CN105858651A - A preparing method of activated carbon - Google Patents
A preparing method of activated carbon Download PDFInfo
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- CN105858651A CN105858651A CN201610195447.8A CN201610195447A CN105858651A CN 105858651 A CN105858651 A CN 105858651A CN 201610195447 A CN201610195447 A CN 201610195447A CN 105858651 A CN105858651 A CN 105858651A
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Abstract
The invention relates to a preparing method of activated carbon, and belongs to the field of chemical engineering. Main raw materials of the activated carbon comprise lignite and a plant biomass material. The preparing method includes weighing the lignite and the plant biomass material, drying, mixing, smashing, sieving with a sieve having a size of 60 meshes, adding a solvent, dipping for 1-24 h, filtering, drying at 105 DEG C for 12-24 h, putting into a horizontal type temperature programmed tube furnace, raising the temperature in a programmed manner to 550-950 DEG C in a mixed atmosphere, carbonizing for 1-12 h, turning off the power of the tube furnace, only feeding a nitrogen atmosphere until room temperature, and taking out to obtain the activated carbon. The method can stabilize active branch chain structures of the lignite and the plant biomass material, increases the intensity of the activated carbon, increases the porosity of micropores and mesopores, increases the effective specific surface area, allows the activated carbon to maintain a branch chain functional group structure and to have enhanced mechanical intensity, increases the repeating utilization rate and further reduces the cost.
Description
[technical field]
The present invention relates to a kind of chemical manufacturing process, the preparation method of a kind of activated carbon.
[technical background]
Activated carbon is made up of the carbon of more than 80%-90%, because its pore structure having complexity and bigger specific surface area, is current
Most widely used adsorbing material, is also a kind of hydrophobic adsorbent.The making raw material of activated carbon can be divided three classes: coal feedstock,
Petroleum and plant material.Petroleum refers to remaining residue fraction in petroleum refining process, owing to its raw material is limited,
Range is less.Coal in China abundant raw material, and its stable in properties, intensity is high, hole is flourishing, specific surface area is big, especially
Micropore volume is big, the most widely used.At present, utilizing plant material to prepare activated carbon, this technology the most still belongs to new technique
Field.Rich in natural plant cell structures in plant material, it it is the good carrier forming microcellular structure；And plant material is mostly
Common being easy to get, cost of manufacture is low.
Brown coal are the abundantest in China's yield, account for more than the 13% of whole nation coal gross reserves.Brown coal are tied containing a large amount of active branched chains
Structure, itself is a kind of respond well adsorbent.The Chinese invention patent of Publication No. CN 102583322 B discloses " one
Plant active brown coal and preparation method thereof ", it is that brown coal are prepared through broken, screening, carbonization, oxidation, activation processing, cooling
The brown coal charcoal that big porosity is higher, pollutant in absorption effluent.Macropore refers to that aperture is more than the hole of 50nm, and we know
Activated carbon is mesopore for processing the live part of dirty water pollutant, is in the hole of 2-50nm because mesopore is aperture, favorably
Spread to micropore in adsorbate, make adsorption more stable.Therefore, this brown coal charcoal is difficult to it and effectively processes Sewage
The purpose of dye.
[summary of the invention]
For the problems referred to above, the present invention proposes the preparation method of a kind of activated carbon.The present invention is by brown coal and plant biological material
Being mixed for preparing activated carbon according to special ratios, the method can stablize brown coal and the active function groups in plant biological material
Active branched chain structure in structure, and brown coal and plant biological material, improve activated carbon intensity, increases micropore, mesopore
Porosity, improves effective ratio area, makes activated carbon the most both save pendant functional groups's structure from damage, can strengthen again its machinery strong
Degree, improves recycling rate of waterused, reduces cost further.
Technical scheme is as follows:
The preparation method of a kind of activated carbon, the primary raw material of described activated carbon includes: brown coal and plant biological material, and it makes
Method comprises the following steps:
(1) by fully dried to brown coal and plant biological material, brown coal and the 1-20 weight portion of 1-50 weight portion are weighed respectively
Plant biological material, after mixing pulverize, cross 60 mesh sieves, obtain mixing raw material；
(2) in above-mentioned mixing raw material, add the solvent of mixing raw material gross mass 1-20 times, after dipping 1-24h, filter, then
12-24h it is dried under the conditions of 105 DEG C；Wherein, described solvent be mass fraction be 10% KOH solution, mass fraction be 10%
NaOH solution, mass fraction be the H of 30%2O2Solution, mass fraction are the HNO of 10%3Any one in solution；
(3) above-mentioned dried mixing raw material is put in pressure-bearing type temperature programming tube furnace, be passed through mixed atmosphere temperature programming extremely
550-950 DEG C, keep temperature, atmosphere constant, carbonization 1-12h；Close tube furnace power supply afterwards, keep being passed through nitrogen atmosphere,
And stop being passed through other atmosphere, until room temperature, take out, obtain activated carbon；Wherein, described mixed atmosphere is: volume flow is
The ammonia of 350-450ml/min, volume flow be the steam of 2-5ml/min, volume flow be the titanium dioxide of 4-8ml/min
Any one or two kinds of in carbon and volume flow are the combination of the nitrogen of 350ml/min.
Further, in step (1), described brown coal: phosphorus content 60%～77%, apparent density is 1.1-1.2g/cm3, wave
Send out composition more than 30%.
Further, in step (1), described plant biological material is any one in straw, coconut husk, Thallus Laminariae (Thallus Eckloniae), wood flour
Or two kinds of combinations.
Further, in step (3), the heating rate of described temperature programming is 5-9 DEG C/min.
The invention provides the preparation method of a kind of activated carbon, compared with prior art, have the advantages that system of the present invention
Standby activated carbon with a certain proportion of brown coal with plant biological material as raw material, the method can stablize brown coal and plant biomass material
Active branched chain structure in material, improves activated carbon intensity.The ammonia atmosphere being passed through in Temperature Programmed Processes can widen space；
The small molecule of steam atmosphere can increase the porosity of micropore, mesopore；Carbon dioxide atmosphere can increase the carbon in activated carbon
Content, improves activated carbon stability and mechanical strength；Nitrogen atmosphere is a kind of noble gas, and activated carbon can be made at carbonisation
Middle holding anaerobic condition, prevents activated carbon excessively oxidated and reduces yield.It is passed through a certain proportion of mixed atmosphere can effectively carry
High-specific surface area, makes activated carbon the most both save pendant functional groups's structure from damage, can strengthen again its mechanical strength, improves and repeats profit
By rate, reduce cost further.
Obtained by the present invention, activated carbon has adsorption, can be applicable to discolor, de-tastes, removes pollutant etc..Can be additionally used in absorption
Heavy metal, for precious metal refineries aspect.No matter in family or industrial, there is good application prospect.
[detailed description of the invention]
The following examples can help those skilled in the art to be more completely understood by the present invention, but cannot limit by any way
The present invention processed.
Embodiment 1
The preparation method of a kind of activated carbon, the primary raw material of described activated carbon includes: brown coal and plant biological material, and it makes
Method comprises the following steps:
(1) by fully dried to brown coal and plant biological material, the plant biological material of 20g brown coal and 20g is weighed respectively,
Pulverize after mixing, cross 60 mesh sieves, obtain mixing raw material；Wherein, described brown coal: phosphorus content 60%, apparent density is 1.1g/cm3,
Volatile ingredient is 30%；Plant biological material is straw, coconut husk two kinds combination；
(2) in above-mentioned mixing raw material, add the solvent of mixing raw material gross mass equivalent, after dipping 1h, filter, then at 105
12h it is dried under the conditions of DEG C；Wherein, described solvent be mass fraction be the KOH solution of 10%；
(3) above-mentioned dried mixing raw material is put in pressure-bearing type temperature programming tube furnace, be passed through mixed atmosphere, with 5 DEG C/min
Heating rate temperature programming to 550 DEG C, keep temperature, atmosphere constant, carbonization 1h；Close tube furnace power supply afterwards, keep
It is passed through nitrogen atmosphere, and stops being passed through other atmosphere, until room temperature, take out, obtain activated carbon；Wherein, described mixed atmosphere
For: volume flow be the ammonia of 350ml/min, volume flow be the carbon dioxide of 5ml/min be 350ml/min with volume flow
The combination of nitrogen.
The index preparing activated carbon is: mesoporous: 35.9%；Microporosity: 48.2%；Specific surface area: 1354m2/kg；Iodine adsorbs
Value: 1100mg/g, methylene blue: 120ml/g.
Embodiment 2
The preparation method of a kind of activated carbon, the primary raw material of described activated carbon includes: brown coal and plant biological material, and it makes
Method comprises the following steps:
(1) by fully dried to brown coal and plant biological material, the plant biological material of 10g brown coal and 20g is weighed respectively,
Pulverize after mixing, cross 60 mesh sieves, obtain mixing raw material；Wherein, described brown coal: phosphorus content 70%, apparent density is 1.2g/cm3,
Volatile ingredient is 30%；Plant biological material is Thallus Laminariae (Thallus Eckloniae), wood flour two kinds combination；
(2) in above-mentioned mixing raw material, add the solvent of mixing raw material gross mass 20 times, after dipping 24h, filter, then at 105
24h it is dried under the conditions of DEG C；Wherein, described solvent be mass fraction be the H of 30%2O2Solution；
(3) above-mentioned dried mixing raw material is put in pressure-bearing type temperature programming tube furnace, be passed through mixed atmosphere, with 7 DEG C/min
Heating rate temperature programming to 750 DEG C, keep temperature, atmosphere constant, carbonization 6h；Close tube furnace power supply afterwards, keep
It is passed through nitrogen atmosphere, and stops being passed through other atmosphere, until room temperature, take out, obtain activated carbon；Wherein, described mixed atmosphere
For: volume flow is the ammonia combination with the nitrogen that volume flow is 350ml/min of 450ml/min.
The index preparing activated carbon is: mesoporous: 38.3%；Microporosity: 45.7%；Specific surface area: 1244m2/kg；Iodine adsorbs
Value: 1070mg/g, methylene blue: 115ml/g.
Embodiment 3
The preparation method of a kind of activated carbon, the primary raw material of described activated carbon includes: brown coal and plant biological material, and it makes
Method comprises the following steps:
(1) by fully dried to brown coal and plant biological material, the plant biological material of 50g brown coal and 20g is weighed respectively,
Pulverize after mixing, cross 60 mesh sieves, obtain mixing raw material；Wherein, described brown coal: phosphorus content 65%, apparent density is 1.2g/cm3,
Volatile ingredient is 35%；Plant biological material is Thallus Laminariae (Thallus Eckloniae), coconut husk two kinds combination；
(2) in above-mentioned mixing raw material, add the solvent of mixing raw material gross mass 10 times, after dipping 12h, filter, then at 105
20h it is dried under the conditions of DEG C；Wherein, described solvent be mass fraction be the NaOH solution of 10%；
(3) above-mentioned dried mixing raw material is put in pressure-bearing type temperature programming tube furnace, be passed through mixed atmosphere, with 9 DEG C/min
Heating rate temperature programming to 950 DEG C, keep temperature, atmosphere constant, carbonization 12h；Close tube furnace power supply afterwards, keep
It is passed through nitrogen atmosphere, and stops being passed through other atmosphere, until room temperature, take out, obtain activated carbon；Wherein, described mixed atmosphere
For: volume flow is the steam combination with the nitrogen that volume flow is 350ml/min of 2ml/min.
The index preparing activated carbon is: mesoporous: 39.7%；Microporosity: 52.4%；Specific surface area: 1213m2/kg；Iodine adsorbs
Value: 1025mg/g, methylene blue: 103ml/g.
Embodiment 4
The preparation method of a kind of activated carbon, the primary raw material of described activated carbon includes: brown coal and biological material, its manufacture method
Comprise the following steps:
(1) by fully dried to brown coal and plant biological material, the plant biological material of 20g brown coal and 15g is weighed respectively,
Pulverize after mixing, cross 60 mesh sieves, obtain mixing raw material；Wherein, described brown coal: phosphorus content 62%, apparent density is 1.2g/cm3,
Volatile ingredient is 33%；Plant biological material is wood flour；
(2) in above-mentioned mixing raw material, add the solvent of mixing raw material gross mass 15 times, after dipping 10h, filter, then at 105
18h it is dried under the conditions of DEG C；Wherein, described solvent be mass fraction be the HNO of 10%3Solution；
(3) above-mentioned dried mixing raw material is put in pressure-bearing type temperature programming tube furnace, be passed through mixed atmosphere, with 9 DEG C/min
Heating rate temperature programming to 650 DEG C, keep temperature, atmosphere constant, carbonization 8h；Close tube furnace power supply afterwards, keep
It is passed through nitrogen atmosphere, and stops being passed through other atmosphere, until room temperature, take out, obtain activated carbon；Wherein, described mixed atmosphere
For: volume flow is the steam combination with the nitrogen that volume flow is 350ml/min of 5ml/min.
The index preparing activated carbon is: mesoporous: 37.8%；Microporosity: 52.7%；Specific surface area: 1464m2/kg；Iodine adsorbs
Value: 1160mg/g, methylene blue: 104ml/g.
Embodiment 5
The preparation method of a kind of activated carbon, the primary raw material of described activated carbon includes: brown coal and plant biological material, and it makes
Method comprises the following steps:
(1) by fully dried to brown coal and plant biological material, the plant biological material of 30g brown coal and 15g is weighed respectively,
Pulverize after mixing, cross 60 mesh sieves, obtain mixing raw material；Wherein, described brown coal: phosphorus content 63%, apparent density is 1.2g/cm3,
Volatile ingredient is 32%；Plant biological material is Thallus Laminariae (Thallus Eckloniae)；
(2) in above-mentioned mixing raw material, add the solvent of mixing raw material gross mass 15 times, after dipping 5h, filter, then at 105
16h it is dried under the conditions of DEG C；Wherein, described solvent be mass fraction be the NaOH solution of 10%；
(3) above-mentioned dried mixing raw material is put in pressure-bearing type temperature programming tube furnace, be passed through mixed atmosphere, with 6 DEG C/min
Heating rate temperature programming to 850 DEG C, keep temperature, atmosphere constant, carbonization 5h；Close tube furnace power supply afterwards, keep
It is passed through nitrogen atmosphere, and stops being passed through other atmosphere, until room temperature, take out and obtain activated carbon；Wherein, described mixed atmosphere is:
Volume flow is the carbon dioxide combination with the nitrogen that volume flow is 350ml/min of 4ml/min.
The index preparing activated carbon is: mesoporous: 37.2%；Microporosity: 47.4%；Specific surface area: 1154m2/kg；Iodine adsorbs
Value: 1360mg/g, methylene blue: 137ml/g.
Embodiment 6
The preparation method of a kind of activated carbon, the primary raw material of described activated carbon includes: brown coal and plant biological material, and it makes
Method comprises the following steps:
(1) by fully dried to brown coal and plant biological material, the plant biological material of 40g brown coal and 15g is weighed respectively,
Pulverize after mixing, cross 60 mesh sieves, obtain mixing raw material；Wherein, described brown coal: phosphorus content 63%, apparent density is 1.2g/cm3,
Volatile ingredient is 32%；Plant biological material is Thallus Laminariae (Thallus Eckloniae) and coconut husk；
(2) in above-mentioned mixing raw material, add the solvent of mixing raw material gross mass 12 times, after dipping 4h, filter, then at 105
15h it is dried under the conditions of DEG C；Wherein, described solvent be mass fraction be the NaOH solution of 10%；
(3) above-mentioned dried mixing raw material is put in pressure-bearing type temperature programming tube furnace, be passed through mixed atmosphere, with 6 DEG C/min
Heating rate temperature programming to 850 DEG C, keep temperature, atmosphere constant, carbonization 3h；Close tube furnace power supply afterwards, keep
It is passed through nitrogen atmosphere, and stops being passed through other atmosphere, until room temperature, take out, obtain activated carbon；Wherein, described mixed atmosphere
For: volume flow is the carbon dioxide combination with the nitrogen that volume flow is 350ml/min of 8ml/min.
The index preparing activated carbon is: mesoporous: 28.2%；Microporosity: 57.4%；Specific surface area: 1024m2/kg；Iodine adsorbs
Value: 1337mg/g, methylene blue: 127ml/g.
Comparative example
The present invention is by substantial amounts of experiment, brown by prepare in Chinese invention patent " a kind of active brown coal and preparation method thereof "
Coal activity charcoal, with various embodiments of the present invention obtained by activated carbon, microporosity contrast, comparing result is as follows:
In table 1 activated carbon of the present invention and brown coal activated carbon, microporosity comparing result
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Brown coal activated carbon | |
| Mesoporous | 35.9% | 38.3% | 39.7% | 37.8% | 37.2% | 28.2% | 10.8% |
| Microporosity | 48.2% | 45.7% | 52.4% | 52.7% | 47.4% | 57.4% | 31.5% |
From table 1 it follows that the activated carbon prepared by the present invention is compared with brown coal activated carbon, there is higher mesoporous and micro-
Porosity, mesoporous reaches more than 3 times of brown coal activated carbon, it is possible to realize more preferable adsorption effect.
Although, the present invention is described in detail the most with a general description of the specific embodiments, but in the present invention
On the basis of, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Therefore, not
Deviate these modifications or improvements on the basis of spirit of the present invention, belong to the scope of protection of present invention.
Claims (4)
1. the preparation method of an activated carbon, it is characterised in that: the primary raw material of described activated carbon includes brown coal and plant biomass
Material, its manufacture method comprises the following steps:
(1) by fully dried to brown coal and plant biological material, brown coal and the 1-20 weight portion of 1-50 weight portion are weighed respectively
Plant biological material, after mixing pulverize, cross 60 mesh sieves, obtain mixing raw material；
(2) in above-mentioned mixing raw material, add the solvent of mixing raw material gross mass 1-20 times, after dipping 1-24h, filter, then
12-24h it is dried under the conditions of 105 DEG C；Wherein, described solvent be mass fraction be 10% KOH solution, mass fraction be 10%
NaOH solution, mass fraction be the H of 30%2O2Solution, mass fraction are the HNO of 10%3Any one in solution；
(3) above-mentioned dried mixing raw material is put in pressure-bearing type temperature programming tube furnace, be passed through mixed atmosphere temperature programming extremely
550-950 DEG C, keep temperature, atmosphere constant, carbonization 1-12h；Close tube furnace power supply afterwards, keep being passed through nitrogen atmosphere,
And stop being passed through other atmosphere, until room temperature, take out, obtain activated carbon；Wherein, described mixed atmosphere is: volume flow is
The ammonia of 350-450ml/min, volume flow be the steam of 2-5ml/min, volume flow be the titanium dioxide of 4-8ml/min
Any one or two kinds of in carbon and volume flow are the combination of the nitrogen of 350ml/min.
The preparation method of activated carbon the most according to claim 1, it is characterised in that: in step (1), described brown coal
Phosphorus content is 60%-77%, and apparent density is 1.1-1.2g/cm3, volatile ingredient is more than 30%.
3. the preparation method of the activated carbon described in claim 1, it is characterised in that: in step (1), described plant biomass
Material is any one or two kinds of combinations in straw, coconut husk, Thallus Laminariae (Thallus Eckloniae), wood flour.
The preparation method of activated carbon the most according to claim 1, it is characterised in that: temperature programming described in step (3)
Heating rate be 5-9 DEG C/min.
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| CN106744941A (en) * | 2017-02-28 | 2017-05-31 | 苏州顶裕节能设备有限公司 | Activated carbon and its method prepared by a kind of utilization discarded object |
| CN107021470A (en) * | 2017-04-27 | 2017-08-08 | 农玉金 | A kind of preparation method of composite biomass carbon material |
| CN107051383A (en) * | 2017-04-27 | 2017-08-18 | 农玉金 | A kind of preparation method of carbon material for sewage disposal |
| CN107381572A (en) * | 2017-08-30 | 2017-11-24 | 章德恩 | A kind of capacitor bio-coal matrix activated carbon material and preparation method thereof |
| CN108010749A (en) * | 2017-11-30 | 2018-05-08 | 浙江海洋大学 | A kind of preparation method based on kelp biomass charcoal super capacitor electrode material |
| CN107996766A (en) * | 2018-01-12 | 2018-05-08 | 广西天昌投资有限公司 | A kind of Camellia nitidissima nano particle and preparation method thereof |
| CN110693290A (en) * | 2019-11-01 | 2020-01-17 | 广西壮族自治区林业科学研究院 | Mildew-proof Buddha incense and processing technology thereof |
| CN110697713A (en) * | 2019-11-01 | 2020-01-17 | 广西壮族自治区林业科学研究院 | Preparation method of cinnamon twig activated carbon |
| CN111908443A (en) * | 2020-06-24 | 2020-11-10 | 西安理工大学 | Preparation method of self-doped porous carbon |
| CN112575575A (en) * | 2020-07-21 | 2021-03-30 | 苏州远浩新纺织科技有限公司 | Hole expanding method for activated carbon fiber |
| CN115193434A (en) * | 2022-08-26 | 2022-10-18 | 山东省科学院能源研究所 | Method and system for cooperatively removing carbon-based catalyst, VOCs and nitrogen oxides |
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| CN106744941A (en) * | 2017-02-28 | 2017-05-31 | 苏州顶裕节能设备有限公司 | Activated carbon and its method prepared by a kind of utilization discarded object |
| CN107051383B (en) * | 2017-04-27 | 2020-06-05 | 台州中知英健机械自动化有限公司 | Preparation method of carbon material for sewage treatment |
| CN107021470A (en) * | 2017-04-27 | 2017-08-08 | 农玉金 | A kind of preparation method of composite biomass carbon material |
| CN107051383A (en) * | 2017-04-27 | 2017-08-18 | 农玉金 | A kind of preparation method of carbon material for sewage disposal |
| CN107381572A (en) * | 2017-08-30 | 2017-11-24 | 章德恩 | A kind of capacitor bio-coal matrix activated carbon material and preparation method thereof |
| CN108010749A (en) * | 2017-11-30 | 2018-05-08 | 浙江海洋大学 | A kind of preparation method based on kelp biomass charcoal super capacitor electrode material |
| CN107996766A (en) * | 2018-01-12 | 2018-05-08 | 广西天昌投资有限公司 | A kind of Camellia nitidissima nano particle and preparation method thereof |
| CN110693290A (en) * | 2019-11-01 | 2020-01-17 | 广西壮族自治区林业科学研究院 | Mildew-proof Buddha incense and processing technology thereof |
| CN110697713A (en) * | 2019-11-01 | 2020-01-17 | 广西壮族自治区林业科学研究院 | Preparation method of cinnamon twig activated carbon |
| CN110693290B (en) * | 2019-11-01 | 2021-06-04 | 广西壮族自治区林业科学研究院 | Mildew-proof Buddha incense and processing technology thereof |
| CN110697713B (en) * | 2019-11-01 | 2021-07-16 | 广西壮族自治区林业科学研究院 | Preparation method of cinnamon twig activated carbon |
| CN111908443A (en) * | 2020-06-24 | 2020-11-10 | 西安理工大学 | Preparation method of self-doped porous carbon |
| CN112575575A (en) * | 2020-07-21 | 2021-03-30 | 苏州远浩新纺织科技有限公司 | Hole expanding method for activated carbon fiber |
| CN115193434A (en) * | 2022-08-26 | 2022-10-18 | 山东省科学院能源研究所 | Method and system for cooperatively removing carbon-based catalyst, VOCs and nitrogen oxides |
| CN115193434B (en) * | 2022-08-26 | 2023-09-29 | 山东省科学院能源研究所 | Method and system for cooperatively removing carbon-based catalyst, VOCs and nitrogen oxides |
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Application publication date: 20160817 |