CN105217627A - A kind of preparation method of coconut husk greying gac - Google Patents
A kind of preparation method of coconut husk greying gac Download PDFInfo
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- CN105217627A CN105217627A CN201510655989.4A CN201510655989A CN105217627A CN 105217627 A CN105217627 A CN 105217627A CN 201510655989 A CN201510655989 A CN 201510655989A CN 105217627 A CN105217627 A CN 105217627A
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Abstract
The invention discloses a kind of preparation method of coconut husk greying gac, directly in carbon raw material, add catalyzer, activator respectively, at 600-1100 DEG C, carbonization-activation can obtain greying gac.And specific surface area and degree of graphitization can be regulated and controled by control activator level and activation temperature, the simplification of its controllability and preparation method, well solves existing gac poorly conductive, specific surface area is less than normal and graphitizing process temperature is too high, complex process is unfavorable for the shortcomings such as commercial applications.
Description
Technical field
The invention belongs to the preparation field of absorbent charcoal material, be specifically related to a kind of preparation method of coconut husk greying gac.
Background technology
Gac is the basic carbonaceous being made up of gac amorphous carbonaceous not graphited in graphited gac crystallite and activated carbon raw material, with advantages such as the gap structure of its prosperity, larger specific surface area, strong adsorptive poweies, is widely used in all trades and professions.Meanwhile, for the gac after graphitization processing, because of the physicochemical property of its uniqueness, progressively there is good electroconductibility, structural stability and special adsorption selection ability.Be employed for electrode conductive material more and more, and as having the support of the catalyst of rock steady structure.
Typically, greying gac needs to obtain activated carbon treatment under inert atmosphere and high-temperature heat treatment condition, or at a lower temperature, carries out low-temperature catalyzed graphitization to activated carbon supported catalyzer.But high-temperature heat treatment greatly can reduce gac specific surface area and pore volume, further limit its application, and energy consumption is high, and is unwell to fairly large production.For the method for catalyzed graphitization, Patents also has report, patent CN102867654A discloses a kind of greying absorbent charcoal material for ultracapacitor and preparation method, the method is that raw material first prepares carbonized material with shell of Semen Ginkgo, then carries out chemical activation, then carries out graphitization processing to obtained activated carbon supported catalyzer, finally carry out pickling, washing process, obviously, preparation technology is very complicated too, and specific surface area is relatively little.Patent CN104071786A discloses a kind of preparation method of greying gac, the method take commercial activated carbons as raw material, after process, degree of graphitization promotes obvious, but its process can produce considerable influence by contrast table area, meanwhile, the regulation and control of its preparation method to activated carbon structure have certain limitation.The people such as Chun-hsienHuang adopt polystyrene triethanol amine resin and triblock copolymer F127 to be template, phenol-formaldehyde resin is carbon source, adding nickelous chloride is graphitization catalyst, obtain perforated structure graphite gac capable of magnetic separating, although have good pore structure and performance, but complicated process of preparation, and cost is high.Therefore, invent a kind of preparation method, allow activation and greying carry out simultaneously, make technical process simple, the greying gac of high specific surface area can be prepared again, particularly important and meaningful with regard to what show.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of preparation method had compared with high-ratio surface coconut husk greying gac is provided.The present invention, by adding catalyzer, activator respectively in the coconut carbon raw material of certain particle size, by controlling activator level and activation temperature, prepares the greying gac of different specific surface area.
For achieving the above object, the present invention is by the following technical solutions:
A kind of preparation method of high-ratio surface coconut husk greying gac: add catalyzer and activator respectively in 50-100 object coconut carbon raw material, under specific atmosphere, at 400-1100 DEG C, process 0.5-5h, then high-specific surface area greying gac can be obtained through strong acid washing, washing.
Specifically comprise the following steps:
(1) first time mixing: by the aqueous impregnation mixing 2-24h of 50-100 object coconut husk material with catalyzer, be then placed in vacuum drying oven, dry 2-10h at 50-100 DEG C;
(2) interpolation of activator: by coconut husk material dry in step (1) and activator mix, flood 1-5h at 50-120 DEG C;
(3) carbonization-activation: the coconut husk material after dipping is placed in atmosphere furnace charing, activation, then uses dust technology, distilled water wash dry successively, namely obtains high-ratio surface greying gac.
Catalyzer described in step (1) is one or more in iron nitrate, Iron nitrate, ferric sulfate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, nickelous nitrate, cobalt chloride, Manganous chloride tetrahydrate and manganous nitrate, and the consumption of catalyzer is the 1%-20% of coconut husk material quality.
Activator described in step (2) is phosphoric acid, and the mass ratio of phosphoric acid and coconut husk material is 0.25 ~ 2.5:1.
Carbonization-activation described in step (3) is: adopt Ar atmosphere, flow control is at 100 ~ 400mL/min, and final temperature controls at 400 ~ 1100 DEG C, maintains 0.5-5h, and it is 5 DEG C/min that temperature rise rate controls.
Diluted acid described in step (3) is the one in hydrochloric acid, sulfuric acid or nitric acid, and adopt circumfluence method to wash, it is 70 DEG C that temperature controls; Then, the gac after pickling is washed, until pH is more than 6, finally at 100 DEG C, dry.
remarkable advantage of the present invention is:
(1) preparation method's process of the present invention is simple, by adding graphitization catalyst and activator, activation and greying being carried out simultaneously, compared with existing technology of preparing, both reduced graphitization temperature, reducing energy consumption, be beneficial to promotion and implementation again;
(2) the present invention is in preparation process, by simply controlling activator level and activation temperature, can obtain the gac of different specific surface, different graphitization degree degree, having good practicality and application prospect.
Figure of description
The Raman figure of the gac of Fig. 1 obtained by each embodiment.
Embodiment
With specific embodiment, technical scheme of the present invention is described below, but the scope that comprises of the present invention is not limited only to this.
Embodiment 1
Get the 50-100 object coconut husk material that 5g is dried, add 5mlFe (NO
3)
3the aqueous solution, catalyst loading is 1% of coconut husk material quality, mixes rear dipping 10h, is then placed in vacuum drying oven, at 50 DEG C, dries 4h; Mixed with phosphoric acid solution by the coconut husk material of drying, it is 0.50 that impregnating ratio controls, at 70 DEG C, flood 5h; Flood complete coconut husk material and be placed in atmosphere furnace, adopt Ar atmosphere, flow control is at 100ml/min, and final temperature is set as 600 DEG C, and temperature rise rate is 5 DEG C/min, constant temperature activation 1h; Activate complete gac, be placed in the nitric acid backflow washing 2h that massfraction is 1%, temperature is 70 DEG C, eventually passes washing, and pH value, to 6-7, is dried, and parameter sees the following form 1.
Embodiment 2
Get the 50-100 object coconut husk material that 5g is dried, add 5mlFe (NO
3)
3the aqueous solution, catalyst loading is 5% of coconut husk material quality, mixes rear dipping 10h, is then placed in vacuum drying oven, at 80 DEG C, dries 4h; Mixed with phosphoric acid solution by the coconut husk material of drying, it is 0.50 that impregnating ratio controls, at 70 DEG C, flood 5h; Flood complete coconut husk material and be placed in atmosphere furnace, adopt Ar atmosphere, flow control is at 100ml/min, and final temperature is set as 800 DEG C, and temperature rise rate is 5 DEG C/min, constant temperature activation 1h; Activate complete gac, be placed in the nitric acid backflow washing 2h that massfraction is 1%, temperature is 70 DEG C, eventually passes washing, and pH value is 6-7, dries, and parameter sees the following form 1.
Embodiment 3
Get the 50-100 object coconut husk material that 5g is dried, add 5mlMnCl
2solution, catalyst loading is 8% of coconut husk material quality, mixes rear dipping 5h, is then placed in vacuum drying oven, at 60 DEG C, dries 4h; Mixed with phosphoric acid solution by the coconut husk material of drying, it is 1.0 that impregnating ratio controls, at 100 DEG C, flood 5h; Flood complete coconut husk material and be placed in atmosphere furnace, adopt Ar atmosphere, flow control is at 200ml/min, and final temperature is set as 900 DEG C, and temperature rise rate is 5 DEG C/min, constant temperature activation 2h; Activate complete gac, be placed in the nitric acid backflow washing 2h that massfraction is 1%, temperature is 70 DEG C, eventually passes washing, and pH value is 6-7, dries, and parameter sees the following form 1.
Embodiment 4
Get the 50-100 object coconut husk material that 5g is dried, add 5mlNi (NO
3)
2solution, catalyst loading is 10% of coconut husk material quality, mixes rear dipping 10h, is then placed in vacuum drying oven, at 80 DEG C, dries 6h; Mixed with phosphoric acid solution by the coconut husk material of drying, it is 0.75 that impregnating ratio controls, at 80 DEG C, flood 5h; Flood complete coconut husk material and be placed in atmosphere furnace, adopt Ar atmosphere, flow control is at 150ml/min, and final temperature is set as 1000 DEG C, and temperature rise rate is 5 DEG C/min, constant temperature activation 3h; Activate complete gac, be placed in the nitric acid backflow washing 2h that massfraction is 1%, temperature is 70 DEG C, eventually passes washing, and pH value is 6-7, dries, and parameter sees the following form 1.
Embodiment 5
Get the 50-100 object coconut husk material that 5g is dried, add 5mlMn (NO
3)
2solution, catalyst loading is 15% of coconut husk material quality, mixes rear dipping 24h, is then placed in vacuum drying oven, at 80 DEG C, dries 5h; Mixed with phosphoric acid solution by the coconut husk material of drying, it is 1.0 that impregnating ratio controls, at 90 DEG C, flood 5h; Flood complete coconut husk material and be placed in atmosphere furnace, adopt Ar atmosphere, flow control is at 100ml/min, and final temperature is set as 1100 DEG C, and temperature rise rate is 5 DEG C/min, constant temperature activation 2h; Activate complete gac, be placed in the nitric acid backflow washing 2h that massfraction is 1%, temperature is 70 DEG C, eventually passes washing, and pH value is 6-7, dries, and parameter sees the following form 1.
The Raman collection of illustrative plates of the activated carbon sample of Fig. 1 prepared by above-mentioned experiment, can find out, all samples all has two different peaks, 1585cm
-1the Raman peaks of left and right is the typical Raman peaks of body phase crystalline graphite, and claim G peak, this peak is the basic vibration mode of graphite crystal, and its intensity is relevant with the size of crystal; 1360cm
1the Raman peaks at place is derived from the vibration at graphite carbon crystalline state edge, is called that D is with; This two places Raman peaks is the typical Raman peaks of class graphite carbon (as graphite, carbon black, activated carbon etc.), and degree of graphitization is usually with IG/ID(intensity level) represent.We are not difficult to find, example 1-5 degree of graphitization improves constantly, the interpolation of catalyzer, and effect is more obvious, and for embodiment 5, the sharpening of G peak, represents graphite-phase degree of crystallinity better.(the heat treated temperature of embodiment 1 to embodiment 5 need reset down, contain 400 DEG C of these points)
Performance Detection:
The performance measurement result of the gac now obtained by embodiment 1-5 presents in Table 1, and the gac that the present invention obtains as can be seen from Table 1 has different specific surface areas, pore structure, shows good Modulatory character.
The character of the gac that table 1 process of the present invention obtains
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application patent change and modify, and all should belong to covering scope of the present invention.
Claims (5)
1. a preparation method for coconut husk greying gac, is characterized in that: comprise the following steps:
(1) first time mixing: by the aqueous impregnation mixing 2-24h of 50-100 object coconut husk material with catalyzer, be then placed in vacuum drying oven, dry 2-10h at 50-100 DEG C;
(2) interpolation of activator: by coconut husk material dry in step (1) and activator mix, flood 1-5h at 50-120 DEG C;
(3) carbonization-activation: the coconut husk material after step (2) being flooded is placed in atmosphere furnace carbonization-activation, then uses diluted acid, distilled water wash dry successively, namely obtains high-ratio surface greying gac.
2. the preparation method of coconut husk greying gac according to claim 1, it is characterized in that: the catalyzer described in step (1) is one or more in iron nitrate, Iron nitrate, ferric sulfate, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, cobalt chloride, nickelous nitrate, Manganous chloride tetrahydrate and manganous nitrate, and the consumption of catalyzer is the 1%-20% of coconut husk material quality.
3. the preparation method of coconut husk greying gac according to claim 1, is characterized in that: the activator described in step (2) is phosphoric acid, the mass ratio of phosphoric acid and coconut husk material is 0.25 ~ 2.5:1.
4. the preparation method of coconut husk greying gac according to claim 1, it is characterized in that: the carbonization-activation in step (3) is: adopt Ar atmosphere, flow control is at 100 ~ 400mL/min, and final temperature controls at 600 ~ 1100 DEG C, maintain 0.5-5h, it is 5 DEG C/min that temperature rise rate controls.
5. the preparation method of coconut husk greying gac according to claim 1, is characterized in that: the diluted acid described in step (3) is the one in hydrochloric acid, sulfuric acid or nitric acid, and adopt circumfluence method to wash, temperature controls at 70 DEG C; Then, the gac after pickling is washed, until pH is more than 6, finally can obtain coconut husk greying gac 100 DEG C of oven dry.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106219545A (en) * | 2016-07-25 | 2016-12-14 | 句容市百诚活性炭有限公司 | A kind of preparation method of sucrose base grading-hole activated carbon |
| CN108083276A (en) * | 2017-12-29 | 2018-05-29 | 北海星石碳材料科技有限责任公司 | The preparation method of ultracapacitor activated carbon |
| CN108298517A (en) * | 2017-01-12 | 2018-07-20 | 中国科学院化学研究所 | A kind of method and its product preparing porous carbon materials using halogenated polyolefin hydrocarbon-based polymeric object as presoma |
| CN111392709A (en) * | 2020-03-30 | 2020-07-10 | 陕西国防工业职业技术学院 | Thick-layer three-dimensional vertical grading multi-pore graphitized active wood source carbon electrode and preparation method thereof |
| CN112938971A (en) * | 2021-04-26 | 2021-06-11 | 中国科学院城市环境研究所 | Coconut shell based mesoporous activated carbon and preparation method and application thereof |
| CN115010129A (en) * | 2022-06-06 | 2022-09-06 | 广州碳加科技有限公司 | Preparation method of special capacitance carbon for super capacitor |
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| CN103011129A (en) * | 2012-12-13 | 2013-04-03 | 黑龙江大学 | Method for preparing high-specific-surface-area porous graphitic nanocarbon plate with coconut shells serving as raw materials |
| CN103086352A (en) * | 2013-01-09 | 2013-05-08 | 上海交通大学 | Preparation method for graphitized porous carbon for supercapacitor |
| CN104944419A (en) * | 2015-06-29 | 2015-09-30 | 中国科学院宁波材料技术与工程研究所 | Graphitized carbon material and preparation method thereof, and supercapacitor |
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| CN103011129A (en) * | 2012-12-13 | 2013-04-03 | 黑龙江大学 | Method for preparing high-specific-surface-area porous graphitic nanocarbon plate with coconut shells serving as raw materials |
| CN103086352A (en) * | 2013-01-09 | 2013-05-08 | 上海交通大学 | Preparation method for graphitized porous carbon for supercapacitor |
| CN104944419A (en) * | 2015-06-29 | 2015-09-30 | 中国科学院宁波材料技术与工程研究所 | Graphitized carbon material and preparation method thereof, and supercapacitor |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106219545A (en) * | 2016-07-25 | 2016-12-14 | 句容市百诚活性炭有限公司 | A kind of preparation method of sucrose base grading-hole activated carbon |
| CN108298517A (en) * | 2017-01-12 | 2018-07-20 | 中国科学院化学研究所 | A kind of method and its product preparing porous carbon materials using halogenated polyolefin hydrocarbon-based polymeric object as presoma |
| CN108083276A (en) * | 2017-12-29 | 2018-05-29 | 北海星石碳材料科技有限责任公司 | The preparation method of ultracapacitor activated carbon |
| CN108083276B (en) * | 2017-12-29 | 2020-12-01 | 北海星石碳材料科技有限责任公司 | Preparation method of super capacitor activated carbon |
| CN111392709A (en) * | 2020-03-30 | 2020-07-10 | 陕西国防工业职业技术学院 | Thick-layer three-dimensional vertical grading multi-pore graphitized active wood source carbon electrode and preparation method thereof |
| CN111392709B (en) * | 2020-03-30 | 2021-06-04 | 陕西国防工业职业技术学院 | Thick-layer three-dimensional vertical grading multi-pore graphitized active wood source carbon electrode and preparation method thereof |
| CN112938971A (en) * | 2021-04-26 | 2021-06-11 | 中国科学院城市环境研究所 | Coconut shell based mesoporous activated carbon and preparation method and application thereof |
| CN115010129A (en) * | 2022-06-06 | 2022-09-06 | 广州碳加科技有限公司 | Preparation method of special capacitance carbon for super capacitor |
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