CN103204502A - Mesoporous coal-based activated carbon and preparation method thereof - Google Patents
Mesoporous coal-based activated carbon and preparation method thereof Download PDFInfo
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- CN103204502A CN103204502A CN2013101474655A CN201310147465A CN103204502A CN 103204502 A CN103204502 A CN 103204502A CN 2013101474655 A CN2013101474655 A CN 2013101474655A CN 201310147465 A CN201310147465 A CN 201310147465A CN 103204502 A CN103204502 A CN 103204502A
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Abstract
The invention relates to the technical field of activated carbon, and discloses mesoporous coal-based activated carbon and a preparation method thereof. The mesoporous coal-based activated carbon is prepared according to the following steps of: 1, crushing coal into 20-100 meshes of granular coal, weighing and evenly mixing the crushed granular coal and a catalyst according to the mass ratio of (100 to 3) to (100 to 7) to form a reaction material; and 2, putting the reaction material into a pyrolysis tube; leading in nitrogen to the pyrolysis tube, and heating the pyrolysis tube, so that the temperature of the material in the pyrolysis tube achieves 400-600 DEG C. A single coal variety is taken as a material; the mesoporous coal-based activated carbon is directly prepared in one step by a vapor activation method under a catalytic effect of the single catalyst; excessive demands on the quality of the coal and the coordination uncertainty between compound catalysts are avoided; and the preparation method has the characteristics that the process is simple, demands on equipment are low, material source is abundant, specific surface area of the obtained mesoporous coal-based activated carbon is large, mesopore volume is large and adsorption capacity is strong; the production cost is reduced; and the production efficiency is improved.
Description
Technical field
The present invention relates to the activated carbon technology field, is a kind of mesopore active carbon from coal and preparation method thereof.
Background technology
Gac is a kind of carbon material adsorbing material that enriches pore texture and huge specific surface area that has; it has, and adsorptivity is strong, good chemical stability; be widely used in fields such as industry, agricultural, national defence, traffic, medical and health, environment protection; in recent years along with the raising day by day of environmental protection requirement; the demand of gac is increasing both at home and abroad, and the development of gac is also more and more rapider.Especially the development of coal mass active carbon, its reason is because the reserves of coal resources are very abundant, cost is lower on the one hand, be because active carbon from coal technology ripe and progressive on the other hand, make that with the coal to be that raw material prepares the research of gac also more and more outstanding.
Some investigators mainly fix on the Preparation of Activated Carbon aspect of pursuing high-specific surface area, high absorption property to sight at present.Wherein, people such as Xing Baolin are raw material with the Taixi anthracite, and KOH is activator, and adopting chemical activation method to make specific surface area is 3215m
2/ g, iodine sorption value reach the high-specific surface area active carbon from coal that 2884mg/g, methylene blue adsorption value reach 548mg/g.Luo Daocheng etc. are raw material with brown coal, and phosphoric acid is activator, and sulfuric acid is additive, adopt charcoal activation single stage method to prepare gac, and gac intensity is 88.2%, and specific surface area is 1158.6m
2/ g, iodine sorption value are that 946.5mg/g, methylene blue adsorption value are 203.4mg/g.Chen Zhanjun mixes the hard coal of high metamorphic grade with low rotten bituminous coal, be binding agent with coal tar, moulding then, and selecting water vapor for use is activator, makes cylindrical particle gac and unsetting charcoal, its specific surface area is 1000m
2About/g, benzene adsorptive value 30% to 35% is about iodine sorption value 1000mg/g.
From forefathers' work, we can see that the development of gac of preparation high-specific surface area mainly concentrates on following several respects: be that to select the hard coal of high-quality for use be raw material on the one hand, adopt chemical activation methods such as KOH, make the gac of high-specific surface area again through charing, activation; Be to adopt technology such as high-quality and low grade coal kneading and compacting on the other hand, make the gac of definite shape.The gac that uses chemical method to make has strict requirement to equipment, has also increased certain cost of investment, is difficult to realize industrialization.Utilize the coal blending legal system to be equipped with gac, extremely strict to the requirement of ature of coal, spent cost is higher, and fabricating technology is complicated.
As everyone knows, gac has very flourishing microvoid structure, the effect fabulous to being adsorbed with of small-molecule substance.But when adsorbate was organism macromole such as polymkeric substance, dyestuff or VITAMIN, micropore had then lost adsorption function, had only big, mesopore could adsorb these macromolecular substance.So, the research in the mesopore aperture of gac is absolutely necessary.People such as Hao Lina have that to adopt manganous nitrate and cupric nitrate be additive, catalytic preparation the mesopore activated carbon of containing metal oxide compound.People's ether such as red legend chief west coal and Datong District's coal are raw material, on the basis of coal blending, add magnesium salts and nitrate composite catalyst, find that additive is conducive to promote the growth in the mesopore aperture of 3nm to 4nm in the gac.Work by forefathers is found, when the preparation gac, utilizes the coal blending technology or adds catalyzer, and be highly effective to development gac mesopore.But, the screening of the strict demand of coal blending ature of coal, coal blending ratio and complicated processing condition thereof, making the coal blending legal system be equipped with mesopore activated carbon has had certain limitation, has also increased the complicacy of experiment and certain production cost simultaneously.And the conformability between composite catalyst, intend the research of proportioning, cause experiment to have many uncertainties, in the composite catalyst that also is difficult to get across which kind of element or which kind of compound promoted the development in aperture.
Summary of the invention
The invention provides a kind of mesopore active carbon from coal and preparation method thereof, overcome the deficiency of above-mentioned prior art, it can effectively solve among the existing mesopore activated carbon preparation method the medium requirement is very high, processing condition are complicated, poor repeatability and the high problem of production cost.
One of technical scheme of the present invention realizes by following measure: a kind of mesopore active carbon from coal, obtain by following step: the first step, coal is crushed to 20 order to 100 purpose particulate coal, and the particulate coal after the fragmentation and catalyzer are that 100:3 to 100:7 takes by weighing and be mixed into reaction raw materials by mass ratio; Second step was placed on reaction raw materials in the thermal decomposition tube, continue to feed nitrogen and heat thermal decomposition tube in thermal decomposition tube, made that material temperature reaches 400 ℃ to 600 ℃ in the thermal decomposition tube, was 400 ℃ to 600 ℃ following constant temperature 1 h to 4h in temperature; The 3rd step, continue the heating thermal decomposition tube, make that material temperature reaches 800 ℃ to 1000 ℃ in the thermal decomposition tube, stop then in thermal decomposition tube, feeding nitrogen, be that the atmidometer of 0.7 kilogram/h to 1.2 kilogram/h continues to feed water vapor in thermal decomposition tube by feeding flow velocity in every kilogram of reaction raw materials, after temperature is 800 ℃ to 1000 ℃ following constant temperature 1 h to 5h, obtain the mesopore active carbon from coal.
Two of technical scheme of the present invention realizes by following measure: a kind of preparation method of mesopore active carbon from coal, undertaken by following step: the first step, coal is crushed to 20 order to 100 purpose particulate coal, and the particulate coal after the fragmentation and catalyzer are that 100:3 to 100:7 takes by weighing and be mixed into reaction raw materials by mass ratio; Second step was placed on reaction raw materials in the thermal decomposition tube, continue to feed nitrogen and heat thermal decomposition tube in thermal decomposition tube, made that material temperature reaches 400 ℃ to 600 ℃ in the thermal decomposition tube, was 400 ℃ to 600 ℃ following constant temperature 1 h to 4h in temperature; The 3rd step, continue the heating thermal decomposition tube, make that material temperature reaches 800 ℃ to 1000 ℃ in the thermal decomposition tube, stop then in thermal decomposition tube, feeding nitrogen, be that the atmidometer of 0.7 kilogram/h to 1.2 kilogram/h continues to feed water vapor in thermal decomposition tube by feeding flow velocity in every kilogram of reaction raw materials, after temperature is 800 ℃ to 1000 ℃ following constant temperature 1 h to 5h, obtain the mesopore active carbon from coal.
Be the further optimization and/or improvements to the foregoing invention technical scheme below:
Above-mentioned catalyzer is urea or ammonium nitrate or Ni (NO
3)
26H
2O or Fe (NO
3)
39H
2O.
In above-mentioned the 3rd step, after temperature is 800 ℃ to 1000 ℃ following constant temperature 1 h to 5h, stop in thermal decomposition tube, feeding water vapor, in thermal decomposition tube, continue to obtain the mesopore active carbon from coal after feeding nitrogen is cooled to room temperature simultaneously.
Above-mentioned second step or/and in the 3rd step the heating rate of thermal decomposition tube be 5 ℃/min to 20 ℃/min.
The flow velocity of above-mentioned nitrogen is 100mL/min to 400mL/min; Or/and the temperature of water vapor is 250 ℃ to 400 ℃.
The present invention is raw material by single coal, under the katalysis of single catalyst, adopt a direct step of steam activation method to make the mesopore active carbon from coal, avoided the harshness requirement of ature of coal and the cooperation uncertainty between composite catalyst, have technology simple, to equipment require low, raw material sources abundant, the big or middle pore volume of mesopore active carbon from coal specific surface area of gained is big and the characteristics of high adsorption capacity, reduce production cost, improved production efficiency.
Description of drawings
Accompanying drawing 1 is mesopore active carbon from coal of the present invention and the attached isothermal curve comparison diagram of suction (taking off) that does not add the blank sample that catalyzer makes in raw material of the present invention.
Accompanying drawing 2 is mesopore active carbon from coal of the present invention and the BJH aperture contrast distribution figure that does not add the blank sample that catalyzer makes in raw material of the present invention.
Embodiment
Embodiment 1, and this mesopore active carbon from coal obtains by following step: the first step, coal is crushed to 20 order to 100 purpose particulate coal, and the particulate coal after the fragmentation and catalyzer are that 100:3 to 100:7 takes by weighing and be mixed into reaction raw materials by mass ratio; Second step was placed on reaction raw materials in the thermal decomposition tube, continue to feed nitrogen and heat thermal decomposition tube in thermal decomposition tube, made that material temperature reaches 400 ℃ to 600 ℃ in the thermal decomposition tube, was 400 ℃ to 600 ℃ following constant temperature 1 h to 4h in temperature; The 3rd step, continue the heating thermal decomposition tube, make that material temperature reaches 800 ℃ to 1000 ℃ in the thermal decomposition tube, stop then in thermal decomposition tube, feeding nitrogen, be that the atmidometer of 0.7 kilogram/h to 1.2 kilogram/h continues to feed water vapor in thermal decomposition tube by feeding flow velocity in every kilogram of reaction raw materials, after temperature is 800 ℃ to 1000 ℃ following constant temperature 1 h to 5h, obtain the mesopore active carbon from coal.
Embodiment 2, and this mesopore active carbon from coal obtains by following step: the first step, coal is crushed to 20 orders or 100 purpose particulate coal, and the particulate coal after the fragmentation and catalyzer are that 100:3 or 100:7 take by weighing and be mixed into reaction raw materials by mass ratio; Second step was placed on reaction raw materials in the thermal decomposition tube, continue to feed nitrogen and heat thermal decomposition tube in thermal decomposition tube, made that material temperature reaches 400 ℃ or 600 ℃ in the thermal decomposition tube, was 400 ℃ or 600 ℃ of following constant temperature 1 h or 4h in temperature; The 3rd step, continue the heating thermal decomposition tube, make that material temperature reaches 800 ℃ or 1000 ℃ in the thermal decomposition tube, stop then in thermal decomposition tube, feeding nitrogen, be that the atmidometer of 0.7 kilogram/h or 1.2 kilograms/h continues to feed water vapor in thermal decomposition tube by feeding flow velocity in every kilogram of reaction raw materials, after temperature is 800 ℃ or 1000 ℃ of following constant temperature 1 h or 5h, obtain the mesopore active carbon from coal.
Embodiment 3, and as the optimization of above-described embodiment, the catalyzer of embodiment 3 is urea or ammonium nitrate or Ni (NO
3)
26H
2O or Fe (NO
3)
39H
2O.
Embodiment 4, be with the difference of above-described embodiment, in the 3rd step of embodiment 4, after temperature is 800 ℃ to 1000 ℃ following constant temperature 1 h to 5h, stop in thermal decomposition tube, feeding water vapor, in thermal decomposition tube, continue to obtain the mesopore active carbon from coal after feeding nitrogen is cooled to room temperature simultaneously.
Embodiment 5, as the optimization of above-described embodiment, second step of embodiment 5 or/and in the 3rd step the heating rate of thermal decomposition tube be 5 ℃/min to 20 ℃/min.
Embodiment 6, and as the optimization of above-described embodiment, the flow velocity of nitrogen is 100mL/min to 400mL/min among the embodiment 6; Embodiment 7, and as the optimization of above-described embodiment, the temperature of water vapor is 250 ℃ to 400 ℃ among the embodiment 7.
The average data contrast that is the mesopore activated carbon that obtains of mesopore active carbon from coal that above-described embodiment is obtained and prior art below is as follows:
The average data contrast of the hard coal mesopore activated carbon that the mesopore active carbon from coal that the present invention obtains and prior art obtain is as shown in table 1.
Table 1
| ? | Specific surface area m 2/g | Total pore volume ml/g |
| The hard coal mesopore activated carbon | 251.0 | 0.26 |
| Mesopore active carbon from coal of the present invention | 574.3 | 0.655 |
As can be seen from Table 1, the average specific surface area of the hard coal mesopore activated carbon that obtains of prior art and average total pore volume are respectively 251.0m
2/ g and 0.26ml/g, the average specific surface area of mesopore active carbon from coal of the present invention and average total pore volume are respectively 574.3m
2/ g and 0.655 ml/g; Mesopore active carbon from coal of the present invention is compared with the hard coal mesopore activated carbon that prior art obtains, and specific surface area has improved 323.3m
2/ g, total pore volume has improved 0.395ml/g, illustrate the specific surface area of the hard coal mesopore activated carbon that the specific surface area of mesopore active carbon from coal of the present invention and total pore volume obtain than prior art and always pore volume be greatly improved.
The average data contrast of the mesopore activated carbon that the mesopore activated carbon that the mesopore active carbon from coal that the present invention obtains and prior art coal blending method make and prior art lower performance commodity charcoal make is as shown in table 2.
Table 2
| ? | Middle pore volume ml/g | Middle porosity % |
| The mesopore activated carbon that the coal blending method makes | <0.40 | <52 |
| The mesopore activated carbon that lower performance commodity charcoal makes | <0.25 | <45 |
| Mesopore active carbon from coal of the present invention | >0.50 | >80 |
The mesopore activated carbon that prior art coal blending method makes in the table 2 is for adding the mesopore activated carbon that composite catalyst makes; The mesopore activated carbon that prior art lower performance commodity charcoal makes is lower performance merchandise active carbon mesopore activated carbon of making of catalysis again under the effect of composite catalyst.
As can be seen from Table 2, the average mesopore of the mesopore activated carbon that makes of prior art coal blending method is held and the average mesopore rate is respectively＜0.40ml/g and＜52%; The average mesopore of the mesopore activated carbon that prior art lower performance commodity charcoal makes is held and the average mesopore rate is respectively＜0.25ml/g and＜45%; The average mesopore of mesopore active carbon from coal of the present invention is held and the average mesopore rate is respectively〉0.50ml/g with 80%; Middle pore volume and the middle porosity of the mesopore activated carbon that the mesopore activated carbon that the middle pore volume of mesopore active carbon from coal of the present invention and middle porosity make than prior art coal blending method and prior art lower performance commodity charcoal make are greatly improved, illustrate that mesopore active carbon from coal of the present invention contains extremely abundant mesopore hole, has great application prospect.
Fig. 1 is mesopore active carbon from coal of the present invention and the attached isothermal curve comparison diagram of suction (taking off) that does not add the blank sample that catalyzer makes in raw material of the present invention.Curve a is illustrated in the attached isothermal curve comparison diagram of suction (taking off) that does not add the blank sample that catalyzer makes in the raw material of the present invention, curve b represents that catalyzer is the attached isothermal curve figure of suction (taking off) of urea in the mesopore active carbon from coal of the present invention, and curve c represents that catalyzer is the attached isothermal curve figure of suction (taking off) of ammonium nitrate in the mesopore active carbon from coal of the present invention; Mesopore active carbon from coal of the present invention has tangible hysteresis loop as can be seen from Figure 1, illustrate that mesopore active carbon from coal of the present invention has abundant central hole structure, by more also finding, curve b and curve c are higher than curve a far away among the present invention, and this has illustrated that single catalyst is conducive to improve the specific surface area of gac.
Fig. 2 is mesopore active carbon from coal of the present invention and the BJH aperture contrast distribution figure that does not add the blank sample that catalyzer makes in raw material of the present invention, and the gac aperture mainly concentrates on 3 nm to 4nm as can be seen from Figure 2.From Fig. 2 it can also be seen that add catalyzer ammonium nitrate after, the aperture of gac concentrates the peak obviously to raise; After adding catalyzer urea, its aperture concentrates the peak all to be higher than the above two, illustrates and adds the development that catalyzer urea extremely is conducive to gac mesopore aperture.
Above technical characterictic has constituted embodiments of the invention, and it has stronger adaptability and implementation result, can increase and decrease non-essential technical characterictic according to actual needs, satisfies the demand of different situations.
Claims (10)
1. mesopore active carbon from coal is characterized in that obtaining by following step: the first step, coal is crushed to 20 order to 100 purpose particulate coal, and the particulate coal after the fragmentation and catalyzer are that 100:3 to 100:7 takes by weighing and be mixed into reaction raw materials by mass ratio; Second step was placed on reaction raw materials in the thermal decomposition tube, continue to feed nitrogen and heat thermal decomposition tube in thermal decomposition tube, made that material temperature reaches 400 ℃ to 600 ℃ in the thermal decomposition tube, was 400 ℃ to 600 ℃ following constant temperature 1 h to 4h in temperature; The 3rd step, continue the heating thermal decomposition tube, make that material temperature reaches 800 ℃ to 1000 ℃ in the thermal decomposition tube, stop then in thermal decomposition tube, feeding nitrogen, be that the atmidometer of 0.7 kilogram/h to 1.2 kilogram/h continues to feed water vapor in thermal decomposition tube by feeding flow velocity in every kilogram of reaction raw materials, after temperature is 800 ℃ to 1000 ℃ following constant temperature 1 h to 5h, obtain the mesopore active carbon from coal.
2. mesopore active carbon from coal according to claim 1 is characterized in that catalyzer is urea or ammonium nitrate or Ni (NO
3)
26H
2O or Fe (NO
3)
39H
2O.
3. mesopore active carbon from coal according to claim 1 and 2, it is characterized in that in the 3rd step, after temperature is 800 ℃ to 1000 ℃ following constant temperature 1 h to 5h, stop in thermal decomposition tube, feeding water vapor, in thermal decomposition tube, continue to obtain the mesopore active carbon from coal after feeding nitrogen is cooled to room temperature simultaneously.
4. according to claim 1 or 2 or 3 described mesopore active carbon from coal, it is characterized in that for second step or/and in the 3rd step the heating rate of thermal decomposition tube be 5 ℃/min to 20 ℃/min.
5. according to claim 1 or 2 or 3 or 4 described mesopore active carbon from coal, the flow velocity that it is characterized in that nitrogen is 100mL/min to 400mL/min; Or/and the temperature of water vapor is 250 ℃ to 400 ℃.
6. the preparation method of a mesopore active carbon from coal, it is characterized in that being undertaken by following step: the first step, coal is crushed to 20 order to 100 purpose particulate coal, and the particulate coal after the fragmentation and catalyzer are that 100:3 to 100:7 takes by weighing and be mixed into reaction raw materials by mass ratio; Second step was placed on reaction raw materials in the thermal decomposition tube, continue to feed nitrogen and heat thermal decomposition tube in thermal decomposition tube, made that material temperature reaches 400 ℃ to 600 ℃ in the thermal decomposition tube, was 400 ℃ to 600 ℃ following constant temperature 1 h to 4h in temperature; The 3rd step, continue the heating thermal decomposition tube, make that material temperature reaches 800 ℃ to 1000 ℃ in the thermal decomposition tube, stop then in thermal decomposition tube, feeding nitrogen, be that the atmidometer of 0.7 kilogram/h to 1.2 kilogram/h continues to feed water vapor in thermal decomposition tube by feeding flow velocity in every kilogram of reaction raw materials, after temperature is 800 ℃ to 1000 ℃ following constant temperature 1 h to 5h, obtain the mesopore active carbon from coal.
7. the preparation method of mesopore active carbon from coal according to claim 6 is characterized in that catalyzer is urea or ammonium nitrate or Ni (NO
3)
26H
2O or Fe (NO
3)
39H
2O.
8. according to the preparation method of claim 6 or 7 described mesopore active carbon from coal, it is characterized in that in the 3rd step, after temperature is 800 ℃ to 1000 ℃ following constant temperature 1 h to 5h, stop in thermal decomposition tube, feeding water vapor, in thermal decomposition tube, continue to obtain the mesopore active carbon from coal after feeding nitrogen is cooled to room temperature simultaneously.
9. according to the preparation method of claim 6 or 7 or 8 described mesopore active carbon from coal, it is characterized in that for second step or/and in the 3rd step the heating rate of thermal decomposition tube be 5 ℃/min to 20 ℃/min.
10. according to claim 6 or 7 or the preparation method of 8 or 9 described mesopore active carbon from coal, the flow velocity that it is characterized in that nitrogen is 100mL/min to 400mL/min; Or/and the temperature of water vapor is 250 ℃ to 400 ℃.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103342360A (en) * | 2013-07-25 | 2013-10-09 | 哈尔滨工业大学 | High-performance mesoporous active carbon suitable for biological enhancement and preparation method thereof |
| CN106976877A (en) * | 2017-04-24 | 2017-07-25 | 句容市百诚活性炭有限公司 | A kind of preparation method of the flourishing activated carbon of mesopore |
| CN107021485A (en) * | 2017-04-24 | 2017-08-08 | 句容市百诚活性炭有限公司 | A kind of preparation method of the flourishing activated carbon of mesopore |
| CN107151017A (en) * | 2017-05-16 | 2017-09-12 | 浙江工业大学 | A kind of coal mass active carbon and preparation method and application |
| CN109796014A (en) * | 2019-03-21 | 2019-05-24 | 上海理工大学 | It is a kind of using ferric nitrate as the preparation method of the mesoporous activated carbon of activator |
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| CN1272454A (en) * | 1999-04-30 | 2000-11-08 | 煤炭科学研究总院北京煤化学研究所 | Production method of coal base mesopore active carbon |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103342360A (en) * | 2013-07-25 | 2013-10-09 | 哈尔滨工业大学 | High-performance mesoporous active carbon suitable for biological enhancement and preparation method thereof |
| CN106976877A (en) * | 2017-04-24 | 2017-07-25 | 句容市百诚活性炭有限公司 | A kind of preparation method of the flourishing activated carbon of mesopore |
| CN107021485A (en) * | 2017-04-24 | 2017-08-08 | 句容市百诚活性炭有限公司 | A kind of preparation method of the flourishing activated carbon of mesopore |
| CN107151017A (en) * | 2017-05-16 | 2017-09-12 | 浙江工业大学 | A kind of coal mass active carbon and preparation method and application |
| CN109796014A (en) * | 2019-03-21 | 2019-05-24 | 上海理工大学 | It is a kind of using ferric nitrate as the preparation method of the mesoporous activated carbon of activator |
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Application publication date: 20130717 |