CN109663509B - 一种多级孔sapo-34分子筛膜的制备方法 - Google Patents
一种多级孔sapo-34分子筛膜的制备方法 Download PDFInfo
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- CN109663509B CN109663509B CN201910048461.9A CN201910048461A CN109663509B CN 109663509 B CN109663509 B CN 109663509B CN 201910048461 A CN201910048461 A CN 201910048461A CN 109663509 B CN109663509 B CN 109663509B
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- 239000012528 membrane Substances 0.000 title claims abstract description 139
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 133
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 239000002149 hierarchical pore Substances 0.000 title abstract description 21
- 238000002360 preparation method Methods 0.000 title abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 109
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 99
- 238000006243 chemical reaction Methods 0.000 claims abstract description 72
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000013078 crystal Substances 0.000 claims abstract description 54
- 229910001868 water Inorganic materials 0.000 claims abstract description 47
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000011148 porous material Substances 0.000 claims abstract description 22
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 20
- 238000003618 dip coating Methods 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 239000010413 mother solution Substances 0.000 claims abstract description 4
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 46
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical group [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 46
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 38
- WEHWNAOGRSTTBQ-UHFFFAOYSA-N dipropylamine Chemical compound CCCNCCC WEHWNAOGRSTTBQ-UHFFFAOYSA-N 0.000 claims description 36
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 30
- 239000012452 mother liquor Substances 0.000 claims description 24
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 22
- 229910019142 PO4 Inorganic materials 0.000 claims description 19
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 19
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 19
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 16
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 15
- 229910052698 phosphorus Inorganic materials 0.000 claims description 15
- 239000011574 phosphorus Substances 0.000 claims description 15
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 239000010703 silicon Substances 0.000 claims description 15
- 239000000919 ceramic Substances 0.000 claims description 11
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- HWCKGOZZJDHMNC-UHFFFAOYSA-M tetraethylammonium bromide Chemical compound [Br-].CC[N+](CC)(CC)CC HWCKGOZZJDHMNC-UHFFFAOYSA-M 0.000 claims description 6
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 4
- 230000008025 crystallization Effects 0.000 claims description 4
- -1 silicate ester Chemical class 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims description 4
- 230000008016 vaporization Effects 0.000 claims description 4
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- BGQMOFGZRJUORO-UHFFFAOYSA-M tetrapropylammonium bromide Chemical compound [Br-].CCC[N+](CCC)(CCC)CCC BGQMOFGZRJUORO-UHFFFAOYSA-M 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 239000012071 phase Substances 0.000 claims 6
- XVMSFILGAMDHEY-UHFFFAOYSA-N 6-(4-aminophenyl)sulfonylpyridin-3-amine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=N1 XVMSFILGAMDHEY-UHFFFAOYSA-N 0.000 claims 1
- 239000007791 liquid phase Substances 0.000 claims 1
- 238000009834 vaporization Methods 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 20
- 230000035699 permeability Effects 0.000 abstract description 5
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 230000000149 penetrating effect Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000012546 transfer Methods 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 description 18
- 239000008367 deionised water Substances 0.000 description 16
- 229910021641 deionized water Inorganic materials 0.000 description 16
- 238000007789 sealing Methods 0.000 description 16
- 238000001035 drying Methods 0.000 description 15
- 238000005406 washing Methods 0.000 description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 14
- 238000002441 X-ray diffraction Methods 0.000 description 11
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- 230000001680 brushing effect Effects 0.000 description 9
- 238000003786 synthesis reaction Methods 0.000 description 9
- 230000007062 hydrolysis Effects 0.000 description 8
- 238000006460 hydrolysis reaction Methods 0.000 description 8
- 239000001569 carbon dioxide Substances 0.000 description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000329 molecular dynamics simulation Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000005373 pervaporation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/028—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
- B01D53/22—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 diffusion
- B01D53/228—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 diffusion characterised by specific membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0048—Inorganic membrane manufacture by sol-gel transition
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
- C01B37/06—Aluminophosphates containing other elements, e.g. metals, boron
- C01B37/08—Silicoaluminophosphates [SAPO compounds], e.g. CoSAPO
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/54—Phosphates, e.g. APO or SAPO compounds
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
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CN114715914B (zh) * | 2022-04-06 | 2024-01-02 | 华南理工大学 | 一种低温脱除sapo-34分子筛膜孔道中有机结构导向剂的方法 |
CN115180633B (zh) * | 2022-06-27 | 2023-09-08 | 中国科学院上海高等研究院 | 一种多级孔sapo-34分子筛及其制备方法、应用 |
Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101443298A (zh) * | 2006-05-15 | 2009-05-27 | 科罗拉多州立大学董事会 | 用于co2/ch4分离的高通量和高选择性的sapo-34膜 |
CN102336414A (zh) * | 2011-06-29 | 2012-02-01 | 同济大学 | 一种使用清澈溶胶法制备高质量sapo-34分子筛膜的方法 |
CN103896300A (zh) * | 2012-12-28 | 2014-07-02 | 中国科学院上海高等研究院 | 高性能sapo-34分子筛膜的制备方法 |
CN104150504A (zh) * | 2014-08-25 | 2014-11-19 | 南京工业大学 | 一种sapo-34分子筛膜的制备方法 |
CN104340993A (zh) * | 2013-08-06 | 2015-02-11 | 中国科学院上海高等研究院 | Sapo-34分子筛膜的制备方法 |
CN104355316A (zh) * | 2014-09-03 | 2015-02-18 | 中国科学院上海高等研究院 | Sapo-34分子筛膜的制备方法 |
CN104525250A (zh) * | 2015-01-09 | 2015-04-22 | 中国科学院上海高等研究院 | 多级孔结构的sapo-34分子筛催化剂及其制备和应用 |
WO2015187311A1 (en) * | 2014-06-06 | 2015-12-10 | Uop Llc | Crystalline porous silicoaluminophosphates and metal-substituted silicoaluminophosphates with a hierarchical pore structure comprising micropores and mesopores, methods for making the same, and processes for converting oxygenates to olefins via reactions catalyzed by the same |
CN105983345A (zh) * | 2015-02-03 | 2016-10-05 | 中国科学院上海高等研究院 | 干凝胶法制备的sapo-34分子筛膜渗透汽化与汽相渗透分离气液/液体混合物的方法 |
CN107285342A (zh) * | 2016-03-31 | 2017-10-24 | 中国科学院上海高等研究院 | 固体酸后处理合成多级孔sapo-34分子筛的方法 |
CN107697925A (zh) * | 2017-10-24 | 2018-02-16 | 中国科学院上海高等研究院 | 一种多级孔sapo‑34分子筛的合成方法 |
CN108128786A (zh) * | 2018-01-09 | 2018-06-08 | 中国科学院上海高等研究院 | 一种超声辅助制备多级孔sapo-11分子筛的方法 |
-
2019
- 2019-01-18 CN CN201910048461.9A patent/CN109663509B/zh active Active
Patent Citations (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101443298A (zh) * | 2006-05-15 | 2009-05-27 | 科罗拉多州立大学董事会 | 用于co2/ch4分离的高通量和高选择性的sapo-34膜 |
CN102336414A (zh) * | 2011-06-29 | 2012-02-01 | 同济大学 | 一种使用清澈溶胶法制备高质量sapo-34分子筛膜的方法 |
CN103896300A (zh) * | 2012-12-28 | 2014-07-02 | 中国科学院上海高等研究院 | 高性能sapo-34分子筛膜的制备方法 |
CN104340993A (zh) * | 2013-08-06 | 2015-02-11 | 中国科学院上海高等研究院 | Sapo-34分子筛膜的制备方法 |
WO2015187311A1 (en) * | 2014-06-06 | 2015-12-10 | Uop Llc | Crystalline porous silicoaluminophosphates and metal-substituted silicoaluminophosphates with a hierarchical pore structure comprising micropores and mesopores, methods for making the same, and processes for converting oxygenates to olefins via reactions catalyzed by the same |
CN104150504A (zh) * | 2014-08-25 | 2014-11-19 | 南京工业大学 | 一种sapo-34分子筛膜的制备方法 |
CN104355316A (zh) * | 2014-09-03 | 2015-02-18 | 中国科学院上海高等研究院 | Sapo-34分子筛膜的制备方法 |
CN104525250A (zh) * | 2015-01-09 | 2015-04-22 | 中国科学院上海高等研究院 | 多级孔结构的sapo-34分子筛催化剂及其制备和应用 |
CN105983345A (zh) * | 2015-02-03 | 2016-10-05 | 中国科学院上海高等研究院 | 干凝胶法制备的sapo-34分子筛膜渗透汽化与汽相渗透分离气液/液体混合物的方法 |
CN107285342A (zh) * | 2016-03-31 | 2017-10-24 | 中国科学院上海高等研究院 | 固体酸后处理合成多级孔sapo-34分子筛的方法 |
CN107697925A (zh) * | 2017-10-24 | 2018-02-16 | 中国科学院上海高等研究院 | 一种多级孔sapo‑34分子筛的合成方法 |
CN108128786A (zh) * | 2018-01-09 | 2018-06-08 | 中国科学院上海高等研究院 | 一种超声辅助制备多级孔sapo-11分子筛的方法 |
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