CN105174255A - Method for preparing super-porous carbon material through persimmon fruit peels - Google Patents
Method for preparing super-porous carbon material through persimmon fruit peels Download PDFInfo
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- CN105174255A CN105174255A CN201510611801.6A CN201510611801A CN105174255A CN 105174255 A CN105174255 A CN 105174255A CN 201510611801 A CN201510611801 A CN 201510611801A CN 105174255 A CN105174255 A CN 105174255A
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- porous carbon
- carbon material
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Abstract
The invention relates to a method for preparing super-porous carbon material through persimmon fruit peels. The method comprises the steps of 1, material preparation; 2, carbonization, wherein dried persimmon fruit peel powder is carbonized for a certain period of time at certain temperature under the atmosphere of inert gas, and a porous carbon material is obtained; 3, screening, wherein the carbon material obtained after carbonization is screened by a screen with the mesh number larger than 100 and smaller than 200 for use; 4, activation, wherein the porous carbon material and an activating agent are mixed according to a certain ratio, and the mixture is activated at certain temperature under the atmosphere of inert gas to obtain a super-porous carbon material crude product; 5, rinsing, wherein suction filtering and washing are carried out on the porous material with activating agent residues till the material is neutral, and meanwhile the activating agent is recycled; 6, redrying. Waste is used as raw materials for preparing the porous carbon material, so that the preparation cost of the porous carbon material is reduced, and the important environmental protection significance is achieved.
Description
Technical field
The present invention relates to an a kind of step rare gas element charring and prepare the super porous carbon MATERIALS METHODS that porous carbon material and activation prepare high-specific surface area, particularly utilize persimmon pericarp discarded in dried persimmon processing process to prepare the method for porous carbon material.
Background technology
Porous carbon material is also known as porous carbon black, and be traditional and the artificial material in modern times, its outward appearance is black powder or unformed particulate state.Its inside has flourishing pore texture, huge specific surface area.Therefore porous carbon material is a kind of carbonaceous material having excellent absorption property.Be applied to the industry-by-industry of industry and national economy, and all respects of environment protection and human lives, as fine chemistry industry, medication chemistry, bio-pharmaceuticals process product are purified, refine, decolour, filtered; The purification of environment-friendly engineering waste water, sanitary wastewater, decolouring, deodorization, COD falls; Improvement of petrochemical industry production, natural gas conditioning, desulfurization, deodorizing, waste gas etc.Extensive just based on porous carbon material Application Areas, makes it have good development prospect.Main raw material prepared by porous carbon material can be almost all organic substances being rich in carbon, as the representative wood chip, charcoal etc. of wooden porous carbon material; The representative Exocarpium cocois (Cocos nucifera L), nut-shell, almond shell etc. of shell porous carbon material; The representative brown coal, mud coal, bituminous coal, hard coal etc. of ature of coal porous carbon material; The representative pitch etc. of petroleum-type porous carbon material; The useless charcoal etc. of the representative of regenerated carbon.These materials containing carbon rich, in tube furnace, are converted into porous carbon material by pyrolysis under certain high temperature and certain pressure.In this reactivation process, the pore texture of huge surface-area and complexity prosperity is formed gradually.Can not enter in the porous carbon blanking aperture less than its hole because of macromole, in adsorption process, the size of these holes has the function of direct adsorption selection to adsorbate.Method prepared by porous carbon material mainly contains the activation of physical activation method, chemical activation method and physical-chemical.
Above-mentioned three kinds of activation methods respectively have relative merits: porous carbon material yield prepared by chemical activation is higher, and hole is flourishing, and absorption property is good, but this method is large to equipment corrosion, and chemical reagent not easily reclaims, and environmental pollution is serious, pyrolysis energy recycling difficulty etc.Although physical activation method technique is simple, pollute less but reaction time consumption is longer, energy loss is high.If prepare porous carbon material in atmosphere of inert gases, by greatly alleviating the shortcoming of activator use procedure, production cost certainly will be reduced simultaneously, there are important market outlook.Up to now, document is not reported in atmosphere of inert gases the technology preparing porous charcoal.
Persimmon, has another name called rice cracker, bezoar from monkeys.Persimmon can up to 20 meters.The wealthy avette or semisphere of tree crown, bark black gray expandable is cleaved into square fritter.Leaf oblong, surperficial deep green, glossy, keratin, autumn has set in, and part leaf reddens, and leaf scar is large, reddish-brown.Flower dioecy or polygamy homophyletic, be born in the axil of newborn branch, brightly yellowish white.5 ~ June of florescence, 9 ~ October of fructescence.Fruit shape is different because of kind, orange or red, sepal Su Cun great, the blunt circle of tip.Persimmon is not only nutritious, containing a large amount of carbohydrates and multivitamin, and has very high pharmaceutical use and economic worth.At present, found to contain various active material in persimmon, comprised carotenoid, flavonoid, lipid acid, phenols and multiple amino acids, trace element, the fields such as medicine, health care and makeup can be widely used in.Wherein, fresh persimmon, dry dried persimmon, persimmon sugar, the calyx and receptacle of a persimmon, persimmon leaf are all good medicines.At present, persimmon is mainly processed into dried persimmon to be sold, and this causes having a large amount of persimmon pericarp to produce every year.Containing abundant nutritive ingredient in persimmon pericarp, as very abundant in carotenoid, total phenol, vitamins C, vitamin A, sugar and crude protein, robust fibre, pectin equal size.Feed feeding chicken can be processed into, pig etc.At present, successfully have developed the products such as persimmon pericarp meals, fibre additive, persimmon pericarp jelly, persimmon pericarp fruit wine and persimmon fruit peel chewy confection, improve the economic worth of persimmon.But it is not to this precious resources, also abundant to its exploitation at present.
Based on this, the present invention is proposed.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method preparing porous carbon material under an inert atmosphere with persimmon pericarp, with discarded persimmon pericarp for porous carbon material prepared by raw material, not only can reduce the cost preparing porous carbon material, and the utilization again of refuse, the treatment of wastes with processes of wastes against one another, turn waste into wealth, there is important environment protection significance.
For achieving the above object, the present invention is achieved by the following technical solutions:
Persimmon pericarp prepares a method for super porous Carbon Materials, comprises the following steps:
(1) get the raw materials ready: by the screening of persimmon pericarp, dipping, drying, pulverize and sieve, obtaining persimmon fruit peel powder last for subsequent use;
(2) carbonize: by the persimmon pericarp powder of drying at rare gas element (as N
2) under atmosphere, carbonize the regular hour at a certain temperature, obtain porous carbon material precursor, i.e. carbonized material;
(3) after sieve: number of being looked over so as to check by the carbonized material obtained after charing is greater than 100 orders and is less than 200 object sieves, for subsequent use;
(4) activate: after carbonized material and activator are mixed by a certain percentage, by compound under atmosphere of inert gases, carry out activating to obtain porous carbon material crude product in certain temperature;
(5) rinsing: filtering and washing is carried out to neutral to the porous carbon material of residual activator, reclaims activator simultaneously;
(6) dry again: to through washing to neutral porous carbon material dry 12h again, to collect and get final product.
The temperature rise rate of described charing is 1-9 DEG C/min, and carbonization temperature is 350-700 DEG C, and carbonization time is 2-3 hour.
The temperature of described activation is 450-850 DEG C, and soak time is 1-2 hour.
Described carbonization and activation step all carry out in carbonization-activation device; Described carbonization-activation device comprises tube furnace, is provided with silica tube in described tube furnace, and described silica tube is connected with nitrogengas cylinder and temperature control unit, and described nitrogengas cylinder is connected to the end of silica tube, and the top of nitrogengas cylinder is provided with under meter.
Described temperature dry is again 120 DEG C.
The activator of described activation is KOH, ZnCl
2, carbonic acid gas, water vapour or oxygen, described activator and persimmon pericarp raw materials quality are than being 3-4:1.
The activator of described activation is KOH or ZnCl
2, described activator KOH or ZnCl
2with the blending means of persimmon pericarp carbonized material for being dry mixed grinding method.
Drying temperature in described step (1) is 120 DEG C, and time of drying is 24h.
Grit number excessively in described step (1) is 30 orders.
Beneficial effect of the present invention is as follows:
Persimmon pericarp of the present invention prepares the method for super porous Carbon Materials, and persimmon pericarp contains a large amount of carbon element, is that porous carbon material prepared by raw material, not only can reduces the cost preparing porous carbon material, and have important environment protection significance with waste; Product is all better at intensity, gas separating property and absorption property.The present invention, in whole production process, does not produce any hazardous and noxious substances, and easy to operate, and yield rate is high.
Accompanying drawing explanation
Fig. 1 is the structural representation of carbonization-activation device of the present invention;
Wherein, 1 be silica tube, 2 be nitrogengas cylinder, 3 be temperature control unit, 4 be under meter, 5 for tube furnace.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to this.
Persimmon pericarp prepares a method for super porous Carbon Materials, comprises the following steps:
(1) get the raw materials ready: by the screening of persimmon pericarp, drying, pulverize and sieve, obtaining persimmon fruit peel powder last for subsequent use; Drying temperature is 120 DEG C, and time of drying is 24h; Crossing grit number is 30 orders.
(2) carbonize: by the persimmon pericarp powder of drying under atmosphere of inert gases, at 350-700 DEG C, carbonize 2-3 hour, temperature rise rate is 1-9 DEG C/min, obtains porous carbon material precursor, i.e. carbonized material;
(3) after sieve: number of being looked over so as to check by the carbonized material obtained after charing is greater than 100 orders and is less than 200 object sieves, for subsequent use;
(4) activate: after carbonized material and activator are mixed by a certain percentage, by compound under atmosphere of inert gases, carry out activation 1-2 hour obtaining porous carbon material crude product the temperature of 450-850 DEG C;
Activator is KOH, ZnCl
2, carbonic acid gas, water vapour or oxygen, activator and persimmon pericarp raw materials quality are than being 3-4:1.
When activator is KOH or ZnCl
2time, activator KOH or ZnCl
2with the blending means of persimmon pericarp carbonized material for being dry mixed grinding method.
(5) rinsing: filtering and washing is carried out to neutral to the porous carbon material of residual activator, reclaims activator simultaneously;
(6) dry again: to through washing to neutral porous carbon material dry 12h again at 120 DEG C, collect and get final product.
Carbonization in the present invention and activation step all carry out in carbonization-activation device; As shown in Figure 1, carbonization-activation device comprises tube furnace 5, is provided with silica tube 1 in tube furnace 5, and silica tube 1 is connected with nitrogengas cylinder 2 and temperature control unit 3, and nitrogengas cylinder 2 is connected to the end of silica tube 1, and the top of nitrogengas cylinder 2 is provided with under meter 4.
In silica tube 1, logical nitrogen does protection gas and H charing and reactivation process produced
2o, CO, CO
2emptying at the other end Deng small molecules; Silica tube 1 refractory brick parcel, keeps constant temperature.Resistance wire and thermopair is had in refractory brick.
The present invention prepares porous carbon material in atmospheric conditions.Adopt KOH for activator, have following reaction:
4KOH+C→K
2CO
3+H
2O+2H
2
A certain amount of carbonized material is mixed postactivated with alkaloids with certain method, roughly can infer and experienced by following process: at 300 ~ 500 DEG C, carbonized material high temperature dehydration, activate within the scope of 600 ~ 800 DEG C, after activation, cooling, is washed with distilled water to neutrality, dry again, just obtain porous carbon material finished product.
Consider that KOH at high temperature decomposes, the reductibility of carbon, in conjunction with the result of study of metal-salt as steam activation catalyzer, know by inference in priming reaction process, may also react:
2KOH→K
2O+H
2O
C+H
2O→H
2+CO
CO+H
2O→H
2+CO
2
K
2O+H
2→2K+H
2O
K
2O+C→2K+CO
K
2O+CO
2→K
2CO
3
K
2CO
3+2C→2K+H
2O
Carry out reaming by above-mentioned reaction, realize porous channel, increase specific surface area, improve application performance
Less than 500 DEG C there is dehydration reaction, under potassium oxide exists, water-gas reaction and gas shift reaction occur, can think that potassium oxide is catalyzer.The carbonic acid gas produced and potassium oxide react and are almost transformed into carbonate completely, and the gas therefore produced mainly hydrogen, only obtains the carbon monoxide of minute quantity, carbonic acid gas, methane and tarry matters.The carbon consumed in reactivation process mainly generates salt of wormwood, thus makes product have very large specific surface area.At about 800 DEG C, potassium oxide is reduced into by hydrogen or carbon and separates out with potassium metal (boiling point 762 DEG C) form, and what the steam of potassium metal constantly clamp-oned that carbon atom forms activates between layers, directly causes porous carbon material to have flourishing aperture.
Conclusion possible is as follows drawn: ZnCl within the scope of 200 ~ 600 DEG C with activator zinc chloride activation persimmon pericarp carbonized material
2as follows to persimmon pericarp role: at 200 ~ 350 DEG C, the volatile matter gasification dehydrogenation in persimmon pericarp; 350 ~ 450 DEG C, ZnCl
2dehydrogenation limit the formation of tar, cause the lignocellulose aromizing in persimmon pericarp; 450 ~ 600 DEG C, ZnCl
2gasification, ZnCl
2skeleton function is played in the inside that molecule is impregnated into carbon, deposits on skeleton after the superpolymer charing of carbon, and after removing ZnCl2 with hot water and pickling, porous carbon material just has huge table specific area and flourishing aperture.
ZnCl
2active principles and KOH similar, CO
2all physical activation method with water vapour or oxygen.
The every test data of method products obtained therefrom that employing the present invention persimmon pericarp prepares porous carbon material is as follows:
| Title | Index |
| Penetrating curve, % | 70-110 |
| Physical strength, % | ＞95％ |
| Iodine sorption value, mg/g | 980～1200 |
| Methylene blue adsorption value, % | 200-240 |
| Adsorption of Phenol value, mg/g | —— |
| Benzene adsorptive value, mg/g | —— |
| Bulk density, g/l | 400～550 |
| Mass ratio surface, m 2/g | 1000～1800 |
From above data, the porous carbon material good adsorption performance obtained.Porous carbon material adsorptive power improves 10 ~ 30%; Bulk density and physical strength high.The porous carbon material that the present invention obtains can be applicable to flue gas desulfurization, sewage disposal, gas sweetening and storage, the fields such as solvent recuperation.
Embodiment 1
By persimmon pericarp 120 DEG C of dry 24h, sieve 30 orders, carbonization temperature 400 DEG C, carbonization time 2h, and temperature rise rate 3 DEG C/min prepares porous carbon material performance:
| Title | Index |
| Penetrating curve, % | 75 |
| Physical strength, % | 96％ |
| Iodine sorption value, mg/g | 254 |
| Methylene blue adsorption value, % | 32 |
| Adsorption of Phenol value, mg/g | 89 |
| Benzene adsorptive value, mg/g | 120 |
| Bulk density, g/l | 513 |
| Mass ratio surface, m 2/g | 465 |
Embodiment 2
By persimmon pericarp 120 DEG C of dry 24h, sieve 30 orders, carbonization temperature 700 DEG C, carbonization time 1h, temperature rise rate 9 DEG C/min; After sieve 100 ~ 200 order; Activation temperature 700 DEG C, soak time 1h, temperature rise rate 7 DEG C/min, KOH than 3: 1, prepares porous carbon material performance with raw materials quality:
| Title | Index |
| Penetrating curve, % | 95 |
| Physical strength, % | 96％ |
| Iodine sorption value, mg/g | 1224 |
| Methylene blue adsorption value, % | 138 |
| Adsorption of Phenol value, mg/g | 343 |
| Benzene adsorptive value, mg/g | 389 |
| Bulk density, g/l | 230 |
| Mass ratio surface, m 2/g | 1229 |
Embodiment 3
By persimmon pericarp 120 DEG C of dry 24h, sieve 30 orders, carbonization temperature 500 DEG C, carbonization time 2h, temperature rise rate 5 DEG C/min, ZnCl
2with raw materials quality than 4: 1,850 DEG C of steam activations, prepare porous carbon material performance:
| Title | Index |
| Penetrating curve, % | 95 |
| Physical strength, % | 96％/ |
| Iodine sorption value, mg/g | 1186 |
| Methylene blue adsorption value, % | 238 |
| Bulk density, g/l | 535 |
| Mass ratio surface, m 2/g | 1186 |
Ultimate analysis
| Sample | Total mass/g | N/％ | C/％ | H/％ |
| Persimmon pericarp | 2.5960 | 1.199 | 46.69 | 5.994 |
Above-described embodiment only illustrates inventive concept of the present invention for explaining, but not the restriction to rights protection of the present invention, all changes utilizing this design the present invention to be carried out to unsubstantiality, all should fall into protection scope of the present invention.
Claims (9)
1. persimmon pericarp prepares a method for super porous Carbon Materials, it is characterized in that comprising the following steps:
(1) get the raw materials ready: by the screening of persimmon pericarp, dipping, drying, pulverize and sieve, obtaining persimmon fruit peel powder last for subsequent use; (2) carbonize: by the persimmon pericarp powder of drying under atmosphere of inert gases, carbonize the regular hour at a certain temperature, obtain porous carbon material precursor, i.e. carbonized material; Charing sample has microchannel structure, and specific surface area can reach 400m
2/ g;
(3) after sieve: number of being looked over so as to check by the carbonized material obtained after charing is greater than 100 orders and is less than 200 object sieves, for subsequent use;
(4) activate: after carbonized material and activator are mixed by a certain percentage, by compound under atmosphere of inert gases, carry out activating to obtain porous carbon material crude product in certain temperature;
(5) rinsing: filtering and washing is carried out to neutral to the porous carbon material of residual activator, reclaims activator simultaneously;
(6) dry again: to through washing to neutral porous carbon material dry 12h again, to collect and get final product.
2. persimmon pericarp prepares the method for super porous Carbon Materials as claimed in claim 1, it is characterized in that: the temperature rise rate of described charing is 1-9 DEG C/min, and carbonization temperature is 350-700 DEG C, and carbonization time is 2-3 hour; After charing, sample has pore structure and comparatively bigger serface.
3. persimmon pericarp prepares the method for super porous Carbon Materials as claimed in claim 1, it is characterized in that: the temperature of described activation is 450-850 DEG C, and soak time is 1-2 hour.
4. as described in claim as arbitrary in claim 1-3, persimmon pericarp prepares the method for super porous Carbon Materials, it is characterized in that: described carbonization and activation step all carry out in carbonization-activation device; Described carbonization-activation device comprises tube furnace, is provided with silica tube in described tube furnace, and described silica tube is connected with nitrogengas cylinder and temperature control unit, and described nitrogengas cylinder is connected to the end of silica tube, and the top of nitrogengas cylinder is provided with under meter.
5. persimmon pericarp prepares the method for super porous Carbon Materials as claimed in claim 1, it is characterized in that: described temperature dry is again 120 DEG C.
6. persimmon pericarp prepares the method for super porous Carbon Materials as claimed in claim 1, it is characterized in that: the activator of described activation is KOH, ZnCl
2, carbonic acid gas, water vapour or oxygen, described activator and persimmon pericarp raw materials quality are than being 3-4:1.
7. persimmon pericarp prepares the method for super porous Carbon Materials as claimed in claim 6, it is characterized in that: the activator of described activation is KOH or ZnCl
2, described activator KOH or ZnCl
2with the blending means of persimmon pericarp carbonized material for being dry mixed grinding method.
8. persimmon pericarp prepares the method for super porous Carbon Materials as claimed in claim 1, it is characterized in that: the drying temperature in described step (1) is 120 DEG C, and time of drying is 24h.
9. persimmon pericarp prepares the method for super porous Carbon Materials as claimed in claim 1, it is characterized in that: the grit number excessively in described step (1) is 30 orders.
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|---|---|---|---|
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111689496A (en) * | 2019-03-12 | 2020-09-22 | 淮阴师范学院 | Persimmon peel-based nitrogen-doped activated carbon and preparation method thereof |
| WO2023087798A1 (en) * | 2021-11-17 | 2023-05-25 | 广东邦普循环科技有限公司 | Method for preparing refractory material from waste battery residues, and use of refractory material |
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| US3917806A (en) * | 1973-09-27 | 1975-11-04 | Kureha Chemical Ind Co Ltd | Method for the preparation of carbon moldings and activated carbon molding therefrom |
| CN101844764A (en) * | 2010-05-27 | 2010-09-29 | 浙江师范大学 | Method for preparing active carbon by using finger citron residue |
| CN102423690A (en) * | 2011-10-17 | 2012-04-25 | 山东大学 | Preparation method of mesoporous tomato stem active carbon |
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2015
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| US3917806A (en) * | 1973-09-27 | 1975-11-04 | Kureha Chemical Ind Co Ltd | Method for the preparation of carbon moldings and activated carbon molding therefrom |
| CN101844764A (en) * | 2010-05-27 | 2010-09-29 | 浙江师范大学 | Method for preparing active carbon by using finger citron residue |
| CN102423690A (en) * | 2011-10-17 | 2012-04-25 | 山东大学 | Preparation method of mesoporous tomato stem active carbon |
Non-Patent Citations (2)
| Title |
|---|
| J.M. ROSAS ET AL.: "On the preparation and characterization of chars and activated carbons from orange skin", 《FUEL PROCESSING TECHNOLOGY》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111689496A (en) * | 2019-03-12 | 2020-09-22 | 淮阴师范学院 | Persimmon peel-based nitrogen-doped activated carbon and preparation method thereof |
| WO2023087798A1 (en) * | 2021-11-17 | 2023-05-25 | 广东邦普循环科技有限公司 | Method for preparing refractory material from waste battery residues, and use of refractory material |
| GB2618499A (en) * | 2021-11-17 | 2023-11-08 | Guangdong Brunp Recycling Technology Co Ltd | Method for preparing refractory material from waste battery residues, and use of refractory material |
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Application publication date: 20151223 |