CN101428794A - Preparation of coir fiber based activated carbon with high specific surface area - Google Patents
Preparation of coir fiber based activated carbon with high specific surface area Download PDFInfo
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- CN101428794A CN101428794A CNA200810177135XA CN200810177135A CN101428794A CN 101428794 A CN101428794 A CN 101428794A CN A200810177135X A CNA200810177135X A CN A200810177135XA CN 200810177135 A CN200810177135 A CN 200810177135A CN 101428794 A CN101428794 A CN 101428794A
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- coir
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Abstract
The invention discloses a preparation method of coir base high specific surface area active carbon, which comprises the following steps: taking coir as raw material to be carbonized and obtaining carbonization material; activating the carbonization material and an alkalescent active agent after being mixed; washing or pickling a product; and then filtering and drying the product. The invention has simple technical process and low cost through taking the coir as the raw material, can effectively enhance the activation of the active agent, and is the preparation method of the active carbon which has the advantages of low cost, high efficiency, environmental protection and the like; and the prepared active carbon has the advantages of high specific surface area, narrow aperture distribution and high middle aperture ratio. The invention can be applied to energy storage materials, capacitors, efficient adsorbent, separating agent and gas adsorbent, hydrogen storage materials, and the like. Furthermore, the invention has wide application prospect.
Description
Technical field
The present invention relates to a kind of preparation method of active carbon, being specifically related to a kind of is raw material with the coir, adopts composite activating agent to prepare high-specific surface area, senior middle school's porosity process of active carbon.
Background technology
Gac is a kind of sorbent material efficiently, and research and the application of present stage to it entered all-round developing period.The development of modern industry and environmental science has occurred such as new variety gacs such as impregnated carbon, ball-type charcoal, fiber charcoals on the one hand; On the other hand, with active carbon fibre peacekeeping super-activated carbon is that high-performance, the specificity gac of representative continually developed, the Application of Brand Active Carbon scope is further enlarged, keep in traditional field such as food, pharmacy, light industry, metallurgy, chemical industry, war industries on the basis of sustainable growth, again constantly to expansions such as field such as environmental protection neck, electronics, medical material and effective catalysts.In hydrogen storage material; gac have hydrogen-storage amount height, suction/desorption rate fast, recycle long and advantage such as accomplish scale production easily of life-span; can significantly promote the development of low cost, mass-producing hydrogen storage technology; the energy, traffic, environmental protection for future have very important significance, and gac has now become a kind of carbonaceous adsorption hydrogen-storing material of having very much potentiality and a competitive power.
Now, the technology of preparing of micropore gac is quite ripe.The raw material type of preparation gac is many, mainly contains timber, rice husk, cotton stalk, English walnut nuclear, bamboo, coal tar, pitch, hard coal etc.The preparation method also is varied, and physical activation method and chemical activation etc. are arranged.The research of activator also is more comprehensive, and the chemical activating agent that uses mainly contains at present: KOH, H
3PO
4, ZnCl
2, NaOH, K
2CO
3, Na
2CO
3Deng, but existing method all is to use single activator, still is very few for the research of composite activating agent.The specific surface area of the gac of existent method preparation at present can be up to 3000m
2More than/the g, absorption property also has significantly raising, but these gacs mainly are based on micropore, central hole structure seldom even do not have, adsorptive power to the small-molecule substance below the 2nm is very strong, but powerless for middle molecule more than the 2nm or macromolecular substance, this is the range of application of restricted activity charcoal largely just.Also there is certain technical barrier and can adsorb macromolecular, as to have central hole structure gac for preparation.
Summary of the invention
The objective of the invention is to provide a kind of preparation method of coir fiber based activated carbon with high specific surface area at the deficiencies in the prior art, be to be that raw material prepares active carbon with high specific surface area with the alkaline activation agent with the coir, improve the specific surface area and the middle porosity of gac by control of process parameters such as carbonization temperature, activator, activation temperature, soak time, temperature rise rates effectively.
The technical solution adopted in the present invention is: be that raw material carries out carbonization and obtains carbonized stock with the coir, carbonized stock mixed the back activating under high temperature with the alkaline activation agent, afterwards again with product washing or pickling, and filter, dry getting final product.
Technological process of the present invention is simple, to measure big inexpensive coir is raw material, cost is low, can strengthen the activation of activator effectively, it is a kind of method for preparation of active carbon with advantages such as low cost, high benefit, environmental protection, the gained gac has characteristics such as specific surface area height, narrow, the middle porosity height of pore size distribution, can be applicable to energy storage material, electrical condenser, high-efficiency adsorbent, separating agent, adsorbent and hydrogen storage material etc., has broad application prospects.
Description of drawings
The isothermal adsorption desorption graphic representation of prepared activated carbon sample among Fig. 1 embodiment one.
The pore size distribution curve figure of prepared activated carbon sample among Fig. 2 embodiment one.
The isothermal adsorption desorption graphic representation of prepared activated carbon sample among Fig. 3 embodiment two.
The pore size distribution curve figure of prepared activated carbon sample among Fig. 4 embodiment two.
The isothermal adsorption desorption graphic representation of prepared activated carbon sample among Fig. 5 embodiment four.
The pore size distribution curve figure of prepared activated carbon sample among Fig. 6 embodiment four.
Embodiment
The invention will be further described below in conjunction with indefiniteness embodiment.
The preparation method of a kind of coir fiber based activated carbon with high specific surface area that the present invention is designed is: be that raw material carries out carbonization and obtains carbonized stock with the coir under 350 ℃～600 ℃ temperature, carbonized stock is mixed back by weight the ratio of 1:2～1:4 with the form of grinding with the alkaline activation agent to be activated under 750 ℃～950 ℃ temperature, afterwards with activation products washings or pickling, and filter, dry getting final product.Described activator is KOH, NaOH+KOH or NaOH+K
2CO
3Described soak time is 90min～120min.
Embodiment one
Present embodiment is to be raw material with the coir, and KOH is an activator.
Earlier the starting material coir is carried out charing 30min under 600 ℃, it is even with the ratio ground and mixed of 1:2 to get 7g carbonized material and KOH, again compound is carried out constant temperature priming reaction 120min under 850 ℃ temperature, and wherein temperature rise rate is 15 ℃/min.Behind the priming reaction, take out product, grind and clean to remove KOH wherein, again with the clean chlorion wherein of distilled water with tap water.Putting into loft drier then can feed 120 ℃ of following oven dry.Prepared gac is to be 1894mg/g based on micropore, iodine sorption value, and specific surface area reaches 2158m
2.g
-1, total pore volume is 1.0466ml.g
-1
As shown in Figure 1 and Figure 2, be respectively the isothermal adsorption graphic representation and the pore size distribution curve figure of present embodiment gained sample.Adsorption isothermal curve among Fig. 1 belongs to first kind isothermal curve, sharply increase in of the increase of periods of low pressure adsorptive capacity with pressure, adsorptive capacity becomes slow gradually with the pressure increase subsequently, when relative pressure is 0.1 left and right sides, adsorptive capacity begin to be one slowly, near linear increase tendency, it is that returning of the adsorption/desorption line ring that stagnates is not obvious that the adsorption/desorption line overlaps more, and this proves absolutely that gac inside contains the abundant microporous structure, but mesopore or macroporous structure are very few.These graph of pore diameter distribution in Fig. 2 are also high-visible.
Embodiment two
Present embodiment is to be raw material with the coir, is composite activating agent with NaOH and KOH.
Earlier with the starting material coir 400 ℃ of following charings, (NaOH:KOH: ratio carbonized material) is ground, is mixed with 3:1:1 to get 20g carbonized material and composite activating agent, compound packed into carry out priming reaction 120min in the stainless steel tube under 900 ℃, the priming reaction temperature rise rate is 15 ℃/min.After priming reaction is finished, take out product, use excessive deionized water wash again, get final product in 150 ℃ of following complete dryinies collections at last with an amount of salt pickling.Prepared gac has higher middle porosity, can reach 24.8%, and its iodine sorption value is 1435.0mg/g, and methylene blue adsorption value is 495mg/g, and specific surface area is 2031.9m
2/ g, productive rate can reach 48.76%.
As shown in Figure 3, Figure 4, be respectively the isothermal adsorption desorption graphic representation and the pore size distribution curve figure of the prepared activated carbon sample of present embodiment.In Fig. 3, sorption isotherm sharply increases in the increase of periods of low pressure adsorptive capacity with pressure, adsorptive capacity becomes slow gradually with the pressure increase subsequently, when relative pressure is 0.4 left and right sides, adsorptive capacity begin to be one slowly, near linear increase tendency, this proves absolutely that gac inside contains the abundant microporous structure.Also can be observed tangible hysteresis loop simultaneously from figure, this illustrates that also gac also has flourishing central hole structure.This pore size distribution curve at Fig. 4 also can obtain proof: the peak value of micropore is the highest, and the peak value of mesopore takes second place, and the aperture of mesopore mainly is distributed in 2-5nm.
Embodiment three
Present embodiment is to be raw material with the coir, is composite activating agent with NaOH and KOH.
Earlier with the starting material coir 500 ℃ of following charings, (NaOH:KOH: ratio carbonized material) is ground, is mixed with 3:1:1 to get 20g carbonized material and composite activating agent, compound packed into carry out priming reaction 150min in the stainless steel tube under 900 ℃, the priming reaction temperature rise rate is 5 ℃/min.After priming reaction is finished, take out product, use excessive deionized water wash again, get final product in 150 ℃ of following complete dryinies collections at last with an amount of salt pickling.Prepared gac has higher middle porosity in the present embodiment, can reach 25.2%, and its iodine sorption value is 1402.05mg/g, and methylene blue adsorption value is 457.5mg/g, and specific surface area is 1547m
2/ g, productive rate can reach 49.59%.
Embodiment four
Present embodiment is to be raw material with the coir, with NaOH and K
2CO
3Be composite activating agent.20g carbonized material and composite activating agent 500 ℃ of following charings, are got with 3:1:1 (NaOH:K with the starting material coir by elder generation
2CO
3: carbonized material) ratio is ground, is mixed, and compound is packed into carry out priming reaction 90min in the stainless steel tube under 850 ℃, and the priming reaction temperature rise rate is 15 ℃/min.After priming reaction is finished, take out product, use excessive deionized water wash again, get final product in 150 ℃ of following complete dryinies collections at last with an amount of salt pickling.Prepared gac has higher middle porosity in the present embodiment, can reach 28%, and its iodine sorption value is 1401.21mg/g, and methylene blue adsorption value is 502.5mg/g, and specific surface area is 1734.5m
2/ g, productive rate can reach 41.65%.As Fig. 5, shown in Figure 6, be respectively the isothermal adsorption desorption graphic representation and the pore size distribution curve figure of the prepared activated carbon sample of present embodiment.
Claims (3)
1, a kind of preparation method of coir fiber based activated carbon with high specific surface area, it is characterized in that: be that raw material carries out carbonization and obtains carbonized stock with the coir under 350 ℃～600 ℃ temperature, carbonized stock is mixed back by weight the ratio of 1:2～1:4 with the form of grinding with the alkaline activation agent to be activated under 750 ℃～950 ℃ temperature, afterwards with activation products washings or pickling, and filter, dry getting final product.
2, the preparation method of coir fiber based activated carbon with high specific surface area according to claim 1 is characterized in that: described activator is KOH, NaOH+KOH or NaOH+K
2CO
3
3, the preparation method of coir fiber based activated carbon with high specific surface area according to claim 1 is characterized in that: described soak time is 90min～120min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830460A (en) * | 2010-05-26 | 2010-09-15 | 中国科学技术大学苏州研究院 | Active carbon particles and preparation method thereof |
| CN102583366A (en) * | 2012-01-19 | 2012-07-18 | 中国科学院山西煤炭化学研究所 | Method for washing active carbon with low water consumption |
| CN102765718A (en) * | 2011-12-23 | 2012-11-07 | 山东轻工业学院 | Method for preparing peach pit active carbon by chemical method |
| CN103252213A (en) * | 2013-05-20 | 2013-08-21 | 绍兴文理学院元培学院 | Active carbon with microporous-mesoporous structure |
| CN105480975A (en) * | 2016-02-25 | 2016-04-13 | 黑龙江省科学院大庆分院 | Method for preparing high-specific-surface-area porous carbon with hemp stems as carbon source |
| CN105923634A (en) * | 2016-05-06 | 2016-09-07 | 海南大学 | Coconut-shell fiber-based activated carbon for supercapacitor and preparation method of activated carbon |
| CN113577981A (en) * | 2021-08-11 | 2021-11-02 | 浙江大学 | Oxygen-containing microporous activated carbon, preparation thereof and application thereof in selective adsorption of ethane |
| CN114275782A (en) * | 2021-12-10 | 2022-04-05 | 海南大学 | Method for preparing full-microporous activated carbon by low-temperature alkali fusion method |
-
2008
- 2008-12-01 CN CNA200810177135XA patent/CN101428794A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101830460A (en) * | 2010-05-26 | 2010-09-15 | 中国科学技术大学苏州研究院 | Active carbon particles and preparation method thereof |
| CN102765718A (en) * | 2011-12-23 | 2012-11-07 | 山东轻工业学院 | Method for preparing peach pit active carbon by chemical method |
| CN102583366A (en) * | 2012-01-19 | 2012-07-18 | 中国科学院山西煤炭化学研究所 | Method for washing active carbon with low water consumption |
| CN103252213A (en) * | 2013-05-20 | 2013-08-21 | 绍兴文理学院元培学院 | Active carbon with microporous-mesoporous structure |
| CN103252213B (en) * | 2013-05-20 | 2015-02-18 | 绍兴文理学院元培学院 | Active carbon with microporous-mesoporous structure |
| CN105480975A (en) * | 2016-02-25 | 2016-04-13 | 黑龙江省科学院大庆分院 | Method for preparing high-specific-surface-area porous carbon with hemp stems as carbon source |
| CN105923634A (en) * | 2016-05-06 | 2016-09-07 | 海南大学 | Coconut-shell fiber-based activated carbon for supercapacitor and preparation method of activated carbon |
| CN105923634B (en) * | 2016-05-06 | 2019-01-15 | 海南大学 | Supercapacitor coir fibre matrix activated carbon and preparation method thereof |
| CN113577981A (en) * | 2021-08-11 | 2021-11-02 | 浙江大学 | Oxygen-containing microporous activated carbon, preparation thereof and application thereof in selective adsorption of ethane |
| CN114275782A (en) * | 2021-12-10 | 2022-04-05 | 海南大学 | Method for preparing full-microporous activated carbon by low-temperature alkali fusion method |
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Open date: 20090513 |