CN107262041A - A kind of sulfhydryl modified biomass char demercuration adsorbent and preparation method thereof - Google Patents
A kind of sulfhydryl modified biomass char demercuration adsorbent and preparation method thereof Download PDFInfo
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- CN107262041A CN107262041A CN201710455347.9A CN201710455347A CN107262041A CN 107262041 A CN107262041 A CN 107262041A CN 201710455347 A CN201710455347 A CN 201710455347A CN 107262041 A CN107262041 A CN 107262041A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/64—Heavy metals or compounds thereof, e.g. mercury
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
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Abstract
The present invention a kind of sulfhydryl modified biomass char demercuration adsorbent is disclosed, be made up of biomass and through sulfhydryl modified biomass char.Invention additionally discloses a kind of preparation method of sulfhydryl modified biomass char demercuration adsorbent, step includes:1) biomass is pre-processed:Biomass material is dried, crushed, powdered biomass is screened out;2) prepared by biomass char:Powdered biomass is sent into pyrolysis oven, the pyrolysis generation biomass char under the mixed atmosphere of vapor and inert gas, then stop being passed through vapor, continued to be passed through inert gas, until biomass char is cooled to less than 100 DEG C, biomass char powder is ground to form after taking-up;3) biomass char is sulfhydryl modified:By sulfydryl aliphatic acid, acetic anhydride, the concentrated sulfuric acid using volume ratio as (180~220):(120~150):Mixed solution is made in (1~2), and biomass char powder is put into the mixed solution and stood, and is then washed with deionized to neutral and dry, is obtained sulfhydryl modified biomass char as demercuration adsorbent.
Description
Technical field
The present invention relates to flue gas demercuration field, and in particular to a kind of sulfhydryl modified biomass char demercuration adsorbent and its preparation
Method.
Background technology
Mercury is a kind of poisonous heavy metal element, and the nervous system of human body and generation of growing can be had a strong impact on.Though
Right mercury is distributed relatively broad in nature, but in all emission sources of mercury, the ratio of anthropogenic discharge is highest.And in people
For in discharge, coal fire discharged ratio is highest again, so coal fire discharged is mercury emissions source maximum in the world.And in the world
In the range of, the Coal-fired capacity of China is maximum, along with the average content of mercury in China's coal is higher by world average level again
0.09mg/kg, so China can not be ignored due to the mercury emissions that fire coal is caused.Therefore, China puts into effect《Thermal power plant's atmosphere pollution
Thing discharge standard》(GB 13223-2011), it is desirable to which the emission limit of mercury and mercuric compounds is less than 30 μ g/ in fire coal boiler fume
Nm3.But with the fast development of China's economy, it is more strict that this standard will certainly be revised.So how efficiently to control
The discharge of coal fired power plant mercury in flue gas pollutant turns into current study hotspot.
For the mercury contaminants in coal fired power plant flue gas, the control technology of more maturation is adsorbent demercuration technology at present.
And for adsorbent demercuration technology, the selection of adsorbent is most important.It is modified activated carbon to apply most adsorbents at present, and
And be applied successfully in Duo Jia power plant of the U.S., show that modified activated carbon has excellent demercuration performance using result.But
The cost of modified activated carbon is too high, and very big financial burden can be brought to coal fired power plant.And the coal fired power plant of China already due to
Minimum discharge causes operating cost significantly to raise, so the too high modified activated carbon demercuration technology of operating cost is not particularly suited for me
The coal fired power plant of state.For this problem, proposition can substitute acticarbon with biomass char.Because biomass has
Wide material sources, rich reserves, clean environment firendly, it is cheap the characteristics of, and biomass char obtained by biomass pyrolytic have with
The similar flourishing pore structure of activated carbon, thus using biomass char as can significantly reduce if demercuration adsorbent demercuration into
This, is easy to commercial introduction and application.
Although substitute activated carbon with biomass char has many advantages, such as demercuration adsorbent, but if directly by ordinary student
Material Jiao (biomass char of i.e. non-modified processing) is used for if adsorbing demercuration, because it is mainly that physics is inhaled between mercury
It is attached, so under the influence of sour gas and moisture in operation temperature and flue gas, the Van der Waals force between mercury and biomass char
It can easily be destroyed, cause mercury to be desorbed from biomass char.In addition, the sour gas in flue gas can also be by shape after absorption
Into mercury compound be reduced to Elemental Mercury and cause the escape of mercury, so as to reduce the removal efficiency of mercury.
The content of the invention
To overcome prior art problem, the present invention provides a kind of sulfhydryl modified biomass char demercuration adsorbent and its preparation side
Method, carries out sulfhydryl modified to biomass char, strengthens its physical absorption ability to mercury and assigns its chemical adsorption capacity, so that
It has the ability of efficient removal Mercury In Coal Combustion Flue Gas.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows:
A kind of sulfhydryl modified biomass char demercuration adsorbent, be made up of biomass and through sulfhydryl modified biomass
It is burnt.
A kind of preparation method of sulfhydryl modified biomass char demercuration adsorbent, step includes:
1) biomass is pre-processed:Biomass material is dried, crushed, powdered biomass is screened out;
2) prepared by biomass char:Powdered biomass is sent into pyrolysis oven, in vapor and the mixed atmosphere of inert gas
Lower pyrolysis generation biomass char, then stops being passed through vapor, continues to be passed through inert gas, until biomass char is cooled to 100
Biomass char powder is ground to form below DEG C, after taking-up;
3) biomass char is sulfhydryl modified:By sulfydryl aliphatic acid, acetic anhydride, the concentrated sulfuric acid using volume ratio as (180~220):
(120~150):Mixed solution is made in (1~2), and biomass char powder is put into the mixed solution and stood, then uses deionized water
Washing obtains sulfhydryl modified biomass char as demercuration adsorbent to neutral and dry.
Further, biomass material lignocellulose-containing, including agricultural crop straw, timber.
Further, the particle diameter of powdered biomass is not more than 5mm.
Further, the mol ratio of hydrone and Inert gas molecule is in the mixed atmosphere of vapor and inert gas
0.5~1.
Further, inert gas includes nitrogen, rare gas etc., wherein the rare gas such as property such as helium, neon, argon gas
The stable gas of matter.
Further, pyrolysis temperature be 300~900 DEG C, when a length of 10~30min.
Further, sulfydryl aliphatic acid includes TGA, mercaptopropionic acid and other many carbon fatty acids with sulfydryl, with
TGA is optimal;Including isomer, such as mercaptopropionic acid includes 2 mercaptopropionic acid (CH3CH(SH)COOH)、3-
Mercaptopropionic acid (CH2(SH)CH2COOH);Effect is to provide the sulfydryl (- SH) that can be complexed with mercury, also provided and biomass char
On hydroxyl (- OH) occur esterification carboxyl (- COOH);For many carbon fatty acids with sulfydryl, it is contemplated that molecule space
The influence that structure and chemical bond etc. are complexed to mercury, using preceding needing to be screened.
Further, sulfydryl aliphatic acid, acetic anhydride, the concentrated sulfuric acid are technical pure.
Further, the particle diameter of biomass char powder is not more than 2mm.
Further, a length of 10~20h when biomass char powder is stood in mixed solution, temperature is 30~60 DEG C.
Biomass char prepared by the present invention is prepared under the mixed atmosphere of inert gas and vapor, it is possible to achieve
Steam activation is carried out to it while biomass char is prepared, is by the preparation of biomass char and steam activation is carried out to it
Two process conformities are a process, can be saved individually with steam activation biomass char when institute calorific requirement.Further, it is also possible to
Make the biomass char of preparation while with bigger serface, moreover it is possible to increase the content of its surface hydroxyl functional group.Because raw
The sulfhydryl modified of material Jiao is to be realized by the hydroxyl on biomass char surface with sulfydryl aliphatic acid generation esterification, so
The content of biomass char surface hydroxyl is higher, and the sulfhydryl content on the burnt surface of the modified biomass prepared will be higher, so logical
Crossing the content of vapor increase hydroxy functional group sulfhydryl modified to biomass char has significant facilitation.
Sulfydryl occurs esterification by sulfydryl aliphatic acid and hydroxyl and is fixed on activated carbon, and the esterification is one
Reversible reaction, to ensure that esterification is smoothed out, the water that must be generated except dereaction can be realized by acetic anhydride.Acetic anhydride
As a kind of strong water absorbent, sent out after can not only promoting the generation of esterification between activated carbon and sulfydryl aliphatic acid, and its water suction
The aliphatic acid that unboiled water solution is produced is alternatively arranged as the catalyst of esterification, will not introduce impurity.
Biomass char adds specific surface area in the presence of vapor, can strengthen the physics to coal fired power plant mercury in flue gas
Adsorption capacity, and the sulfydryl on surface can form highly stable complex compound with mercury, realize the chemisorbed to mercury, effectively prevent
Mercury after absorption is reduced to Elemental Mercury by the sour gas in flue gas, therefore compared with existing biomass char, this is sulfhydryl modified
Biomass char has stronger adsorption capacity to mercury in flue gas.
Brief description of the drawings
Fig. 1 is the schematic diagram for preparing sulfhydryl modified biomass char.
Fig. 2 is the mercury adsorbance comparison diagram of sulfhydryl modified biomass char and common biomass char.
Embodiment
To enable the features described above and advantage of the present invention to become apparent, special embodiment below, and coordinate institute's accompanying drawing work
Describe in detail as follows.
Embodiment 1
The present embodiment discloses a kind of preparation method of sulfhydryl modified biomass char demercuration adsorbent, as shown in figure 1, step bag
Include:
1) biomass is pre-processed:Biomass material selects the agricultural crop straw of lignocellulose-containing, by the biomass material
It is dried, crushes, screens out the powder that particle diameter is less than 5mm;
2) prepared by biomass char:Powdered biomass is sent into pyrolysis oven, vapor and nitrogen mol ratio for 0.5 it is mixed
Close and be pyrolyzed under atmosphere, pyrolysis temperature is maintained at 300 DEG C, and duration 30min generates biomass char;Then stop being passed through water steaming
Gas, continues to be passed through nitrogen, until biomass char is cooled to less than 100 DEG C, the powder that particle diameter is less than 2mm is ground to form after taking-up;
3) biomass char is sulfhydryl modified:By commercially pure TGA, acetic anhydride, the concentrated sulfuric acid using volume ratio as 180:120:
1 is made mixed solution, and biomass char powder is put into the mixed solution and stands 10h, and temperature is maintained at 60 DEG C, then spend from
Sub- water washing obtains sulfhydryl modified biomass char as demercuration adsorbent to neutral and dry.
Embodiment 2
The present embodiment discloses a kind of preparation method of sulfhydryl modified biomass char demercuration adsorbent, and Step By Condition is with implementing
Example 1 is roughly the same, and difference is:Biomass material selects the timber of lignocellulose-containing;Inert gas selects helium, water
Steam and helium mol ratio are 1;Pyrolysis temperature is maintained at 900 DEG C, when a length of 10min;Sulfydryl aliphatic acid selects 2 mercaptopropionic acid,
It is 220 with acetic anhydride, concentrated sulfuric acid volume ratio:150:2, it is technical pure;When biomass char powder is stood in mixed solution
A length of 20h, temperature is 30 DEG C.
Embodiment 3
The present embodiment discloses a kind of preparation method of sulfhydryl modified biomass char demercuration adsorbent, and Step By Condition is with implementing
Example 1 is roughly the same, and difference is:Inert gas selects neon, and vapor and neon mol ratio are 0.7;Pyrolysis temperature is protected
Hold at 600 DEG C, when a length of 20min;Sulfydryl aliphatic acid selects 3- TGAs, and it is 200 with acetic anhydride, concentrated sulfuric acid volume ratio:
140:1.5, it is technical pure;Biomass char powder a length of 15h when being stood in mixed solution, temperature is 50 DEG C.
It is real that the sulfhydryl modified biomass char prepared by embodiment 1 carries out following mercury absorption with existing common biomass char
Test:
Sulfhydryl modified biomass char and common biomass char are made into five groups of samples respectively, on ADSORPTION IN A FIXED BED experimental bench
Verify mercury adsorption features.Fixture bed experiment platform occurs system, fixed bed reactors, mercury vapourmeter etc. by simulated flue gas and constituted, wherein
Simulated flue gas is made up of high pure nitrogen, and simulated flue gas total flow is 2L/min.Mercury vapour is by being placed in U-shaped high-boron-silicon glass pipe
Mercury osmos tube is produced, and the mercury vapour of generation is taken out of by high pure nitrogen as carrier gas.High pure nitrogen flow is 200ml/min, remaining
For as the nitrogen of Balance Air, fixed bed entrance mercury vapour concentration see the table below.In view of sulfydryl stability, adsorption temp is no more than
80 DEG C, adsorption time is 150min.The sample mercury adsorbance (amount of every gram of sample adsorption mercury) tested out is as shown in the table.
Fig. 2 is the line chart drawn based on above table, can be, it is evident that sulfhydryl modified biology by list data and the figure
The burnt mercury adsorbance of matter is higher than common biomass char, is calculated from data and understands that the former is about 1.5 times or so of the latter (different real
Test condition and measurement accuracy, data difference), show that sulfhydryl modified biomass char is stronger to the adsorption capacity of mercury.In addition, by
Figure it can also be seen that, within the specific limits, the increase of mercury vapour concentration can improve mercury adsorbance, therefore sulfhydryl modified biomass char is more applicable
In the absorption of higher mercury concentration.
Why higher to the adsorption capacity of mercury sulfhydryl modified biomass char is as demercuration adsorbent, is because its Adsorption of Mercury
Using two ways:
First, physical absorption:Biomass char prepared by the present invention is made under the mixed atmosphere of vapor and inert gas
Standby, it is possible to achieve steam activation is carried out to it while biomass char is prepared, is that will prepare and steam activation two
Process conformity is a process, can save and individually use steam activation biomass char when institute calorific requirement, and make the life of preparation
Material Jiao possesses bigger serface, and the physical absorption ability to mercury is stronger;
2nd, chemisorbed:Vapor can increase the hydroxyl quantity on biomass char surface, pass through hydroxyl and TGA
Esterification carries out complex reaction generation complex compound to carry sulfydryl (i.e. sulfhydryl modified) using sulfydryl and mercury, so as to realize pair
The chemisorbed of mercury, this is not available for existing common biomass char, and the firmness of the chemical bond of sulfydryl and mercury
Far above the Van der Waals force of physical absorption.
The process of chemical reaction is as follows:
Biomass char of the surface with hydroxyl (- OH) is (with B- (OH)nRepresent) and TGA (CH2SHCOOH) occur such as
Lower esterification (non-row reaction condition):
B-(OH)n+nCH2SHCOOH→B-(OOCCH2SH)n+nH2O;
Sulfydryl (- SH) on biomass char band is made by above-mentioned esterification, thus realize it is sulfhydryl modified, so biomass char
The content of surface hydroxyl is higher, and the sulfhydryl content on the burnt surface of the modified biomass prepared will be higher, and sulfydryl can and fire
Mercury in coal generating plant flue gas forms highly stable complex compound, reaches that mercury adsorbs purpose, the reaction equation of such as following signals (does not arrange anti-
Answer condition):
B-(OOCCH2SH)n+nHg→B-(OOCCH2SH…Hg)n。
Claims (10)
1. a kind of sulfhydryl modified biomass char demercuration adsorbent, be made up of biomass and through sulfhydryl modified biomass char.
2. a kind of preparation method of sulfhydryl modified biomass char demercuration adsorbent, step includes:
1) biomass material is dried, crushed, screen out powdered biomass;
2) powdered biomass is sent into pyrolysis oven, the pyrolysis generation biomass under the mixed atmosphere of vapor and inert gas
Jiao, then stops being passed through vapor, continues to be passed through inert gas, until biomass char is cooled to less than 100 DEG C, ground after taking-up
Into biomass char powder;
3) by sulfydryl aliphatic acid, acetic anhydride, the concentrated sulfuric acid with volume ratio (180~220):(120~150):Mixing is made in (1~2)
Solution, biomass char powder is put into the mixed solution and stood, then is washed with deionized to neutral and dry, obtains sulfydryl
Modified biomass Jiaozhuo is demercuration adsorbent.
3. preparation method according to claim 2, it is characterised in that biomass material lignocellulose-containing, including farming
Thing stalk, timber.
4. preparation method according to claim 2, it is characterised in that the particle diameter of powdered biomass is not more than 5mm.
5. preparation method according to claim 2, it is characterised in that moisture in the mixed atmosphere of vapor and inert gas
The mol ratio of son and Inert gas molecule is 0.5~1.
6. the preparation method according to claim 2 or 5, it is characterised in that inert gas includes nitrogen, rare gas.
7. preparation method according to claim 2, it is characterised in that pyrolysis temperature is 300~900 DEG C, when a length of 10~
30min。
8. preparation method according to claim 2, it is characterised in that sulfydryl aliphatic acid includes TGA, mercaptopropionic acid.
9. preparation method according to claim 2, it is characterised in that the particle diameter of biomass char powder is not more than 2mm.
10. preparation method according to claim 2, it is characterised in that when biomass char powder is stood in mixed solution
A length of 10~20h, temperature is 30~60 DEG C.
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Citations (5)
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---|---|---|---|---|
CN101474551A (en) * | 2008-12-22 | 2009-07-08 | 重庆大学 | S-loaded activated carbon for mercury removal from flue gas and preparation method thereof |
CN101985099A (en) * | 2010-11-22 | 2011-03-16 | 东南大学 | Flue gas demercuration adsorbent and preparation method thereof |
CN103252212A (en) * | 2013-04-22 | 2013-08-21 | 南京师范大学 | Biomass carbon-based flue gas demercuration adsorbent and preparation method thereof |
CN105771902A (en) * | 2016-05-27 | 2016-07-20 | 北京三聚环保新材料股份有限公司 | Preparation method and application of sulfhydryl activated carbon mercury removal agent |
CN106000317A (en) * | 2016-08-01 | 2016-10-12 | 华北电力大学(保定) | Efficient demercuration absorbent for biomass char |
-
2017
- 2017-06-16 CN CN201710455347.9A patent/CN107262041A/en active Pending
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---|---|---|---|---|
CN101474551A (en) * | 2008-12-22 | 2009-07-08 | 重庆大学 | S-loaded activated carbon for mercury removal from flue gas and preparation method thereof |
CN101985099A (en) * | 2010-11-22 | 2011-03-16 | 东南大学 | Flue gas demercuration adsorbent and preparation method thereof |
CN103252212A (en) * | 2013-04-22 | 2013-08-21 | 南京师范大学 | Biomass carbon-based flue gas demercuration adsorbent and preparation method thereof |
CN105771902A (en) * | 2016-05-27 | 2016-07-20 | 北京三聚环保新材料股份有限公司 | Preparation method and application of sulfhydryl activated carbon mercury removal agent |
CN106000317A (en) * | 2016-08-01 | 2016-10-12 | 华北电力大学(保定) | Efficient demercuration absorbent for biomass char |
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Title |
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