CN103043659A - Preparation method for modified actived carbons - Google Patents
Preparation method for modified actived carbons Download PDFInfo
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- CN103043659A CN103043659A CN2012105487221A CN201210548722A CN103043659A CN 103043659 A CN103043659 A CN 103043659A CN 2012105487221 A CN2012105487221 A CN 2012105487221A CN 201210548722 A CN201210548722 A CN 201210548722A CN 103043659 A CN103043659 A CN 103043659A
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Abstract
The invention discloses a preparation method for modified actived carbons. The modified active carbons are actived carbons modified by adopting hydrogen inhibitor; and the hydrogen inhibitor is lead oxide loaded on the surfaces of the actived carbons. The preparation process comprises the following steps: firstly, lead ions are absorbed by using the actived carbons; then the lead ions are deposited on the surfaces of the actived carbons by using alkali; and finally, lead hydrogen is decomposed to lead oxide through the heat treatment, and the lead oxide is loaded on the surfaces of the actived carbons; the actived carbons, lead salt and the alkali are chemically reacted through the ball milling method, and are treated at the high temperature under the protecting air environment to prepare the modified actived carbons. The method has the advantages of simple preparation technique, short production period, facilitation of industrial production, lower equipment investment, environmental friendliness and wide application, and can increase the specific capacitance of the active carbons.
Description
Technical field
The present invention relates to technical field of chemical power, especially a kind of preparation method of modified activated carbon.
Background technology
Along with the fast development of society, environmental pollution and traditional energy shortage, people need more efficient, and more the energy of environmental protection substitutes or additional traditional energy, and this causes the demand of mixed power electric car, power truck more and more.Carbon is a kind of energy storage material commonly used, in water system electric capacity or water system battery, adds activity charcoal powder and can improve this energy-storage travelling wave tube energy density and power density, can improve the cycle life of battery.
But carbon class material is lower at the hydrogen-evolution overpotential of aqueous electrochemical system, can accelerate the decomposition of water at charge and discharge process, therefore in the aqueous electrochemical system, electrical condenser or the battery operated voltage of carbon class material are lower, improve the decomposition voltage of water, must start with from the modification of gac.
Summary of the invention
For solving above-mentioned drawback, technical problem to be solved by this invention is that a kind of preparation method with modified activated carbon of high hydrogen-evolution overpotential is provided.In order to solve the problems of the technologies described above, the technical solution used in the present invention is, a kind of modified activated carbon preparation method is characterized in that, described modified activated carbon is the gac that adopts the hydrogen inhibitor modification; Described hydrogen inhibitor is the plumbous oxide that loads on activated carbon surface;
The preparation process of described modified activated carbon is: use first the charcoal absorption lead ion 1.; 2. re-use alkali lead ion is deposited on activated carbon surface; 3. make lead hydroxide resolve into plumbous oxide by thermal treatment at last, and load on activated carbon surface;
Then gac, lead salt and alkali prepare by pyroprocessing under protection compression ring border by ball milling method generation chemical reaction; Described lead salt is taken from the mixture of one or both arbitrary proportions of lead sulfate or plumbic acetate; Described alkali is taken from a kind of of potassium hydroxide, sodium hydroxide.
Its main chemical reactions is as follows:
Use lead sulfate to prepare presoma: PbSO
4+ KOH → Pb (OH)
2+ K
2SO
4
Use plumbic acetate to prepare presoma: PbAC+KOH → Pb (OH)
2+ KAC
Thermal treatment: Pb (OH)
2→ PbO+H
2O.
Commercially available capacitor stage gac is taken from the charcoal source of modified activated carbon of the present invention, and described capacitor stage gac will satisfy following technical indicator:
Preferably, the preparation method of described modified activated carbon specifically comprises the steps:
The first step: take by weighing quantitative gac, lead salt is put into ball grinder, the control ratio of grinding media to material is 10:1～50:1, and wherein lead salt is equivalent to 5%～15% of gac weight, with said mixture ball milling 10～30min, raw material is smashed;
Second step: get a certain amount of sodium hydroxide or potassium hydroxide and add in the described ball grinder of the first step, wherein the mole number of sodium hydroxide or potassium hydroxide is equivalent to 2.1～2.3 times of lead salt mole number in the first step, and adding deionized water, the weight of deionized water is 1%～5% of lead salt weight, with said mixture ball milling 20min～30min, obtain the black powder of activated carbon supported lead;
The 3rd step: with the powder oven dry that second step makes, the control bake out temperature is 80 ℃～90 ℃, and the time is 0.5～1 hour;
The 4th step: the 3rd step gained powder put into place tube furnace lead to argon shield, argon flow amount is 70～80ml/min, and at the uniform velocity intensification is heat-treated; thermal treatment temp is 600～850 ℃; and be incubated 1～2h, and tube furnace is naturally cooled to room temperature, namely get described modified activated carbon.
Beneficial effect of the present invention is:
1, preparation technology of the present invention is simple, and is with short production cycle, is easy to suitability for industrialized production, and facility investment is less, is a kind of low input, the new technology project of high production.
2, not producing waste gas, waste water, waste residue in the preparation process of the present invention, is a kind of production technology of environmental protection, without any byproduct, does not need to carry out water treatment and gas processing.
3, the prepared modified activated carbon of the present invention is a kind of high hydrogen overpotential powdered carbon that presses down, and operating voltage is higher, can be used on numerous water system batteries or electric capacity, such as plumbous carbon battery, nickel metal hydride battery, carbon supercapacitor, nickel-zinc cell etc.
4, modified activated carbon since load metal oxide, therefore produce fake capacitance in the working cycle meeting, can increase the ratio electric capacity of gac.
5, the overpotential of hydrogen evolution of PbO is higher, and low price.
The present invention will be further described below in conjunction with the drawings and specific embodiments.
Description of drawings
Accompanying drawing is that the modified activated carbon of example 1-3 preparation and commercially available gac are made respectively working electrode and carried out constant current charge-discharge and test resulting voltage/time plot.
Embodiment
Embodiment 1: the first step: take by weighing 100 gram gacs, 5 gram lead nitrates are put into ball grinder, and the control ratio of grinding media to material is 25:1, with said mixture ball milling 20min, raw material is smashed.
Second step: get potassium hydroxide 1.9 grams and put into the described ball grinder of the first step, and add 0.1 gram deionized water, with said mixture ball milling 20min, obtain the black powder of activated carbon supported lead.
The 3rd step: with the powder oven dry that second step makes, the control bake out temperature is 85 ℃, and the time is 0.5 hour.
The 4th step: the 3rd step gained powder put into place tube furnace to lead to argon shield; argon flow amount is that 70ml/min heat-treats with the speed intensification of 5 ℃/min; thermal treatment temp is 650 ℃; and insulation 1.5h; tube furnace is naturally cooled to room temperature, namely obtain the modified activated carbon of the present invention's preparation.
Embodiment 2: the first step: take by weighing 500 gram gacs, 50 gram lead nitrates are put into ball grinder, and the control ratio of grinding media to material is 10:1, with said mixture ball milling 25min, raw material is smashed.
Second step: get potassium hydroxide 20 grams and put into the described ball grinder of the first step, and add 1.5 gram deionized waters, with said mixture ball milling 30min, obtain the black powder of activated carbon supported lead.
The 3rd step: with the powder oven dry that second step makes, the control bake out temperature is 90 ℃, and the time is 0.5 hour.
The 4th step: the 3rd step gained powder put into place tube furnace to lead to argon shield; argon flow amount is that 75ml/min heat-treats with the speed intensification of 5 ℃/min, and thermal treatment temp is 750 ℃, and insulation 2h; tubular type is naturally cooled to room temperature, namely obtain the modified activated carbon of the present invention's preparation.
Embodiment 3: the first step: take by weighing 1000 gram gacs, 50 gram plumbic acetates are put into ball grinder, and the control ratio of grinding media to material is 20:1, with said mixture ball milling 28min, raw material is smashed.
Second step: get potassium hydroxide 19 grams and put into the described ball grinder of the first step, and add 2 gram deionized waters, with said mixture ball milling 30min, obtain the black powder of activated carbon supported lead.
The 3rd step: with the powder oven dry that second step makes, the control bake out temperature is 80 ℃, and the time is 1 hour.
The 4th step: the 3rd step gained powder put into place tube furnace to lead to argon shield; argon flow amount is that 80ml/min heat-treats with the speed intensification of 5 ℃/min, and thermal treatment temp is 850 ℃, and insulation 2h; tubular type is naturally cooled to room temperature, namely obtain the modified activated carbon of the present invention's preparation.
The performance perameter of the modified activated carbon that the various embodiments described above are prepared sees the following form:
| Specific surface area | Compare electric capacity | The D50 pore size distribution | |
| Example 1 | 853m 2/g | 100F/g | 8nm |
| Example 2 | 1450m 2/g | 140F/g | 12nm |
| Example 3 | 1600m 2/g | 145F/g | 13nm |
Take by weighing the modified activated carbon of example 1-3 preparation and each 10mg of carbon electrode of commercially available gac preparation, the ptfe emulsion that adds respectively 5% massfraction is binding agent, is evenly coated on the nickel foam, at 300kg/cm
2Pressure under be pressed into working electrode, the two electrodes test system is adopted in constant current charge-discharge test, under 25 ℃ of conditions of room temperature, tests curve such as accompanying drawing at the CHI660C electrochemical workstation with the 0.5A/g electric current.
Claims (2)
1. the preparation method of a modified activated carbon is characterized in that, described modified activated carbon is the gac that adopts the hydrogen inhibitor modification; Described hydrogen inhibitor is the plumbous oxide that loads on activated carbon surface;
The preparation process of described modified activated carbon is: use first the charcoal absorption lead ion 1.; 2. re-use alkali lead ion is deposited on activated carbon surface; 3. make lead hydroxide resolve into plumbous oxide by thermal treatment at last, and load on activated carbon surface;
Then gac, lead salt and alkali prepare by pyroprocessing under protection compression ring border by ball milling method generation chemical reaction; Described lead salt is taken from the mixture of one or both arbitrary proportions of lead sulfate or plumbic acetate; Described alkali is taken from a kind of of potassium hydroxide, sodium hydroxide.
2. the preparation method of a kind of modified activated carbon as claimed in claim 1 is characterized in that, the preparation method of described modified activated carbon specifically comprises the steps:
The first step: take by weighing quantitative gac, lead salt is put into ball grinder, the control ratio of grinding media to material is 10:1～50:1, and wherein lead salt is equivalent to 5%～15% of gac weight, with said mixture ball milling 10～30min, raw material is smashed;
Second step: get a certain amount of sodium hydroxide or potassium hydroxide and add in the described ball grinder of the first step, wherein the mole number of sodium hydroxide or potassium hydroxide is equivalent to 2.1～2.3 times of lead salt mole number in the first step, and adding deionized water, the weight of deionized water is 1%～5% of lead salt weight, with said mixture ball milling 20min～30min, obtain the black powder of activated carbon supported lead;
The 3rd step: with the powder oven dry that second step makes, the control bake out temperature is 80 ℃～90 ℃, and the time is 0.5～1 hour;
The 4th step: the 3rd step gained powder put into place tube furnace to lead to argon shield, argon flow amount is 70～80ml/min, and intensification is heat-treated; thermal treatment temp is 600～850 ℃; and be incubated 1～2h, and tube furnace is naturally cooled to room temperature, namely get described modified activated carbon.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105489887A (en) * | 2015-11-05 | 2016-04-13 | 中国电力科学研究院 | Negative lead paste for lead-carbon battery |
| CN106206063A (en) * | 2016-08-13 | 2016-12-07 | 代相臣 | Water system hybrid super capacitor and preparation method thereof |
| CN106941166A (en) * | 2017-04-13 | 2017-07-11 | 安徽理士电源技术有限公司 | A kind of lead titanium Si-C composite material and preparation method thereof |
| CN107425196A (en) * | 2017-06-07 | 2017-12-01 | 常州市丰瑞电子有限公司 | A kind of preparation method of special four basic lead sulphate of lead accumulator |
| CN108899492A (en) * | 2018-06-21 | 2018-11-27 | 华中科技大学 | A kind of lead carbon composite, preparation method and application |
| CN111320173A (en) * | 2020-03-06 | 2020-06-23 | 浙江省林业科学研究院 | Preparation method of modified activated carbon material for capacitor |
| CN111509197A (en) * | 2019-01-31 | 2020-08-07 | 山东欧铂新材料有限公司 | Modified activated carbon composite material for negative electrode of lead-carbon battery, preparation method of modified activated carbon composite material and lead-carbon battery |
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| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| CN102306784A (en) * | 2011-06-29 | 2012-01-04 | 哈尔滨工业大学 | Modified activated carbon with high hydrogen evolution potential and preparation method thereof as well as lead-acid battery negative lead paste containing modified activated carbon |
| CN102823037A (en) * | 2009-12-11 | 2012-12-12 | 艾纳G2技术公司 | Carbon materials comprising an electrochemical modifier |
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2012
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| CN102823037A (en) * | 2009-12-11 | 2012-12-12 | 艾纳G2技术公司 | Carbon materials comprising an electrochemical modifier |
| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| CN102306784A (en) * | 2011-06-29 | 2012-01-04 | 哈尔滨工业大学 | Modified activated carbon with high hydrogen evolution potential and preparation method thereof as well as lead-acid battery negative lead paste containing modified activated carbon |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105489887A (en) * | 2015-11-05 | 2016-04-13 | 中国电力科学研究院 | Negative lead paste for lead-carbon battery |
| CN105489887B (en) * | 2015-11-05 | 2020-07-24 | 中国电力科学研究院 | Negative lead paste of lead-carbon battery |
| CN106206063A (en) * | 2016-08-13 | 2016-12-07 | 代相臣 | Water system hybrid super capacitor and preparation method thereof |
| CN106941166B (en) * | 2017-04-13 | 2019-04-23 | 安徽理士电源技术有限公司 | A kind of lead titanium Si-C composite material and preparation method thereof |
| CN106941166A (en) * | 2017-04-13 | 2017-07-11 | 安徽理士电源技术有限公司 | A kind of lead titanium Si-C composite material and preparation method thereof |
| CN107425196A (en) * | 2017-06-07 | 2017-12-01 | 常州市丰瑞电子有限公司 | A kind of preparation method of special four basic lead sulphate of lead accumulator |
| CN107425196B (en) * | 2017-06-07 | 2020-05-05 | 泉州市圣能电源科技有限公司 | Preparation method of tetrabasic lead sulfate special for lead storage battery |
| CN108899492B (en) * | 2018-06-21 | 2020-05-19 | 华中科技大学 | Lead-carbon composite material, and preparation method and application thereof |
| CN108899492A (en) * | 2018-06-21 | 2018-11-27 | 华中科技大学 | A kind of lead carbon composite, preparation method and application |
| CN111509197A (en) * | 2019-01-31 | 2020-08-07 | 山东欧铂新材料有限公司 | Modified activated carbon composite material for negative electrode of lead-carbon battery, preparation method of modified activated carbon composite material and lead-carbon battery |
| CN111509197B (en) * | 2019-01-31 | 2021-11-19 | 山东欧铂新材料有限公司 | Modified activated carbon composite material for negative electrode of lead-carbon battery, preparation method of modified activated carbon composite material and lead-carbon battery |
| CN111320173A (en) * | 2020-03-06 | 2020-06-23 | 浙江省林业科学研究院 | Preparation method of modified activated carbon material for capacitor |
| CN111320173B (en) * | 2020-03-06 | 2022-10-11 | 浙江省林业科学研究院 | Preparation method of modified activated carbon material for capacitor |
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Application publication date: 20130417 |