CN106731648B - A kind of modification of chitosan is that raw material prepares sulfur and mercury removing agent and preparation method thereof - Google Patents
A kind of modification of chitosan is that raw material prepares sulfur and mercury removing agent and preparation method thereof Download PDFInfo
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- CN106731648B CN106731648B CN201611200898.2A CN201611200898A CN106731648B CN 106731648 B CN106731648 B CN 106731648B CN 201611200898 A CN201611200898 A CN 201611200898A CN 106731648 B CN106731648 B CN 106731648B
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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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/81—Solid phase processes
- B01D53/82—Solid phase processes with stationary reactants
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- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/50—Sulfur oxides
- B01D53/508—Sulfur oxides by treating the gases with solids
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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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
- B01D53/46—Removing components of defined structure
- B01D53/64—Heavy metals or compounds thereof, e.g. mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/60—Heavy metals or heavy metal compounds
- B01D2257/602—Mercury or mercury compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The present invention relates to sulfur and mercury removing agent technical fields, especially a kind of modification of chitosan is that raw material prepares sulfur and mercury removing agent and preparation method thereof, sulfur and mercury removing agent is prepared by the way that modification of chitosan and pyrolusite are carried out mix and match, its raw material is easy to get, cost is relatively low, it can not only realize to the oxidizing sulfur dioxide in flue gas at sulfuric acid, but also the elemental mercury oxidation in flue gas can be entered in solution at ionic mercury, and it is added into modification of chitosan complex-precipitation and gets off, so that mercury ingredient is separated by filter cup, so that the content of sulfur dioxide and mercury ingredient in discharge flue gas is close to zero, so that removal efficiency reaches 98% or more.
Description
Technical field
The present invention relates to sulfur and mercury removing agent technical field, especially a kind of modification of chitosan is that raw material prepares sulfur and mercury removing agent
And preparation method thereof.
Background technique
Coal, in occupation of leading position, accounts for national non-renewable energy yield in the production of energy and consumption structure in China
70% or so.Under the so abundant environment of the coal energy, so that pattern of the power generation energy resource based on coal will maintain for a long time.
Coal-fired thermal power generation unit is occupied an leading position in China's power industry, and still, the burning of coal is along with the tight of ecological environment
Deteriorate again, so that after needing to handle coal in recent years, then it is used for thermal power plant's application, it otherwise needs to fire thermal power plant
The discharge of coal tail gas is handled, and reason is: containing a large amount of sulphur, mercury ingredient in China's coal resource, sulphur ingredient enters
After in environment, be easy to cause the generation of acid rain, mercury in the environment, enters organism, can and methyl form methyl mercury, and methyl
Mercury is with severe toxicity, it will seriously affects the metabolism of organism.
In the prior art, relatively more for the sulphur ingredient removing sulfuldioxide research during coal fire discharged, such as in power plant soot
Limestone-gypsum desulphurization system is installed, so that sulphur ingredient qualified discharge in exhanst gas outlet on exhaust pipe；And for above-mentioned dress
It sets, is but difficult to the mercury ingredient removing in flue gas, and handled using above-mentioned apparatus, a large amount of gypsum can be made to generate,
Post-processing burden is caused to increase, the sulphur ingredient of processing flue gas Hu cannot get reasonable utilization.
For this purpose, having researcher to be combined using pyrolusite, manganese carbonate is configured to ore pulp processing, so that two in pyrolusite
Manganese oxide carries out catalysis oxidation to sulfur dioxide and Elemental Mercury, so that the sulfur dioxide in flue gas can be realized qualified discharge；
Simultaneously it is also possible that Elemental Mercury therein is converted to ionic mercury enters in ore pulp, so that realizing desulfuration demercuration；Also have using soft
The method that manganese ore dry method carries out sulphur in removing flue gas, mercury, but ore pulp is either used, or use dry process flue gas,
It is lower for the removal efficiency of sulphur, mercury, is merely capable of realizing that sulfur removal rate reaches 70% or so, reaches 64% for the removal efficiency of mercury
Left and right still be easy to cause the pollution of environment so that still containing a large amount of sulphur, mercury ingredient in flue gas.
Based on this, and there is researcher to study sulfur and mercury removing agent, using manganese dioxide, magnetic iron oxide iron
Fe21.333O32For active constituent, by active constituent in conjunction with carrier, so that 99% or more has been reached to sulphur, mercury removal rate, still,
Since the preparation cost that magnetic iron oxide Fe21.333O32 ingredient therein is is higher, it is difficult to obtain so that industrial applications at
This is higher, it is difficult to realize industrial applications.
Summary of the invention
In order to solve the above technical problems existing in the prior art, it is raw material system that the present invention, which provides a kind of modification of chitosan,
Standby sulfur and mercury removing agent and preparation method thereof.
It is achieved particular by following technical scheme:
A kind of modification of chitosan is that raw material prepares sulfur and mercury removing agent, and material composition is modification of chitosan 1-3 in parts by weight
Part, 10-20 parts of pyrolusite, water, dosage are 3-7:1 to enable to liquid-solid ratio；Wherein modification of chitosan is using thiosemicarbazides
After mixing with chitosan according to mass ratio for 1:1.3-2.1, potassium metaperiodate is instilled, infusion volume accounts for thiosemicarbazides quality 0.3-1.1
Times, it stirs evenly.
The pyrolusite is 20-100 mesh powder.
The pyrolusite is crossed by microwave radiation processing.
The microwave radiation, radiant power 130-180W, radiated time 8-15min.
Above-mentioned modification of chitosan is that raw material prepares sulfur and mercury removing agent preparation method, comprising the following steps:
(1) pyrolusite is crushed, grind into powder, and placed it in using microwave radiation processing 8-15min, radiant power
For 130-180W, water is added, forms ore pulp；
It (2) is that 1:1.3-2.1 is mixed according to mass ratio with chitosan by thiosemicarbazides, instillation accounts for thiosemicarbazides quality 0.3-
1.1 times of potassium metaperiodate, stirs evenly, and obtains modification of chitosan；
(3) ore pulp is added in modification of chitosan, and add water adjust its liquid-solid ratio be 3-7:1 to get.
The step (1), pyrolusite are pulverized last, are added water, after being prepared into ore pulp, then are used microwave
Radiation treatment 8-15min, radiant power 130-180W.
The preparation method of the invention, step can also be according to following progress:
(1) pyrolusite is taken, is crushed, grinding, microwave radiation 8-15min, radiant power 130-180W add water, prepare mine
Slurry；
(2) it is that 1:1.3-2.1 is mixed according to mass ratio with chitosan by thiosemicarbazides, ore pulp is added, is stirred evenly, is adjusted
Whole liquid-solid ratio be 3-7:1 to get.
The potassium metaperiodate is replaced using potassium permanganate.
The modification of chitosan of the invention prepares sulfur and mercury removing agent for raw material and takes off applied to coal-fired power plant flue gas desulfurization
Mercury processing.
The coal-fired power plant flue-gas temperature is≤170 DEG C.
Compared with prior art, technical effect of the invention is embodied in:
The sulfur and mercury removing agent raw material of the invention is easy to get, and cost is relatively low, can not only realize to the titanium dioxide in flue gas
Sulphur is oxidized into sulfuric acid, but also can enter the elemental mercury oxidation in flue gas in solution at ionic mercury, and be added into modification
Chitosan complex precipitates, so that mercury ingredient is separated by filter cup, so that sulfur dioxide and mercury in discharge flue gas
The content of ingredient is close to zero, so that removal efficiency reaches 98% or more.
It is lower than 170 DEG C particularly with flue-gas temperature, removal efficiency is more more excellent, effectively avoids sulfur and mercury removing agent
Decomposition and the more defect for causing removal effect poor of steam, are preferably answered in the desulfuration demercuration field of coal-fired power plant flue gas
With.
Chitosan and the effect of thiosemicarbazides Jining are modified by the invention, so that the complexing function of modified chitosan
Enhancing, and the activity of thiosemicarbazides is more excellent, can be realized good modification, enhances the complexing function to heavy metal ion, makes
It obtains during flue gas desulfurizing and hydrargyrum-removing, can significantly reduce component content therein, but also can play in the solution
Buffer function, so that pyrolusite is in carrying out catalysis oxidation generation sulfuric acid process, pH value is stablized, and enhances to sulfur dioxide
Removing so that removal efficiency reaches 98% or more.
The preparation process of the invention is simple, and preparation energy consumption is lower, and cost is relatively low, and chitosan belongs to wadding
The native compound of solidifying effect enhances mercury ion from solution so that can be realized rapid precipitation after complexing heavy metal mercury ion
In detach so that can be realized during flue gas desulfurizing and hydrargyrum-removing and recycle manganese sulfate, reduce mercury to manganese sulfate pair
The pollution of product improves the added value of flue gas desulfurizing and hydrargyrum-removing.
Specific embodiment
It is limited below with reference to specific embodiment technical solution of the present invention is further, but claimed
Range is not only limited to made description.
In certain embodiments, the pyrolusite is 20-100 mesh powder.
In certain embodiments, the pyrolusite is crossed by microwave radiation processing.
In certain embodiments, the microwave radiation, radiant power 130-180W, radiated time 8-15min.
In certain embodiments, modification of chitosan is that raw material prepares sulfur and mercury removing agent preparation method, comprising the following steps:
(1) pyrolusite is crushed, grind into powder, and placed it in using microwave radiation processing 8-15min, radiant power
For 130-180W, water is added, forms ore pulp；
It (2) is that 1:1.3-2.1 is mixed according to mass ratio with chitosan by thiosemicarbazides, instillation accounts for thiosemicarbazides quality 0.3-
1.1 times of potassium metaperiodate, stirs evenly, and obtains modification of chitosan；
(3) ore pulp is added in modification of chitosan, and add water adjust its liquid-solid ratio be 3-7:1 to get.
In certain embodiments, the step (1), pyrolusite are pulverized last, are added water, are prepared into ore pulp
Afterwards, microwave radiation processing 8-15min, radiant power 130-180W are used then.
In certain embodiments, preparation method can also be according to following progress:
(1) pyrolusite is taken, is crushed, grinding, microwave radiation 8-15min, radiant power 130-180W add water, prepare mine
Slurry；
(2) it is that 1:1.3-2.1 is mixed according to mass ratio with chitosan by thiosemicarbazides, ore pulp is added, is stirred evenly, is adjusted
Whole liquid-solid ratio be 3-7:1 to get.
In certain embodiments, the potassium metaperiodate is replaced using potassium permanganate.
In certain embodiments, it is handled for coal-fired power plant flue gas desulfurizing and hydrargyrum-removing；Coal-fired power plant flue-gas temperature be≤
170℃。
Embodiment 1
After taking pyrolusite powder to be broken into powder, itself plus water are prepared into ore pulp, liquid-solid ratio 3:1, and be used for thermal power plant
The desulfuration demercuration of coal-fired flue-gas is handled, and the result is shown in shown in table 1.
Embodiment 2
After taking pyrolusite powder to be broken into powder, itself plus water are prepared into ore pulp, liquid-solid ratio 3:1, and using at microwave radiation
15min, radiant power 130W are managed, and is used for the desulfuration demercuration processing of coal-fired power plant flue gas, the result is shown in 1 institutes of table
Show.
Embodiment 3
After taking pyrolusite powder to be broken into powder, using microwave radiation processing 15min, radiant power 130W, by itself plus water system
For at ore pulp, liquid-solid ratio 3:1, for the desulfuration demercuration processing of coal-fired power plant flue gas, the result is shown in shown in table 1.
Embodiment 4
After taking pyrolusite powder to be broken into powder, using microwave radiation processing 8min, radiant power 180W, by itself plus water preparation
At ore pulp, liquid-solid ratio 7:1, the desulfuration demercuration for coal-fired power plant flue gas is handled, and the result is shown in shown in table 1.
Embodiment 5
It takes pyrolusite powder to be broken into powder, takes modification of chitosan, the modification of modification of chitosan is by thiosemicarbazides and chitosan
It is after 1:1.3 is mixed, to instill potassium metaperiodate, infusion volume accounts for 0.3 times of thiosemicarbazides quality, stirs evenly, and obtains according to mass ratio；
After pyrolusite powder is mixed with modification of chitosan according to mass ratio for 20:1, it is 5:1 that water, which is added, and is modulated into liquid-solid ratio, for fire
The desulfuration demercuration of power plant soot fume is handled, and the result is shown in shown in table 1.
Embodiment 6
It takes pyrolusite powder to be broken into powder, takes modification of chitosan, the modification of modification of chitosan is by thiosemicarbazides and chitosan
It is after 1:2.1 is mixed, to instill potassium metaperiodate, infusion volume accounts for 1.1 times of thiosemicarbazides quality, stirs evenly, and obtains according to mass ratio；
After pyrolusite powder is mixed with modification of chitosan according to mass ratio for 10:3, it is 6:1 that water, which is added, and is modulated into liquid-solid ratio, for fire
The desulfuration demercuration of power plant soot fume is handled, and the result is shown in shown in table 1.
Embodiment 7
It takes pyrolusite powder to be broken into powder, modification of chitosan is taken using microwave radiation processing 10min, radiant power 150W,
The modification of modification of chitosan is after mixing thiosemicarbazides for 1:1.5 according to mass ratio with chitosan, to instill potassium metaperiodate, is instilled
Amount accounts for 0.7 times of thiosemicarbazides quality, stirs evenly, and obtains；It according to mass ratio is 15:2 by pyrolusite powder and modification of chitosan
After mixing, it is 4:1 that water, which is added, and is modulated into liquid-solid ratio, and the desulfuration demercuration for coal-fired power plant flue gas is handled, and the result is shown in 1 institutes of table
Show.
Embodiment 8
It takes pyrolusite powder to be broken into powder, water is added to be prepared into ore pulp, using microwave radiation processing 13min, radiant power is
140W, takes modification of chitosan, and the modification of modification of chitosan is to mix thiosemicarbazides for 1:1.3 according to mass ratio with chitosan
Afterwards, potassium metaperiodate is instilled, infusion volume accounts for 0.7 times of thiosemicarbazides quality, stirs evenly, and obtains；By ore pulp with pyrolusite powder quality
Meter is after 13:2.5 is mixed according to mass ratio with modification of chitosan, and it is 5.5:1 that water, which is added, and is modulated into liquid-solid ratio, is fired for thermal power plant
The desulfuration demercuration of flue-gas is handled, and the result is shown in shown in table 1.
Embodiment 9
Pyrolusite is crushed, grind into powder, and placed it in using microwave radiation processing 14min, radiant power is
Water is added in 180W, forms ore pulp；Thiosemicarbazides is mixed with chitosan according to mass ratio for 1:1.7, instillation accounts for thiosemicarbazides matter
The potassium metaperiodate of 0.3 times of amount, stirs evenly, obtains modification of chitosan；Ore pulp is added to modified shell in terms of pyrolusite powder quality
In glycan, and add water adjust its liquid-solid ratio be 3:1 to get.Desulfuration demercuration for coal-fired power plant flue gas is handled, the result is shown in
Shown in table 1.
Embodiment 10
Pyrolusite is crushed, grind into powder, and placed it in using microwave radiation processing 11min, radiant power is
Water is added in 160W, forms ore pulp；Thiosemicarbazides is mixed with chitosan according to mass ratio for 1:1.9, instillation accounts for thiosemicarbazides matter
The potassium metaperiodate of 0.5 times of amount, stirs evenly, obtains modification of chitosan；Ore pulp is added to modified shell in terms of pyrolusite powder quality
In glycan, and add water adjust its liquid-solid ratio be 7:1 to get.Desulfuration demercuration for coal-fired power plant flue gas is handled, the result is shown in
Shown in table 1.
Embodiment 11
Pyrolusite is taken, is crushed, grinding, microwave radiation 9min, radiant power 180W add water, prepare ore pulp；By amino sulphur
Urea is that 1:1.3 is mixed according to mass ratio with chitosan, ore pulp is added in terms of pyrolusite powder quality, so that pyrolusite powder and shell are poly-
Sugared mass ratio be 15:2, stir evenly, adjustment liquid-solid ratio be 7:1 to get.At desulfuration demercuration for coal-fired power plant flue gas
Reason, the result is shown in shown in table 1.
Embodiment 12
Pyrolusite is taken, is crushed, grinding, microwave radiation 15min, radiant power 130W add water, prepare ore pulp；By amino
Thiocarbamide is that 1:2.1 is mixed according to mass ratio with chitosan, ore pulp is added in terms of pyrolusite powder quality, so that pyrolusite powder and shell
Glycan mass ratio be 17:2, stir evenly, adjustment liquid-solid ratio be 5:1 to get.At desulfuration demercuration for coal-fired power plant flue gas
Reason, the result is shown in shown in table 1.
Embodiment 13
Potassium metaperiodate in embodiment 10 is replaced using potassium permanganate, at the desulfuration demercuration for coal-fired power plant flue gas
Reason, the result is shown in shown in table 1.
Desulfuration demercuration efficiency rating (experiment is to carry out the test effect evaluation of simulation process in the lab):
In above-described embodiment 1-13 in the desulfuration demercuration processing for coal-fired power plant flue gas, the temperature of flue gas≤
170 DEG C, be the sulfur and mercury removing agent by above-mentioned preparation in spray-absorption device during processing, by flue gas from absorption
Tower bottom enters, and spray liquid gets off from top spray, realizes that flue gas and sulfur and mercury removing agent carry out gas-liquid contact effect, removes flue gas
In sulphur, mercury ingredient, and for each embodiment enter spray column before flue gas in sulphur, mercury composition detection, to spray-absorption
The detection of the sulphur, mercury ingredient in tower flue gas exit comments the effect of the sulfur and mercury removing agent by the comparison of removing front and back
Valence, the results are shown in Table 1:
Table 1
Modification of chitosan in the invention is only to carry out each raw material according to the proportion simply in modifying process
Be uniformly mixed, this is uniformly mixed so that interact between each ingredient, can so that after it is mixed with pyrolusite pulp
Effectively promoting the removing of the sulphur, mercury ingredient in flue gas, and each raw material is easy to get, preparation process is simple, and it is at low cost, it is applied to
Cost is relatively low in industry, and chitosan belongs to pure natural compound, is not easy to bring secondary pollution to environment.
By the data of above-mentioned table 1 show it can be seen from the invention sulfur and mercury removing agent to temperature lower than 170 DEG C
When flue gas carries out spray process, desulfuration demercuration efficiency can be effectively made to reach 98% or more.
It is elaborated although the present invention has passed through specific embodiment, this profession ordinary skill
Personnel should be understood that made on this basis without departing from any form of claims and the variation of details,
Belong to invention which is intended to be protected.
Claims (9)
1. a kind of modification of chitosan is that raw material prepares sulfur and mercury removing agent, which is characterized in that material composition is modified in parts by weight
1-3 parts of chitosan, 10-20 parts of pyrolusite, water, dosage are 3-7:1 to enable to liquid-solid ratio；Wherein modification of chitosan is to use
Thiosemicarbazides is after 1:1.3-2.1 is mixed, to instill potassium metaperiodate according to mass ratio with chitosan, and infusion volume accounts for thiosemicarbazides quality
It 0.3-1.1 times, stirs evenly；
The preparation, method the following steps are included:
(1) pyrolusite is crushed, grind into powder, and placed it in using microwave radiation processing 8-15min, radiant power is
Water is added in 130-180W, forms ore pulp；
It (2) is that 1:1.3-2.1 is mixed according to mass ratio with chitosan by thiosemicarbazides, instillation accounts for thiosemicarbazides quality 0.3-1.1
Potassium metaperiodate again, stirs evenly, obtains modification of chitosan；
(3) ore pulp is added in modification of chitosan, and add water adjust its liquid-solid ratio be 3-7:1 to get.
2. modification of chitosan as described in claim 1 is that raw material prepares sulfur and mercury removing agent, which is characterized in that the pyrolusite
For 20-100 mesh powder.
3. modification of chitosan as claimed in claim 1 or 2 is that raw material prepares sulfur and mercury removing agent, which is characterized in that described is soft
Manganese ore is crossed by microwave radiation processing.
4. modification of chitosan as claimed in claim 3 is that raw material prepares sulfur and mercury removing agent, which is characterized in that the microwave spoke
It penetrates, radiant power 130-180W, radiated time 8-15min.
5. modification of chitosan as described in claim 1 is that raw material prepares sulfur and mercury removing agent, which is characterized in that the step
(1), pyrolusite is pulverized last, adds water, after being prepared into ore pulp, then is used microwave radiation processing 8-15min, spoke
Penetrating power is 130-180W.
6. modification of chitosan as described in claim 1 is that raw material prepares sulfur and mercury removing agent, which is characterized in that the step,
It is according to following progress:
(1) pyrolusite is taken, is crushed, grinding, microwave radiation 8-15min, radiant power 130-180W add water, prepare ore pulp；
(2) it is that 1:1.3-2.1 is mixed according to mass ratio with chitosan by thiosemicarbazides, ore pulp is added, is stirred evenly, liquid is adjusted
Gu than be 3-7:1 to get.
7. modification of chitosan as described in claim 1 is that raw material prepares sulfur and mercury removing agent, which is characterized in that the periodic acid
Potassium is replaced using potassium permanganate.
8. if the described in any item modification of chitosan of claim 1-7 are that raw material prepares sulfur and mercury removing agent applied to coal-fired power plant
Flue gas desulfurizing and hydrargyrum-removing processing.
9. application as claimed in claim 8, which is characterized in that the coal-fired power plant flue-gas temperature is≤170 DEG C.
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