CN103396835B - Method for simultaneously preparing clean gaseous fuel and adsorbent by sludge - Google Patents
Method for simultaneously preparing clean gaseous fuel and adsorbent by sludge Download PDFInfo
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- CN103396835B CN103396835B CN201310273025.4A CN201310273025A CN103396835B CN 103396835 B CN103396835 B CN 103396835B CN 201310273025 A CN201310273025 A CN 201310273025A CN 103396835 B CN103396835 B CN 103396835B
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- sludge
- mud
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The invention provides a method for simultaneously preparing a clean gaseous fuel and an adsorbent by sludge, comprising the following steps of: orderly adding an iron-containing oxidizing agent and a calcium-based conditioning agent into the slurry, stirring to mix, and mechanically dehydrating to obtain dehydrated sludge; and carrying out steam gasification after crushing the dehydrated sludge, to obtain the cleaning gaseous fuel rich in H2, CO and CH4, and gasifying obtained solid products to obtain a sludge ash-based adsorbent. The method starts from sludge treatment and resource utilization, improves gasification characteristics of the sludge, raises adsorption activity of solid products, implants a composite conditioning and dehydrating process, makes the iron-containing oxidizing agent and the calcium-based conditioning agent with catalytic activity to be more uniformly distributed in sludge particles by a wet-mixing manner, raises a generation amount of the gaseous fuel and the catalytic activity of the solid products in the gasification process by the cooperative effect between the iron-containing oxidizing agent and the calcium-based conditioning agent, inhibits release of pollutants in the whole process, and implements sludge utilization with low cost, low energy consumption, low pollution and high output.
Description
Technical field
The invention belongs to specific resistance to filtration and recycling field, be specifically related to a kind of method that mud prepares clean air fuel and sorbent material simultaneously.
Background technology
Mud is the by product of sewage disposal, and its wetting ability is strong, and organic content is usually up to 40% ~ 80%, and easily corruption is smelly.In recent years, along with the newly-built and reorganization and expansion of the large quantities of sewage work in the whole nation, sludge quantity sharply increases, and directly enters environment, easily causes serious secondary pollution.If but adopt appropriate measures, mud can " be turned waste into wealth ", except completing minimizing, stabilization, innoxious solid waste process disposal target, can also realize its effective resource utilization.
At present, recycling sludge utilizes technical development rapid, wherein prepares geseous fuel and mud all effectively can be converted into high value added product by carbon-based adsorbent, therefore obtains and studies widely and approve.Chinese patent CN101775315A, CN102994152A, CN202705199U, CN202193763U, CN202881204U are all the exploitation aspects from the gasification type of furnace, improve sludge gasification efficiency.Chinese patent CN102557361A discloses a kind of sludge gasification method, will add flocculation agent, and the sludge slurry layering after acid treatment, and taking precipitate sends into gasifying reactor, causes carbonaceous material and supercritical water generating gasification to be reacted, and obtains geseous fuel.
In the preparation of sludge based sorbent material, prior art is all started with from the different activation method of exploitation, makes full use of organic matter and prepares active sludge carbon.Such as, Chinese patent CN100418621C adopts ZnCl
2solution mixes with mud, obtained wet mud carbonization sorbent material after pyrolysis, washing.Chinese patent CN101559354B, CN101537342B, CN101869825B have selected solid NaHCO respectively
3, the tensio-active agent such as cetyl trimethylammonium bromide, containing sulfydryl aqueous polyurethane emulsion as chemical activating agent, improve the activity of active sludge carbon.Municipal sludge mixes with damaged tire and aluminum oxide industry red mud by CN102728321A, CN102886247A respectively, then prepares sorbent material through processes such as follow-up dipping, carbonizations.
Prior art still open question is:
(1) mud is prepared into geseous fuel or sorbent material respectively, the organic and inorganic components in mud cannot be utilized simultaneously, realize recycling to greatest extent;
(2) in preparation process, especially carbonization, pyrolysis or gasifying stage, high temperature can make N and S in mud discharge with the form of sulfur-bearing nitrogenous gas pollutent, therefore fails to realize harmony in recycling and pollution reduction.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of high yield be provided, method that less energy-consumption, oligosaprobic mud prepare clean air fuel and sorbent material simultaneously.
In order to realize foregoing invention object, the technical scheme of the embodiment of the present invention is as follows:
Mud prepares a method for clean air fuel and sorbent material simultaneously, comprises the steps:
In sludge slurry, interpolation contains ferroxidant and calcium base conditioning agent successively, is uniformly mixed and carries out mechanical dehydration to obtain dewatered sludge;
Directly steam gasification is carried out afterwards to the dewatered sludge fragmentation obtained, obtains and be rich in H
2, CO, CH
4clean air fuel, gasification gained solid product is sludge ash base adsorbent.
Further, the described ferroxidant that contains specifically comprises the following several component by mud butt weight ratio added successively: H
2sO
4or CH
3cOOH is 0% ~ 3%; FeSO
4or Fe
2(SO
4)
3or Fe
2(S
2o
8)
3be 0.3% ~ 15%; H
2o
2be 0% ~ 3%.
Further, described calcium base conditioning agent is CaO, Ca (OH)
2, CaCO
3in one or more mixing, the consumption of described calcium base conditioning agent is 5% ~ 50% of mud butt weight.
Further, the coal dust of 30% ~ 80% of its quality is also mixed to calcium base conditioning agent.
Further, before to dewatered sludge fragmentation, also carry out heat drying in short-term to it, mummification temperature is 45 DEG C ~ 200 DEG C, and drying time is 0min ~ 30min.
Further, steam gasification temperature is 600 DEG C ~ 1000 DEG C, and steam/hydrocarbons ratio is 1.2 ~ 2.2:1.
Further, the sludge returning after fragmentation is 0.045mm ~ 5mm.
Further, described sludge slurry is municipal sludge and/or paper mill sludge and/or oily sludge, and its water ratio is 90% ~ 99%.
In general, compared with prior art, effect and Advantages found exist the above technical scheme conceived by the present invention:
Because the present invention will improve sludge gasification characteristic, improve solid product adsorption activity process implantation combined cooker dehydration.Compare physical mixed, dipping and ion-exchange; wet-mixed mode is adopted to make the material having katalysis or improve calorific value effect mix with mud granule more fully, be more evenly distributed; thus more effectively improve the factor of created gase of sludge gasification, especially produce hydrogen rate.Direct utilization remains in molysite, calcium salt (or mixture of calcium salt and coal dust) in mud cake, can also reduce medicament and running cost, realize the recycling of the mud organic matter of efficient energy-saving.
Meanwhile, the interaction of molysite, calcium salt and sludge ash matrix, effectively can improve porosity and the specific surface area of solid product, and increase Ca content, and obtained sludge based sorbent material has higher adsorption activity, realizes the high-value-use of inorganic residue.
In addition, in whole gasification, the thermochemical study product of molysite and calcium salt effectively can fix the sulphur in mud, and promotes that N in mud is to N
2transform, reduce SO
x, NO
xand the generation of precursor, the discharge of effective control polluted articles, achieves low cost, high yield, oligosaprobic sludge gasification and absorbent preparation.
Accompanying drawing explanation
Fig. 1 is the inventive method schematic flow sheet.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.In addition, if below in described each embodiment of the present invention involved technical characteristic do not form conflict each other and just can mutually combine.
The invention provides a kind of method that mud prepares clean air fuel and sorbent material simultaneously.Raw sludge slurry comprises municipal sludge, paper mill sludge and oily sludge etc., and water ratio is 90% ~ 99%.Flow process is as shown in Figure 1:
Add in sludge slurry and carry out combined cooker containing ferroxidant and calcium base conditioning agent, then adopt mechanical dehydration.After solid-liquid separation, be present in the mud cake of solid phase with the form of molysite (comprising ferrous salt), calcium salt (or mixture of calcium salt and modification coal dust) respectively containing ferroxidant and calcium base conditioning agent.
Two implementation paths are had from being dewatered to gasification:
One is, dry 5min ~ 30min at dewatered sludge being placed in 45 DEG C ~ 200 DEG C, and being then broken into particle diameter is after the mud granule of 0.045mm ~ 5mm, then carries out steam gasification.Due to through combined cooker modifying process, in mud, the existence form of moisture changes, and very easily evaporates, and therefore drying process is consuming time short, consumes energy low.
Another kind is, dewatered sludge being broken into particle diameter is after the mud granule of 0.045mm ~ 5mm, directly delivers to gasification burner.Residual water can replace partial gasification medium, reduces water vapour consumption.In addition, compare the outside water vapour added, the moisture that granule interior evaporates contacts tightr with mud carbon, gasification result is better.Moisture flash evapn at high temperature makes to produce in solid residue larger more pore texture.
Steam gasification process and absorbent preparation course synchronization, control steam/hydrocarbons ratio is 1.2 ~ 2.2:1, and temperature of reaction is 600 DEG C ~ 1000 DEG C.Remain in and be dispersed in mud granule inside containing ferroxidant and calcium base conditioning agent in mud cake, add the content of the elements such as Fe, Ca, C in mud, and work from three aspects:
In preparing gas fuel, molysite can improve the speed of reaction of sludge gasification, and CO, CH can be improved in supplementary C source
4, hydrocarbon gas output.High reactivity CaO facilitates the fracture of mud granule surface carbon hydrogen bond and carbon-carbon bond, causes macromole to resolve into small molecules, and form pore texture in particle, increases the specific surface area of mud granule.Meanwhile, the cracking of CaO energy catalytic tar
and realize catching of carbonic acid gas
make water gas shift reaction
steam gasification reacts
react with steam reforming
move right, thus effective raising synthetic gas especially hydrogen output.
In affecting performance of the adsorbent, consistent with above-mentioned principle, remaining solid product hole is flourishing and be rich in highly active calcium oxide, is particularly suitable for the absorption of sulfurous gas and removes.
In pollutant catabolic gene, between calcium salt and molysite, there is synergistic effect, react with the N in mud, thus reduce NO
xand the generation of precursor.In addition, in calcium salt and mud trace S or containing the S-phase mutual effect in ferroxidant, generate CaSO
4, CaSO
3deng, inhibit the release of sulfurous gas.
The following several component by mud butt weight ratio added successively is specifically comprised: H containing ferroxidant
2sO
4or CH
3cOOH is 0% ~ 3%; FeSO
4or Fe
2(SO
4)
3or Fe
2(S
2o
8)
3be 0.3% ~ 15%; H
2o
2be 0% ~ 3%, said components can arbitrary combination.
Described calcium base conditioning agent is CaO, Ca (OH)
2, CaCO
3in one or more mixing, the consumption of described calcium base conditioning agent is 5% ~ 50% of mud butt weight.
Now prepare the method for clean air fuel and sorbent material for concrete mud simultaneously, the present invention is further elaborated.
Embodiment 1
Get the municipal sludge that water ratio is 99%, in sludge slurry, add solid-state FeSO successively
4, throwing amount is 11% of mud butt weight, adds H after mixing
2o
2, throwing amount is 0.9% of mud butt weight, stirring reaction 15min; Add 30%CaO again as calcium base conditioning agent, mixing.
After adopting plate-and-frame filter press dehydration, gained dewatered sludge is broken into the mud granule that particle diameter is 0.5mm ~ 2mm.Directly carry out steam gasification, gasification temperature is 800 DEG C, and steam/hydrocarbons ratio is 1.2:1.
H
2, CO, CH
4output be respectively 500mL/gDS, 350mL/gDS, 63mL/gDS.
Obtained sludge ash base adsorbent BET specific surface area is 182m
2/ g, active CaO content is 34%.
Embodiment 2
Get the paper mill sludge that water ratio is 95%, in sludge slurry, add the H of 0.5% successively
2sO
4solution, 0.3% FeSO
4solution, the H of 0.6%
2o
2, stirring reaction 10min; Add the calcium base conditioning agent of 50% again, mixing.Calcium base conditioning agent is CaO, CaCO
3with the mixture of coal dust, coal dust volume is 80% of calcium base conditioning agent weight.
Adopt centrifuge dehydration, gained dewatered sludge is dried 30min at 45 DEG C, is then broken into the mud granule that particle diameter is 0.045mm ~ 0.106mm.Next, at 1000 DEG C, carry out steam gasification, steam/hydrocarbons ratio is 2.2:1.
H
2, CO, CH
4output be respectively 800mL/gDS, 890mL/gDS, 160mL/gDS.
The BET specific surface area of obtained sludge ash base adsorbent is 297m
2/ g, active CaO content is 10%.
Embodiment 3
Get the oily sludge that water ratio is 90%, in sludge slurry, add the H of 3% successively
2sO
4solution, 15% FeSO
4solution, the H of 3%
2o
2, reaction 30min; Add the Ca (OH) of 15% again
2, be uniformly mixed.
Employing belt filter press dewaters, and gained dewatered sludge is dried 5min at 200 DEG C, is then broken into the mud granule that particle diameter is 0.180mm ~ 0.250mm.Next, at 600 DEG C, carry out steam gasification, steam/hydrocarbons ratio is 1.7:1.
H
2, CO, CH
4output be respectively 280mL/gDS, 130mL/gDS, 68mL/gDS.
The BET specific surface area of obtained sludge ash base adsorbent is 101m
2/ g, active CaO content is 11%.
Embodiment 4
Get the municipal sludge that water ratio is 96%, in sludge slurry, add the CH of 0.5% successively
3cOOH solution, 8% solid-state Fe
2(SO
4)
3, the H of 1.5%
2o
2, reaction 15min; Add the CaO of 50% again, be uniformly mixed.
Employing plate-and-frame filter press dewaters, and gained dewatered sludge is broken into the mud granule that particle diameter is 2mm ~ 5mm.Next, at 1000 DEG C, carry out steam gasification, steam/hydrocarbons ratio is 1.7:1.
H
2, CO, CH
4output be respectively 550mL/gDS, 396mL/gDS, 98mL/gDS.
The BET specific surface area of obtained sludge ash base adsorbent is 269m
2/ g, active CaO content is 48%.
Embodiment 5
Get the municipal sludge that water ratio is 95%, in sludge slurry, add the FeSO of 7% successively
4solution, the H of 1.1%
2o
2, reaction 15min; Add the calcium base conditioning agent of 50% again, mixing.Calcium base conditioning agent is the mixture of CaO and coal dust, and coal dust volume is 30% of calcium base conditioning agent weight.
Employing plate-and-frame filter press dewaters, and gained dewatered sludge is dried 15min at 105 DEG C, is then broken into the mud granule that particle diameter is 0.180mm ~ 0.250mm.At 800 DEG C, carry out steam gasification, steam/hydrocarbons ratio is 1.7:1.
H
2, CO, CH
4output be respectively 306mL/gDS, 154mL/gDS, 72mL/gDS.
The BET specific surface area of obtained sludge ash base adsorbent is 136m
2/ g, active CaO content is 31%.
Embodiment 6
Get the municipal sludge that water ratio is 95%, in sludge slurry, add the solid-state FeSO of 11% successively
4, the H of 0.9%
2o
2, reaction 15min; Add the Ca (OH) of 5% again
2, mixing.
Employing plate-and-frame filter press dewaters, and gained dewatered sludge is dried 15min at 105 DEG C, is then broken into the mud granule that particle diameter is 0.180mm ~ 0.250mm.Next, at 800 DEG C, carry out steam gasification, steam/hydrocarbons ratio is 1.9:1.
H
2, CO, CH
4output be respectively 436mL/gDS, 174mL/gDS, 83mL/gDS.
The BET specific surface area of obtained sludge ash base adsorbent is 145m
2/ g, active CaO content is 1%.
Embodiment 7
Get the municipal sludge that water ratio is 94%, in sludge slurry, add the Fe of 8% successively
2(S
2o
8)
3solution, reaction 5min; Add the CaO of 35% again, be uniformly mixed.
Employing plate-and-frame filter press dewaters, and gained dewatered sludge is dried 30min at 45 DEG C, is then broken into the mud granule that particle diameter is 0.106mm ~ 0.180mm.At 1000 DEG C, carry out steam gasification, steam/hydrocarbons ratio is 1.7:1.
H
2, CO, CH
4output be respectively 663mL/gDS, 352mL/gDS, 109mL/gDS.
The BET specific surface area of obtained sludge ash base adsorbent is 268m
2/ g, active CaO content is 39%.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. mud prepares a method for clean air fuel and sorbent material simultaneously, comprises the steps:
In sludge slurry, interpolation contains ferroxidant and calcium base conditioning agent successively, is uniformly mixed and carries out mechanical dehydration to obtain dewatered sludge;
Directly steam gasification is carried out afterwards to the dewatered sludge fragmentation obtained, obtains and be rich in H
2, CO, CH
4clean air fuel, gasification gained solid product is sludge ash base adsorbent;
The described ferroxidant that contains specifically comprises the following several component by mud butt weight ratio added successively: H
2sO
4or CH
3cOOH is 0% ~ 3%; FeSO
4or Fe
2(SO
4)
3or Fe
2(S
2o
8)
3be 0.3% ~ 15%; H
2o
2be 0% ~ 3%;
Described calcium base conditioning agent is CaO, Ca (OH)
2, CaCO
3in one or more mixing, the consumption of described calcium base conditioning agent is 5% ~ 50% of mud butt weight;
Described steam gasification temperature is 600 DEG C ~ 1000 DEG C, and steam/hydrocarbons ratio is 1.2 ~ 2.2:1;
Described dewatered sludge is broken into the mud granule that particle diameter is 0.045mm ~ 5mm.
2. method according to claim 1, is characterized in that, also mixes the coal dust of 30% ~ 80% of its quality to calcium base conditioning agent.
3. method according to claim 1 and 2, is characterized in that, before to dewatered sludge fragmentation, also carry out heat drying in short-term to it, and mummification temperature is 45 DEG C ~ 200 DEG C, and drying time is 5min ~ 30min.
4. method according to claim 1 and 2, is characterized in that, described sludge slurry is municipal sludge and/or paper mill sludge and/or oily sludge, and its water ratio is 90% ~ 99%.
5. what prepare according to method described in Claims 1 to 4 any one claim is rich in H
2, CO, CH
4clean air fuel and sludge ash base adsorbent.
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|---|---|---|---|
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|---|---|---|---|
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| CN103396835B true CN103396835B (en) | 2014-12-31 |
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| CN105688805A (en) * | 2016-01-08 | 2016-06-22 | 中国环境科学研究院 | Method for synthesizing mesoporous carbon material by catalyzing sludge of urban sewage treatment plant through alkaline-earth metal method |
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| CN111269729A (en) * | 2020-02-24 | 2020-06-12 | 徐州工程学院 | Method and system for preparing biochar by co-pyrolysis of sludge and waste tires |
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| CN115261076A (en) * | 2022-08-15 | 2022-11-01 | 内蒙古大唐国际克什克腾煤制天然气有限责任公司 | Coal and organic waste cooperative gasification treatment method |
| CN115340283A (en) * | 2022-08-22 | 2022-11-15 | 中国科学院广州能源研究所 | Municipal sludge energy utilization method |
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