CN113952931A - Supported desulfurizer and preparation method and application thereof - Google Patents
Supported desulfurizer and preparation method and application thereof Download PDFInfo
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- CN113952931A CN113952931A CN202111454344.6A CN202111454344A CN113952931A CN 113952931 A CN113952931 A CN 113952931A CN 202111454344 A CN202111454344 A CN 202111454344A CN 113952931 A CN113952931 A CN 113952931A
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- desulfurizer
- furfural
- metal compound
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical group O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 claims abstract description 73
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- 238000002791 soaking Methods 0.000 claims abstract description 35
- 238000001035 drying Methods 0.000 claims abstract description 30
- 239000005539 carbonized material Substances 0.000 claims abstract description 29
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 29
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 239000004094 surface-active agent Substances 0.000 claims abstract description 20
- 150000001875 compounds Chemical class 0.000 claims abstract description 18
- 238000003763 carbonization Methods 0.000 claims abstract description 13
- 239000012744 reinforcing agent Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000012216 screening Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- 238000005470 impregnation Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 13
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 13
- 239000003945 anionic surfactant Substances 0.000 claims description 11
- 239000002736 nonionic surfactant Substances 0.000 claims description 11
- 238000010000 carbonizing Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000006477 desulfuration reaction Methods 0.000 claims description 9
- 230000023556 desulfurization Effects 0.000 claims description 9
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 8
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 230000003009 desulfurizing effect Effects 0.000 claims description 5
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 3
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 3
- 229920005610 lignin Polymers 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- 235000019698 starch Nutrition 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 2
- 238000001354 calcination Methods 0.000 claims 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims 1
- 229910052681 coesite Inorganic materials 0.000 claims 1
- 229910052906 cristobalite Inorganic materials 0.000 claims 1
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 229910052682 stishovite Inorganic materials 0.000 claims 1
- 229910052905 tridymite Inorganic materials 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000002912 waste gas Substances 0.000 abstract description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 14
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 12
- 229910052938 sodium sulfate Inorganic materials 0.000 description 11
- 235000011152 sodium sulphate Nutrition 0.000 description 11
- 239000002904 solvent Substances 0.000 description 7
- 239000003623 enhancer Substances 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 5
- 125000000373 fatty alcohol group Chemical group 0.000 description 5
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(III) nitrate Inorganic materials [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 150000002191 fatty alcohols Chemical class 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 235000013162 Cocos nucifera Nutrition 0.000 description 3
- 244000060011 Cocos nucifera Species 0.000 description 3
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 125000004434 sulfur atom Chemical group 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Inorganic materials [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 150000003568 thioethers Chemical class 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- -1 Sodium fatty alcohol Chemical class 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 235000012343 cottonseed oil Nutrition 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 235000021190 leftovers Nutrition 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002803 maceration Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28061—Surface area, e.g. B.E.T specific surface area being in the range 100-500 m2/g
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
-
- 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
-
- 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
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
Abstract
The invention discloses a supported desulfurizer as well as a preparation method and application thereof, wherein the preparation method comprises the following steps: 1) washing, screening and drying the furfural residues, and putting the furfural residues into a carbonization furnace for carbonization to obtain a furfural residue carbonized material; 2) dissolving a metal compound, a compound surfactant, a pore-increasing agent and a strength reinforcing agent in an organic solvent, and fully mixing to obtain an impregnation liquid; 3) soaking the furfural residue carbonized material in an impregnation solution, and filtering and drying to obtain a carrier loaded with an active metal compound; 4) and (3) soaking the carrier loaded with the active metal compound in a sodium hydroxide solution, filtering, drying and roasting to obtain the supported desulfurizer. The carbonized material is prepared by taking the furfural residues as the raw material, so that the furfural residues can be reasonably recycled, the pollution to the environment is eliminated, and the production cost of the desulfurizer is reduced; and the carbonized material is loaded with the activated metal, so that the method has high adsorption efficiency on sulfide in the waste gas.
Description
Technical Field
The invention relates to a desulfurizer, and particularly relates to a supported desulfurizer as well as a preparation method and application thereof.
Background
With the rapid development of global economy, a large amount of fossil fuels are being exploited. SO produced by combustion of fossil fuelsxSulfate particles have adverse effects on the environment and on human health.
Adsorption desulfurization is a technique of performing desulfurization by effectively adsorbing sulfur-containing compounds in fuel oil with an adsorbent. The advantages of adsorption desulfurization are: for low concentration SO2Has high purification efficiency, simple equipment, convenient operation and effective recovery of SO2. In recent years, activated carbon has attracted much attention as an adsorbent in desulfurization because of its advantages such as low production cost and large adsorption amount. Patent CN105126597B, CN104338435B, etc. disclose an adsorption-type desulfurizing agent using activated carbon as a carrier, but the traditional activated carbon is adopted, and the traditional activated carbon production method is easy to cause waste of coal and wood, so there is a need to find a cheap and renewable alternative material.
Although CN102500323B discloses a coconut shell activated carbon, the coconut shell activated carbon is limited due to the production area, and is not suitable for large-scale production due to high price.
The furfural residue is a biomass substance, such as biomass waste generated by hydrolyzing polypentaose component in corncobs, cornstalks, rice husks, cottonseed hulls and leftovers of agricultural and sideline product processing to produce furfural (furfural). The furfural residue as a biomass waste contains a large amount of cellulose, hemicellulose and lignin, and has good recycling value. Therefore, the furfural residues are reasonably recycled, the pollution to the environment is eliminated, and the problem to be solved is urgently needed to be solved for recycling the furfural residues.
Disclosure of Invention
Aiming at the problems in the prior art, the technical problem to be solved by the invention is to provide a supported desulfurizer, and a preparation method and application thereof.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a supported desulfurizer comprises the following steps:
1) washing, screening and drying the furfural residues, putting the furfural residues into a carbonization furnace, carbonizing the furfural residues at 350-450 ℃ for 30-45min, and cooling the furfural residues to room temperature to obtain a furfural residue carbonized material;
2) dissolving a metal compound, a compound surfactant, a pore-increasing agent and a strength reinforcing agent in an organic solvent, and fully mixing to obtain an impregnation liquid; the metal compound is selected from one or more of metal compounds of Zn, Fe, Cu, Al and Mg;
3) soaking the furfural residue carbonized material in an impregnation solution, and filtering and drying to obtain a carrier loaded with an active metal compound;
4) and (3) soaking the carrier loaded with the active metal compound in a sodium hydroxide solution, filtering, drying and roasting to obtain the supported desulfurizer.
Further, in the step 2), the compound surfactant consists of a nonionic surfactant and an anionic surfactant, and the mass ratio of the nonionic surfactant to the anionic surfactant is 1-2: 1.
further, the nonionic surfactant is fatty alcohol-polyoxyethylene ether sodium sulfate, and the anionic surfactant is selected from sodium dodecyl benzene sulfonate and/or sodium dodecyl sulfate.
After the pore-increasing agent is added, a large number of irregular pores are formed in the desulfurizer, the surface area of the desulfurizer is increased, and the adsorption capacity of gas is improved.
While the specific surface area and the pore structure of the carbonized material are kept to be increased by using the pore-increasing agent, the desulfurizing agent can be developed towards light weight, and in order to optimize the structure of the desulfurizing agent, a strength reinforcing agent SiO is introduced2And the compressive strength and the mechanical property of the desulfurizer are enhanced while the combination degree of the raw materials is improved.
Further, in step 2), the organic solvent is selected from one of methanol, ethanol, isopropanol and dimethyl sulfoxide.
Further, in the step 2), the molar ratio of the metal compound, the compound surfactant, the pore-increasing agent and the strength enhancer is 4-5: 1-2: 0.1-0.2: 0.2-0.3.
Further, in the step 3), the carbonized material is immersed in the immersion liquid for 30-40 min.
Further, in the step 4), the roasting temperature is 500-700 ℃, and the roasting time is 3-7 hours; and soaking the carrier loaded with the active metal compound in a sodium hydroxide solution for 30-40 min.
The supported desulfurizer prepared by the method.
The supported desulfurizer is applied to waste gas treatment.
Has the advantages that: compared with the prior art, the invention has the advantages that:
1) the carbonization material is prepared by taking the furfural residues as the raw material, the furfural residues can be reasonably recycled, the pollution to the environment is eliminated, waste is turned into wealth, the reutilization value is good, the production cost of the desulfurizer is greatly reduced, and the carbonization material is more favorable for large-scale production and application of the desulfurizer compared with coconut shell activated carbon.
2) The composite surfactant, the pore-increasing agent and the strength reinforcing agent are adopted, so that the specific surface area and the pore structure of the carbonized material are increased, and the mechanical strength of the carbonized material is also enhanced.
3) This application is through loading activated metal on the carbomorphism material, adsorbs the sulfur atom in the sulphide, makes it remain on the adsorbent, has very high adsorption efficiency to the sulphide in the waste gas.
Detailed Description
The invention is further described with reference to specific examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. Modifications or substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and scope of the invention. In the following examples, unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
The furfural residue used in the following examples was obtained from Tianguan Furfural chemical Co., Ltd, Shandong.
Sodium fatty alcohol polyoxyethylene ether sulfate, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate are all purchased from King Kong surfactant, Jiangsu King Kong.
Example 1
A preparation method of a supported desulfurizer comprises the following steps:
1) washing, screening and drying the furfural residues, putting the furfural residues into a carbonization furnace, carbonizing the furfural residues at 350 ℃ for 45min, and cooling the furfural residues to room temperature to obtain a furfural residue carbonized material;
2) a metal compound (ZnAc)2、Fe(NO3)3) And a compound surfactant (the nonionic surfactant is fatty alcohol polyoxyethylene ether sodium sulfate, the anionic surfactant is sodium dodecyl benzene sulfonate, and the mass ratio of the fatty alcohol polyoxyethylene ether sodium sulfate to the sodium dodecyl benzene sulfonate is 1: 1) starch as pore-increasing agent and SiO as strength enhancer2Dissolving in methanol solvent, and mixing to obtain soaking solution;
wherein the molar ratio of the metal compound, the compound surfactant, the pore-increasing agent and the strength reinforcing agent is 4: 1: 0.1: 0.2;
3) soaking the furfural residue carbonized material in the soaking solution for 30min, and filtering and drying to obtain a carrier loaded with an active metal compound;
4) and (3) soaking the carrier loaded with the active metal compound in a sodium hydroxide solution for 30min, filtering, drying, and roasting at 580 ℃ for 6h to obtain the supported desulfurizer D1.
Example 2
A preparation method of a supported desulfurizer comprises the following steps:
1) washing, screening and drying the furfural residues, putting the furfural residues into a carbonization furnace, carbonizing the furfural residues for 30min at 450 ℃, and cooling the furfural residues to room temperature to obtain a furfural residue carbonized material;
2) a metal compound (ZnAc)2、Fe(NO3)3、Mg(NO3)2) And a compound surfactant (the nonionic surfactant is fatty alcohol polyoxyethylene ether sodium sulfate, and the anionic surfactant is sodium dodecyl sulfate)And the mass ratio of the fatty alcohol-polyoxyethylene ether sodium sulfate to the lauryl sodium sulfate is 2: 1) carboxymethyl cellulose as pore-increasing agent and SiO as strength reinforcing agent2Dissolving in dimethyl sulfoxide solvent, and mixing to obtain soaking solution;
wherein the molar ratio of the metal compound to the compound surfactant to the pore-increasing agent to the strength reinforcing agent is 5: 2: 0.2: 0.3;
3) soaking the furfural residue carbonized material in the soaking solution for 35min, and filtering and drying to obtain a carrier loaded with an active metal compound;
4) and (3) soaking the carrier loaded with the active metal compound in a sodium hydroxide solution for 35min, filtering, drying, and roasting at 680 ℃ for 4h to obtain the supported desulfurizer D2.
Example 3
A preparation method of a supported desulfurizer comprises the following steps:
1) washing, screening and drying the furfural residues, putting the furfural residues into a carbonization furnace, carbonizing the furfural residues for 30min at 450 ℃, and cooling the furfural residues to room temperature to obtain a furfural residue carbonized material;
2) mixing metal compound (Cu (NO)3)2、AlCl3) And a compound surfactant (the nonionic surfactant is fatty alcohol polyoxyethylene ether sodium sulfate, the anionic surfactant is lauryl sodium sulfate, and the mass ratio of the fatty alcohol polyoxyethylene ether sodium sulfate to the lauryl sodium sulfate is 2: 1) carboxymethyl cellulose as pore-increasing agent and SiO as strength reinforcing agent2Dissolving in ethanol solvent, and mixing to obtain soaking solution;
wherein the molar ratio of the metal compound, the compound surfactant, the pore-increasing agent and the strength reinforcing agent is 4: 1: 0.1: 0.2;
3) soaking the furfural residue carbonized material in the soaking solution for 40min, and filtering and drying to obtain a carrier loaded with an active metal compound;
4) and soaking the carrier loaded with the active metal compound in a sodium hydroxide solution for 40min, filtering, drying, and roasting at 520 ℃ for 7h to obtain the supported desulfurizer D3.
Example 4
A preparation method of a supported desulfurizer comprises the following steps:
1) washing, screening and drying the furfural residues, putting the furfural residues into a carbonization furnace, carbonizing the furfural residues at 400 ℃ for 40min, and cooling the furfural residues to room temperature to obtain a furfural residue carbonized material;
2) mixing metal compound (Cu (NO)3)2、Mg(NO3)2) And a compound surfactant (the nonionic surfactant is fatty alcohol polyoxyethylene ether sodium sulfate, the anionic surfactant is sodium dodecyl benzene sulfonate, and the mass ratio of the fatty alcohol polyoxyethylene ether sodium sulfate to the sodium dodecyl benzene sulfonate is 1: 1) lignin as pore-increasing agent and SiO as strength enhancer2Dissolving in isopropanol as solvent, and mixing to obtain maceration extract;
wherein the molar ratio of the metal compound, the compound surfactant, the pore-increasing agent and the strength reinforcing agent is 4: 2: 0.2: 0.3;
3) soaking the furfural residue carbonized material in the soaking solution for 38min, and filtering and drying to obtain a carrier loaded with an active metal compound;
4) and (3) soaking the carrier loaded with the active metal compound in a sodium hydroxide solution for 38min, filtering, drying, and roasting at 640 ℃ for 5h to obtain the supported desulfurizer D4.
Comparative example 1
A preparation method of a supported desulfurizer comprises the following steps:
1) washing, screening and drying the furfural residues, putting the furfural residues into a carbonization furnace, carbonizing the furfural residues at 350 ℃ for 45min, and cooling the furfural residues to room temperature to obtain a furfural residue carbonized material;
2) a metal compound (ZnAc)2、Fe(NO3)3) Starch as pore-increasing agent and SiO as strength enhancer2Dissolving in methanol solvent, and mixing to obtain soaking solution;
wherein the molar ratio of the metal compound to the pore-increasing agent to the strength enhancer is 4: 0.1: 0.2;
3) soaking the furfural residue carbonized material in the soaking solution for 30min, and filtering and drying to obtain a carrier loaded with an active metal compound;
4) and (3) soaking the carrier loaded with the active metal compound in a sodium hydroxide solution for 30min, filtering, drying, and roasting at 580 ℃ for 6h to obtain the supported desulfurizer C1.
Comparative example 2
A preparation method of a supported desulfurizer comprises the following steps:
1) washing, screening and drying the furfural residues, putting the furfural residues into a carbonization furnace, carbonizing the furfural residues at 350 ℃ for 45min, and cooling the furfural residues to room temperature to obtain a furfural residue carbonized material;
2) a metal compound (ZnAc)2、Fe(NO3)3) And a compound surfactant (the nonionic surfactant is fatty alcohol polyoxyethylene ether sodium sulfate, the anionic surfactant is sodium dodecyl benzene sulfonate, and the mass ratio of the fatty alcohol polyoxyethylene ether sodium sulfate to the sodium dodecyl benzene sulfonate is 1: 1) dissolving in methanol solvent, and mixing to obtain soaking solution;
wherein the molar ratio of the metal compound to the compound surfactant is 4: 1;
3) soaking the furfural residue carbonized material in the soaking solution for 30min, and filtering and drying to obtain a carrier loaded with an active metal compound;
4) and (3) soaking the carrier loaded with the active metal compound in a sodium hydroxide solution for 30min, filtering, drying, and roasting at 580 ℃ for 6h to obtain the supported desulfurizer C2.
Comparative example 3
A preparation method of a supported desulfurizer comprises the following steps:
1) washing, screening and drying the furfural residues, putting the furfural residues into a carbonization furnace, carbonizing the furfural residues at 350 ℃ for 45min, and cooling the furfural residues to room temperature to obtain a furfural residue carbonized material;
2) a metal compound (ZnAc)2、Fe(NO3)3) Dissolving in methanol as solvent to obtain soaking solution;
3) soaking the furfural residue carbonized material in the soaking solution for 30min, and filtering and drying to obtain a carrier loaded with an active metal compound;
4) and (3) soaking the carrier loaded with the active metal compound in a sodium hydroxide solution for 30min, filtering, drying, and roasting at 580 ℃ for 6h to obtain the supported desulfurizer C3.
Example 5
Specific surface, mechanical strength and desulfurization rate were measured with respect to the supported desulfurization agents prepared in examples 1 to 4 and comparative examples 1 to 3, and the results are shown in table 1, and the specific test methods are as follows:
specific surface area: testing was performed with reference to GB/T19587-2004;
compressive strength: horizontally placing the sample on the center of a lower supporting plate of a microcomputer-controlled full-automatic folding testing machine, starting the testing machine, slowly contacting the upper pressure plate with the sample and starting to extrude the sample, and recording the pressure when the sample is broken.
Desulfurization degree: h2The concentration of S is 800 mu L/L, and the space velocity is 3000h-1Normal temperature and pressure.
TABLE 1
As can be seen from table 1, the desulfurizer prepared by the present application employs a compound surfactant, a pore-increasing agent and a strength enhancer, and enhances the mechanical strength while maintaining the increase of the specific surface area and pore structure of the carbonized material, and at the same time, the carbonized material is loaded with an activated metal to adsorb sulfur atoms in sulfides, so that the sulfur atoms are retained on the adsorbent, and the adsorbent has high adsorption efficiency on sulfides in waste gas.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. The preparation method of the supported desulfurizer is characterized by comprising the following steps:
1) washing, screening and drying the furfural residues, putting the furfural residues into a carbonization furnace, carbonizing the furfural residues at 350-450 ℃ for 30-45min, and cooling the furfural residues to room temperature to obtain a furfural residue carbonized material;
2) dissolving a metal compound, a compound surfactant, a pore-increasing agent and a strength reinforcing agent in an organic solvent, and fully mixing to obtain an impregnation liquid; the metal compound is selected from one or more of metal compounds of Zn, Fe, Cu, Al and Mg;
3) soaking the furfural residue carbonized material in an impregnation solution, and filtering and drying to obtain a carrier loaded with an active metal compound;
4) and (3) soaking the carrier loaded with the active metal compound in a sodium hydroxide solution, filtering, drying and roasting to obtain the supported desulfurizer.
2. The preparation method of the supported desulfurizer according to claim 1, wherein in the step 2), the compound surfactant is composed of a nonionic surfactant and an anionic surfactant, and the mass ratio of the nonionic surfactant to the anionic surfactant is 1-2: 1.
3. the method for preparing the supported desulfurizing agent according to claim 2, wherein the non-ionic surfactant is sodium fatty alcohol-polyoxyethylene ether sulfate; the anionic surfactant is selected from sodium dodecyl benzene sulfonate and/or sodium dodecyl sulfate.
4. The method for preparing the supported desulfurizer according to claim 1, wherein in step 2), the pore-increasing agent is selected from one or more of starch, lignin or carboxymethyl cellulose; the strength reinforcing agent is SiO2 。
5. The method for preparing a supported desulfurizer according to claim 1, wherein in step 2), the organic solvent is selected from one of methanol, ethanol, isopropanol and dimethyl sulfoxide.
6. The preparation method of the supported desulfurizer according to claim 1, wherein in the step 2), the molar ratio of the metal compound to the built surfactant to the pore-increasing agent to the strength-enhancing agent is 4 to 5: 1-2: 0.1-0.2: 0.2-0.3.
7. The method for preparing a supported desulfurizing agent according to claim 1, wherein in step 3), the carbonized material is immersed in the immersion liquid for 30-40 min.
8. The method for preparing a supported desulfurizer as claimed in claim 1, wherein in the step 4), the calcination temperature is 500-700 ℃ and the calcination time is 3-7 hours; and soaking the carrier loaded with the active metal compound in a sodium hydroxide solution for 30-40 min.
9. A supported desulfurization agent prepared by the process according to any one of claims 1 to 8.
10. Use of the supported desulfurization agent of claim 9 in the treatment of exhaust gas.
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