CN105749858A - Preparation method of carbon monoxide absorbent - Google Patents
Preparation method of carbon monoxide absorbent Download PDFInfo
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- CN105749858A CN105749858A CN201610014247.8A CN201610014247A CN105749858A CN 105749858 A CN105749858 A CN 105749858A CN 201610014247 A CN201610014247 A CN 201610014247A CN 105749858 A CN105749858 A CN 105749858A
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- molecular sieve
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- carbon monooxide
- carbon monoxide
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- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000002250 absorbent Substances 0.000 title claims abstract description 26
- 230000002745 absorbent Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910002091 carbon monoxide Inorganic materials 0.000 title abstract description 9
- 239000002808 molecular sieve Substances 0.000 claims abstract description 56
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000007789 gas Substances 0.000 claims abstract description 34
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000003463 adsorbent Substances 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 238000001994 activation Methods 0.000 claims description 9
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 8
- 230000004913 activation Effects 0.000 claims description 8
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 10
- 238000000746 purification Methods 0.000 abstract description 4
- 238000005342 ion exchange Methods 0.000 abstract description 3
- 239000013543 active substance Substances 0.000 abstract description 2
- 239000003546 flue gas Substances 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 229910021592 Copper(II) chloride Inorganic materials 0.000 abstract 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 abstract 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 230000005855 radiation Effects 0.000 abstract 1
- 238000004064 recycling Methods 0.000 abstract 1
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- 238000010521 absorption reaction Methods 0.000 description 7
- 239000012159 carrier gas Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000012065 filter cake Substances 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 238000010298 pulverizing process Methods 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000002356 single layer Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000010668 complexation reaction Methods 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005057 refrigeration Methods 0.000 description 3
- 230000002269 spontaneous effect Effects 0.000 description 3
- VMQMZMRVKUZKQL-UHFFFAOYSA-N Cu+ Chemical compound [Cu+] VMQMZMRVKUZKQL-UHFFFAOYSA-N 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000002079 cooperative effect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 206010002660 Anoxia Diseases 0.000 description 1
- 241000976983 Anoxia Species 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 108010003320 Carboxyhemoglobin Proteins 0.000 description 1
- 206010010071 Coma Diseases 0.000 description 1
- 108010054147 Hemoglobins Proteins 0.000 description 1
- 102000001554 Hemoglobins Human genes 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- 229910000805 Pig iron Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000002156 adsorbate Substances 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000007953 anoxia Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000018109 developmental process Effects 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
- 238000007598 dipping method Methods 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 235000013980 iron oxide Nutrition 0.000 description 1
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- CCEKAJIANROZEO-UHFFFAOYSA-N sulfluramid Chemical group CCNS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F CCEKAJIANROZEO-UHFFFAOYSA-N 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
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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
- B01J20/10—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
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
- B01J20/3204—Inorganic carriers, supports or substrates
-
- 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
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
- B01J20/3234—Inorganic material layers
-
- 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
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of carbon monoxide absorbent which is mainly applicable to the resource recycling of carbon monoxide in yellow phosphorus tail gas and belongs to the field of flue gas purification.The preparation method includes: using NaY type molecular sieve as the carrier to prepare CuCl2 solution, adding the molecular sieve into the CuCl2 solution, adding an appropriate amount cerium nitrate, using a microwave radiation method to perform ion exchanging on the molecular sieve, drying, and calcining the molecular sieve after the exchanging to obtain the absorbent.The absorbent needs to be reductively activated by oxygen before being used, and the used molecular sieve can be desorbed through vacuumizing or heating.The prepared absorbent is short in modification time, high in ion exchanging degree, even in active substance dispersion, high in molecular sieve catalytic activity and promising in industrial application prospect.
Description
Technical field
The preparation method that the present invention relates to a kind of absorbent for carbon monooxide, belongs to filed of flue gas purification.
Background technology
Carbon monoxide background concentration in atmosphere convection layer is about 0.1～2ppm, and this content is harmless.Due to countries in the world transportation cause, industrial and mining establishment's development, the consumption sustainable growth of the fuel such as coal and oil, the discharge capacity of carbon monoxide also increases therewith.According to incomplete statistics in 1970, whole world carbon monoxide total release reached 3.71 hundred million tons.Wherein the output of automobile exhaust gas, accounts for 2.37 hundred million tons, accounts for 64%, becomes the pollution source that urban atmosphere is day by day serious.The use of heating and tea-urn cooking stove, not only pollutes room air, has also increased the weight of the atmospheric pollution in city.Some natural disasters, such as volcano eruption, forest fire, pit blast and the Disaster Event such as earthquake, will also result in increasing of some areas carbonomonoxide concentration.Smoking will also result in carbon monoxide pollution harm.Carbon monoxide in conjunction with hemoglobin production carboxyhemoglobin, can cause human body anoxia, to such an extent as to go into a coma or dead.Need the carbon monoxide in air is processed.
CO can as gaseous fuel, it is also possible in metal smelting, and industrial conventional CO reducing iron oxides carry out manUfaCtUre of pig iron.It is also used as the unstripped gas etc. of synthesizing methanol, vinyl acetate, methyl formate.Metallurgical, chemistry, graphite electrode manufacture and household fuel gas or coal stove, vehicle exhaust all there is CO to exist.
And CO and Cu(I) complexation time formed electronics accept key, mutually promote, produce cooperative effect.Due to CO2, nitrogen, methane, hydrogen etc. will not produce above-mentioned cooperative effect with Cu (I), therefore Absorptive complex wave will not occur.Therefore, if loaded Cu (I) on the sorbent, then can to CO selective absorption, it is achieved the purification to CO.Additionally, owing to Absorptive complex wave is reversible, the bond energy of complexation is more much smaller than general covalent bond energy, therefore is conducive to the regeneration of adsorbent.Therefore Absorptive complex wave has become the Main way of CO absorption.
The main sorting method of current CO has separation by deep refrigeration, cuprammonia absorption process, membrane separation process and solid absorption partition method etc..Wherein separation by deep refrigeration recovery system and refrigeration system are complicated so that process energy consumption is high, and cuprammonia absorption method also has the shortcomings such as the CO evolution degree of purification is not high, cuprous ion is unstable.With the present invention relatively have the NA type rare earth composite adsorbent that Nanjing University of Technology makes, it uses activated carbon as carrier, by dipping, roasting, activation process molding, CO pressure-variable adsorption amount can maintain about 12.5ml/g, but the H of trace in unstripped gas2Rare earth composite adsorbent is had large effect by the existence of O, and when the mass concentration of water is only 250mg/L, the pressure-variable adsorption amount of CO reduces about 35%, and NA adsorbent is to CO2Adsorbance bigger.In Japanese Unexamined Patent Publication 2003-311148 publication, can using adsorbent as removing CO under room temperature, disclose Cu-ZSM5 type zeolite, the pre-treatment of adsorbent needs the high-temperature process under 700 degree, and under its normal temperature and pressure, CO adsorption capacity is 28ml/g, and adsorption effect is relatively low.In patent CN1035253A, use Al2O3Or Al2O3--—SiO2As carrier, contact with the mixed solution of the mantoquita in solvent and reducing agent or dispersion, then remove solvent and prepare the adsorbent absorbing CO.Its desorption performance is not good, and assimilation effect is not outstanding.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of absorbent for carbon monooxide, specifically includes following steps:
(1) NaY type molecular sieve cleaned, calcine, after being then ground to powder, cross 60 ~ 200 mesh sieves；
(2) NaY type molecular sieve powder step (1) obtained in the ratio that solid-to-liquid ratio is 1:5 ~ 1:15 is immersed in the CuCl of 1 ~ 2mol/L2In solution, then adding cerous nitrate and obtain mixed impregnant liquor, the addition of cerous nitrate is the 3% ~ 5% of molecular sieve quality；
(3) with nitrogen as protection gas, mixed impregnant liquor step (2) obtained carries out microwave exposure in microwave oven；
(4) molecular sieve that step (3) obtains is carried out sucking filtration, then by after filtration cakes torrefaction, pass into N2Adsorbent is obtained after calcining 2 ~ 4h as protection gas at 500 ~ 600 DEG C；
(5), before using, adsorbent step (4) obtained is at 300 ~ 500 DEG C of temperature, at H2With N2Mixing gas in activation 3 ~ 5h.
Preferably, calcination condition described in step of the present invention (1) is: calcine 3 ~ 5h at 300 ~ 500 DEG C.
Preferably, in step of the present invention (3), the speed that passes into of nitrogen is 300 ~ 600ml/min.
Preferably, in step of the present invention (3), the condition of microwave exposure is: react 5 ~ 7min under 450 ~ 850W.
Preferably, step of the present invention (4) drying condition is dry 10 ~ 15min in 300 ~ 400W.
Preferably, H of the present invention2With N2Volume ratio be 1:5 ~ 1:10, passing into speed is 200 ~ 500ml/min.
Principles of the invention: spontaneous Monolayer Dispersion principle refers to oxide or salt can spontaneously form Monolayer Dispersion on the surface of carrier, reason is that this Monolayer Dispersion process can make total free energy of system decline, this principle is also applied for the dispersion in molecular sieve surfaces externally and internally and hole of oxide or salt, this dispersion is the dispersion of atomic level, it can occur in molecular sieve surfaces externally and internally and hole, is a kind of fairly common thermodynamics spontaneous process.And Absorptive complex wave separation is based on the principle that can form complex bonds between adsorbate with adsorbent and realizes the technology that mixture separates.Complexation belongs to the category of weak chemical bond.Therefore, compared with traditional physical absorption utilizing Van der Waals force or electrostatic force, its active force is strong, has higher adsorptive selectivity；And with general chemistry Adsorption Phase ratio, its weak Bonding Properties makes desorption process easily via reducing pressure or raising the mode of temperature and be achieved.CO molecule can form complex with monovalence Cu, so utilizing spontaneous Monolayer Dispersion principle load monovalence Cu over a molecular sieve to can be used to CO absorption.
Beneficial effects of the present invention: the molecular sieve modified time is short, ion-exchange degree is high, and active substance dispersion is comparatively uniform, and the catalysis activity ultimately resulting in molecular sieve is higher；Energy consumption of the present invention is little, and small investment is cheap, it is easy to desorption, and adsorption efficiency is higher, has good industrial applications prospect.
Accompanying drawing explanation
Fig. 1 is the structural representation of microwave oven used by the embodiment of the present invention.
In figure: 1-nitrogen cylinder；2-mass flowmenter；3-quartz glass reactor；4-microwave generator；5-thermocouple thermometer.
Detailed description of the invention
By the examples below the present invention is described in further detail, but scope is not limited to described content.
Embodiment 1
The preparation method of absorbent for carbon monooxide described in the present embodiment, specifically includes following steps:
(1) NaY type molecular sieve is carried out, then puts into afterwards and Muffle furnace is calcined 3h at 300 DEG C, after pulverizing, cross 60 mesh sieves；
(2) NaY type molecular sieve powder step (1) obtained in the ratio that solid-to-liquid ratio is 1:5 is immersed in the CuCl of 1mol/L2In solution, then adding cerous nitrate and obtain mixed impregnant liquor, the addition of cerous nitrate is the 5% of molecular sieve quality；
(3) molecular sieve solution is put in reactor, pass into N with the speed that passes into of 300ml/min2As protection gas, carry out irradiation reaction 5min with 450W power.
(4) molecular sieve that step (3) obtains is carried out sucking filtration, then by filter cake in the reactor, after the dry 10min of 400W power, to be then placed in tube furnace and to pass into N2At 550 DEG C, calcine 3h as protection gas and obtain adsorbent；
(5), before using, molecular sieve step (4) obtained at 300 DEG C is at H2With N2Mixing gas in carry out activation 3h after obtain absorbent for carbon monooxide, H2With N2Volume ratio be 1:5, passing into speed is 200ml/min.
Taking 20g adsorbent and put in reactor, passing into the CO(carrier gas that volume fraction is 24% is Ar), use gas chromatographic measurement CO content, calculating CO, to penetrate adsorbance be 19ml/g.
Embodiment 2
The preparation method of absorbent for carbon monooxide described in the present embodiment, specifically includes following steps:
(1) NaY type molecular sieve is carried out, then puts into afterwards and Muffle furnace is calcined 3.5h at 400 DEG C, after pulverizing, cross 80 mesh sieves；
(2) NaY type molecular sieve powder step (1) obtained in the ratio that solid-to-liquid ratio is 1:8 is immersed in the CuCl of 1.2mol/L2In solution, then adding cerous nitrate and obtain mixed impregnant liquor, the addition of cerous nitrate is the 3% of molecular sieve quality；
(3) molecular sieve solution is put in reactor, pass into N with the speed that passes into of 500ml/min2As protection gas, carry out irradiation reaction 5.5min with 550W power.
(4) molecular sieve that step (3) obtains is carried out sucking filtration, then by filter cake in the reactor, after the dry 15min of 300W power, to be then placed in tube furnace and to pass into N2At 500 DEG C, calcine 3.5h as protection gas and obtain adsorbent；
(5), before using, molecular sieve step (4) obtained at 350 DEG C is at H2With N2Mixing gas in carry out activation 3.3h after obtain absorbent for carbon monooxide, H2With N2Volume ratio be 1:6, passing into speed is 300ml/min.
Taking 20g adsorbent and put in reactor, passing into the CO(carrier gas that volume fraction is 24% is Ar), use gas chromatographic measurement CO content, calculating CO, to penetrate adsorbance be 29ml/g.
Embodiment 3
The preparation method of absorbent for carbon monooxide described in the present embodiment, specifically includes following steps:
(1) NaY type molecular sieve is carried out, then puts into afterwards and Muffle furnace is calcined 3h at 350 DEG C, after pulverizing, cross 120 mesh sieves；
(2) NaY type molecular sieve powder step (1) obtained in the ratio that solid-to-liquid ratio is 1:10 is immersed in the CuCl of 1.4mol/L2In solution, then adding cerous nitrate and obtain mixed impregnant liquor, the addition of cerous nitrate is the 3.5% of molecular sieve quality；
(3) molecular sieve solution is put in reactor, pass into N with the speed that passes into of 600ml/min2As protection gas, carry out irradiation reaction 6min with 650W power.
(4) molecular sieve that step (3) obtains is carried out sucking filtration, then by filter cake in the reactor, after the dry 10min of 450W power, to be then placed in tube furnace and to pass into N2At 520 DEG C, calcine 2.5h as protection gas and obtain adsorbent；
(5), before using, molecular sieve step (4) obtained at 400 DEG C is at H2With N2Mixing gas in carry out activation 3.5h after obtain absorbent for carbon monooxide, H2With N2Volume ratio be 1:7, passing into speed is 350ml/min.
Taking 20g adsorbent and put in reactor, passing into the CO(carrier gas that volume fraction is 24% is Ar), use gas chromatographic measurement CO content, calculating CO, to penetrate adsorbance be 38ml/g.
Embodiment 4
The preparation method of absorbent for carbon monooxide described in the present embodiment, specifically includes following steps:
(1) NaY type molecular sieve is carried out, then puts into afterwards and Muffle furnace is calcined 5h at 500 DEG C, after pulverizing, cross 140 mesh sieves；
(2) NaY type molecular sieve powder step (1) obtained in the ratio that solid-to-liquid ratio is 1:12 is immersed in the CuCl of 1.6mol/L2In solution, then adding cerous nitrate and obtain mixed impregnant liquor, the addition of cerous nitrate is the 4.3% of molecular sieve quality；
(3) molecular sieve solution is put in reactor, pass into N with the speed that passes into of 400ml/min2As protection gas, carry out irradiation reaction 6.7min with 850W power.
(4) molecular sieve that step (3) obtains is carried out sucking filtration, then by filter cake in the reactor, after the dry 12min of 350W power, to be then placed in tube furnace and to pass into N2At 560 DEG C, calcine 3.5h as protection gas and obtain adsorbent；
(5), before using, molecular sieve step (4) obtained at 450 DEG C is at H2With N2Mixing gas in carry out activation 4.5h after obtain absorbent for carbon monooxide, H2With N2Volume ratio be 1:8, passing into speed is 400ml/min.
Taking 20g adsorbent and put in reactor, passing into the CO(carrier gas that volume fraction is 24% is Ar), use gas chromatographic measurement CO content, calculating CO, to penetrate adsorbance be 31ml/g.
Embodiment 5
The preparation method of absorbent for carbon monooxide described in the present embodiment, specifically includes following steps:
(1) NaY type molecular sieve is carried out, then puts into afterwards and Muffle furnace is calcined 5h at 450 DEG C, after pulverizing, cross 160 mesh sieves；
(2) NaY type molecular sieve powder step (1) obtained in the ratio that solid-to-liquid ratio is 1:14 is immersed in the CuCl of 1.8mol/L2In solution, then adding cerous nitrate and obtain mixed impregnant liquor, the addition of cerous nitrate is the 4.8% of molecular sieve quality；
(3) molecular sieve solution is put in reactor, pass into N with the speed that passes into of 450ml/min2As protection gas, carry out irradiation reaction 7min with 750W power.
(4) molecular sieve that step (3) obtains is carried out sucking filtration, then by filter cake in the reactor, after the dry 15min of 400W power, to be then placed in tube furnace and to pass into N2At 580 DEG C, calcine 4h as protection gas and obtain adsorbent；
(5), before using, molecular sieve step (4) obtained at 500 DEG C is at H2With N2Mixing gas in carry out activation 4h after obtain absorbent for carbon monooxide, H2With N2Volume ratio be 1:9, passing into speed is 450ml/min.
Taking 20g adsorbent and put in reactor, passing into the CO(carrier gas that volume fraction is 24% is Ar), use gas chromatographic measurement CO content, calculating CO, to penetrate adsorbance be 21ml/g.
Embodiment 6
The preparation method of absorbent for carbon monooxide described in the present embodiment, specifically includes following steps:
(1) NaY type molecular sieve is carried out, then puts into afterwards and Muffle furnace is calcined 5h at 300 DEG C, after pulverizing, cross 200 mesh sieves；
(2) NaY type molecular sieve powder step (1) obtained in the ratio that solid-to-liquid ratio is 1:15 is immersed in the CuCl of 2mol/L2In solution, then adding cerous nitrate and obtain mixed impregnant liquor, the addition of cerous nitrate is the 3.5% of molecular sieve quality；
(3) molecular sieve solution is put in reactor, pass into N with the speed that passes into of 550ml/min2As protection gas, carry out irradiation reaction 5.8min with 500W power.
(4) molecular sieve that step (3) obtains is carried out sucking filtration, then by filter cake in the reactor, after the dry 13min of 400W power, to be then placed in tube furnace and to pass into N2At 600 DEG C, calcine 2h as protection gas and obtain adsorbent；
(5), before using, molecular sieve step (4) obtained at 480 DEG C is at H2With N2Mixing gas in carry out activation 5h after obtain absorbent for carbon monooxide, H2With N2Volume ratio be 1:10, passing into speed is 500ml/min.
Taking 20g adsorbent and put in reactor, passing into the CO(carrier gas that volume fraction is 24% is Ar), use gas chromatographic measurement CO content, calculating CO, to penetrate adsorbance be 27ml/g.
Claims (6)
1. the preparation method of an absorbent for carbon monooxide, it is characterised in that specifically include following steps:
(1) NaY type molecular sieve cleaned, calcine, after being then ground to powder, cross 60 ~ 200 mesh sieves；
(2) NaY type molecular sieve powder step (1) obtained in the ratio that solid-to-liquid ratio is 1:5 ~ 1:15 is immersed in the CuCl of 1 ~ 2mol/L2In solution, then adding cerous nitrate and obtain mixed impregnant liquor, the addition of cerous nitrate is the 3% ~ 5% of molecular sieve quality；
(3) with nitrogen as protection gas, mixed impregnant liquor step (2) obtained carries out microwave exposure in microwave oven；
(4) molecular sieve that step (3) obtains is carried out sucking filtration, then by after filtration cakes torrefaction, pass into N2Molecular sieve after being impregnated after calcining 2 ~ 4h as protection gas at 500 ~ 600 DEG C；
(5), before using, adsorbent step (4) obtained is at 300 ~ 500 DEG C of temperature, at H2With N2Mixing gas in activation 3 ~ 5h.
2. the preparation method of absorbent for carbon monooxide according to claim 1, it is characterised in that: calcination condition described in step (1) is: calcine 3 ~ 5h at 300 ~ 500 DEG C.
3. the preparation method of absorbent for carbon monooxide according to claim 1, it is characterised in that: in step (3), the speed that passes into of nitrogen is 300 ~ 600ml/min.
4. the preparation method of absorbent for carbon monooxide according to claim 1, it is characterised in that: in step (3), the condition of microwave exposure is: react 5 ~ 7min under 450 ~ 850W.
5. the preparation method of absorbent for carbon monooxide according to claim 1, it is characterised in that: step (4) drying condition is dry 10 ~ 15min in 300 ~ 400W.
6. the preparation method of absorbent for carbon monooxide according to claim 1, it is characterised in that: H2With N2Volume ratio be 1:5 ~ 1:10, passing into speed is 200 ~ 500ml/min.
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| CN110548481A (en) * | 2019-09-09 | 2019-12-10 | 内江师范学院 | Hollow-structure CO adsorbent with nano copper salt coated by Y-type molecular sieve and preparation method and application thereof |
| CN111375373A (en) * | 2018-12-29 | 2020-07-07 | 中国石油化工股份有限公司 | Adsorbent using active carbon as carrier and preparation method thereof |
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