CN115350694A - Method for preparing molded acid gas adsorbent by using iron-containing waste residues and molded acid gas adsorbent prepared by using method - Google Patents
Method for preparing molded acid gas adsorbent by using iron-containing waste residues and molded acid gas adsorbent prepared by using method Download PDFInfo
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- CN115350694A CN115350694A CN202210644802.0A CN202210644802A CN115350694A CN 115350694 A CN115350694 A CN 115350694A CN 202210644802 A CN202210644802 A CN 202210644802A CN 115350694 A CN115350694 A CN 115350694A
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- containing waste
- waste residue
- iron
- adsorbent
- acid gas
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 98
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000002699 waste material Substances 0.000 title claims abstract description 82
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 40
- 239000002253 acid Substances 0.000 title claims abstract description 35
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000002893 slag Substances 0.000 claims abstract description 9
- 230000002378 acidificating effect Effects 0.000 claims abstract description 8
- 239000011148 porous material Substances 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 44
- 238000001035 drying Methods 0.000 claims description 41
- 229910052782 aluminium Inorganic materials 0.000 claims description 35
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 35
- 239000011230 binding agent Substances 0.000 claims description 33
- 229910052710 silicon Inorganic materials 0.000 claims description 31
- 239000010703 silicon Substances 0.000 claims description 31
- 238000002156 mixing Methods 0.000 claims description 30
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 23
- 238000000227 grinding Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000003513 alkali Substances 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 238000001125 extrusion Methods 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000002594 sorbent Substances 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 239000002956 ash Substances 0.000 claims description 4
- 239000010881 fly ash Substances 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000003245 coal Substances 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 244000275012 Sesbania cannabina Species 0.000 claims description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 2
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical group [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 2
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 2
- 229910052726 zirconium Inorganic materials 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 43
- 239000007789 gas Substances 0.000 abstract description 35
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 abstract description 17
- 229910000037 hydrogen sulfide Inorganic materials 0.000 abstract description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 11
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 abstract description 11
- 229910000041 hydrogen chloride Inorganic materials 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 5
- 239000002440 industrial waste Substances 0.000 abstract description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 24
- 239000011787 zinc oxide Substances 0.000 description 12
- 230000035515 penetration Effects 0.000 description 8
- 239000002808 molecular sieve Substances 0.000 description 6
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000006477 desulfuration reaction Methods 0.000 description 3
- 230000023556 desulfurization Effects 0.000 description 3
- 239000008188 pellet Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 229910052878 cordierite Inorganic materials 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000003009 desulfurizing effect Effects 0.000 description 2
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Images
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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
-
- 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
- B01J20/28014—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 form
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/20—Halogens or halogen compounds
- B01D2257/204—Inorganic halogen compounds
- B01D2257/2045—Hydrochloric acid
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/502—Carbon monoxide
-
- 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
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
Abstract
The invention discloses a method for preparing a molded acid gas adsorbent by using iron-containing waste residues and the molded acid gas adsorbent prepared by the method. The invention utilizes the industrial wastes such as the waste slag containing iron to prepare the adsorbent powder, and then the formed adsorbent with uniformly mixed components, stable effect and smooth surface is obtained by secondary forming. The prepared molded adsorbent has high strength, low density and large number of pores, the internal adsorbent can be fully contacted with acidic gases such as hydrogen sulfide, hydrogen chloride and the like, the adsorption quantity and the utilization rate of the adsorbent are improved, and the molded adsorbent has excellent adsorption capacity. The invention has the advantages of cheap and easily obtained raw materials, simple forming process, low requirement on equipment and suitability for popularization and application.
Description
Technical Field
The invention relates to an adsorbent and a preparation and forming method thereof, in particular to an acidic gas adsorbent containing silicon, aluminum and iron-containing waste residues and a preparation and forming method thereof.
Background
Hydrogen sulfide and hydrogen chloride are common acidic harmful gases, which pollute the environment and damage human health. At present, wet absorption is a common acid gas treatment method, has a good effect, is easy to corrode equipment, and also faces the problem of wastewater treatment. The dry method for removing the acid gas has the advantages of simple process, no corrosion to equipment and high adsorption selectivity, so that the method is widely researched by scholars.
The dry powdered adsorbent is difficult to be applied industrially due to the adverse factors of high pressure drop, poor mass and heat transfer performance, large diffusion resistance, low contact efficiency and the like. In order to solve these problems, it is common to form a supported adsorbent or a formed monolithic adsorbent by supporting a powder on a carrier or adding a binder. The formed adsorbent has uniform quality and high strength, compared with a load type adsorbent, the formed adsorbent has no problem that a carrier occupies an adsorption space, and the utilization rate of a product is increased.
The formed desulfurization adsorbent commonly used in the market at present is mainly two metal oxide adsorbents of ferric oxide and zinc oxide. The ferric oxide has wide raw material source and low cost, and is an excellent choice for low-precision desulfurization in the market. But the adsorption capacity and the adsorption efficiency are low, so that the method is not suitable for high-precision desulfurization application. The zinc oxide is a hydrogen sulfide adsorbent with good effect and high precision in the currently realized commercial desulfurizer, and is widely applied to removing hydrogen sulfide in raw materials such as natural gas, coal field gas, refinery gas and the like. But the application cost is higher, the bulk density of the zinc oxide is too high, the internal zinc oxide can not fully react with hydrogen sulfide gas, and the utilization rate of the zinc oxide is reduced. In recent years, experts and scholars have started to research adsorbing materials such as activated carbon, zeolite, metal organic framework and the like, but it is still difficult to research a commercial desulfurizing agent which replaces iron oxide and zinc oxide.
At present, the adsorption of low-concentration hydrogen chloride mainly adopts metal oxide adsorption, but the problem that the adsorption selectivity is low and the deep removal of hydrogen chloride cannot be achieved is mainly solved. The hydrogen chloride gas is adsorbed by scholars through molecular sieves, but the problem of too low adsorption quantity exists. How to improve the adsorption capacity and the adsorption effect at the same time and achieve the purpose of deeply removing hydrogen sulfide at low cost still needs to be researched.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects in the prior art, provide a method for preparing a formed acid gas adsorbent by using iron-containing waste residues and the formed acid gas adsorbent prepared by using the method, provide a method for preparing and forming the acid gas adsorbent containing silicon, aluminum and iron-containing waste residues, and prepare the formed acid gas adsorbent with high adsorption capacity and adsorption efficiency at low cost by using the iron-containing waste residues as raw materials through a simple forming process.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
a method for preparing a molded acid gas adsorbent by using iron-containing waste residues comprises the following steps:
(1) Pretreating aluminum-containing waste residues and silicon-containing waste residues in a liquid phase according to a certain proportion, filtering and drying to obtain a mixture A;
the aluminum content in the aluminum-containing waste residue is 30-50 wt.%, and the silicon content in the silicon-containing waste residue is 30-50 wt.%; the molar mass ratio of aluminum in the aluminum-containing waste residue to silicon in the silicon-containing waste residue is (1) - (1); the pretreatment conditions of the aluminum-containing waste residue and the silicon-containing waste residue are that water is added according to the solid-to-liquid ratio of 1; the drying temperature is not lower than 105 ℃, and the drying time is 1-2 h;
(2) Mixing the mixture A and an alkali source according to a certain proportion, and calcining to obtain a mixture B;
the mixture A and the alkali source are mixed according to the mass ratio of 2; the calcination temperature is 300-500 ℃, and the calcination time is 2-4 h;
(3) Taking iron-containing waste residues, drying, grinding and sieving to 50 meshes;
the iron mass percent content of the iron-containing waste residue is 40-60 wt.%; the drying temperature is not lower than 105 ℃, and the drying time is 2-4 h;
(4) Grinding the mixture B to 50 meshes, and mixing the mixture B with the iron-containing waste residue treated in the step (3) according to a certain proportion to obtain a mixture C;
the mass ratio of the mixture B to the iron-containing waste residue treated in the step (3) is (2);
(5) Mixing the mixture C and water according to a certain proportion, stirring, standing, stirring again, drying, grinding, and sieving to 50 meshes to obtain raw adsorbent powder;
the mixture C and water are mixed according to the solid-liquid ratio of 1; the stirring temperature is 50-70 ℃, and the stirring time is at least 2h; the standing time is 6-12 h; the re-stirring temperature is 90-150 ℃, and the re-stirring time is 6-12 h; the drying temperature is not lower than 105 ℃, and the drying time is 1-2 h;
(6) Mixing an organic binder and an inorganic binder according to a certain proportion, adjusting the pH to 6-8 by using ammonia water with the concentration of not less than 0.01mol/L, and stirring for a period of time to obtain the required mixed binder;
the mass ratio of the organic binder to the inorganic binder is 2:1 to 1:2; the stirring time is 0.5-1 h;
(7) Taking a proper amount of raw adsorbent powder, adding a proper amount of mixed binder, fully mixing for a period of time by using a mixing machine, and drying to obtain a mixture of the adsorbent and the binder;
the mass ratio of the raw adsorbent powder to the mixed binder is 4:3 to 3:4; the mixing time is 20-50 min;
(8) Placing the mixture in a hydraulic forming machine, and extruding the mixture through a strip-shaped cylindrical die according to a certain horizontal inclination angle to obtain a primary wet forming body; then placing the wet forming body in a hydraulic forming machine again for extrusion to obtain a secondary wet forming body;
the horizontal inclination angle of the hydraulic forming machine during extrusion is 30-90 degrees; the diameter phi of the cylindrical strip-shaped die is = 3-4 mm;
(9) And drying the secondary wet forming body at the temperature of not less than 105 ℃ for 1-2 h to obtain the formed acidic gas adsorbent.
Preferably, in the step (1), the aluminum-containing waste residue is at least one of aluminum ash, aluminum slag, high-alumina fly ash and aluminum sulfate waste residue; the silicon-containing waste residue is at least one of high-silicon fly ash, steel slag, coal slag and incineration ash.
Preferably, in the step (1), the molar mass ratio of aluminum in the aluminum-containing waste residue to silicon in the silicon-containing waste residue subjected to mixing is 1; the pretreatment conditions of the aluminum-containing waste residue and the silicon-containing waste residue are that water is added according to the solid-to-liquid ratio of 1; the drying temperature is 105 ℃, and the drying time is 2h.
Preferably, in the step (2), the alkali source is at least one of sodium hydroxide, aluminum hydroxide, calcium hydroxide and sodium carbonate.
Preferably, in the step (2), the mass ratio of the mixture A to the alkali source is 1; the calcination temperature is 400-500 ℃, and the calcination time is 3-4 h.
Preferably, in the step (3), the iron-containing waste residue is ferrous sulfate waste residue.
Preferably, in the step (3), the drying temperature is 105 ℃, and the drying time is 3-4 h.
Preferably, in the step (4), the mixture B and the iron-containing waste slag treated in the step (3) are mixed in a mass ratio of 2.
Preferably, in the step (5), the mixture C and water are mixed according to a solid-liquid ratio of 1; the stirring temperature is 50-60 ℃, and the stirring time is 2 hours; the standing time is 7-10 h; the re-stirring temperature is 90-110 ℃, and the re-stirring time is 8-12 h; the drying temperature is 105 ℃, and the drying time is 2h.
Preferably, in the step (6), the organic binder is at least one of sodium carboxymethyl cellulose sol, sesbania powder hydrosol, epoxy resin and glycerol, and the inorganic binder is at least one of silica sol, aluminum sol, zirconium sol and pseudo-boehmite gel.
Preferably, in the step (6), the organic binder and the inorganic binder are mixed in a mass ratio of 1:1 to 1:2; the stirring time is 0.5h.
Preferably, in the step (7), the drying temperature is not lower than 105 ℃, and the drying time is 1-2 h.
Preferably, in the step (7), the mass ratio of the raw adsorbent powder to the mixed binder is 4:3 to 1:1.
preferably, in the step (8), the horizontal inclination angle of the hydraulic molding machine during extrusion is 60 ° to 90 °; the diameter phi of the cylindrical strip-shaped die is =3mm.
Preferably, in the step (9), the secondary wet-formed body is dried at 105 ℃ for 2 hours.
The molded acid gas adsorbent is prepared by the method for preparing the molded acid gas adsorbent by using the iron-containing waste residues, and the specific surface area of the molded acid gas adsorbent is not less than 88.33m 2 Per g, pore volume of not less than 0.21cm 3 /g。
Compared with the prior art, the invention has the following obvious substantive characteristics and remarkable advantages:
1. the method takes the waste slag containing iron as the raw material to prepare the adsorbent, has low cost and simultaneously achieves the aim of preparing waste by using waste;
2. the adsorbent prepared by the invention has high strength, low density and large pore number, and the internal adsorbent can be fully contacted with acidic gases such as hydrogen sulfide, hydrogen chloride and the like, so that the adsorption capacity, the adsorption efficiency and the utilization rate of the adsorbent are improved;
3. according to the invention, through secondary extrusion forming, the formed adsorbent and the binder are mixed more uniformly, the effect is more stable, and the surface is smoother;
4. the invention has the advantages of cheap and easily obtained raw materials, simple forming process, low requirement on equipment and suitability for popularization and application.
Drawings
FIG. 1 is a pictorial representation of the shaped acid gas sorbent prepared by the method of example 1 of the present invention.
FIG. 2 is a graph showing the comparison of the hydrogen sulfide adsorption effect of the shaped adsorbents of examples 1 to 2 and the zinc oxide adsorbent of comparative example 2 according to the present invention.
FIG. 3 is a temperature programmed CO desorption curve before and after adsorption in examples 1 and 2 of the present invention.
Detailed Description
To make the objects, technical solutions and advantages of the present invention clearer, the following detailed descriptions of implementation procedures and beneficial effects of the present invention through specific examples are intended to help readers to better understand the essence and features of the present invention, and are not intended to limit the implementable scope of the present invention.
The above-described embodiments are further illustrated below with reference to specific examples, in which preferred embodiments of the invention are detailed below:
example 1
In this embodiment, a method for preparing a shaped acid gas adsorbent from iron-containing waste residue includes the following steps:
(1) The mass percent of aluminum in the aluminum-containing waste residue is 45wt.%, and the mass percent of silicon in the silicon-containing waste residue is 48wt.%; fully mixing aluminum-containing waste residues and silicon-containing waste residues in a liquid phase according to the molar mass ratio of 1;
(2) Mixing the mixture A and an alkali source according to the proportion of 1;
(3) Taking iron-containing waste residues with the iron content of 52wt.%, drying at 105 ℃ for 2h, grinding, and sieving to 50 meshes;
(4) Grinding the mixture B to 50 meshes, and mixing the mixture B with the iron-containing waste residue treated in the step (3) according to a ratio of 1;
(5) Mixing the mixture C and water according to a solid-to-liquid ratio of 1;
(6) Mixing an organic binder and an inorganic binder according to a ratio of 1;
(7) Adding raw adsorbent powder and a mixed binder according to the mass ratio of 1; fully mixing for 30min by using a mixing machine to obtain a mixture of the adsorbent and the binder;
(8) Placing the mixture in a hydraulic forming machine, and extruding the mixture through a cylindrical die with phi =4mm according to a horizontal inclination angle of 60 degrees to obtain a primary wet forming body; then placing the wet forming body in a hydraulic forming machine again for extrusion to obtain a secondary wet forming body;
(9) And drying the secondary wet forming body for 2 hours at the temperature of not less than 105 ℃ to obtain the formed acid gas adsorbent.
The shaped acid gas sorbent prepared in this example is shown in figure 1.
Example 2
This embodiment is substantially the same as embodiment 1, and is characterized in that:
in this embodiment, a method for preparing a shaped acidic gas adsorbent from iron-containing waste residues includes the following steps:
(1) The mass percent of aluminum in the aluminum-containing waste residue is 45wt.%, and the mass percent of silicon in the silicon-containing waste residue is 41wt.%; fully mixing aluminum-containing waste residues and silicon-containing waste residues in a liquid phase according to the molar mass ratio of 1;
(2) Mixing the mixture A and an alkali source according to the proportion of 2;
(3) Taking iron-containing waste residue with iron content of 52wt.%, drying at 105 deg.C for 2h, grinding, and sieving to 50 mesh;
(4) Grinding the mixture B to 50 meshes, and mixing the mixture B with the iron-containing waste residue treated in the step (3) according to a ratio of 3;
(5) Mixing the mixture C and water according to a solid-liquid ratio of 1 to 6, stirring at 50 ℃ for 2h, standing for 7h, stirring again for 8h, drying at 105 ℃ for 2h, grinding, and sieving to 50 meshes to obtain adsorbent raw powder;
(6) Mixing an organic binder and an inorganic binder according to a ratio of 2;
(7) Adding raw adsorbent powder and a mixed binder according to the mass ratio of 4; fully mixing for 30min by using a mixing machine to obtain a mixture of the adsorbent and the binder;
(8) Placing the mixture in a hydraulic forming machine, and extruding the mixture through a cylindrical die with phi =3mm according to a horizontal inclination angle of 60 degrees to obtain a primary wet forming body; then placing the wet forming body in a hydraulic forming machine again for extrusion to obtain a secondary wet forming body;
(9) And drying the secondary wet forming body for 2 hours at the temperature of not less than 105 ℃ to obtain the formed acid gas adsorbent.
Comparative example 1:
TABLE 1 results of testing specific surface area and pore volume before and after forming in examples 1 to 2
| Item | EXAMPLE 1 Prior to Molding | EXAMPLE 1 after Molding | EXAMPLE 2 Prior to Molding | EXAMPLE 2 after Molding |
| Specific surface area (m) 2 /g) | 98.61 | 88.87 | 96.92 | 88.33 |
| Pore volume (cm) 3 /g) | 0.22 | 0.21 | 0.22 | 0.22 |
As is clear from Table 1, the adsorbent produced by the present method showed little change in specific surface area before and after molding. For the compression resistance tests of the embodiments 1-2, the compression strength of the embodiment 2 is improved by 16 percent compared with the embodiment 1, the requirement on the strength during transportation can be completely met, and the specific surface area and the pore volume are basically kept unchanged.
Performance test
The adsorption effects of the shaped adsorbents prepared in examples 1-2 were compared with those of the shaped zinc oxide desulfurizing agent. Defining the position of the outlet end with the concentration of the hydrogen sulfide of 0.01ppm as a penetration point, and calculating the penetration time; the breakthrough capacity of the adsorbent was calculated according to the following equation:
wherein S is cap Represents the total adsorption capacity, Q, of the adsorbent H2S Represents the mass flow rate of hydrogen sulfide, m represents the mass of adsorbent used, t represents the time elapsed until saturation of adsorption is reached, C in And C out Representing the inlet and outlet hydrogen sulfide concentrations, respectively.
250g of the molded adsorbent of example 1, the molded adsorbent of example 2 and the zinc oxide adsorbent were placed in S304 stainless steel tubes having an inner diameter of 100mm and subjected to inert treatment with polytetrafluoroethylene, respectively, in a catalytic evaluation apparatus, and the bottom of the adsorbents was packed with cordierite having an outer diameter of 98 mm. The whole system was purged with nitrogen and stabilized for 30min. Hydrogen sulfide was then passed into the tube at a feed gas concentration of 6000ppm and the breakthrough time and adsorption capacity before breakthrough were calculated.
Fig. 2 is a graph of hydrogen sulfide sorption breakthrough for the shaped sorbents and the shaped zinc oxide sorbents prepared in examples 1 and 2. The adsorption experiments were carried out under the above conditions, and examples 1 and 2 exhibited excellent adsorption performance at a mass space velocity of 1.5L/min. Wherein the penetration time of the formed zinc oxide adsorbent is 80min, and the adsorption capacity before penetration is 24 mg/g; the penetration time of the formed adsorbent in the embodiment 2 can reach 290min, and the adsorption capacity before penetration is 87mg/g, which is 3-4 times of that of the zinc oxide adsorbent.
Comparative example 2:
the adsorption effects of the molded adsorbents prepared in examples 1 to 2 were compared with those of the molded Y-type molecular sieve and alumina pellets, and the point at which the concentration of hydrogen sulfide at the outlet end varied by more than 0.2ppm per minute was defined as the breakthrough point, and the breakthrough time was calculated.
250g of the molded adsorbent of example 1, the molded adsorbent of example 2, the molded Y-type molecular sieve and alumina were placed in a Teflon inert-treated S304 stainless steel tube of a catalytic evaluation apparatus having an inner diameter of 100mm, and the bottom of the adsorbent was packed with cordierite having an outer diameter of 98 mm. The whole system was purged with nitrogen and stabilized for 30min. Then the steel industrial waste gas containing 500-1000 ppm (dynamic change) of hydrogen chloride is introduced into the tube at a mass space velocity of 1.5L/min, and the adsorption efficiency before penetration and the penetration time are calculated.
TABLE 2 comparison of HCl adsorption data for the shaped adsorbents of examples 1-2 with the shaped Y-type molecular sieves and alumina pellets
| Example 1 | Example 2 | Formed Y-type molecular sieve | Alumina pellets | |
| Adsorption efficiency before breakthrough | 99.8％ | 99.8％ | 99.0％ | 95.7％ |
| Time of adsorption breakthrough | 52min | 57min | 7min | 36min |
Table 2 is a comparison of the results of the adsorption experiments, and it can be seen that the adsorption efficiency before breakthrough is higher and the breakthrough time is longer in examples 1 and 2; the adsorption efficiency of the Y-type molecular sieve and the alumina balls cannot achieve the effect of removing the hydrogen chloride with high precision, and the adsorption breakthrough time is far shorter than that of the examples 1 and 2.
Comparative example 3:
FIG. 3 is a temperature programmed CO desorption curve before and after adsorption of the adsorbents in examples 1 to 2. As can be seen from the figure, before adsorption, a large number of weakly basic sites exist at 150 ℃ to 400 ℃ and a large number of strongly basic sites exist at 600 ℃ to 700 ℃. After adsorption, the alkaline sites disappear, which indicates that the alkaline sites in the adsorbent are the key factors for generating the chemical adsorption effect. From the variation in the number of basic sites in examples 1-2, it can be seen that: with the increase of the alkaline sites, the selectivity of the adsorbent to acidic gases such as hydrogen sulfide, hydrogen chloride and the like is improved, so that the adsorbent is favorably combined with the gases and fully reacts, and the adsorption quantity is improved.
The invention discloses a preparation and forming method of an adsorbent, and particularly relates to a preparation and forming method of an acid gas adsorbent containing silicon, aluminum and iron-containing waste residues. According to the embodiment of the invention, the adsorbent powder is prepared from the industrial wastes such as the iron-containing waste residues, and the formed adsorbent with uniformly mixed components, stable effect and smooth surface is obtained through secondary forming. The formed adsorbent prepared by the embodiment has high strength, low density and large pore number, the internal adsorbent can be fully contacted with acid gases such as hydrogen sulfide, hydrogen chloride and the like, the adsorption capacity and the utilization rate of the adsorbent are improved, and the formed adsorbent has excellent adsorption capacity. The raw materials of the embodiment of the invention are cheap and easy to obtain, the forming process is simple, the requirement on equipment is not high, and the invention is suitable for popularization and use
The embodiments of the present invention have been described above with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made according to the purpose of the invention, and all changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be made in the form of equivalent substitution, so long as the invention is in accordance with the purpose of the invention, and the invention shall fall within the protection scope of the present invention as long as the technical principle and the inventive concept of the present invention are not departed from the present invention.
Claims (10)
1. A method for preparing a molded acid gas adsorbent by using iron-containing waste residues is characterized by comprising the following steps:
(1) Pretreating aluminum-containing waste residues and silicon-containing waste residues in a liquid phase according to a certain proportion, filtering and drying to obtain a mixture A;
the aluminum content in the aluminum-containing waste residue is 30-50 wt.%, and the silicon content in the silicon-containing waste residue is 30-50 wt.%; the molar mass ratio of aluminum in the aluminum-containing waste residue to silicon in the silicon-containing waste residue is 1; the pretreatment conditions of the aluminum-containing waste residue and the silicon-containing waste residue are that water is added according to the solid-liquid ratio of 1 to 3-1; the drying temperature is not lower than 105 ℃, and the drying time is 1-2 h;
(2) Mixing the mixture A and an alkali source according to a certain proportion, and calcining to obtain a mixture B;
the mixture A and the alkali source are mixed according to the mass ratio of 2; the calcination temperature is 300-500 ℃, and the calcination time is 2-4 h;
(3) Taking iron-containing waste residues, drying, grinding and sieving to 50 meshes;
the iron mass percent content of the iron-containing waste residue is 40-60 wt.%; the drying temperature is not lower than 105 ℃, and the drying time is 2-4 h;
(4) Grinding the mixture B to 50 meshes, and mixing the mixture B with the iron-containing waste residue treated in the step (3) according to a certain proportion to obtain a mixture C;
the mass ratio of the mixture B to the iron-containing waste residue treated in the step (3) is (2);
(5) Mixing the mixture C and water according to a certain proportion, stirring, standing, stirring again, drying, grinding, and sieving to 50 meshes to obtain raw adsorbent powder;
the mixture C and water are mixed according to the solid-liquid ratio of 1; the stirring temperature is 50-70 ℃, and the stirring time is at least 2h; the standing time is 6-12 h; the re-stirring temperature is 90-150 ℃, and the re-stirring time is 6-12 h; the drying temperature is not lower than 105 ℃, and the drying time is 1-2 h;
(6) Mixing an organic binder and an inorganic binder according to a certain proportion, adjusting the pH to 6-8 by using ammonia water with the concentration of not less than 0.01mol/L, and stirring for a period of time to obtain the required mixed binder;
the mass ratio of the organic binder to the inorganic binder is 2:1 to 1:2; the stirring time is 0.5-1 h;
(7) Taking a proper amount of raw adsorbent powder, adding a proper amount of mixed binder, fully mixing for a period of time by using a mixing machine, and drying to obtain a mixture of the adsorbent and the binder;
the mass ratio of the adsorbent raw powder to the mixed binder is 4:3 to 3:4; the mixing time is 20-50 min;
(8) Placing the mixture in a hydraulic forming machine, and extruding the mixture through a strip-shaped cylindrical die according to a certain horizontal inclination angle to obtain a primary wet forming body; then placing the wet forming body in a hydraulic forming machine again for extrusion to obtain a secondary wet forming body;
the horizontal inclination angle of the hydraulic forming machine during extrusion is 30-90 degrees; the diameter phi of the cylindrical strip-shaped die is = 3-4 mm;
(9) And drying the secondary wet forming body at the temperature of not less than 105 ℃ for 1-2 h to obtain the formed acidic gas adsorbent.
2. The method for preparing the molded acid gas adsorbent from the iron-containing waste residue according to claim 1, wherein: in the step (1), the aluminum-containing waste residue is at least one of aluminum ash, aluminum slag, high-alumina fly ash and aluminum sulfate waste residue; the silicon-containing waste residue is at least one of high-silicon fly ash, steel slag, coal slag and incineration ash.
3. The method for preparing the molded acid gas adsorbent from the iron-containing waste residue according to claim 1, wherein: in the step (1), the molar mass ratio of aluminum in the aluminum-containing waste residue to silicon in the silicon-containing waste residue for mixing is 1; the pretreatment conditions of the aluminum-containing waste residue and the silicon-containing waste residue are that water is added according to the solid-to-liquid ratio of 1; the drying temperature is 105 ℃, and the drying time is 2h.
4. The method for preparing the molded acid gas adsorbent by using the iron-containing waste residue according to claim 1, wherein the molding step comprises the following steps: in the step (2), the alkali source is at least one of sodium hydroxide, aluminum hydroxide, calcium hydroxide and sodium carbonate.
5. The method for preparing the molded acid gas adsorbent from the iron-containing waste residue according to claim 1, wherein: in the step (2), the mass ratio of the mixture A to the alkali source is 1; the calcination temperature is 400-500 ℃, and the calcination time is 3-4 h.
6. The method for preparing the molded acid gas adsorbent from the iron-containing waste residue according to claim 1, wherein: in the step (3), the iron-containing waste residue is ferrous sulfate waste residue.
7. The method for preparing the molded acid gas adsorbent by using the iron-containing waste residue according to claim 1, wherein the molding step comprises the following steps: in the step (3), the drying temperature is 105 ℃, and the drying time is 3-4 h.
8. The method for preparing the molded acid gas adsorbent from the iron-containing waste residue according to claim 1, wherein: in the step (6), the organic binder is at least one of sodium carboxymethylcellulose sol, sesbania powder hydrosol, epoxy resin and glycerol, and the inorganic binder is at least one of silica sol, aluminum sol, zirconium sol and pseudo-boehmite gel.
9. The method for preparing the molded acid gas adsorbent from the iron-containing waste residue according to claim 1, wherein: in the step (7), the drying temperature is not lower than 105 ℃, and the drying time is 1-2 h.
10. A shaped acid gas sorbent characterized by: the method for preparing the shaped acid gas adsorbent by using the iron-containing waste residue as claimed in claim 1, wherein the specific surface area of the shaped acid gas adsorbent is not less than 88.33m 2 Per g, pore volume is not less than 0.21cm 3 /g。
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