CN103480336A - Modified biomass activated coke mercury removal adsorbent and preparation method thereof - Google Patents
Modified biomass activated coke mercury removal adsorbent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a modified biomass activated coke mercury removal adsorbent and a preparation method thereof. The mercury removal adsorbent is biomass activated coke undergoing phosphoric acid activation and halogenated ammonium salt modification dual treatment. The preparation method includes: immersing biomass particles into a phosphoric acid solution to conduct continuous stirring impregnation, performing filtering and drying, then under an N2 atmosphere, carrying out pyrolysis activation on the biomass particles subjected to phosphoric acid impregnation treatment; then conducting washing till the filtrate has a pH value of 6-7, and performing drying under 45-50DEG C; immersing the biomass activated coke into a halogenated ammonium salt solution, and carrying out continuous stirring impregnation for 1-2h; and conducting filtering and drying so as to obtain the modified biomass activated coke mercury removal adsorbent, which has the advantages of convenience and simplicity, less pollution, easy industrial popularization and the like.
Description
Technical field
The invention belongs to comprehensive utilization and the industrial waste gas demercuration field of biomass resource, relate to a kind of method of utilizing phosphoric acid activation and ammonium halide salt modified biomass Jiao to prepare demercuration adsorbent.
Background technology
Mercury and mercuric compounds is a class poisonous and harmful substance, the mercury of micro-dosage can cause huge harm to natural environments such as health and ecological water and soil atmosphere, and has the features such as interzone is migrated, the interior enrichment of organism, the transmission of food chain toxicity, strong latency.Except natural cause, the human activity such as fossil-fuel-fired, metal smelt, manufacture of cement, chlorine industry, Municipal Industry day by day becomes the important sources of mercury pollution in atmosphere.At present, the many countries in the whole world have formulated the laws and regulations and the industry standard that limit for industrial processes mercury emissions such as waste incineration, mineral processing, coal fired power generations specially.
From removal efficiency, scrap build, operation difficulty, on the existing equipment impact and whether introduce many-sided comprehensive consideration such as new pollutant, adsorbent flue gas injection technology is considered to the mercury removal technology of tool industrial prospect, and on the solid waste burning device of city, be used widely, be also the plan that China carries out the first-selection of mercury pollution control in industrial waste gas.Adsorbent the most commonly used is the business active carbon at present, and obtain operation examination on site in the U.S., Europe etc., obtain preferably demercuration effect, but its still have competitive Adsorption, temperature window is narrow, operating cost is high, regenerability is poor, affect the problems such as byproduct quality.Visible, the key issue of active carbon flue gas injection demercuration is its high operating cost after all, the method that derivative two classes reduce costs thus: the one, adsorbent is carried out to modification, strengthening unit mass mercury adsorption features, thereby the total flow of minimizing adsorbent; The 2nd, actively seek the alternative adsorbent of Cheap highly effective.
Living beings have that wide material sources, reserves are abundant, clean environment firendly, the advantage such as cheap, the traditional energy be on the rise tighten and the dual-pressure of problem of environmental pollution under, become the focus of domestic and international association area.Biomass pyrolytic, activation gained living beings activation Jiao have the flourishing pore structure similar to active carbon, thereby possesses certain physical absorption ability, it is carried out to chemical modification, be formed with the functional group that is beneficial to mercury absorption on its surface, likely obtain the demercuration adsorbent with efficient adsorption ability, realization replaces the high-carbon energy active carbon with low-carbon (LC) agriculture and forestry discarded object, reduces the cost of demercuration adsorbent, is convenient to industrial promotion and application.
Summary of the invention
technical problem:the present invention is directed to the deficiency that existing active carbon demercuration adsorbent exists, provide a kind of and utilized living beings to there is the modified biomass that efficiently removes the ability of mercury in industrial waste gas after simple pyrolysis, activation and modification to activate burnt demercuration adsorbent and preparation method thereof.
technical scheme:the method for preparing modified biomass activation coke adsorbent of the present invention comprises the following steps:
(1) according to the mass ratio 1:1 ~ 1:3 of living beings and phosphoric acid, biological particles by granularity below 100 orders immerses in the phosphoric acid solution that mass percent is 20% ~ 60%, and use magnetic stirring apparatus continuous stirring 12 ~ 24 h, obtain phosphoric acid living beings liquid-solid mixture;
(2) the phosphoric acid living beings liquid-solid mixture that filtration step (1) obtains is dried gained biological particles after the elimination clear liquid under 45 ~ 50 ℃;
(3) at N
2under atmosphere, the biological particles after phosphate impregnation is processed, at 400 ~ 600 ℃ of lower pyrolysis activation 30 ~ 90 min, obtains activated material;
(4) take out the activated material that step (3) obtains, and with the deionized water washing, to the pH value of wash filtrate be 6 ~ 7, then under 45 ~ 50 ℃, dry, make living beings activation Jiao;
(5) the mass ratio 100:1 ~ 1:1 with ammonium halide salt according to living beings activation Jiao, immerse step (4) gained living beings activation Jiao in the ammonium halide salt solution that mass percent is 0.1% ~ 1%, and use magnetic stirring apparatus continuous stirring 1 ~ 2 h;
(6) living beings activation Jiao after filtration step (5) processing and the liquid-solid mixture of ammonium halide salt solution are dried gained living beings activation Jiao after the elimination clear liquid under 45 ~ 50 ℃, make modified biomass and activate burnt demercuration adsorbent.
In preparation method of the present invention, the ammonium halide salt in step (5) is ammonium chloride or ammonium bromide.
The modified biomass that the present invention also provides a kind of above-mentioned preparation method to obtain activates burnt demercuration adsorbent.
Industrial waste gas demercuration adsorbent in the present invention be take living beings as raw material, and living beings comprise root, stem, leaf and leaf, sawmilling powder of the crops such as paddy rice, wheat, corn, cotton etc.
Mechanism of the present invention is in living beings to contain higher volatile matter, in inert atmosphere, middle hot conditions, issues the reaction of heat-dissipating solution, and separating out of volatile matter can be at living beings surface and the large hole of inner formation; In addition, under certain external condition, the organic structures such as avicel cellulose in phosphoric acid solubilized biomass material, permeate preferably and spread in living beings inside, after washing away the phosphoric acid activation agent, and can be at the flourishing pore structure of the inner acquisition of living beings; Biomass active Jiao through pyrolysis activation process gained, the parameter of the sign such as specific area, micropore volume microscopic appearance all is significantly improved, be aided with the modification of ammonium halide salt solution chemistry dipping, when not affecting the efficient physical mercury adsorption capacity that original biomass active Jiao possesses, can more in depth enter the living beings activation burnt inner, support the halogen active sites that is beneficial to demercuration on its surface, further improve living beings and activate burnt chemical mercury absorption conversion capability.
beneficial effect:the present invention compared with prior art, has following advantage:
(1) the biomass pyrolytic activation is burnt for the preparation of the industrial waste gas demercuration adsorbent, it is the brand-new mode of living beings Renewable Energy Resources utilization, the theory that meets scientific development and environmental protection, utilize the agriculture and forestry discarded object significantly to reduce production costs simultaneously, promote sorbent injection to remove the popularization of mercury in industrial waste gas;
(2) adopt phosphoric acid activation method, at biological particles surface and the inner flourishing pore structure that forms and develop certain degree, both overcome problem of environmental pollution aspect commercial Application simultaneously, also lower to the damage of activation equipment;
(3) utilize the ammonium halide salt modification, halogen is supported effectively in the burnt surface of living beings activation, form the effective active position, improved its absorption to mercury in industrial waste gas and conversion capability;
The present invention organically combines high temperature pyrolysis, phosphoric acid activation and ammonium halide salt modification in living beings, utilize the characteristics that the living beings volatile matter is high, form flourishing pore structure after Volatile, by phosphoric acid method, activate, the reaming of further clearing the way, when improving biomass char physical absorption ability, also for follow-up dipping modification, provide the solution infiltration lane, while is for the special physico-chemical character of mercury, the ammonium halide salt of take activates burnt chemical impregnation modification as modifier carries out living beings, further improves its demercuration performance.According to above-mentioned steps and method, successfully prepare the modified biomass activation coke adsorbent for the industrial waste gas high-efficiency mercury removal, keep nearly 100% demercuration efficiency in short time at 1 ~ 10 min, also can maintain the demercuration efficiency more than 90% in 120 ~ 240 min are long-time, and, through biomass active Jiao of phosphoric acid activation and ammonium halide salt modification Duplex treatment, its demercuration efficiency is better than carrying out merely the biomass char of ammonium halide salt modification more than 20% all the time.
The specific embodiment
According to following embodiment, the present invention may be better understood.Yet, those skilled in the art will readily understand, the described concrete material proportion of embodiment, preparation condition and result thereof be only for the present invention is described, and should also can not limit the present invention described in detail in claims.
Embodiment 1:
It is 40% that the SPA that is 85% by mass percent is diluted to mass percent, and broken dry rice husk, sieve, and chooses the following particle of particle diameter 100 orders standby.Take 10 g rice husk particles and be placed in phosphoric acid solution after the above-mentioned dilution of 75 g (rice husk particle with phosphoric acid quality than being 1:3), and use magnetic stirring apparatus continuous stirring 24 h, filter, gained rice husk particle is dried under 45 ~ 50 ℃, at N
2under atmosphere, the rice husk particle risen to after 500 ℃ after phosphate impregnation is processed until furnace temperature is sent into pyrolysis activation in stove, taking out and be placed in drier after 60 min preserves, take out the rice husk activated material and wash by deionized water, pH value to wash filtrate is 6 ~ 7, dry under 45 ~ 50 ℃, make the rice husk activation burnt.
Take 1 g ammonium bromide and be placed in beaker, add deionized water, stir and be mixed with the ammonium bromide solution that mass percent is 1%.By the burnt beaker (rice husk activation Jiao is 1:1 with the ammonium bromide mass ratio) that fills 1% ammonium bromide solution of putting into of load weighted 1 g rice husk activation in advance, and use magnetic stirring apparatus continuous stirring 1 h, filter, under 45 ~ 50 ℃, dry, be placed in reagent bottle and preserve, make ammonium bromide modification rice husk and activate burnt demercuration adsorbent.
Embodiment 2:
It is 60% that the SPA that is 85% by mass percent is diluted to mass percent, and broken dry rice straw, sieve, and chooses the following particle of particle diameter 100 orders standby.Take 10 g rice straw particles and be placed in phosphoric acid solution after the above-mentioned dilution of 50 g (rice straw particle with phosphoric acid quality than being 1:3), and use magnetic stirring apparatus continuous stirring 12 h, filter, gained rice straw particle is dried under 45 ~ 50 ℃, at N
2under atmosphere, the rice straw particle risen to after 600 ℃ after phosphate impregnation is processed until furnace temperature is sent into pyrolysis activation in stove, taking out and be placed in drier after 30 min preserves, take out the rice straw activated material and wash by deionized water, pH value to wash filtrate is 6 ~ 7, dry under 45 ~ 50 ℃, make the rice straw activation burnt.
Take 0.5 g ammonium bromide and be placed in beaker, add deionized water, stir and be mixed with the ammonium bromide solution that mass percent is 0.5%.By the burnt beaker (rice straw activation Jiao is 10:1 with the ammonium bromide mass ratio) that fills 0.5% ammonium bromide solution of putting into of load weighted 5 g rice straw activation in advance, and use magnetic stirring apparatus continuous stirring 2 h, filter, under 45 ~ 50 ℃, dry, be placed in reagent bottle and preserve, make ammonium bromide modification rice straw and activate burnt demercuration adsorbent.
Embodiment 3:
It is 20% that the SPA that is 85% by mass percent is diluted to mass percent, and broken dry sawdust, sieve, and chooses the following particle of particle diameter 100 orders standby.Take 10 g sawdust particles and be placed in phosphoric acid solution after the above-mentioned dilution of 50 g (sawdust particle with phosphoric acid quality than being 1:1), and use magnetic stirring apparatus continuous stirring 18 h, filter, gained sawdust particle is dried under 45 ~ 50 ℃, at N
2under atmosphere, the sawdust particle risen to after 400 ℃ after phosphate impregnation is processed until furnace temperature is sent into pyrolysis activation in stove, taking out and be placed in drier after 90 min preserves, take out the sawdust activated material and wash by deionized water, pH value to wash filtrate is 6 ~ 7, dry under 45 ~ 50 ℃, make the sawdust activation burnt.
Take 1 g ammonium chloride and be placed in beaker, add deionized water, stir and be mixed with the ammonium chloride solution that mass percent is 0.1%.By the burnt beaker (sawdust activation Jiao is 100:1 with the ammonium chloride mass ratio) that fills 0.1% ammonium chloride solution of putting into of load weighted 100 g sawdust activation in advance, and use magnetic stirring apparatus continuous stirring 1.5 h, filter, under 45 ~ 50 ℃, dry, be placed in reagent bottle and preserve, make ammonium chloride modification sawdust and activate burnt demercuration adsorbent.
Embodiment 4:
It is 40% that the SPA that is 85% by mass percent is diluted to mass percent, and broken dry cotton stalk, sieve, and chooses the following particle of particle diameter 100 orders standby.Take the cotton stalk particles of 10 g and be placed in phosphoric acid solution after the above-mentioned dilution of 50 g (cotton stalk particle with phosphoric acid quality than being 1:2), and use magnetic stirring apparatus continuous stirring 24 h, filter, the cotton stalk particle of gained is dried under 45 ~ 50 ℃, at N
2under atmosphere, the cotton stalk particle risen to after 500 ℃ after phosphate impregnation is processed until furnace temperature is sent into pyrolysis activation in stove, taking out and be placed in drier after 90 min preserves, take out cotton stalk activated material and wash by deionized water, pH value to wash filtrate is 6 ~ 7, dry under 45 ~ 50 ℃, make cotton stalk activation burnt.
Take 0.5 g ammonium chloride and be placed in beaker, add deionized water, stir and be mixed with the ammonium chloride solution that mass percent is 0.5%.By the burnt beaker (cotton stalk activation Jiao is 20:1 with the ammonium chloride mass ratio) that fills 0.5% ammonium chloride solution of putting into of the cotton stalk activation of load weighted 10 g in advance, and use magnetic stirring apparatus continuous stirring 2 h, filter, under 45 ~ 50 ℃, dry, be placed in reagent bottle and preserve, make the cotton stalk of ammonium chloride modification and activate burnt demercuration adsorbent.
Embodiment 5:
The applicant selects the ammonium bromide modification rice husk of preparation in embodiment 1 to activate burnt demercuration adsorbent, its absorption property of checking on the ADSORPTION IN A FIXED BED experimental bench.The ADSORPTION IN A FIXED BED experimental bench is comprised of simulated flue gas generation systems, fixed bed reactors, mercury measurement device, device for purifying and treating tail gas etc., and wherein simulated flue gas adopts high-purity N
2, total gas flow rate is 2 L/min.Mercury vapour is produced by the mercury osmos tube (U.S. VICI Metronics company) be placed in U-shaped high-boron-silicon glass pipe, and by high-purity N
2take out of as carrier gas, carry mercury N
2flow is 150 ml/min.Fixed bed entrance mercury concentration is 32 ± 1.0 μ g/m
3.Experimental result shows, the initial mercury adsorption efficiency of the adsorbent of embodiment 1 is that after 100%, 120 min, adsorption efficiency is 93%, and in its 120 min, accumulation mercury adsorbance is 31.59 μ g/g.
Embodiment 6:
Optional embodiment 2,3,4 or the demercuration adsorbent of being prepared by other biomass material, according to the experimental technique of embodiment 5, carry out the demercuration experimental verification, all can produce good demercuration effect.
Claims (3)
1. one kind prepares the method that modified biomass activates burnt demercuration adsorbent, it is characterized in that, the method comprises the following steps:
(1) according to the mass ratio 1:1 ~ 1:3 of living beings and phosphoric acid, biological particles by granularity below 100 orders immerses in the phosphoric acid solution that mass percent is 20% ~ 60%, and use magnetic stirring apparatus continuous stirring 12 ~ 24 h, obtain phosphoric acid living beings liquid-solid mixture;
(2) the phosphoric acid living beings liquid-solid mixture that filtration step (1) obtains is dried gained biological particles after the elimination clear liquid under 45 ~ 50 ℃;
(3) at N
2under atmosphere, the biological particles after phosphate impregnation is processed, at 400 ~ 600 ℃ of lower pyrolysis activation 30 ~ 90 min, obtains activated material;
(4) take out the activated material that described step (3) obtains, and with deionized water washing, to the pH value of wash filtrate be 6 ~ 7, then under 45 ~ 50 ℃, dry, make living beings activation Jiao;
(5) the mass ratio 100:1 ~ 1:1 with ammonium halide salt according to living beings activation Jiao, immerse step (4) gained living beings activation Jiao in the ammonium halide salt solution that mass percent is 0.1% ~ 1%, and use magnetic stirring apparatus continuous stirring 1 ~ 2 h;
(6) living beings of filtering after described step (5) is processed activate liquid-solid mixture burnt and ammonium halide salt solution, by the burnt oven dry under 45 ~ 50 ℃ of gained living beings activation after the elimination clear liquid, make modified biomass and activate burnt demercuration adsorbent.
2. according to claim 1ly prepare the method that modified biomass activates burnt demercuration adsorbent, it is characterized in that, the ammonium halide salt in described step (5) is ammonium chloride or ammonium bromide.
3. a modified biomass activates burnt demercuration adsorbent, it is characterized in that, this demercuration adsorbent prepares according to the described method of claim 1 or 2.
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US10449492B2 (en) | 2014-05-30 | 2019-10-22 | Ada Carbon Solutions, Llc | Catalytically enhanced compositions for efficient removal of contaminants in flue gas streams |
US10780396B2 (en) | 2014-05-30 | 2020-09-22 | Ada Carbon Solutions, Llc | Methods for the treatment of a flue gas stream using catalytically-enhanced sorbent compositions |
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CN106466590A (en) * | 2015-08-14 | 2017-03-01 | Ada碳解决方案有限责任公司 | The adsorbent composition with amorphous halogen species for pollutant chelating |
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US11285459B2 (en) | 2015-08-14 | 2022-03-29 | Ada Carbon Solutions, Llc | Sorbent compositions having amorphous halogen species for the sequestration of contaminants |
CN107182652A (en) * | 2017-04-22 | 2017-09-22 | 枞阳县横山生态农业有限公司 | A kind of regional paddy rice planting method of mercury pollution |
CN110252245A (en) * | 2019-06-27 | 2019-09-20 | 南京理工大学 | The preparation method of modified carbon-based demercuration adsorbent |
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CN112705164A (en) * | 2020-12-31 | 2021-04-27 | 南京理工大学 | Sulfur-resistant demercuration adsorbent and modification method thereof |
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