continue to calcine 3-4 hour in 700-750 ° of C under the protection of nitrogen, cooling, pulverizing can obtain.
Advantage of the present invention is: the modification acetylene black that the present invention adds has and enhances electric conductivity and improve the advantages such as high-rate charge-discharge capability, the iron manganese phosphate for lithium of doping has higher energy density, also there is good charging and discharging circulation reversibility energy, compensate for straw base charcoal as the not high difficult problem of electrode material energy density.
specific embodiments
Below by instantiation, the present invention is described in detail.
A kind of doping phosphoric acid ferromanganese lithium straw base charcoal combination electrode material, is made up of the raw material of following weight portion (kilogram): iron manganese phosphate for lithium 5, diethylenetriamines 1, methyl silicate 1, butyl titanate 2, ammonium persulfate 0.2, waterglass 1, stalk 1200, zinc chloride 11, citric acid 6, modification acetylene black 5, distilled water 140;
Described modification acetylene black is made up of the raw material of following weight portion (kilogram): barium sulfate 4, acetylene black 55, lignin 1, molybdenum bisuphide 4, silicon tetrachloride 7, polyvinyl alcohol 2, distilled water 17; Preparation method is: be added in the solution of silicon tetrachloride by barium sulfate, lignin, molybdenum bisuphide, ultrasonic disperse 1-2 hour, again by the material suction filtration post-drying of gained, be added in the aqueous solution of polyvinyl alcohol and form suspension-turbid liquid, again suspension-turbid liquid is coated in the acetylene black after ozone activation, under the condition of 600-700 ° of C, sinter 3-5 hour, after naturally cooling to room temperature, grind to form 200-400 order powder.
A kind of doping phosphoric acid ferromanganese lithium straw base charcoal combination electrode material of the present invention, be made up of following concrete step:
(1) powder of straw is broken into fine particle shape, clean up post-drying, moisture controls at about 20-25%, again zinc chloride and citric acid are added in distilled water, add stalk after stirring and soak 4-8 hour, be added to after drying dewaters in retort, first low-temperature carbonization 1-2 hour under 250-350 ° of C, raised temperature, to 450-550 ° of C, continues charing for subsequent use after 1-2 hour;
(2) butyl titanate, methyl silicate, waterglass are added in distilled water, be heated to 60-70 ° of C stir, add the material of iron manganese phosphate for lithium, diethylenetriamines, ammonium persulfate and step (1) again, stirring reaction 1-2 hour, to be added in microwave dryer dry 3-5 hour under 130-150 ° of C after reaction terminates;
(3) by the product of step (2) and the mixing of modification acetylene black, ball milling 2-3 hour under the atmosphere of nitrogen, then be added in calciner and continue to calcine 3-4 hour in 700-750 ° of C under the protection of nitrogen, cooling, pulverizing can obtain.
Electrode material and conductive agent, binding agent are proportionally mixed, laminated by roller machine, be pressed in after drying on stainless (steel) wire collector, make ultracapacitor, its reference electrode is saturated calomel electrode, electrolyte is the sodium hydroxide solution of 9mol/l, in the voltage range of-0.2V to 0.8V, carry out constant current charge-discharge test, when electric current is 0.2A/g, ratio capacitance is 253F/g, when electric current is 10A/g, ratio capacitance is 162F/g.
Claims (2)
1. a doping phosphoric acid ferromanganese lithium straw base charcoal combination electrode material, it is characterized in that, be made up of the raw material of following weight portion: iron manganese phosphate for lithium 3-5, diethylenetriamines 1-2, methyl silicate 1-2, butyl titanate 1-2, ammonium persulfate 0.2-0.4, waterglass 1-2, stalk 1000-1200, zinc chloride 8-12, citric acid 4-7, modification acetylene black 3-5, distilled water 100-150;
Described modification acetylene black is made up of the raw material of following weight portion: barium sulfate 3-5, acetylene black 40-60, lignin 1-2, molybdenum bisuphide 4-5, silicon tetrachloride 5-7, polyvinyl alcohol 2-3, distilled water 10-20; Preparation method is: be added in the solution of silicon tetrachloride by barium sulfate, lignin, molybdenum bisuphide, ultrasonic disperse 1-2 hour, again by the material suction filtration post-drying of gained, be added in the aqueous solution of polyvinyl alcohol and form suspension-turbid liquid, again suspension-turbid liquid is coated in the acetylene black after ozone activation, under the condition of 600-700 ° of C, sinter 3-5 hour, after naturally cooling to room temperature, grind to form 200-400 order powder.
2. a kind of doping phosphoric acid ferromanganese lithium straw base charcoal combination electrode material according to claim 1, is characterized in that, be made up of following concrete step:
(1) powder of straw is broken into fine particle shape, clean up post-drying, moisture controls at about 20-25%, again zinc chloride and citric acid are added in distilled water, add stalk after stirring and soak 4-8 hour, be added to after drying dewaters in retort, first low-temperature carbonization 1-2 hour under 250-350 ° of C, raised temperature, to 450-550 ° of C, continues charing for subsequent use after 1-2 hour;
(2) butyl titanate, methyl silicate, waterglass are added in distilled water, be heated to 60-70 ° of C stir, add the material of iron manganese phosphate for lithium, diethylenetriamines, ammonium persulfate and step (1) again, stirring reaction 1-2 hour, to be added in microwave dryer dry 3-5 hour under 130-150 ° of C after reaction terminates;
(3) by the product of step (2) and the mixing of modification acetylene black, ball milling 2-3 hour under the atmosphere of nitrogen, then be added in calciner and continue to calcine 3-4 hour in 700-750 ° of C under the protection of nitrogen, cooling, pulverizing can obtain.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510157770.1A CN104851614A (en) | 2015-04-03 | 2015-04-03 | Doped lithium manganese iron phosphate-straw-based carbon composite electrode material and preparation method thereof |
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| CN201510157770.1A CN104851614A (en) | 2015-04-03 | 2015-04-03 | Doped lithium manganese iron phosphate-straw-based carbon composite electrode material and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050196336A1 (en) * | 2004-03-05 | 2005-09-08 | Chatterjee Arup K. | Activated graphitic carbon and metal hybrids thereof |
| CN102583333A (en) * | 2012-01-18 | 2012-07-18 | 黑龙江大学 | Method for synthesizing porous nanographite flakes by using corn stalks as carbon source |
| CN102651484A (en) * | 2012-05-10 | 2012-08-29 | 中国第一汽车股份有限公司 | Energy storage device combining with characteristics of lithium ion battery and super-capacitor |
| CN102786052A (en) * | 2012-07-16 | 2012-11-21 | 太仓市联林活性炭厂 | Method for preparation of activated carbon through rice hull desilication |
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- 2015-04-03 CN CN201510157770.1A patent/CN104851614A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050196336A1 (en) * | 2004-03-05 | 2005-09-08 | Chatterjee Arup K. | Activated graphitic carbon and metal hybrids thereof |
| CN102583333A (en) * | 2012-01-18 | 2012-07-18 | 黑龙江大学 | Method for synthesizing porous nanographite flakes by using corn stalks as carbon source |
| CN102651484A (en) * | 2012-05-10 | 2012-08-29 | 中国第一汽车股份有限公司 | Energy storage device combining with characteristics of lithium ion battery and super-capacitor |
| CN102786052A (en) * | 2012-07-16 | 2012-11-21 | 太仓市联林活性炭厂 | Method for preparation of activated carbon through rice hull desilication |
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