CN102580679B - A kind of preparation method of modified microwave activated carbon sorbent - Google Patents
A kind of preparation method of modified microwave activated carbon sorbent Download PDFInfo
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- CN102580679B CN102580679B CN201210064995.9A CN201210064995A CN102580679B CN 102580679 B CN102580679 B CN 102580679B CN 201210064995 A CN201210064995 A CN 201210064995A CN 102580679 B CN102580679 B CN 102580679B
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- microwave activated
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Abstract
The invention discloses a kind of preparation method of modified microwave activated carbon sorbent, the method is using microwave activated carbon as carrier, and alkali metal ion K ion carries out modification as active component, adopts ultrasonic wave equivalent impregnation, obtained modified microwave activated carbon sorbent; The inventive method is simple, and easy to operate, cost is low, the adsorbent prepared by the inventive method, advantages of good adsorption effect, can obtain higher CO
2/ CH
4adsorption equilibrium selective factor B.
Description
Technical field
The present invention relates to a kind of preparation method of modified microwave activated carbon sorbent, specifically 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 biogas under normal circumstances
4content be about 60% ~ 70%, CO
2content is about 30% ~ 40%, also has a small amount of O in addition
2, N
2deng other gas.Reclaim from refuse landfill and utilize the CH biogas
4gas, technically with in economic benefit be all feasible, and be reduce discharging CH
4an effective way of gas.The concentrated refuse landfill in a city has a large amount of CH
4gas, if used, has just reduced discharging a considerable amount of greenhouse gases, and has provided new energy sources approach; And simultaneously CO
2existence greatly reduce the energy value of unit volume gas, the biogas scope of application now and limited, and efficiency is lower.In addition, CO
2existence also can corrode transport pipeline, work the mischief.Therefore how to CH
4and CO
2effectively be separated, and be used respectively, current, there is important strategic importance.In China, the biogas that a large amount of medium and small methane-generating pit in rural area produces is mainly used for cooking and throwing light on, and has not given play to larger economic benefit; And in Europe and North America, the biogas of production is by being incorporated to gas distributing system, for biogas fuel cell generating, cogeneration of heat and power after purification or be used as motor vehicle fuel, larger economic benefit can be produced.
Effective separation of C H
4and CO
2method have absorption process, membrane separation process, cryogenic distillation process and pressure swing adsorption method etc.Absorption process often adopts alkaline solution to do absorbent divided gas flow, and technical operation is complicated, and energy consumption is large, and easily produces contaminated wastewater.Chinese patent CN101693169A reports a kind of separation of C O
2, CH
4the preparation method of the composite membrane of mist, by will to CO
2have that the SAPO-34 of strong adsorption property is molecular sieve doped to be entered in the precursor liquid of charcoal molecular film, thus facilitate composite membrane to CO
2selectively penetrating, improve CO
2/ CH
4selective.But adopt membrane separation process usually to need dehydration and filter process, add the complexity of operating procedure.
Absorption method has that product purity is high, energy consumption is low, technological process is simple, automaticity advantages of higher, and the application in being separated of purification and biogas of natural gas also more and more comes into one's own, 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 conventional have natural zeolite, molecular sieve, silica gel, active carbon etc.Chinese patent CN126871A reports with the rich sodium clinoptilolite of natural formation as adsorbent, adopts pressure swing adsorption method bulk separation of carbon dioxide from methane.A large amount of most of carbon dioxide can be deviate from low operating pressures.This absorption adsorbing separation effect is better, but uses natural zeolite cost higher.Active carbon has flourishing microcellular structure, and adsorption capacity is large, cheap, is widely used in gas absorption separation field.Chinese patent CN101255945A discloses a kind of technology utilizing activated carbon microballon adsorbent to remove carbon dioxide in natural, the carbon dioxide content in natural gas can be reduced to 0.05 volume % by about 10.0 volume %.Activated carbon microballon adsorbent desorption in this invention is simple, can circulate and recycle, but adsorptive selectivity is not high at ambient pressure.Along with the development of science and technology, the active carbon utilizing microwave heating process obtained is heated evenly because of it, with low cost, produces conveniently, advantages such as 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, also be applied in some field of gas purification, Chinese patent CN101693162A discloses and a kind ofly utilizes active carbon under microwave to the method for boiler smoke simultaneous SO_2 and NO removal, invention make use of the selective heating properties of microwave, in conjunction with the reducing power of charcoal to SO2 and NOX, substantially increase the efficiency of desulphurization and denitration simultaneously, the desulfurization degree of more than 95% and the denitration rate of more than 90% can be reached.Microwave activated carbon is at adsorbing separation CO
2/ CH
4application in gas field, there is not been reported.
Summary of the invention
The present invention has aimed to provide a kind of preparation method of modified microwave activated carbon sorbent, and the adsorbent prepared by the present invention to be separated CO absorption
2and CH
4the modified microwave activated carbon sorbent of gas.
Using microwave activated carbon as carrier in the present invention, alkali metal ion K ion carries out modification as active component, adopts ultrasonic wave equivalent impregnation, obtained adsorbent.The concrete preparation method of modified adsorbent comprises the steps:
(1) ground, be sized to 40 ~ 60 orders by microwave activated carbon, with distilled water washing 3 ~ 4 times, at 100 ~ 120 DEG C, dry 12 ~ 24h, is naturally down to room temperature in drying basin;
(2) add the alkali metal soln of 2 ~ 4ml by 1g active carbon, the active carbon processed is placed in alkali metal soln and carries out ultrasonic wave dipping 0.5 ~ 4h, then dry 12 ~ 24h at 100 ~ 120 DEG C;
(3) roasting 2 ~ 5h at the microwave activated carbon that (2) step is obtained being placed on 200 ~ 650 DEG C, is naturally down to room temperature, obtains modified microwave activated carbon sorbent in drying basin.
Alkali metal soln described in the present invention is a kind of in potassium hydroxide, potassium nitrate, potash, 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 DEG C, carries out under ultrasonic frequency 28 ~ 45KHz condition.
In the present invention, microwave activated carbon used adopts conventional method, through the active carbon that microwave treatment obtains, as obtained with reference to method disclosed in Chinese patent application 200810233530.5.
The present invention has following advantages and effect:
The inventive method is simple, and cost is lower, sorbent used carrier simple to operate and maceration extract, cheap, easily obtains, and modified adsorbent is by adsorption CO
2and CH
4gas, to CO
2adsorption capacity improve, CH
4adsorption capacity reduce, thus obtain higher CO
2/ CH
4adsorption equilibrium selective factor B, adsorbent prepared by preparation method of the present invention is CH in adsorbing separation biogas
4and CO
2gas provides a kind of economically viable approach, and separating effect is better.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but scope is not limited to described content.
embodiment 1:a preparation method for modified microwave activated carbon sorbent, concrete operations are as follows:
(1) microwave cocoanut active charcoal is ground, is sized to 40 orders, get 17g active carbon distilled water and wash 3 times, at 100 DEG C after dry 24h, in drying basin, be naturally down to room temperature;
(2) active carbon processed is placed in 0.5mol/L solution of potassium carbonate 34ml, at 30 DEG C, ultrasonic frequency is under 28KHz condition, dipping 4h, then dry 24h at 100 DEG C in thermostatic drying chamber;
(3) finally active carbon is placed in Muffle furnace roasting 4h at 350 DEG C, in drying basin, is naturally down to room temperature, obtains modified microwave activated carbon sorbent.
(4) modified microwave activated carbon sorbent 2.0g is got, adsorbing separation CO at 25 DEG C
2and CH
4gas, CO
2and CH
4the concentration of volume percent of gas is respectively 99.99% and 99.9%; Static Volumetric Method is utilized to record CH
4and CO
2the adsorpting data of gas, test result is as shown in table 1.
embodiment 2:a preparation method for modified microwave activated carbon sorbent, concrete operations are as follows:
(1) microwave coal mass active carbon is ground, is sized to 50 orders, get 17g active carbon distilled water and wash 4 times, at 110 DEG C after dry 18h, in drying basin, be naturally down to room temperature;
(2) active carbon processed is placed in 1mol/L Klorvess Liquid 51ml, at 40 DEG C, ultrasonic frequency is under 35KHz condition, dipping 2h, then dry 18h at 110 DEG C in thermostatic drying chamber;
(3) finally active carbon is placed in Muffle furnace roasting 5h at 200 DEG C, in drying basin, is naturally down to room temperature, obtains modified microwave activated carbon sorbent.
(4) modified microwave activated carbon sorbent 2.0g is got, adsorbing separation CO at 25 DEG C
2and CH
4gas, CO
2and CH
4the concentration of volume percent of gas is respectively 99.99% and 99.9%; Static Volumetric Method is utilized to record CH
4and CO
2the adsorpting data of gas, test result is as shown in table 1.
embodiment 3:a preparation method for modified microwave activated carbon sorbent, concrete operations are as follows:
(1) microwave cocoanut active charcoal is ground, is sized to 60 orders, get 17g active carbon distilled water and wash 3 times, at 120 DEG C after dry 12h, in drying basin, be naturally down to room temperature;
(2) active carbon processed is placed in 2mol/L potassium hydroxide solution 68ml, at 35 DEG C, ultrasonic frequency is under 45KHz condition, dipping 0.5h, then dry 12h at 120 DEG C in thermostatic drying chamber;
(3) finally active carbon is placed in Muffle furnace roasting 2h at 650 DEG C, in drying basin, is naturally down to room temperature, obtains modified microwave activated carbon sorbent.
(4) modified microwave activated carbon sorbent 2.0g is got, adsorbing separation CO at 25 DEG C
2and CH
4gas, CO
2and CH
4the concentration of volume percent of gas is respectively 99.99% and 99.9%; Static Volumetric Method is utilized to record CH
4and CO
2the adsorpting data of gas, test result is as shown in table 1.
embodiment 4:a preparation method for modified microwave activated carbon sorbent, concrete operations are as follows:
(1) microwave tobacco rod matrix activated carbon is ground, is sized to 45 orders, get 17g active carbon distilled water and wash 3 times, at 115 DEG C after dry 20h, in drying basin, be naturally down to room temperature;
(2) active carbon processed is placed in 1.5mol/L potassium nitrate solution 51ml, at 35 DEG C, ultrasonic frequency is under 40KHz condition, dipping 1h, then dry 16h at 120 DEG C in thermostatic drying chamber;
(3) finally active carbon is placed in Muffle furnace roasting 3h at 450 DEG C, in drying basin, is naturally down to room temperature, obtains modified microwave activated carbon sorbent.
(4) modified microwave activated carbon sorbent 2.0g is got, adsorbing separation CO at 25 DEG C
2and CH
4gas, CO
2and CH
4the concentration of volume percent of gas is respectively 99.99% and 99.9%; Static Volumetric Method is utilized 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
As can be seen from Table 1, compared with blank microwave activated carbon, through modified adsorbent to CO
2adsorption capacity increase, and to CH
4adsorption capacity reduce, adsorption equilibrium selective factor B is greater than blank microwave activated carbon.
The microwave activated carbon adopted in above-described embodiment all prepares with reference to method disclosed in Chinese patent application 200810233530.5.
Claims (3)
1. a preparation method for modified microwave activated carbon sorbent, is characterized in that carrying out as follows:
(1) microwave activated carbon is ground, is sized to 40 ~ 60 orders, with distilled water washing 3 ~ 4 times, at 100 ~ 120 DEG C after dry 12 ~ 24h, be naturally down to room temperature;
(2) add the alkali metal soln of 2 ~ 4mL by 1g microwave activated carbon, the microwave activated carbon processed is placed in alkali metal soln and carries out ultrasonic wave dipping 0.5 ~ 4h, then dry 12 ~ 24h at 100 ~ 120 DEG C;
(3) finally by microwave activated carbon roasting 2 ~ 5h at 200 ~ 650 DEG C, in drying basin, be naturally down to room temperature, obtain modified microwave activated carbon sorbent;
Described alkali metal soln is a kind of in potassium hydroxide, potassium nitrate, potash, Klorvess Liquid.
2. the preparation method of modified microwave activated carbon sorbent according to claim 1, is characterized in that: alkali metal soln concentration is 0.5 ~ 2mol/L.
3. the preparation method of modified microwave activated carbon sorbent according to claim 1, is characterized in that: ultrasonic wave is immersed in 30 ~ 40 DEG C, carries out under ultrasonic frequency 28 ~ 45KHz condition.
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| CN103232036B (en) * | 2013-05-09 | 2016-01-20 | 贺守印 | A kind of preparation method of desulphurization denitration active carbon |
| CN103754977B (en) * | 2014-01-17 | 2015-04-01 | 哈尔滨工业大学 | Active carbon modification method for emergently treating sudden organic pollution of drinking water |
| CN104907045B (en) * | 2014-03-10 | 2017-10-31 | 江苏瑞丰科技实业有限公司 | High-efficiency carbon dioxide material for trapping |
| CN105251444B (en) * | 2015-10-30 | 2018-01-16 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of method of trace potassium hydroxide modified activated carbon base propane adsorbent |
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| CN108126660A (en) * | 2018-01-23 | 2018-06-08 | 大连理工大学盘锦产业技术研究院 | A kind of CO based on Immesion active carbon2Solid absorbent, preparation method and its usage |
| CN108392942A (en) * | 2018-03-16 | 2018-08-14 | 东华大学 | A kind of amino modified alkali metal base CO2Adsorbent and preparation method thereof |
| CN108525463A (en) * | 2018-04-20 | 2018-09-14 | 辽宁石油化工大学 | A kind of CO2/CH4CO in mixed gas2Separation method |
| TWI657859B (en) * | 2018-04-30 | 2019-05-01 | 國立成功大學 | Regeneration method of carbon dioxide absorbent material |
| CN110653247B (en) * | 2019-09-30 | 2021-11-19 | 中国矿业大学 | Soil phosphorus condition improvement method based on red mud-based composite solid waste material recycling |
| CN110935420A (en) * | 2019-12-11 | 2020-03-31 | 福州大学 | Normal pressure CO2Preparation method of hierarchical pore activated carbon adsorbent |
| CN111905691B (en) * | 2020-06-01 | 2022-11-08 | 农业部沼气科学研究所 | Rapid oxidation modification method of biomass charcoal, product and application thereof |
| CN113786798B (en) * | 2021-10-14 | 2023-09-29 | 辽宁科技大学 | Method for preparing flue gas adsorbent by cooperatively treating industrial waste residues by coupling external fields |
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