CN113083222A - Modified adsorbent for adsorption separation and preparation method and application thereof - Google Patents
Modified adsorbent for adsorption separation and preparation method and application thereof Download PDFInfo
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- CN113083222A CN113083222A CN202110341409.XA CN202110341409A CN113083222A CN 113083222 A CN113083222 A CN 113083222A CN 202110341409 A CN202110341409 A CN 202110341409A CN 113083222 A CN113083222 A CN 113083222A
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- isomers
- separating
- adsorbent
- modified adsorbent
- molecular sieve
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 63
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 31
- 238000000926 separation method Methods 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000002808 molecular sieve Substances 0.000 claims abstract description 35
- 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 34
- 239000003054 catalyst Substances 0.000 claims abstract description 31
- 230000004048 modification Effects 0.000 claims abstract description 12
- 238000012986 modification Methods 0.000 claims abstract description 12
- 125000003118 aryl group Chemical class 0.000 claims abstract description 7
- 150000004985 diamines Chemical class 0.000 claims abstract description 7
- 229920005862 polyol Chemical class 0.000 claims abstract description 7
- 150000003077 polyols Chemical class 0.000 claims abstract description 7
- 239000002912 waste gas Substances 0.000 claims abstract description 7
- 239000002351 wastewater Substances 0.000 claims abstract description 7
- 230000018044 dehydration Effects 0.000 claims abstract description 6
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 6
- 230000003197 catalytic effect Effects 0.000 claims abstract description 5
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 5
- 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 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims description 48
- 239000000243 solution Substances 0.000 claims description 23
- 239000002131 composite material Substances 0.000 claims description 21
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 229910052710 silicon Inorganic materials 0.000 claims description 12
- 239000010703 silicon Substances 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- 235000019353 potassium silicate Nutrition 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 10
- 239000000945 filler Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000012266 salt solution Substances 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 5
- NXXYKOUNUYWIHA-UHFFFAOYSA-N 2,6-Dimethylphenol Chemical compound CC1=CC=CC(C)=C1O NXXYKOUNUYWIHA-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 claims description 4
- 230000000274 adsorptive effect Effects 0.000 claims description 4
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- -1 inorganic acid salt Chemical class 0.000 claims description 4
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000004005 microsphere Substances 0.000 claims description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 3
- 229940015975 1,2-hexanediol Drugs 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 241000219793 Trifolium Species 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- OWBTYPJTUOEWEK-UHFFFAOYSA-N butane-2,3-diol Chemical compound CC(O)C(C)O OWBTYPJTUOEWEK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 239000010919 dye waste Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
- FHKSXSQHXQEMOK-UHFFFAOYSA-N hexane-1,2-diol Chemical compound CCCCC(O)CO FHKSXSQHXQEMOK-UHFFFAOYSA-N 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- WCVRQHFDJLLWFE-UHFFFAOYSA-N pentane-1,2-diol Chemical compound CCCC(O)CO WCVRQHFDJLLWFE-UHFFFAOYSA-N 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 229910052702 rhenium Inorganic materials 0.000 claims description 2
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims 2
- 238000006317 isomerization reaction Methods 0.000 claims 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 7
- 239000000969 carrier Substances 0.000 abstract description 3
- 238000001833 catalytic reforming Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000004811 liquid chromatography Methods 0.000 abstract description 3
- 238000005457 optimization Methods 0.000 abstract description 3
- 238000004227 thermal cracking Methods 0.000 abstract description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical class O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003208 petroleum Substances 0.000 abstract description 2
- 150000002989 phenols Chemical class 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 17
- 230000008569 process Effects 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 6
- 150000007529 inorganic bases Chemical class 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 239000005995 Aluminium silicate Substances 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 235000012211 aluminium silicate Nutrition 0.000 description 4
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 4
- 239000012670 alkaline solution Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000004323 potassium nitrate Substances 0.000 description 3
- 235000010333 potassium nitrate Nutrition 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound 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 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 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 description 2
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003889 chemical engineering Methods 0.000 description 2
- 150000001896 cresols Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- IWDCLRJOBJJRNH-UHFFFAOYSA-N p-cresol Chemical compound CC1=CC=C(O)C=C1 IWDCLRJOBJJRNH-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 229910007570 Zn-Al Inorganic materials 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 229960000892 attapulgite Drugs 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052625 palygorskite Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000036314 physical performance Effects 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005303 weighing 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
-
- 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
- B01J20/02—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
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a modified adsorbent for adsorption separation and a preparation method and application thereof, belonging to the technical field of petroleum and chemical industry. The invention is based on industrial molecular sieve or catalyst, and through modification optimization, on the premise of ensuring that the original surface microstructure is not damaged, the modified zeolite is endowed with better specific surface area, adsorption capacity, diffusivity, directional selectivity and mechanical strength. The catalyst can be widely applied to the fields of aromatic isomers, diamine isomers, phenol isomers and polyol isomers in the liquid chromatography adsorption separation technology, and further has wide applicability in the fields of adsorption dehydration, catalyst carriers, removal of organic matters in waste water and waste gas and the like, particularly cordierite honeycomb catalytic modules with higher mechanical strength requirements are mainly applied to the fields of rapid thermal cracking catalytic reforming and the like, and meanwhile, the more stable catalyst or molecular sieve adsorbent is more easily applicable to adsorption of harmful substances such as indoor formaldehyde and the like.
Description
Technical Field
The invention belongs to the technical field of petroleum and chemical engineering, and particularly relates to a modified adsorbent for adsorption separation and a preparation method and application thereof.
Background
As is well known, the excellent performance of a catalyst or a molecular sieve is widely applied in the fields of chemical industry, industrial catalysis, chemical product production and the like, however, no matter the supported catalyst or the molecular sieve is used directly or conventionally, a forming process is required, some fillers such as kaolin and attapulgite and auxiliaries such as water glass and silica sol are added in the process, the active ingredients of the catalyst or the molecular sieve are sprayed on the surface of cordierite honeycomb ceramic to prepare a regular honeycomb catalytic module, and the physical performance of the surface of the catalyst or the molecular sieve is influenced to a certain extent by the use of a large amount of fillers and auxiliaries in the process, so that the adsorption performance of the catalyst or the molecular sieve is influenced; the unreasonable proportion can not reach the expected molding requirement, and the mechanical strength is weak.
The existing literature data refers to, for example, the peak is considered, and the like, the Y zeolite is synthesized in situ by kaolin microspheres in a low liquid-solid ratio system, the chemical engineering progress is 2012,32(10): 2234-2238; refining group of Changling oil refinery institute, investigation of aging process of synthesized Y-type molecular sieve crystallization guiding agent, oil refining 1978, 22-25; wangzhen, et al, the synthesis of high-silicon Y-type molecular sieves from water glass, petrochemical, 1973,3:218-222, 230; yuan in amber, alkali treatment process research of small sphere binding phase of molecular sieve adsorbent, Yanshan petrochemical, 1992,2:78-82. adopting alkali liquor treatment mode, the problems of weak mechanical strength, reduced adsorption capacity and the like caused by adding auxiliary agent or filler can be improved, it is generally considered that after the formed catalyst or molecular sieve industrial product is calcined at the temperature of more than 550 ℃, the auxiliary agent or filler loses most of interlayer water, the formed catalyst or filler becomes amorphous containing silicon and aluminum oxide, the ratio of silicon and aluminum is close to 2, the surface filler structure can be washed away by using alkali treatment, the silicon source and the aluminum source can be separated out, the silicon source and the aluminum source can be dissolved out from the inner and outer pores of the flow-through system particles, or the corresponding silicon source and aluminum source are added, for example, Honghai Liu, etc. FCC catalyst synthesis in situ atmosphere of Y zeon Kaolin clay, 168: 163. water heating, 168: 163. under the conditions of suitable water heating, the crystal transformation is carried out on the surfaces of the catalyst or molecular sieve particles and among the catalyst or molecular sieve particles in situ to generate tree-shaped cross-linked substances, thereby enhancing the mechanical strength of the catalyst or molecular sieve particles. However, the literature also mentions that the use of an alkaline solution with too high concentration is likely to cause a serious desiliconization phenomenon, destroy the surface physical microstructure, not only does not achieve the effect of improving, but also causes the silicon-aluminum ratio to decrease, even the structure to be destroyed and collapse, and the like, while industrial molecular sieves or catalysts are often formed structures, are relatively stable and not easy to crystallize in situ, and can perform a certain modification effect by using a composite alkaline solution containing a silicon source and an aluminum source, but generally have a long crystallization time, are likely to generate P and other mixed crystals, and are not optimal process conditions.
Patent CN 111482157a discloses a method for preparing pure silicalite-3 adsorbent without adhesive, which uses silica as adhesive, pure silicalite-1 as precursor, and water vapor to synthesize pure silicalite-3 adsorbent without adhesive by gas-solid phase crystal transformation.
In the related patents at present, for example, CN111097372A, CN101497022B, CN105263616A, etc., generally aim at a specific type of catalyst or molecular sieve raw powder, a certain amount of filler is added to prepare particles with a specified shape, and then the particles are treated by alkali liquor and finally exchanged for specific metal ions, so that the whole process has certain limitations, is not convenient for wide application, and has low applicability.
Disclosure of Invention
The invention provides a modified adsorbent for adsorption separation and a preparation method thereof, and aims to solve the problems of the prior art, and the like, and particularly relates to a modified adsorbent for adsorption separation and a preparation method thereof, which are based on the prior molded catalyst or molecular sieve industrial product, and endow the modified adsorbent with high specific surface area, high adsorption capacity, easy expansibility, directional selectivity and better mechanical strength on the premise of ensuring that the prior surface microstructure is not damaged through modification optimization, and have wide practicability, low cost and high efficiency.
Can be widely applied to the fields of aromatic isomers, diamine isomers, cresol isomers and polyol isomers in the liquid chromatography adsorption separation technology, and further has wide applicability in the fields of adsorption dehydration, catalyst carriers, removal of organic matters in waste water and waste gas and the like.
The invention provides a modified adsorbent for adsorption separation, and the adsorbent prepared by the method has good mechanical strength, low ignition loss rate, good adsorption selectivity and good mass transfer diffusion performance.
A preparation method of modified adsorbent for adsorption separation comprises the following steps:
(1) purifying industrial products; putting an industrial molecular sieve into a reaction tank containing softened water, stirring at a proper temperature, cooling to room temperature, standing, filtering, and removing water-soluble impurities to obtain a primary modified adsorbent;
(2) surface modification; putting the primary modified adsorbent obtained in the step (1) into a reaction tank containing alkali solution, stirring at a proper temperature, repeatedly washing with warm water until the pH value is 9-11, and drying to obtain a secondary modified adsorbent;
(3) surface modification; putting the secondary modified adsorbent obtained in the step (2) into a reaction tank containing a soluble salt solution, stirring at a proper temperature, repeatedly washing with warm water until the pH value is 8-9, and drying to obtain an adsorbent precursor;
(4) dehydrating and activating; and (4) placing the adsorbent precursor obtained in the step (3) into a muffle furnace for roasting to obtain the modified adsorbent for adsorption separation.
Further, the industrial molecular sieves in the step (1) comprise one, two or more of NaY, 13X, ZSM-5, H beta, MCM-41, activated carbon and Zn-Al multilayer filler; preferably NaY, 13X, ZSM-5 catalyst or molecular sieve.
The shapes of the industrial molecular sieves comprise one, two or more than two of powder, particles, microspheres, strips, clovers and polygons; preferably a microspheroidal, particulate catalyst or molecular sieve.
Further, the suitable temperature in step (1) is 60-100 ℃, preferably 75 ℃; the stirring time is 5-10h, preferably 7 h; the liquid-solid ratio of the softened water to the molecular sieve is 5-15, and the optimized ratio is 12; standing for 12-24 h.
Further, the alkali solution in the step (2) includes but is not limited to one, two or more of inorganic alkali, organic alkali, silica sol, water glass and composite alkali solution; the inorganic base and the water glass are preferably used in a composite way, wherein the mass ratio of the water glass to the inorganic base is 1.1-2.3, and the water glass and the inorganic base can also be used independently.
Further, the suitable temperature is 85-100 ℃, preferably 95 ℃; the stirring time is 1-5h, preferably 2 h; the liquid-solid ratio of the alkali solution to the primary modified adsorbent is 1-5, preferably 1.4; the drying temperature is 105-120 ℃, and the drying time is 24-48 h.
Further, the mass ratio of the composite alkali liquor is SiO2:Al2O3:Na2O:H2O＝(3.2-10.5):1:(1.5-7.5):(120-260)。
The addition amount of the composite alkali liquor is 0.5-5 wt%, and the stirring time is preferably prolonged by 2-3 h.
Further, the concentration of the alkali solution is 0.2-2mol/L, and the silicon content is 0-2.5 wt%; more preferably, the concentration of the inorganic alkali is 1-1.8mol/L, the silicon content is 1-1.5 wt%, and the composite alkali liquor is added by 0.5-1.2 wt%.
Further, adding water glass, silica sol, organic alkali, inorganic alkali and composite alkali liquor in the aqueous alkali, wherein the adding sequence is sequentially organic alkali and/or inorganic alkali, water glass and/or silica sol and composite alkali liquor or not; the addition sequence of the inorganic base and the composite alkali liquor includes, but is not limited to, front and back, and can also be added in a plurality of times in batches, more preferably, the inorganic base is added after 1h of treatment, the treatment temperature is preferably between 95 and 100 ℃, and the total treatment time is preferably 4 to 5 h.
Further, the silicon source in the composite alkali liquor is selected from one, two or more than two of water glass, sodium silicate, silica sol, white carbon black, active silica, fumed silica, precipitated silica and bio-based silica, and preferably is sodium silicate, active silica and bio-based silica.
Further, the aluminum source in the composite alkali liquor is selected from one, two or more of aluminum hydroxide, pseudo-boehmite, sodium metaaluminate and aluminum sulfate, preferably pseudo-boehmite, sodium metaaluminate and aluminum sulfate.
Further, the soluble salt solution in step (3) includes, but is not limited to, one, two or more of inorganic acid salt, organic acid salt, chloride or oxide containing barium, cobalt, potassium, magnesium, calcium, gallium, rhenium, etc., preferably nitrate, halide; the suitable temperature is 65-100 ℃, preferably 80 ℃; the stirring time is 1-5h, preferably 2; the liquid-solid mass ratio of the soluble salt solution to the secondary modified adsorbent is 5-10, preferably 10; the drying temperature is 105-120 ℃, and the drying time is 24-48 h.
Further, the temperature of the roasting in the step (4) is 150-; the roasting time is 3-8h, preferably 6 h; the heating rate is 5-10K/min, and more preferably the temperature is programmed in a stepwise manner at 110 ℃ for 1.5h, 350 ℃ for 1h and 550 ℃ for 6 h.
A modified adsorbent prepared by the method for adsorption separationThe adsorption capacity and the mechanical strength of the adsorbent are improved compared with the unmodified adsorbent, and the specific surface area S is obviouslyBETAn increase of 2.5-15%, more preferably 13.07%; pore volume VtotalIncrease by 1.5-9.5%, more preferably 9.09%; mechanical Strength K130N/％、K250N/％Respectively increasing to 25-55%, 30-65%, more preferably 49.02%, 62.03%; the ignition loss is reduced by 12-30%, and more preferably 29.54%; and the exchange degree is improved by 1 to 5 percent, and is more preferably 4.81 percent.
An application of the modified adsorbent for adsorptive separation, which comprises the following 1) to 7):
1) separating the aromatic isomers;
2) separating the diamine isomers;
3) separating the phenolic isomers;
4) separating the polyol isomers;
5) a dehydration adsorbent;
6) a catalyst support;
7) and removing organic matters in the waste water and the waste gas.
Further, the separation of aromatic isomers includes separation of mixed industrial feedstocks of toluene, xylene, ethylbenzene; separating the diamine isomers comprises separating the 1, 5-pentanediamine industrial raw material; separating phenol isomers comprises separating mixed industrial raw materials such as m-cresol and p-cresol, 2, 6-dimethylphenol and the like; the separation of the polyol isomers comprises the separation of industrial raw materials such as 2, 3-butanediol, 1, 2-pentanediol, 1, 2-hexanediol and the like; the dehydration adsorbent comprises water moisture purification; the catalyst carrier comprises a cordierite honeycomb catalytic module and is suitable for the fields of rapid thermal cracking catalytic reforming and the like; the organic matter removal in the waste water and the waste gas comprises the treatment of acidic organic dye waste water and VOC, and is more preferably suitable for the adsorption of harmful substances such as indoor formaldehyde and the like.
By adopting the technical scheme, the following positive benefits can be realized:
the invention discloses a modified adsorbent for adsorption separation and a preparation method thereof, which can effectively solve the problem of the deficiency of the prior art, and particularly, based on the formed catalyst or molecular sieve industrial product, the surface adsorption capacity of the adsorbent is expanded on the premise of ensuring that the surface physical property of the original microstructure is not damaged by the modification optimization procedures of surface purification, alkali solution modification, soluble salt solution functionalization and the like, so that the adsorbent is endowed with high specific surface area and high adsorption capacity, and has directional selectivity, easy expansibility and better mechanical strength, and has wide practicability, low cost and high efficiency. Through reasonable alkali solution process collocation, the desiliconization problem caused by high-concentration alkali solution can be effectively overcome, and meanwhile, the composite alkali solution in the preparation method only needs shorter crystallization time, so that the defects of easy generation of P and other mixed crystals, influence on performance and the like due to long-time crystallization can be effectively overcome.
The catalyst can be widely applied to the fields of aromatic isomers, diamine isomers, cresol isomers and polyol isomers in the liquid chromatography adsorption separation technology, further has wide applicability in the fields of adsorption dehydration, catalyst carriers, removal of organic matters in waste water and waste gas and the like, particularly has important application in the fields of rapid thermal cracking catalytic reforming and the like for a cordierite honeycomb catalytic module with higher requirement on mechanical strength, and is more stable and high in adsorption capacity for catalysts or molecular sieve adsorbents, so that the catalyst or the molecular sieve adsorbents are more easily suitable for adsorbing harmful substances such as indoor formaldehyde and the like.
Drawings
FIG. 1 is a schematic diagram of a process for preparing a modified adsorbent for adsorptive separation according to the present invention.
FIG. 2 is a schematic diagram of the possible surface modification principle of the catalyst or molecular sieve in the modified adsorbent for adsorptive separation according to the present invention.
Detailed Description
The following further description of the preferred embodiments with reference to the attached drawings will make the advantages and features of the present invention easier to understand by those skilled in the art, and thus the scope of the present invention will be clearly and clearly defined.
Example 1
(1) The preparation of primary modified adsorbent is carried out by weighing industrial NaY molecular sieve particles (0.3-0.8 mm; Si/Al 4.37;) 5kg, putting into reaction pot with 50L softened water, stirring at 80 deg.C for 5h, cooling to room temperature, naturally settling for 24-48h, separating supernatant, removing water-soluble impurities, wherein the impurities are unshaped raw powder micro-slag or soluble fine powder such as kaolin adhesive, and recovering filtrate for next use.
(2) Preparing composite alkali liquor 5.2SiO2:Al2O3:3.2Na2O:220H2O, the composite alkali liquor can be prepared firstly or stored for a plurality of days in a closed manner and then used, the alkali liquor and the primary modified adsorbent are mixed and contacted, the temperature is maintained at 100 ℃, the duration time is 4 hours, and the filtrate is recycled for next use; obtaining the surface modified secondary modified adsorbent.
(3) And (3) mixing and contacting the secondary modified adsorbent with 0.1-0.5mol/L potassium nitrate solution, stirring for 2-4h at 75-90 ℃, and recovering the filtrate for next use to obtain an adsorbent precursor.
(4) Activating and dehydrating in a high-temperature muffle furnace at 110 ℃ for 1.5h, 350 ℃ for 1h and 550 ℃ for 6h to obtain the dry-based 1-4 wt% functional modified adsorbent A.
Example 2
The preparation method in the example 1 is repeated, the composite alkali liquor in the step (2) in the example 1 is replaced by NaOH with the concentration of 1.1mol/L, the NaOH is used together with water glass, the silicon content in the composite alkali liquor is 1.8 wt%, and the liquid-solid mass ratio is maintained to be 1.3: 1; and (3) at the temperature of 95 ℃, treating for 5 hours to obtain the functional modified adsorbent B.
Example 3
The preparation method in the example 1 is repeated, the composite alkali liquor in the step (2) in the example 1 is changed into NaOH with the concentration of 1.6mol/L, no other NaOH is added, and the liquid-solid ratio is maintained to be 1.4: 1; at the temperature of 90 ℃, the treatment time is 2 hours, and the functional modified adsorbent C is obtained.
Example 4
The preparation method in the embodiment 3 is repeated, and the alkali solution treatment time in the embodiment 3 is divided into two sections, namely, firstly, the pretreatment is carried out for 1-2h by using an alkali solution with the concentration of 1.6mol/L NaOH, the compound alkali solution in the embodiment 1 is dropwise added in the latter section, and the treatment is continued for 3-4h at the same temperature, so as to obtain the functional modified adsorbent D.
Example 5
Example 1 was repeatedThe preparation method of (3) is to adjust the mixture ratio of the composite alkali liquor in the step (2) of the embodiment 1 to 8.5SiO2:Al2O3:3.5Na2O:180H2O, naturally storing for more than 5 days, and maintaining the liquid-solid ratio of 1.3: 1; and (3) at the temperature of 100 ℃, treating for 4-5h to obtain the functional modified adsorbent E.
Example 6
The preparation process of example 1 was repeated, the industrial molecular sieve of example 1, step (1), was replaced with NaX molecular sieve (0.3-0.8 mm; Si/Al 2.32;), and the mass ratio of the composite lye of step (2) was adjusted to 3.5SiO2:Al2O3:6.5Na2O:204H2O; and (3) replacing the 0.1-0.5mol/L potassium nitrate solution with 0.1-2mol/L barium nitrate solution to obtain the functional modified adsorbent F.
Example 7
The preparation process in example 6 was repeated, and the 0.1 to 2mol/L barium nitrate solution in step (3) in example 6 was replaced with a mixed solution of barium chloride and potassium chloride at a mass concentration ratio of 10 to 15:1 and a total mass concentration of 11.2%, and the mixture was stirred at 75 ℃ for 4 hours to obtain functionally modified adsorbent G.
Example 8
The preparation process in example 3 was repeated, using the alkaline solution scheme described in example 3, to replace the 0.1 to 0.5mol/L potassium nitrate solution with the 0.25 to 0.5mol/L magnesium nitrate solution in step (3) of example 1, and treated at a temperature of 80 ℃ for 2 hours to obtain a functionally modified adsorbent H.
Example 9
The preparation process of example 1 was repeated without any modification treatment, except for the unmodified adsorbent I obtained in accordance with steps (3) and (4).
TABLE 1 Properties of the functionally modified adsorbents obtained in examples 1 to 9
1Z-M is Z-molecular sieve and M-active component;2K130N/％、K250N/% -is respectively inBreakage under 130N, 250N pressure;3the ignition loss rate refers to the condition of mass change before and after roasting at 850-;
the above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (10)
1. A preparation method of a modified adsorbent for adsorption separation is characterized by comprising the following steps:
(1) purifying industrial products; putting an industrial molecular sieve into a reaction tank containing softened water, stirring at a proper temperature, cooling to room temperature, standing, filtering, and removing water-soluble impurities to obtain a primary modified adsorbent;
(2) surface modification; putting the primary modified adsorbent obtained in the step (1) into a reaction tank containing alkali solution, stirring at a proper temperature, repeatedly washing with warm water until the pH value is 9-11, and drying to obtain a secondary modified adsorbent;
(3) surface modification; putting the secondary modified adsorbent obtained in the step (2) into a reaction tank containing a soluble salt solution, stirring at a proper temperature, repeatedly washing with warm water until the pH value is 8-9, and drying to obtain an adsorbent precursor;
(4) dehydrating and activating; and (4) placing the adsorbent precursor obtained in the step (3) into a muffle furnace for roasting to obtain the modified adsorbent for adsorption separation.
2. The preparation method according to claim 1, wherein the industrial molecular sieve in step (1) comprises one, two or more of NaY, 13X, ZSM-5, H β, MCM-41, activated carbon, Zn — Al multi-layer filler; the shape of the industrial molecular sieve comprises one, two or more than two of powder, particles, microspheres, strips, clovers and polygons.
3. The method according to claim 1, wherein the suitable temperature in step (1) is 60 to 100 ℃; stirring for 5-10 h; the liquid-solid mass ratio of the softened water to the molecular sieve is 5-15; standing for 12-24 h.
4. The preparation method according to claim 1, wherein the alkali solution in the step (2) comprises one, two or more of inorganic alkali, organic alkali, silica sol, water glass and composite alkali liquor; the suitable temperature is 85-100 ℃; stirring for 1-5 h; the liquid-solid mass ratio of the alkali solution to the primary modified adsorbent is 1-5; the concentration of the alkali solution is 0.2-2.0mol/L, and the silicon content in the alkali solution is 0-2.5 wt%; the drying temperature is 105-120 ℃, and the drying time is 24-48 h.
5. The preparation method of claim 4, wherein the mass ratio of the composite alkali liquor is SiO2:Al2O3:Na2O:H2O＝(3.2-10.5):1:(1.5-7.5):(120-260)。
6. The method according to claim 1, wherein the soluble salt solution in the step (3) comprises one, two or more of inorganic acid salt, organic acid salt, chloride or oxide containing barium, cobalt, potassium, magnesium, calcium, gallium or rhenium; the suitable temperature is 65-100 ℃; stirring for 1-5 h; the liquid-solid mass ratio of the soluble salt solution to the secondary modified adsorbent is 5-10; the drying temperature is 105-120 ℃, and the drying time is 24-48 h.
7. The preparation method as claimed in claim 1, wherein the calcination temperature in step (4) is 150 ℃ and 600 ℃ and the calcination time is 3-8 h.
8. A modified adsorbent for adsorptive separation prepared by the production process according to any one of claims 1 to 7.
9. The use of the modified adsorbent of claim 8, comprising the following 1) to 7):
1) separating the aromatic isomers;
2) separating the diamine isomers;
3) separating the phenolic isomers;
4) separating the polyol isomers;
5) dehydrating and adsorbing;
6) a catalyst support;
7) and removing organic matters in the waste water and the waste gas.
10. The use of claim 9, wherein separating aromatic isomers comprises separating mixed industrial feedstocks of toluene, xylene, ethylbenzene; separating the diamine isomers comprises separating the 1, 5-pentanediamine industrial raw material; separating phenol isomerization comprises separating industrial raw materials such as m-cresol, 2, 6-dimethylphenol and the like; the separation of the polyol isomers comprises the separation of industrial raw materials such as 2, 3-butanediol, 1, 2-pentanediol, 1, 2-hexanediol and the like; the dehydration adsorption comprises separating moisture; the catalyst carrier includes a cordierite honeycomb catalytic module; the removal of organic matters in the waste water and waste gas comprises the treatment of acidic organic dye waste water and VOC.
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