CN102580679A - Method for preparing modified microwave activated carbon sorbent - Google Patents
Method for preparing modified microwave activated carbon sorbent Download PDFInfo
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- CN102580679A CN102580679A CN2012100649959A CN201210064995A CN102580679A CN 102580679 A CN102580679 A CN 102580679A CN 2012100649959 A CN2012100649959 A CN 2012100649959A CN 201210064995 A CN201210064995 A CN 201210064995A CN 102580679 A CN102580679 A CN 102580679A
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- modification
- microwave activity
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- active carbon
- alkali metal
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title abstract description 25
- 239000002594 sorbent Substances 0.000 title abstract description 5
- 230000000694 effects Effects 0.000 claims abstract description 35
- 238000012986 modification Methods 0.000 claims abstract description 26
- 230000004048 modification Effects 0.000 claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 claims description 46
- 239000003463 adsorbent Substances 0.000 claims description 33
- 238000002360 preparation method Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 239000003610 charcoal Substances 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 229910052783 alkali metal Inorganic materials 0.000 claims description 8
- 150000001340 alkali metals Chemical class 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000007598 dipping method Methods 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 229940072033 potash Drugs 0.000 claims description 2
- 235000015320 potassium carbonate Nutrition 0.000 claims description 2
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 14
- 238000005470 impregnation Methods 0.000 abstract description 2
- 229910021645 metal ion Inorganic materials 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 23
- 238000000926 separation method Methods 0.000 description 20
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- 230000008901 benefit Effects 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 239000001569 carbon dioxide Substances 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 3
- 235000013162 Cocos nucifera Nutrition 0.000 description 2
- 244000060011 Cocos nucifera Species 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 239000003345 natural gas Substances 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241000208125 Nicotiana Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- JYIBXUUINYLWLR-UHFFFAOYSA-N aluminum;calcium;potassium;silicon;sodium;trihydrate Chemical compound O.O.O.[Na].[Al].[Si].[K].[Ca] JYIBXUUINYLWLR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910001603 clinoptilolite Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002803 maceration Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000002120 nanofilm Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Abstract
The invention discloses a method for preparing a modified microwave activated carbon sorbent. The method is characterized in that microwave activated carbon is taken as the carrier, loading alkaline metal ions K are taken as active components for modification, and the modified microwave activated carbon sorbent is prepared through adoption of ultrasonic wave equivalent impregnation. The method provided by the invention is simple, easy to operate and low in cost; and the sorbent prepared through the method has a good sorption effect, and more adsorption equilibrium selection factors of CO2/CO4 can be obtained.
Description
Technical field
The present invention relates to a kind of preparation method of modification microwave activity carbon adsorbent, specifically is a kind of adsorbing separation CO
2And CH
4The preparation method of modified activated carbon absorbent, belong to gas separation technique field.
Background technology
At present, energy crisis and environmental problem are on the rise, and many countries develop biogas in succession as the energy.Biogas is a kind of clean energy resource, and its main component is CH
4And CO
2, CH in the biogas generally
4Content be about 60%～70%, CO
2Content is about 30%～40%, also has a spot of O in addition
2, N
2Wait other gas.Reclaim and utilize the CH the biogas from refuse landfill
4Gas, technically with economic benefit on all be feasible, and be to reduce discharging CH
4An effective way of gas.The concentrated refuse landfill in a city has a large amount of CH
4Gas if it is used, has just reduced discharging a considerable amount of greenhouse gases, and new energy sources approach is provided; And while CO
2Existence greatly reduce the energy value of unit volume gas, the biogas scope of application of this moment and limited, and efficient is lower.In addition, CO
2Existence also can corrode transport pipeline, work the mischief.Therefore how to CH
4And CO
2Effectively separate, and be used respectively, have an important strategic meaning current.In China, a large amount of biogas that medium and small methane-generating pit produced in rural area mainly is to be used to cook and throw light on, and has not given play to bigger economic benefit; And in Europe and North America, the biogas of production is incorporated gas distributing system into through after purifying, is used for the biogas fuel cell power generation, cogeneration of heat and power or as motor vehicle fuel, can produce bigger economic benefit.
Effective separation of C H
4And CO
2Method absorption process, membrane separation process, low temperature distillation method and pressure swing adsorption method etc. are arranged.Absorption process often adopts alkaline solution to do the absorbent divided gas flow, technological complicated operation, and energy consumption is big, and is easy to generate contaminated wastewater.Chinese patent CN101693169A has reported a kind of separation of C O
2, CH
4The preparation method of the composite membrane of mist is through will be to CO
2Have in the precursor liquid of the molecular sieve doped entering charcoal of SAPO-34 molecular film of strong adsorption property, thereby promoted composite membrane CO
2Selectively penetrating, improved CO
2/ CH
4Selectivity.But adopt membrane separation process need dewater usually and filter process, increased the complexity of operating procedure.
Absorption method has the product purity height, energy consumption is low, technological process is simple, the automaticity advantages of higher, also more and more comes into one's own in the purification of natural gas and the applications in separation of biogas, and many scholars both domestic and external study adsorbing separation CO energetically
2/ CH
4Technology.The key of adsorption method of separation is exactly the selection of adsorbent.At separation of C O
2/ CH
4Absorbing process in commonly used natural zeolite, molecular sieve, silica gel, active carbon etc. are arranged.Chinese patent CN126871A has reported that rich sodium clinoptilolite with natural formation as adsorbent, adopts pressure swing adsorption method bulk separation of carbon dioxide from methane.Under low operating pressure, can deviate from a large amount of most of carbon dioxide.This absorption adsorbing separation effect is better, but uses the natural zeolite cost higher.Active carbon has flourishing microcellular structure, and adsorption capacity is big, and is cheap, in the gas absorption separation field, has obtained using widely.Chinese patent CN 101255945A discloses a kind of technology of utilizing the activated carbon microballon adsorbent to remove carbon dioxide in natural, can the carbon dioxide content in the natural gas be reduced to 0.05 volume % by about 10.0 volume %.Activated carbon microballon adsorbents adsorb desorption in this invention is simple, can circulate and recycle, but adsorptive selectivity is not high under normal pressure.Along with development of science and technology, advantage such as the active carbon that utilizes microwave heating to handle to make is heated evenly because of it, and is with low cost, produces convenience, and absorption property is good and become the focus of research.At present; Active carbon through microwave treatment is widely used in water treatment and field of purification, in some gas purification fields, also is applied, and Chinese patent CN101693162A has announced and a kind ofly utilized active carbon under the microwave radiation to the boiler smoke method of desulphurization denitration simultaneously; Invention has utilized the selectivity heating properties of microwave; In conjunction with the reducing power of charcoal to SO2 and NOX, improved the efficient of desulfurization simultaneously, denitration greatly, can reach the denitration rate more than the desulfurization degree and 90% 95% or more.The microwave activity charcoal is at adsorbing separation CO
2/ CH
4The gas Application for Field is not appeared in the newspapers as yet.
Summary of the invention
The present invention has aimed to provide a kind of preparation method of modification microwave activity carbon adsorbent, and the adsorbent for preparing through the present invention is to separate CO absorption
2And CH
4The modification microwave activity carbon adsorbent of gas.
Among the present invention with the microwave activity charcoal as carrier, carrying alkali metal ion K ion carries out modification as active component, adopts the ultrasonic wave equivalent impregnation, makes adsorbent.The concrete preparation method of modified adsorbent comprises the steps:
(1) the microwave activity charcoal is ground, is sized to 40～60 orders, with distilled water washing 3～4 times, 100～120 ℃ of down dry 12～24h reduce to room temperature naturally in drying basin;
(2) press the alkali metal soln that the 1g active carbon adds 2～4ml, place alkali metal soln to carry out ultrasonic wave dipping 0.5～4h active carbon processed, then at 100～120 ℃ of down dry 12～24h;
(3) the microwave activity charcoal that (2) step is made is placed on 200～650 ℃ of following roasting 2～5h, in drying basin, reduces to room temperature naturally, promptly gets modification microwave activity carbon adsorbent.
Alkali metal soln described in the present invention is a kind of in potassium hydroxide, potassium nitrate, potash, the Klorvess Liquid.
The concentration of alkali metal soln described in the present invention is 0.5～2mol/L.
Ultrasonic wave described in the present invention is immersed in 30～40 ℃, carries out under ultrasonic frequency 28～45KHz condition.
Used microwave activity charcoal is to adopt conventional method among the present invention, and the active carbon that obtains through microwave treatment is as making with reference to disclosed method in the one Chinese patent application 200810233530.5.
The present invention has advantage and effect:
The inventive method is simple, and cost is lower, and sorbent used carrier simple to operate and maceration extract are cheap, obtains easily, and adsorbent is through surface adsorption CO after the modification
2And CH
4Gas is to CO
2Adsorption capacity improve CH
4Adsorption capacity reduce, thereby obtain higher CO
2/ CH
4Adsorption equilibrium select the factor, the adsorbent of preparation method's preparation of the present invention is CH in the adsorbing separation biogas
4And CO
2Gas provides a kind of economically viable approach, and separating effect is better.
The specific embodiment
Below in conjunction with embodiment the present invention is done further explain, but protection domain of the present invention is not limited to said content.
Embodiment 1:A kind of preparation method of modification microwave activity carbon adsorbent, concrete operations are following:
(1) the microwave cocoanut active charcoal is ground, is sized to 40 orders, get the 17g active carbon, behind 100 ℃ of following dry 24h, in drying basin, reduce to room temperature naturally with distilled water washing 3 times;
(2) active carbon processed is placed 0.5mol/L solution of potassium carbonate 34ml, at 30 ℃, ultrasonic frequency is under the 28KHz condition, dipping 4h, 100 ℃ of following dry 24h in thermostatic drying chamber then;
(3) place Muffle furnace at 350 ℃ of following roasting 4h active carbon at last, in drying basin, reduce to room temperature naturally, promptly get modification microwave activity carbon adsorbent.
(4) get modification microwave activity carbon adsorbent 2.0g, at 25 ℃ of following adsorbing separation CO
2And CH
4Gas, CO
2And CH
4The concentration of volume percent of gas is respectively 99.99% and 99.9%; Utilize Static Volumetric Method to record CH
4And CO
2The adsorpting data of gas, test result is as shown in table 1.
Embodiment 2:A kind of preparation method of modification microwave activity carbon adsorbent, concrete operations are following:
(1) the microwave coal mass active carbon is ground, is sized to 50 orders, get the 17g active carbon, behind 110 ℃ of following dry 18h, in drying basin, reduce to room temperature naturally with distilled water washing 4 times;
(2) active carbon processed is placed 1mol/L Klorvess Liquid 51ml, at 40 ℃, ultrasonic frequency is under the 35KHz condition, dipping 2h, 110 ℃ of following dry 18h in thermostatic drying chamber then;
(3) place Muffle furnace at 200 ℃ of following roasting 5h active carbon at last, in drying basin, reduce to room temperature naturally, promptly get modification microwave activity carbon adsorbent.
(4) get modification microwave activity carbon adsorbent 2.0g, at 25 ℃ of following adsorbing separation CO
2And CH
4Gas, CO
2And CH
4The concentration of volume percent of gas is respectively 99.99% and 99.9%; Utilize Static Volumetric Method to record CH
4And CO
2The adsorpting data of gas, test result is as shown in table 1.
Embodiment 3:A kind of preparation method of modification microwave activity carbon adsorbent, concrete operations are following:
(1) the microwave cocoanut active charcoal is ground, is sized to 60 orders, get the 17g active carbon, behind 120 ℃ of following dry 12h, in drying basin, reduce to room temperature naturally with distilled water washing 3 times;
(2) active carbon processed is placed 2mol/L potassium hydroxide solution 68ml, at 35 ℃, ultrasonic frequency is under the 45KHz condition, dipping 0.5h, 120 ℃ of following dry 12h in thermostatic drying chamber then;
(3) place Muffle furnace at 650 ℃ of following roasting 2h active carbon at last, in drying basin, reduce to room temperature naturally, promptly get modification microwave activity carbon adsorbent.
(4) get modification microwave activity carbon adsorbent 2.0g, at 25 ℃ of following adsorbing separation CO
2And CH
4Gas, CO
2And CH
4The concentration of volume percent of gas is respectively 99.99% and 99.9%; Utilize Static Volumetric Method to record CH
4And CO
2The adsorpting data of gas, test result is as shown in table 1.
Embodiment 4:A kind of preparation method of modification microwave activity carbon adsorbent, concrete operations are following:
(1) microwave tobacco rod matrix activated carbon is ground, is sized to 45 orders, get the 17g active carbon, behind 115 ℃ of following dry 20h, in drying basin, reduce to room temperature naturally with distilled water washing 3 times;
(2) active carbon processed is placed 1.5mol/L potassium nitrate solution 51ml, at 35 ℃, ultrasonic frequency is under the 40KHz condition, dipping 1h, 120 ℃ of following dry 16h in thermostatic drying chamber then;
(3) place Muffle furnace at 450 ℃ of following roasting 3h active carbon at last, in drying basin, reduce to room temperature naturally, promptly get modification microwave activity carbon adsorbent.
(4) get modification microwave activity carbon adsorbent 2.0g, at 25 ℃ of following adsorbing separation CO
2And CH
4Gas, CO
2And CH
4The concentration of volume percent of gas is respectively 99.99% and 99.9%; Utilize Static Volumetric Method to record CH
4And CO
2The adsorpting data of gas, test result is as shown in table 1.
Table 1: modified adsorbent adsorbing separation CH
4And CO
2The experimental result of gas
Can find out from table 1, compare that the adsorbent after the process modification is to CO with blank microwave activity charcoal
2Adsorption capacity increase, and to CH
4Adsorption capacity reduce, adsorption equilibrium selects the factor greater than blank microwave activity charcoal.
The microwave activity charcoal that adopts in the foregoing description all prepares with reference to disclosed method in the one Chinese patent application 200810233530.5.
Claims (4)
1. the preparation method of a modification microwave activity carbon adsorbent is characterized in that carrying out as follows:
(1) the microwave activity charcoal is ground, is sized to 40～60 orders,, behind 100～120 ℃ of down dry 12～24h, reduce to room temperature naturally with distilled water washing 3～4 times;
(2) press the alkali metal soln that the 1g active carbon adds 2～4ml, place alkali metal soln to carry out ultrasonic wave dipping 0.5～4h active carbon processed, then at 100～120 ℃ of down dry 12～24h;
(3) at last with active carbon at 200～650 ℃ of following roasting 2～5h, in drying basin, reduce to room temperature naturally, promptly get modification microwave activity carbon adsorbent.
2. the preparation method of modification microwave activity carbon adsorbent according to claim 1 is characterized in that: alkali metal soln is a kind of in potassium hydroxide, potassium nitrate, potash, the Klorvess Liquid.
3. the preparation method of modification microwave activity carbon adsorbent according to claim 2 is characterized in that: alkali metal soln concentration is 0.5～2mol/L.
4. the preparation method of modification microwave activity carbon adsorbent according to claim 1 is characterized in that: ultrasonic wave is immersed in 30～40 ℃, carries out under ultrasonic frequency 28～45KHz condition.
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|---|---|---|---|
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|---|---|---|---|
| CN201210064995.9A CN102580679B (en) | 2012-01-13 | 2012-01-13 | A kind of preparation method of modified microwave activated carbon sorbent |
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| CN102580679A true CN102580679A (en) | 2012-07-18 |
| CN102580679B CN102580679B (en) | 2016-01-20 |
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| CN103232036A (en) * | 2013-05-09 | 2013-08-07 | 贺守印 | Preparation method of desulfurization and denitrification active carbon |
| CN103754977A (en) * | 2014-01-17 | 2014-04-30 | 哈尔滨工业大学 | Active carbon modification method for emergently treating sudden organic pollution of drinking water |
| CN104907045A (en) * | 2014-03-10 | 2015-09-16 | 江苏瑞丰科技实业有限公司 | Efficient carbon dioxide catching material |
| CN105251444A (en) * | 2015-10-30 | 2016-01-20 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for modifying activated carbon-based propane adsorbent with trace potassium hydroxide |
| CN105597709A (en) * | 2016-03-08 | 2016-05-25 | 湖南凯美特气体股份有限公司 | Preparing and modifying method for carbon material for adsorbing CO2 |
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