CN107051379A - A kind of preparation method of the modified straw charcoal biogas desulfurizer of loaded metal ion - Google Patents
A kind of preparation method of the modified straw charcoal biogas desulfurizer of loaded metal ion Download PDFInfo
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- CN107051379A CN107051379A CN201710174976.4A CN201710174976A CN107051379A CN 107051379 A CN107051379 A CN 107051379A CN 201710174976 A CN201710174976 A CN 201710174976A CN 107051379 A CN107051379 A CN 107051379A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
- C10L3/101—Removal of contaminants
- C10L3/102—Removal of contaminants of acid contaminants
- C10L3/103—Sulfur containing contaminants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
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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
- B01D2257/30—Sulfur compounds
- B01D2257/304—Hydrogen sulfide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/05—Biogas
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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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
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/20—Capture or disposal of greenhouse gases of methane
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract
A kind of preparation method of the modified straw charcoal biogas desulfurizer of loaded metal ion, belongs to marsh gas purifying field.Problem to be solved is existing biogas removing H2Desulfurized effect present in S technologies is poor, the high shortcoming of desulphurization cost.Methods described is, by dry crops stalk crushing, by sulfuric acid solution dipping to be prepared by the agricultural crop straw of crushing into charcoal, then charcoal is modified with KOH solution, finally uses modified straw charcoal and contains Mg2+、Zn2+、Cu2+、Ag+、Ni+The aqueous solution in impregnate, then in N2It is calcined in atmosphere, the modified straw charcoal biogas desulfurizer of loaded metal ion is can obtain after cooling.
Description
Technical field
The invention belongs to technical field of methane purification, more particularly to a kind of biogas desulfurizer
Technical background
The New research progress of marsh gas purifying technology is mainly reflected in the new development of desulfurization technology.Existing desulfurization technology according to
Principle can be divided into physico-chemical process desulfurization, biological oxidation process desulfurization, change energy type biological desulphurization and Electrochemistry Desulfurization method etc..Physico-chemical process takes off
Sulphur is a kind of traditional marsh gas purifying technology, and technology relative maturity, maximum shortcoming is that desulfurizer regeneration is difficult, and operating cost is high
Secondary pollution is produced with easy.Biological oxidation process desulfurization is under conditions of aerobic, will to be vulcanized by the metabolism of sulfur bacteria
Hydrogen is converted into elemental sulfur, and its advantage is not need catalyst, no chemical sludge, consume energy low, recyclable elemental sulfur, hydrogen sulfide to go
Except rate is high, but this method is higher to technological requirement, complex operation.Change the weight that energy type biological desulfurizing technology is Recent study
Point, laboratory research and practical engineering application all achieve greater advance.It is big that change energy type Biogas Biological Desulphurization Reactor is divided into two
Class：Batch reactor and flow reactor.Biological scrubber, biofilter and bio-trickling filter three in flow reactor
Class is the focus of currentization energy type biological desulphurization reactor research.The Electrochemistry in Desulfurization of biogas comes power plant tail gas, work
The desulfurization technology of industry coal gas etc., not only with equipment investment is few, operating cost is low, it is pollution-free the features such as, also hydrogen sulfide is gone
Except rate is also very high, wherein " ferric trichloride absorption-electrochemical regeneration " method is up-and-coming one kind in biogas desulfurization technology
Method.
In today of scientific development, it has been found that every all living things containing cellulose, hemicellulose and lignin
Matter, by series of process process, can produce charcoal class new material, charcoal is occurred in that immediately.The technology is abroad
Early have been widely used, the U.S. smelts extraordinary synthesis steel using sawdust, domestic heating stove burns with sawdust carbon in South Korea；Hongkong, day
Charcoal is used for the catering trades such as barbecue by sheet, Taiwan etc..
It is also at the early-stage to the research of straw biological charcoal both at home and abroad at present, the processing of main research straw biological charcoal and
Application in sewage disposal, the research applied in biogas desulfurization technology has not been reported, so research is forward-looking.This hair
Bright to start with from the structure of charcoal, research modified straw charcoal loaded metal ion is studied the effect of biogas desulfurization,
Its desulphurization mechanism is sought, theoretical foundation is provided for charcoal biogas desulfurization.Meanwhile, it is the life of inexpensive, efficient desulfurizing agent
Production provides data and supported, so the present invention has research and the double meaning used.
The content of the invention
To solve, desulfurized effect present in existing biogas desulfurization technology is poor, production cost is high lacks the purpose of the present invention
Point, and a kind of preparation method of the modified straw charcoal biogas desulfurizer of the loaded metal ion provided.
The preparation method of the modified straw charcoal biogas desulfurizer of a kind of loaded metal ion in the present invention, by following step
It is rapid to realize：
Step 1: taking stalk fragment to be added to sulfuric acid to 5mm-10mm length fragments dry crops stalk crushing
Impregnated in solution, remove sulfuric acid solution, obtain the first sediment, the first sediment is cooled to 15 DEG C -25 DEG C, that is, obtained
Straw biological carbon；
Step 2: the straw biological carbon obtained in step one is placed in KOH solution, shaken, remove KOH solution and obtain
To the second sediment, the second sediment is cleaned with distilled water, then in N2Dried under atmosphere, that is, obtain modified straw life
Thing charcoal；
Step 3: the modified straw charcoal of loaded metal ion is prepared, the modified straw obtained in step 2 is biological
Charcoal is successively containing Mg2+、Zn2+、Cu2+、Ag+、Ni+The aqueous solution in impregnate to exchange equilibrium, two kinds contain metal cation solution
Impregnate between modified straw charcoal, modified straw charcoal is subjected to drying and processing；
Step 4: the modified straw charcoal after being handled through step 3 is in N2It is calcined under atmosphere, that is, obtains carried metal
The modified straw charcoal biogas desulfurizer of ion.
The invention has the advantages that
The modified straw charcoal biogas desulfurizer for the loaded metal ion that the present invention is provided is to the H in biogas2S is inhaled
It is attached to remove, H in biogas2S removal efficiency is higher by 30% than common straw biological charcoal desulfurized effect up to 95%, is a kind of economical, high
The biogas desulfurizer technology of preparing of effect, using agricultural wastes as raw material, mitigates the pollution to environment, cost of material is low, modification
Straw biological charcoal afterwards, the more difficult identification of biological structure, has reached nanoscale, and regular, and biogas desulfurization effect increases greatly
By force, the biogas after purification may be used as motor vehicle fuel, be incorporated to natural gas grid, and biogas fuel cell generates electricity, filling storage transport etc.
High-end applications, play bigger economic value.
Brief description of the drawings
Fig. 1 schemes for undressed straw biological charcoal SEM；
Fig. 2 schemes for the modified straw charcoal SEM of loaded metal ion；
Fig. 3 is the modified straw charcoal desulfurized effect comparison diagram of untreated straw biological charcoal and loaded metal ion.
Embodiment
Embodiment one：The system of the modified straw charcoal biogas desulfurizer of loaded metal ion in present embodiment
Preparation Method is realized according to the following steps：
Step 1: taking stalk fragment to be added to sulfuric acid to 5mm-10mm length fragments dry crops stalk crushing
Impregnated in solution, remove sulfuric acid solution, obtain the first sediment, the first sediment is cooled to 15 DEG C -25 DEG C, that is, obtained
Straw biological charcoal；
Step 2: the straw biological charcoal obtained in step one is placed in KOH solution, shaken, remove KOH solution and obtain
To the second sediment, the second sediment is cleaned with distilled water, then in N2Dried under atmosphere, that is, obtain modified straw life
Thing charcoal；
Step 3: the modified straw charcoal of loaded metal ion is prepared, the modified straw obtained in step 2 is biological
Charcoal is successively containing Mg2+、Zn2+、Cu2+、Ag+、Ni+The aqueous solution in impregnate to exchange equilibrium, two kinds contain metal cation solution
Impregnate between modified straw charcoal, modified straw charcoal is subjected to drying and processing；
Step 4: the modified straw charcoal after being handled through step 3 is in N2It is calcined under atmosphere, that is, obtains carried metal
The modified straw charcoal biogas desulfurizer of ion.
Embodiment two：Different from embodiment one is：Agricultural crop straw described in step one is jade
The stalk of rice, sorghum or wheat.Other steps and parameter are identical with embodiment one
Embodiment three：Different from embodiment one or two is：Sulfuric acid solution mole in step one
Concentration is 0.1mol-0.2mol/L, and dip time is 2h-3h.Other steps and parameter are identical with embodiment one or two.
Embodiment four：Unlike one of embodiment one to three：Sulfuric acid described in step one is molten
Liquid quality is 20-40 with agricultural crop straw mass ratio:1.Other steps and parameter are identical with one of embodiment one to three.
Embodiment five：Unlike one of embodiment one to four：The quality of KOH solution in step 2
Concentration is 5%-15%, and the concussion time is 16h-24h.Other steps and parameter are identical with one of embodiment one to four.
Embodiment six：Unlike one of embodiment one to five：The second sediment is used in step 2
Distilled water is cleaned untill the pH value of filtrate is 7-8, then in N2Under atmosphere, temperature be 100 DEG C -200 DEG C at dry.Other steps
Rapid and parameter is identical with one of embodiment one to five.
Embodiment seven：Unlike one of embodiment one to six：Contain Mg described in step 32+、
Zn2+、Cu2+、Ag+、Ni+Solution respectively by Mg (Cl)2、Zn(Cl)2、Cu(Cl)2、AgNO3, NiCl solution provide.Other steps
It is identical with one of embodiment one to six with parameter.
Embodiment eight：Unlike one of embodiment one to seven：Two kinds of gold described in step 3
Progress drying and processing is in 70 DEG C of -90 DEG C of bars by modified straw charcoal between belonging to cationic solution dipping modified straw charcoal
Dried 2-4 hours under part.Other steps and parameter are identical with one of embodiment one to seven.
Embodiment nine：Unlike one of embodiment one to eight：Contain Mg described in step 32+、Zn2 +、Cu2+、Ag+、Ni+The aqueous solution mass concentration of ion is 40-50%.Other steps and parameter and embodiment one to
One of eight is identical.
Embodiment ten：Unlike one of embodiment one to nine：Sintering temperature described in step 4
For 100 DEG C -150 DEG C, roasting time is 3h-4h.Other steps and parameter are identical with one of embodiment one to nine.
Embodiment
A kind of preparation method of the modified straw biological carbon biogas desulfurizer of loaded metal ion, it is real according to the following steps
Existing：
Step one：By dry crops stalk crushing to 5mm-10mm length fragments, the addition of 500g stalks fragment is weighed
In being 0.15mol/L sulfuric acid solutions to 10L molar concentrations concentration, 2.5h is impregnated, sulfuric acid solution is removed, obtains the first sediment,
First sediment is cooled to 15 DEG C -25 DEG C, that is, obtains straw biological charcoal.
Step 2：The straw biological charcoal obtained in step one is placed in the KOH solution that mass concentration is 5%, shaken
Swing 16-24 hours, remove KOH solution and obtain the second sediment, be by the pH value that the second sediment is cleaned with distilled water to filtrate
Untill 7-8, then in N2Under atmosphere, 100 DEG C -200 DEG C of temperature dried, that is, obtain modified straw charcoal；
Step 3：
1st, prepared by mass concentration 40% and contain Mg2+、Zn2+、Cu2+、Ag+、Ni+The aqueous solution：Take Mg (Cl)294g、Zn
(Cl)2126g、Cu(Cl)2 134g、AgNO3166g, Ni Cl 92g prepare the solution respectively；
2nd, by 200 grams of addition Mg (Cl) of modified straw charcoal2In the aqueous solution impregnate 2 hours, take out straw biological charcoal in
80 DEG C dry 3 hours；
3rd, the modified straw charcoal that step 2 is treated adds Zn (Cl)2Impregnated 1.5 hours in the aqueous solution, taking-up changes
Property straw biological charcoal in 80 DEG C dry 3 hours；
4th, the modified straw charcoal that step 3 is treated adds Cu (Cl)2Impregnated in the aqueous solution and extremely exchange within 1.5 hours flat
Weighing apparatus, takes out modified straw charcoal and is dried 3 hours in 80 DEG C.
5th, the modified straw charcoal that step 4 is treated adds AgNO3Impregnated in the aqueous solution and extremely exchange within 1.5 hours flat
Weighing apparatus, takes out modified straw charcoal and is dried 3 hours in 80 DEG C.
6th, the modified straw charcoal that step 5 is treated, which is added in the NiCl aqueous solution, impregnates 1.5 hours to exchange equilibrium,
Modified straw charcoal is taken out to dry 3 hours in 80 DEG C.
Step 4: the modified straw charcoal by the treated loaded metal ion of step 3 step 6 in N2Atmosphere
In and 150 DEG C at be calcined 3 hours, cooling obtains the modified straw charcoal biogas desulfurizer of loaded metal ion.
Modified straw charcoal biogas desulfurizer electromicroscopic photograph such as Fig. 2 institutes of loaded metal ion manufactured in the present embodiment
Show, contrasted with the straw biological charcoal without any processing, undressed straw biological charcoal is as shown in figure 1, maintain jade
Biological structure before rice stalk preparation, can clearly identify the conduit and screen casing of stalk；Its surface sediment many tiny
Grain, charcoal aperture is larger, from 1 micron to 10 microns.And pass through KOH solution and contain Mg2+、Zn2+、Cu2+、Ag+、Ni+
The straw biological charcoal shape of the aqueous solution processing of ion is more in small, broken bits, and the more difficult identification of biological structure originally has reached nanoscale,
And it is regular, biogas desulfurization effect will be greatly enhanced.The modified straw of loaded metal ion manufactured in the present embodiment is given birth to
Thing charcoal biogas desulfurizer carries out contrasting as shown in Figure 3 with the straw biological charcoal desulfurized effect without any processing.
Claims (10)
1. a kind of preparation method of the modified straw charcoal biogas desulfurizer of loaded metal ion, it is characterised in that carried metal
The preparation method of the modified straw charcoal biogas desulfurizer of ion is realized according to the following steps：
Step 1: taking stalk fragment to be added to sulfuric acid solution to 5mm-10mm length fragments dry crops stalk crushing
It is middle to be impregnated, sulfuric acid solution is removed, the first sediment is obtained, the first sediment is cooled to 15 DEG C -25 DEG C, that is, obtains stalk
Biological carbon；
Step 2: the straw biological carbon obtained in step one is placed in KOH solution, shaken, remove KOH solution and obtain the
Two sediments, the second sediment are cleaned with distilled water, then in N2Dried under atmosphere, that is, obtain modified straw biological
Charcoal；
Step 3: prepare the modified straw charcoal of loaded metal ion, by the modified straw charcoal obtained in step 2 according to
It is secondary containing Mg2+、Zn2+、Cu2+、Ag+、Ni+The aqueous solution in impregnate to exchange equilibrium, two kinds containing metal cation solution impregnate
Between modified straw charcoal, modified straw charcoal is subjected to drying and processing；
Step 4: the modified straw charcoal after being handled through step 3 is in N2It is calcined under atmosphere, that is, obtains loaded metal ion
Modified straw charcoal biogas desulfurizer.
2. the preparation method of the modified straw charcoal biogas desulfurizer of loaded metal ion according to claim 1, its
It is characterised by the stalk that the agricultural crop straw described in step one is corn, sorghum or wheat.
3. the preparation method of the modified straw charcoal biogas desulfurizer of loaded metal ion according to claim 1 or 2,
It is characterized in that the sulfuric acid solution molar concentration in step one is 0.1mol/L-0.2mol/L, dip time is 2h-3h.
4. the preparation method of the modified straw charcoal biogas desulfurizer of loaded metal ion according to claim 3, its
The sulfuric acid solution quality and agricultural crop straw mass ratio being characterised by described in step one are 20-40:1.
5. the preparation method of the modified straw charcoal biogas desulfurizer of loaded metal ion according to claim 4, its
The mass concentration for being characterised by KOH solution in step 2 is 5%-15%, and the concussion time is 16h-24h.
6. the preparation method of the modified straw charcoal biogas desulfurizer of loaded metal ion according to claim 5, its
It is characterised by step 2 that the second sediment is cleaned untill the pH value of filtrate is 7-8 with distilled water, then in N2Under atmosphere, temperature
Spend to dry at 100 DEG C -200 DEG C.
7. the preparation method of the modified straw charcoal biogas desulfurizer of loaded metal ion according to claim 6, its
It is characterised by containing Mg described in step 32+、Zn2+、Cu2+、Ag+、Ni+Solution respectively by Mg (Cl)2、Zn(Cl)2、Cu
(Cl)2、AgNO3, NiCl solution provide.
8. the preparation method of the modified straw charcoal biogas desulfurizer of loaded metal ion according to claim 7, its
Progress drying and processing is between being characterised by two described in step 3 kinds of metal cation solution dipping modified straw charcoals
Modified straw charcoal is dried 2-4 hours under the conditions of 70 DEG C -90 DEG C.
9. the preparation method of the modified straw charcoal biogas desulfurizer of loaded metal ion according to claim 8, its
It is characterised by containing Mg described in step 32+、Zn2+、Cu2+、Ag+、Ni+The aqueous solution mass concentration of ion is 40-50%.
10. the preparation method of the modified straw charcoal biogas desulfurizer of loaded metal ion according to claim 9, its
It is 100 DEG C -150 DEG C to be characterised by sintering temperature described in step 4, and roasting time is 3h-4h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113244888A (en) * | 2021-05-17 | 2021-08-13 | 内蒙古工业大学 | Modified lignite-based adsorption material and preparation method and application thereof |
| CN113403346A (en) * | 2021-07-01 | 2021-09-17 | 黑龙江省农业科学院农村能源与环保研究所 | Method for producing biogas by joint anaerobic fermentation of pig farm liquid dung and corn straws treated by biochar loaded with nano zero-valent iron |
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| CN101608141A (en) * | 2009-07-16 | 2009-12-23 | 黑龙江省农业科学院农村能源研究所 | The method of producing biomass solid shaping fuel by catalytic mild carbonization |
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| CN101608141A (en) * | 2009-07-16 | 2009-12-23 | 黑龙江省农业科学院农村能源研究所 | The method of producing biomass solid shaping fuel by catalytic mild carbonization |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113244888A (en) * | 2021-05-17 | 2021-08-13 | 内蒙古工业大学 | Modified lignite-based adsorption material and preparation method and application thereof |
| CN113244888B (en) * | 2021-05-17 | 2023-10-20 | 内蒙古工业大学 | Modified brown coal-based adsorption material and preparation method and application thereof |
| CN113403346A (en) * | 2021-07-01 | 2021-09-17 | 黑龙江省农业科学院农村能源与环保研究所 | Method for producing biogas by joint anaerobic fermentation of pig farm liquid dung and corn straws treated by biochar loaded with nano zero-valent iron |
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