CN103480336B - A kind of modified biomass activates burnt demercuration adsorbent and preparation method thereof - Google Patents
A kind of modified biomass activates burnt demercuration adsorbent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of modified biomass and activate burnt demercuration adsorbent and preparation method thereof.This demercuration adsorbent is utilize the living beings activation of phosphoric acid activation and ammonium halide salt modification Duplex treatment burnt.Biological particles immerses in phosphoric acid solution and stirs dipping continuously, at N after filtering drying by preparation method
2under atmosphere, by the biological particles pyrolysis activation after phosphate impregnation process; Dry at the pH value of then washing to filtrate is 6 ~ 7,45 ~ 50 DEG C; Burnt for living beings activation immersion in ammonium halide salt solution is stirred dipping 1 ~ 2h continuously; After filtering drying, namely obtained modified biomass activates burnt demercuration adsorbent.The present invention have convenient and simple, pollute less, be convenient to the advantages such as commercial introduction.
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 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 air, and have that interzone is migrated, the feature such as enrichment in organism, food chain toxicity are transmitted, 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 air.At present, the many countries in the whole world have formulated the special laws and regulations for industrial processes mercury emissions restrictions such as waste incineration, mineral processing, coal fired power generations and professional standard.
From removal efficiency, scrap build, operation difficulty, on existing equipment impact and whether introduce many-sided comprehensive considerations such as new pollutant, adsorbent flue gas injection technology is considered to the mercury removal technology of most industrial prospect, and be used widely on the solid waste burning device of city, Yi Shi China carries out the plan of the first-selection of mercury pollution control in industrial waste gas.Adsorbent the most conventional is at present commercial activated carbons, and obtain operation examination on site in the U.S., Europe etc., obtain preferably demercuration effect, but its still there is 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, derives the method that two classes reduce costs thus: one is carry out modification to adsorbent, strengthening unit mass mercury adsorption features, thus reduces the total flow of adsorbent; Two is the alternative adsorbents actively seeking Cheap highly effective.
Living beings have wide material sources, rich reserves, clean environment firendly, the advantage such as cheap, the traditional energy be on the rise tighten and problem of environmental pollution dual-pressure 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, thus certain physical absorption ability is possessed, chemical modification is carried out to it, the functional group being beneficial to mercury absorption is formed on its surface, then likely obtain the demercuration adsorbent with efficient adsorption ability, realize replacing high-carbon energy active carbon with low-carbon (LC) agriculture and forestry discarded object, reduce the cost of demercuration adsorbent, be convenient to commercial introduction 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 modified biomass utilizing living beings to have the ability of mercury in efficient removal industrial waste gas after simple pyrolysis, activation and modification and activate burnt demercuration adsorbent and preparation method thereof.
technical scheme:the method 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, it is in the phosphoric acid solution of 20% ~ 60% that the biological particles of granularity below 100 orders is immersed mass percent, and uses magnetic stirring apparatus to stir 12 ~ 24h continuously, obtains phosphoric acid living beings liquid-solid mixture;
(2) the phosphoric acid living beings liquid-solid mixture that obtains of filtration step (1), dries gained biological particles after elimination clear liquid at 45 ~ 50 DEG C;
(3) at N
2under atmosphere, by the pyrolysis activation 30 ~ 90min at 400 ~ 600 DEG C of the biological particles after phosphate impregnation process, obtain activated material;
(4) take out the activated material that step (3) obtains, and spend deionized water, the pH value to wash filtrate is 6 ~ 7, then dries at 45 ~ 50 DEG C, and obtained living beings activation is burnt;
(5) according to living beings activation is burnt and the mass ratio 100:1 ~ 1:1 of ammonium halide salt, it is in the ammonium halide salt solution of 0.1% ~ 1% that step (4) gained living beings activation Jiao is immersed mass percent, and uses magnetic stirring apparatus to stir 1 ~ 2h continuously;
(6) living beings after filtration step (5) process activate liquid-solid mixture that is burnt and ammonium halide salt solution, and by burnt for gained living beings activation after elimination clear liquid oven dry at 45 ~ 50 DEG C, namely obtained modified biomass activates 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 take living beings as raw material, and living beings comprise the root of the crops such as paddy rice, wheat, corn, cotton, stem, leaf and leaf, sawmilling powder etc.
Mechanism of the present invention is that issue raw pyrolytic reaction in inert atmosphere, middle hot conditions, the precipitation of volatile matter can form large hole at biological surface and inside containing higher volatile matter in living beings; In addition, under certain external condition, the organic structures such as the avicel cellulose in phosphoric acid solubilized biomass material, permeate preferably in living beings inside and spread, and after washing away phosphoric acid activation agent, can obtain flourishing pore structure in living beings inside; Biomass active through pyrolysis activation process gained is burnt, the parameter that specific area, micropore volume etc. characterize microscopic appearance is all significantly improved, be aided with the modification of ammonium halide salt solution chemistry dipping, while not affecting the burnt efficient physical mercury adsorption capacity possessed of original biomass active, more in depth can enter living beings activation burnt inner, support the halogen active sites being beneficial to demercuration on its surface, further improve the chemical mercury absorption conversion capability that living beings activation is burnt.
beneficial effect:compared with prior art, tool has the following advantages in the present invention:
(1) biomass pyrolytic is activated Jiao for the preparation of industrial waste gas demercuration adsorbent, it is the new way that living beings Renewable Energy Resourcesization utilizes, meet the theory of scientific development and environmental protection, utilize agriculture and forestry discarded object significantly can reduce production cost simultaneously, promote that sorbent injection removes the popularization of mercury in industrial waste gas;
(2) adopt phosphoric acid activation method, formed on biological particles surface and inside and develop the flourishing pore structure of certain degree, in commercial Application, both overcoming problem of environmental pollution simultaneously, also lower to the damage of activation equipment;
(3) utilize ammonium halide salt modification, halogen is supported effectively in the burnt surface of living beings activation, form effective active sites, improve it to the absorption of mercury in industrial waste gas and conversion capability;
High temperature pyrolysis, phosphoric acid activation and ammonium halide salt modification in living beings organically combine by the present invention, utilize the feature that living beings volatile matter is high, namely flourishing pore structure is formed after Volatile, activate by phosphoric acid method, to clear the way further reaming, while raising biomass char physical absorption ability, also solution infiltration lane is provided for follow-up dipping modification, simultaneously for the special physico-chemical character of mercury, be that modifier carries out the burnt chemical impregnation modification of living beings activation with ammonium halide salt, improve its demercuration performance further.According to above-mentioned steps and method, successfully prepare the modified biomass activation coke adsorbent for industrial waste gas high-efficiency mercury removal, the demercuration efficiency of nearly 100% is kept within 1 ~ 10min short time, also the demercuration efficiency of more than 90% can be maintained in 120 ~ 240min is long-time, and burnt through the biomass active of phosphoric acid activation and ammonium halide salt modification Duplex treatment, its demercuration efficiency is better than the biomass char more than 20% carrying out merely ammonium halide salt modification all the time.
Detailed description of the invention
According to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, concrete material proportion, preparation condition and result thereof described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
Embodiment 1:
By mass percent be 85% SPA to be diluted to mass percent be 40%, broken dry rice husk, sieve, the particle choosing below particle diameter 100 order is for subsequent use.Take 10g rice husk particle and be placed in phosphoric acid solution after the above-mentioned dilution of 75g (rice husk particle and phosphoric acid quality are than being 1:3), and use magnetic stirring apparatus to stir 24h continuously, filter, gained rice husk particle is dried at 45 ~ 50 DEG C, at N
2under atmosphere, rise to after 500 DEG C until furnace temperature and the rice husk particle after phosphate impregnation process is sent into pyrolysis activation in stove, take out after 60min and be placed in drier and preserve, take out rice husk activated material and spend deionized water, pH value to wash filtrate is 6 ~ 7, dry at 45 ~ 50 DEG C, obtained rice husk activation is burnt.
Take 1g ammonium bromide and be placed in beaker, add deionized water, stir and be mixed with the ammonium bromide solution that mass percent is 1%.The beaker (rice husk activation Jiao is 1:1 with ammonium bromide mass ratio) filling 1% ammonium bromide solution is put into by burnt for load weighted 1g rice husk activation in advance, and use magnetic stirring apparatus to stir 1h continuously, filter, dry at 45 ~ 50 DEG C, be placed in reagent bottle to preserve, namely obtained ammonium bromide modification rice husk activates burnt demercuration adsorbent.
Embodiment 2:
By mass percent be 85% SPA to be diluted to mass percent be 60%, broken dry rice straw, sieve, the particle choosing below particle diameter 100 order is for subsequent use.Take 10g rice straw particle and be placed in phosphoric acid solution after the above-mentioned dilution of 50g (rice straw particle and phosphoric acid quality are than being 1:3), and use magnetic stirring apparatus to stir 12h continuously, filter, gained rice straw particle is dried at 45 ~ 50 DEG C, at N
2under atmosphere, rise to after 600 DEG C until furnace temperature and the rice straw particle after phosphate impregnation process is sent into pyrolysis activation in stove, take out after 30min and be placed in drier and preserve, take out rice straw activated material and spend deionized water, pH value to wash filtrate is 6 ~ 7, dry at 45 ~ 50 DEG C, obtained rice straw activation is burnt.
Take 0.5g 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%.The beaker (rice straw activation Jiao is 10:1 with ammonium bromide mass ratio) filling 0.5% ammonium bromide solution is put into by burnt for load weighted 5g rice straw activation in advance, and use magnetic stirring apparatus to stir 2h continuously, filter, dry at 45 ~ 50 DEG C, be placed in reagent bottle to preserve, namely obtained ammonium bromide modification rice straw activates burnt demercuration adsorbent.
Embodiment 3:
By mass percent be 85% SPA to be diluted to mass percent be 20%, broken dry sawdust, sieve, the particle choosing below particle diameter 100 order is for subsequent use.Take 10g sawdust particle and be placed in phosphoric acid solution after the above-mentioned dilution of 50g (sawdust particle and phosphoric acid quality are than being 1:1), and use magnetic stirring apparatus to stir 18h continuously, filter, gained sawdust particle is dried at 45 ~ 50 DEG C, at N
2under atmosphere, rise to after 400 DEG C until furnace temperature and the sawdust particle after phosphate impregnation process is sent into pyrolysis activation in stove, take out after 90min and be placed in drier and preserve, take out sawdust activated material and spend deionized water, pH value to wash filtrate is 6 ~ 7, dry at 45 ~ 50 DEG C, obtained sawdust activation is burnt.
Take 1g 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%.The beaker (sawdust activation Jiao is 100:1 with ammonium chloride mass ratio) filling 0.1% ammonium chloride solution is put into by burnt for load weighted 100g sawdust activation in advance, and use magnetic stirring apparatus to stir 1.5h continuously, filter, dry at 45 ~ 50 DEG C, be placed in reagent bottle to preserve, namely obtained ammonium chloride sawdust activates burnt demercuration adsorbent.
Embodiment 4:
By mass percent be 85% SPA to be diluted to mass percent be 40%, broken dry cotton stalk, sieve, the particle choosing below particle diameter 100 order is for subsequent use.Take the cotton stalk particle of 10g be placed in the above-mentioned dilution of 50g after phosphoric acid solution (cotton stalk particle and phosphoric acid quality are than being 1:2), and use magnetic stirring apparatus to stir 24h continuously, filter, cotton for gained stalk particle is dried, at N at 45 ~ 50 DEG C
2under atmosphere, rise to after 500 DEG C until furnace temperature and the cotton stalk particle after phosphate impregnation process is sent into pyrolysis activation in stove, take out after 90min and be placed in drier and preserve, take out cotton stalk activated material and spend deionized water, pH value to wash filtrate is 6 ~ 7, dry at 45 ~ 50 DEG C, obtained cotton stalk activation is burnt.
Take 0.5g 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%.The beaker (cotton stalk activation Jiao is 20:1 with ammonium chloride mass ratio) filling 0.5% ammonium chloride solution is put into by burnt for load weighted 10g cotton stalk activation in advance, and use magnetic stirring apparatus to stir 2h continuously, filter, dry at 45 ~ 50 DEG C, be placed in reagent bottle to preserve, namely the cotton stalk of obtained ammonium chloride activates burnt demercuration adsorbent.
Embodiment 5:
Applicant selects the ammonium bromide modification rice husk of preparation in embodiment 1 to activate burnt demercuration adsorbent, and ADSORPTION IN A FIXED BED experimental bench is verified its absorption property.ADSORPTION IN A FIXED BED experimental bench is made up 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 2L/min.Mercury vapour is produced by the mercury osmos tube be placed in U-shaped high-boron-silicon glass pipe (VICIMetronics company of the U.S.), and by high-purity N
2take out of as carrier gas, carry mercury N
2flow is 150ml/min.Fixed bed entrance mercury concentration is 32 ± 1.0 μ g/m
3.Experimental result shows, the initial mercury adsorption efficiency of adsorbent of embodiment 1 is that after 100%, 120min, adsorption efficiency is 93%, and in its 120min, accumulation mercury adsorbance is 31.59 μ g/g.
Embodiment 6:
Optional embodiment 2,3,4 or the demercuration adsorbent prepared by other biomass material, according to the experimental technique of embodiment 5, carry out demercuration experimental verification, all can produce good demercuration effect.
Claims (3)
1. prepare 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, it is in the phosphoric acid solution of 20% ~ 60% that the biological particles of granularity below 100 orders is immersed mass percent, and use magnetic stirring apparatus to stir 12 ~ 24h continuously, obtain phosphoric acid living beings liquid-solid mixture, described living beings are the root of paddy rice or wheat or corn or cotton, stem, leaf, leaf or sawmilling powder;
(2) the phosphoric acid living beings liquid-solid mixture that obtains of filtration step (1), dries gained biological particles after elimination clear liquid at 45 ~ 50 DEG C;
(3) at N
2under atmosphere, by the pyrolysis activation 30 ~ 90min at 400 ~ 600 DEG C of the biological particles after phosphate impregnation process, obtain activated material;
(4) take out the activated material that described step (3) obtains, and spend deionized water, the pH value to wash filtrate is 6 ~ 7, then dries at 45 ~ 50 DEG C, and namely obtained living beings activation is burnt;
(5) according to living beings activation is burnt and the mass ratio 100:1 ~ 1:1 of ammonium halide salt, it is in the ammonium halide salt solution of 0.1% ~ 1% that step (4) gained living beings activation Jiao is immersed mass percent, and uses magnetic stirring apparatus to stir 1 ~ 2h continuously;
(6) living beings of filtering after described step (5) process activate liquid-solid mixture that is burnt and ammonium halide salt solution, and by burnt for gained living beings activation after elimination clear liquid oven dry at 45 ~ 50 DEG C, namely obtained modified biomass activates 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. modified biomass activates a burnt demercuration adsorbent, it is characterized in that, this demercuration adsorbent method according to claim 1 or 2 prepares.
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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 |
| US11285459B2 (en) | 2015-08-14 | 2022-03-29 | Ada Carbon Solutions, Llc | Sorbent compositions having amorphous halogen species for the sequestration of contaminants |
| US11219878B2 (en) | 2015-08-14 | 2022-01-11 | 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 |
| CN112175685B (en) * | 2019-07-02 | 2022-05-10 | 中国石油天然气股份有限公司 | System and method for reducing deposited mercury volatilization in natural gas processing equipment |
| CN112705164B (en) * | 2020-12-31 | 2023-05-09 | 南京理工大学 | Sulfur-resistant mercury removal adsorbent and modification method thereof |
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| US20070184976A1 (en) * | 2005-03-30 | 2007-08-09 | Tiejun Zhang | Activated carbon for fuel purification |
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