CN114534693B - Preparation method of transparent hydrophobic spherical silica aerogel adsorbent - Google Patents
Preparation method of transparent hydrophobic spherical silica aerogel adsorbent Download PDFInfo
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- CN114534693B CN114534693B CN202210149350.9A CN202210149350A CN114534693B CN 114534693 B CN114534693 B CN 114534693B CN 202210149350 A CN202210149350 A CN 202210149350A CN 114534693 B CN114534693 B CN 114534693B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 239000003463 adsorbent Substances 0.000 title claims abstract description 45
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 38
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000001179 sorption measurement Methods 0.000 claims abstract description 47
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- 239000010703 silicon Substances 0.000 claims abstract description 11
- 150000001412 amines Chemical class 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000000352 supercritical drying Methods 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- 230000004048 modification Effects 0.000 claims abstract description 3
- 238000012986 modification Methods 0.000 claims abstract description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 24
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 16
- 239000011240 wet gel Substances 0.000 claims description 16
- 239000000741 silica gel Substances 0.000 claims description 15
- 229910002027 silica gel Inorganic materials 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000499 gel Substances 0.000 claims description 11
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 239000003960 organic solvent Substances 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 239000000839 emulsion Substances 0.000 claims description 7
- 238000001879 gelation Methods 0.000 claims description 7
- 238000007654 immersion Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000010008 shearing Methods 0.000 claims description 7
- 239000012798 spherical particle Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 6
- 239000003607 modifier Substances 0.000 claims description 6
- 229920000428 triblock copolymer Polymers 0.000 claims description 6
- 230000001112 coagulating effect Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- 229920002873 Polyethylenimine Polymers 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 3
- 239000002285 corn oil Substances 0.000 claims description 3
- 235000005687 corn oil Nutrition 0.000 claims description 3
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 claims description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- 235000019198 oils Nutrition 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 2
- 238000002210 supercritical carbon dioxide drying Methods 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 10
- 238000002336 sorption--desorption measurement Methods 0.000 description 8
- 239000004964 aerogel Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- -1 amine compound Chemical class 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 239000005431 greenhouse gas Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007783 nanoporous material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 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
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000013305 flexible fiber Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- 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
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
- B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
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- 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
- B01D2257/504—Carbon dioxide
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- 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
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
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- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention relates to a preparation method of a transparent hydrophobic spherical silica aerogel adsorbent. Preparing silicon source, surfactant, gel catalyst and solvent into sol, and preparing the sol by ball drop method, amine modification and supercritical drying. The invention adopts the water system as the main solvent, has convenient process, easily obtained raw materials, environmental protection, cost saving and easy realization of large-scale industrial production. The prepared transparent hydrophobic spherical silica aerogel adsorbent has the characteristics of excellent mechanical property, excellent hydrophobic property, high-efficiency gas circulation adsorption property and the like, and is an ideal high-performance gas adsorption material.
Description
Technical Field
The invention belongs to the field of preparation of new materials, and particularly relates to a preparation method of a transparent hydrophobic spherical silica aerogel adsorbent.
Background
Since the industrial revolution, with the development of economy and society, the emission of greenhouse gases has increased year by year, the global warming has become serious, serious climate and environmental problems have been caused, and serious challenges have been brought to the survival and development of human society, so that a high-efficiency novel adsorbent material is needed. Traditional adsorbents such as silica gel and activated alumina have the problems of limited adsorption capacity, complex preparation process, limited adsorption conditions, weak adsorption selectivity, poor recycling capability and the like, and are difficult to meet the requirement of treating large-scale greenhouse gas adsorption. Activated carbon is a relatively common adsorbent, but activated carbon has a relatively short service life and needs to be replaced periodically, which also increases cost. Therefore, the adsorbent material which is environment-friendly, low in cost, high in adsorptivity, recyclable and selective in adsorption is favored.
The nano porous material with high porosity and specific surface area has good application in adsorption. The silica aerogel is a nano porous material formed by nano particles, has high porosity, large specific surface area and other excellent properties, and is an ideal high-performance adsorption material. The amine compound has stronger chemical interaction with CO 2, so the adsorption medium is an ideal CO 2 adsorption medium. The existing aerogel adsorbent is modified by amines, and the morphology is mainly powder or block. The powder adsorbent is difficult to recycle, and secondary pollution can be caused; meanwhile, the inside of the block adsorbent is difficult to contact with an acting medium, waste is easy to cause, adsorption kinetic efficiency is low, and engineering application is difficult to realize in the adsorption field truly.
Patent application number CN201610560599.3 discloses a preparation method of carbon fiber aerogel circulating adsorbent taking flexible fibers as raw materials, but aims at adsorbing organic liquid, dye and the like, but does not show high-efficiency selective adsorption performance for gases such as CO 2 and the like. The patent with the application number of CN201910682903.5 discloses a preparation method of a spherical amino modified silicon oxide aerogel material, which adopts water glass as a silicon source, has poor inherent mechanical property and opaque material, has no hydrophobic property, is difficult to recycle, can cause secondary pollution in the use process, and has weak circulation stability and gas selective adsorption property.
Disclosure of Invention
In order to solve the problems of low adsorption rate, weak adsorption selectivity, poor recycling capability, poor mechanical property and the like of the conventional aerogel adsorption material, the invention provides a preparation method of a transparent hydrophobic spherical silica aerogel adsorbent. The method has the advantages of convenient process, easily obtained raw materials and easy realization of mass production. The prepared transparent hydrophobic spherical silica aerogel adsorbent has the characteristics of excellent mechanical properties, excellent hydrophobic properties, high-efficiency gas circulation adsorption performance and the like, is beneficial to the circulation use and the high-efficiency recovery in practical engineering application, and has high-efficiency selective adsorption performance on gases such as carbon dioxide, formaldehyde and the like.
The technical scheme of the invention is as follows: the preparation method of the transparent hydrophobic spherical silica aerogel adsorbent comprises the following specific steps:
(1) Under the condition of high-speed shearing and stirring at the rotating speed of 6000-20000 rpm, uniformly mixing an acid solution with a certain concentration, a surfactant and a gel catalyst, dripping a silicon source, continuously stirring to obtain a uniform emulsion, and standing for defoaming to obtain a clear and transparent silica sol;
(2) Preheating the silica sol obtained in the step (1), dripping the silica sol into a coagulating bath at 20-100 ℃ by using an automatic ball dripping device with a certain inner diameter, and standing for a period of time to carry out gelation reaction to obtain spherical silica wet gel;
(3) Washing the silica wet gel obtained in the step (2) with deionized water, and then replacing the silica wet gel with an organic solvent to obtain spherical silica gel;
(4) Mixing an amine modifier and an organic solvent according to a certain proportion to obtain a modified liquid, wherein the volume ratio of the modified liquid is that the amine modifier: organic solvent = 1: (1-10);
(5) Immersing the spherical silica gel obtained in the step (3) into the modified liquid prepared in the step (4) at 20-60 ℃, modifying for a certain time under the auxiliary condition, and performing supercritical CO 2 drying to obtain the transparent hydrophobic spherical silica aerogel adsorbent.
Preferably, the acid solution in the step (1) is one of acetic acid aqueous solution, oxalic acid aqueous solution, carbonic acid aqueous solution, phosphoric acid aqueous solution or boric acid aqueous solution, and the concentration is 0.1-10 mM; the surfactant is one of sodium dodecyl benzene sulfonate, cetyltrimethylammonium bromide, cetyltrimethylammonium chloride, triblock copolymer F127 or triblock copolymer P123; the gel catalyst is one of pyridine, urea, ammonium bicarbonate, triethylamine or hydrazine hydrate; the silicon source is one of methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane, trimethylmethoxysilane or hexamethyldisiloxane.
Preferably, the molar ratio of the silicon source, the acid solution, the surfactant and the gel catalyst in the step (1) is 1: (10-50): (0.016-0.048): (0.1-2.0); the dropping speed of the silicon source is 1-10 mL/min.
Preferably, the preheating time in the step (2) is 5-30 min, and the preheating temperature is 50-90 ℃; the inner diameter of the automatic ball dropping device is 0.5-10 mm; the standing time is 1-10 min; the coagulating bath is one of paraffin, n-hexane, corn oil, silicone oil or pump oil.
Preferably, the deionized water washing conditions in the step (3) are as follows: washing for 3-5 times at 20-100 ℃ for 1-12 h each time; the organic solvent is one of methanol, ethanol, acetonitrile, isopropanol or acetone; the replacement conditions are as follows: the temperature is 20-80 ℃, the replacement is carried out for 3-5 times, and each time lasts for 8-12 hours.
Preferably, the amine modifier in the step (4) is one of ethylenediamine, hexamethylenediamine, 3-aminopropyl triethoxysilane, polyethyleneimine or tetraethylenepentamine; the organic solvent is one of ethanol, acetonitrile, isopropanol, n-hexane or acetone.
Preferably, the immersion mode in the step (5) is one of normal pressure immersion, vacuum immersion or pressurized immersion; the auxiliary condition is one of ultrasonic, quartz lamp irradiation or water bath shaking table oscillation; the modification time is 0.5-36 h; the supercritical drying conditions of the CO 2 are as follows: the drying temperature is 45-80 ℃, and the pressure of the reaction kettle is 8-30 MPa.
The transparent hydrophobic spherical silica aerogel adsorbent prepared by the invention is spherical particles with the average particle diameter of 0.5-10 mm, the bulk density of 0.02-0.2 g/cm 3, the apparent density of 0.08-0.8 g/cm 3, the specific surface area of 520.6-1007.1 m 2/g, the water contact angle of 132.0-155.5 degrees, the CO 2 adsorption capacity of 1.64-4.69 mmol/g and the formaldehyde adsorption capacity of 5.85-8.28 mmol/g. The adsorption efficiency is maintained at 95-99% after 10 adsorption-desorption cycles.
The beneficial effects are that:
The preparation method of the transparent hydrophobic spherical silica aerogel adsorbent has the following characteristics:
(1) The preparation method provided by the invention is simple and quick, has wide raw material sources, low cost, environmental protection and environment friendliness, is high in safety, does not pollute the environment, and is easy to realize quantitative production.
(2) Compared with the massive and powdery silicon-based aerogel adsorption materials, the hydrophobic spherical silicon oxide aerogel adsorbent has excellent hydrophobic property and mechanical property, expands the application range, and can be applied to fixed bed and fluidized bed environments.
(3) The transparent hydrophobic spherical silica aerogel adsorbent prepared by the invention can be recycled, gas absorbed in the adsorbent can be separated by adopting means of heating, extraction and the like, and the adsorption efficiency is still maintained to be more than 95% after repeated adsorption-desorption cycles, so that the adsorbent has excellent cycle stability.
Drawings
FIG. 1 is an infrared plot of the transparent hydrophobic spherical silica aerogel adsorbent prepared in example 1;
FIG. 2 is a hydrophobic plot of the transparent hydrophobic spherical silica aerogel adsorbent prepared in example 1;
FIG. 3 is a graph of the CO 2 cycle adsorption of the transparent hydrophobic spherical silica aerogel adsorbent prepared in example 1.
Detailed Description
Example 1
Under the condition of high-speed shearing and stirring at the speed of 20000rpm, 20mol of acetic acid aqueous solution with the concentration of 1mM, 0.016mol of sodium dodecyl benzene sulfonate and 0.2mol of pyridine are uniformly mixed, 1mol of methyltrimethoxysilane is dripped into the mixed solution at the speed of 10mL/min, the uniform emulsion is obtained by continuous stirring, and the transparent silica sol is obtained by standing and defoaming. Preheating the sol at 90 ℃ for 5min, dripping the sol into 65 ℃ paraffin by using an automatic ball dripping device with the inner diameter of 3mm, and standing for 5min for gelation reaction to obtain spherical silica wet gel. The wet gel was washed with deionized water at 70℃for 3 times, 6 hours each time, and replaced with methanol at 50℃for 3 times, 10 hours each time, to obtain spherical silica gel. 100ml of ethylenediamine and 100ml of ethanol were mixed to obtain a modified solution. At 60 ℃, spherical silica gel is immersed in the modifying liquid in a normal pressure immersing way, and modified for 8 hours under the ultrasonic condition. And (3) carrying out CO 2 supercritical drying on the modified gel, wherein the drying temperature is 50 ℃, and the pressure of a reaction kettle is 10MPa, so as to obtain the transparent hydrophobic spherical silica aerogel adsorbent. The adsorbent is spherical particles with an average particle diameter of 3mm, the bulk density is 0.02g/cm 3, the apparent density is 0.08g/cm 3, the specific surface area is 520.6m 2/g, the water contact angle is 155.5 degrees, the CO 2 adsorption amount is 4.69mmol/g, and the formaldehyde adsorption amount is 8.28mmol/g. The adsorption efficiency was maintained at 99% through 10 adsorption-desorption cycles.
The infrared diagram of the prepared transparent hydrophobic spherical silica aerogel adsorbent is shown in figure 1. In the figure, the peaks at 2884cm -1 are attributed to hydrophobic methyl groups, the peaks at 1630, 1573 and 1484cm -1 are attributed to amine modified introduced ammonium salts or protonated ammonium NH 3+. These two groups can give excellent hydrophobic and selective adsorption properties to the material.
The hydrophobic diagram of the prepared transparent hydrophobic spherical silica aerogel adsorbent is shown in fig. 2. As can be seen from the figure, the prepared transparent hydrophobic spherical silica aerogel adsorbent material has a water contact angle of 155.5 degrees and excellent hydrophobicity.
The CO 2 cyclic adsorption curve chart of the prepared transparent hydrophobic spherical silica aerogel adsorbent is shown in figure 3. The measurement results show that: after 10 adsorption-desorption cycles, the adsorption capacity of CO 2 of the prepared transparent hydrophobic spherical silica aerogel adsorbent is reduced from 4.69 to 4.63mmol/g, the adsorption efficiency is 99%, and the transparent hydrophobic spherical silica aerogel adsorbent has excellent cycle stability.
Example 2
Under the high-speed shearing stirring condition with the speed of 18000rpm, 10mol of oxalic acid aqueous solution with the concentration of 5mM, 0.016mol of cetyltrimethylammonium bromide and 0.1mol of urea are uniformly mixed, 1mol of methyltriethoxysilane is dripped into the mixed solution at the speed of 6mL/min, the uniform emulsion is obtained by continuous stirring, and the transparent silica sol is obtained by standing and defoaming. Preheating the sol at 80 ℃ for 10min, dripping the sol into n-hexane at 20 ℃ by using an automatic ball dripping device with the inner diameter of 1mm, and standing for 10min to carry out gelation reaction to obtain spherical silica wet gel. Washing the wet gel with deionized water at 20deg.C for 5 times each for 12 hr, and replacing with ethanol at 20deg.C for 5 times each for 12 hr to obtain spherical silica gel. 100ml of hexamethylenediamine and 200ml of acetonitrile were mixed to obtain a modified liquid. At 50 ℃, the spherical silica gel is immersed in the modifying liquid in a pressurized dipping mode, and is modified for 24 hours under the oscillating condition of a water bath shaking table. And (3) carrying out CO 2 supercritical drying on the modified gel, wherein the drying temperature is 70 ℃, and the pressure of a reaction kettle is 20MPa, so as to obtain the transparent hydrophobic spherical silica aerogel adsorbent. The adsorbent is spherical particles with an average particle diameter of 1mm, the bulk density is 0.09g/cm 3, the apparent density is 0.32g/cm 3, the specific surface area is 664.3m 2/g, the water contact angle is 138.5 degrees, the CO 2 adsorption capacity is 3.89mmol/g, and the formaldehyde adsorption capacity is 7.82mmol/g. The adsorption efficiency was maintained at 98% through 10 adsorption-desorption cycles.
Example 3
Under the condition of high-speed shearing and stirring at the speed of 15000rpm, 30mol of carbonic acid aqueous solution with the concentration of 0.1mM, 0.032mol of cetyltrimethylammonium chloride and 0.8mol of ammonium bicarbonate are uniformly mixed, 1mol of dimethyl dimethoxy silane is dripped into the mixed solution at the speed of 4.5mL/min, the uniform emulsion is obtained by continuous stirring, and clear and transparent silica sol is obtained by standing and defoaming. Preheating the sol at 70 ℃ for 15min, dripping the sol into corn oil at 80 ℃ by using an automatic ball dripping device with the inner diameter of 5mm, and standing for 3min to carry out gelation reaction to obtain spherical silica wet gel. The wet gel was washed 3 times with 80 ℃ deionized water for 4 hours each time, and replaced with 60 ℃ acetonitrile for 4 times for 9 hours each time to obtain spherical silica gel. 100ml of 3-aminopropyl triethoxysilane and 500ml of isopropanol were mixed to obtain a modified liquid. At 40 ℃, the spherical silica gel is immersed in the modifying liquid in a vacuum impregnation mode, and modified for 0.5h under the irradiation condition of a quartz lamp. And (3) carrying out CO 2 supercritical drying on the modified gel, wherein the drying temperature is 60 ℃, and the pressure of a reaction kettle is 15MPa, so as to obtain the transparent hydrophobic spherical silica aerogel adsorbent. The adsorbent is spherical particles with an average particle diameter of 5mm, the bulk density is 0.12g/cm 3, the apparent density is 0.53g/cm 3, the specific surface area is 727.1m 2/g, the water contact angle is 142.5 degrees, the CO 2 adsorption capacity is 2.64mmol/g, and the formaldehyde adsorption capacity is 6.98mmol/g. The adsorption efficiency was maintained at 97% through 10 adsorption-desorption cycles.
Example 4
Under the condition of high-speed shearing and stirring at the speed of 9000rpm, 50mol of phosphoric acid aqueous solution with the concentration of 0.5mM, 0.048mol of triblock copolymer F127 and 2.0mol of triethylamine are uniformly mixed, 1mol of hexamethyldisiloxane is dripped into the mixed solution at the speed of 1.5mL/min, and stirring is continued to obtain uniform emulsion, and standing and defoaming are carried out to obtain clear and transparent silica sol. Preheating the sol at 50 ℃ for 30min, dripping the sol into 60 ℃ silicone oil by using an automatic ball dripping device with the inner diameter of 0.5mm, and standing for 1min to carry out gelation reaction to obtain spherical silica wet gel. The wet gel was washed 3 times with deionized water at 90℃for 1 hour each, and replaced with isopropanol at 70℃for 5 times for 8 hours each to obtain spherical silica gel. 100ml of polyethyleneimine and 1000ml of n-hexane were mixed to obtain a modified liquid. At 20 ℃, the spherical silica gel is immersed in the modifying liquid in a normal pressure immersing way, and modified for 2 hours under the ultrasonic condition. And (3) carrying out CO 2 supercritical drying on the modified gel, wherein the drying temperature is 45 ℃, and the pressure of a reaction kettle is 30MPa, so as to obtain the transparent hydrophobic spherical silica aerogel adsorbent. The adsorbent is spherical particles with an average particle diameter of 0.5mm, a bulk density of 0.16g/cm 3, an apparent density of 0.66g/cm 3, a specific surface area of 987.2m 2/g, a water contact angle of 144.0 DEG, an adsorption capacity of CO 2 of 1.98mmol/g and an adsorption capacity of formaldehyde of 6.28mmol/g. The adsorption efficiency was maintained at 96% through 10 adsorption-desorption cycles.
Example 5
Under the high-speed shearing stirring condition with the speed of 6000rpm, 40mol of boric acid aqueous solution with the concentration of 10mM, 0.032mol of triblock copolymer P123 and 1.0mol of hydrazine hydrate are uniformly mixed, 1mol of trimethylmethoxysilane is dripped into the mixed solution at the speed of 1mL/min, the uniform emulsion is obtained by continuous stirring, and the transparent silica sol is obtained by standing and defoaming. Preheating the sol at 60 ℃ for 20min, dripping the sol into pump oil at 100 ℃ by using an automatic ball dripping device with the inner diameter of 10mm, and standing for 8min to carry out gelation reaction to obtain spherical silica wet gel. The wet gel was washed 3 times with 100 ℃ deionized water for 1 hour each time, and replaced 3 times with 80 ℃ acetone for 8 hours each time to obtain spherical silica gel. 100ml of tetraethylenepentamine and 750ml of acetone were mixed to obtain a modified liquid. At 30 ℃, the spherical silica gel is immersed in the modifying liquid in a pressurized dipping mode, and is modified for 36 hours under the oscillating condition of a water bath shaking table. And (3) carrying out CO 2 supercritical drying on the modified gel, wherein the drying temperature is 80 ℃, and the pressure of a reaction kettle is 8MPa, so as to obtain the transparent hydrophobic spherical silica aerogel adsorbent. The adsorbent is spherical particles with an average particle diameter of 10mm, the bulk density is 0.2g/cm 3, the apparent density is 0.8g/cm 3, the specific surface area is 1007.1m 2/g, the water contact angle is 132.0 degrees, the CO 2 adsorption capacity is 1.64mmol/g, and the formaldehyde adsorption capacity is 5.85mmol/g. The adsorption efficiency was maintained at 95% through 10 adsorption-desorption cycles.
Claims (8)
1. The preparation method of the transparent hydrophobic spherical silica aerogel adsorbent comprises the following specific steps:
(1) Under the condition of high-speed shearing and stirring at the rotating speed of 6000-20000 rpm, uniformly mixing an acid solution with a certain concentration, a surfactant and a gel catalyst, dripping a silicon source, continuously stirring to obtain a uniform emulsion, and standing for defoaming to obtain a clear and transparent silica sol; the silicon source is one of methyltrimethoxysilane, methyltriethoxysilane, dimethyldimethoxysilane, trimethylmethoxysilane or hexamethyldisiloxane;
(2) Preheating the silica sol obtained in the step (1), dripping the silica sol into a coagulating bath at 20-100 ℃ by using an automatic ball dripping device with a certain inner diameter, and standing for a period of time to carry out gelation reaction to obtain spherical silica wet gel;
(3) Washing the silica wet gel obtained in the step (2) with deionized water, and then replacing the silica wet gel with an organic solvent to obtain spherical silica gel;
(4) Mixing an amine modifier and an organic solvent according to a certain proportion to obtain a modified liquid, wherein the volume ratio of the modified liquid is that the amine modifier: organic solvent = 1: (1-10);
(5) Immersing the spherical silica gel obtained in the step (3) into the modified liquid prepared in the step (4) at 20-60 ℃, modifying for a certain time under the auxiliary condition, and performing supercritical CO 2 drying to obtain the transparent hydrophobic spherical silica aerogel adsorbent; wherein the conditions of supercritical drying of CO 2 are as follows: the drying temperature is 45-80 ℃, and the pressure of the reaction kettle is 8-30 MPa.
2. The method according to claim 1, wherein the acid solution in the step (1) is one of an aqueous acetic acid solution, an aqueous oxalic acid solution, an aqueous carbonic acid solution, an aqueous phosphoric acid solution or an aqueous boric acid solution, and the concentration is 0.1-10 mM; the surfactant is one of sodium dodecyl benzene sulfonate, cetyltrimethylammonium bromide, cetyltrimethylammonium chloride, triblock copolymer F127 or triblock copolymer P123; the gel catalyst is one of pyridine, urea, ammonium bicarbonate, triethylamine or hydrazine hydrate.
3. The method according to claim 1, wherein the molar ratio of the silicon source, the acid solution, the surfactant and the gel catalyst in the step (1) is 1: (10-50): (0.016-0.048): (0.1-2.0); the dropping speed of the silicon source is 1-10 mL/min.
4. The preparation method according to claim 1, wherein the preheating time in the step (2) is 5 to 30 minutes, and the preheating temperature is 50 to 90 ℃; the inner diameter of the automatic ball dropping device is 0.5-10 mm; the standing time is 1-10 min; the coagulating bath is one of paraffin, n-hexane, corn oil, silicone oil or pump oil.
5. The method according to claim 1, wherein the deionized water washing conditions in the step (3) are: washing for 3-5 times at 20-100 ℃ for 1-12 h each time; the organic solvent is one of methanol, ethanol, acetonitrile, isopropanol or acetone; the replacement conditions are as follows: the temperature is 20-80 ℃, the replacement is carried out for 3-5 times, and each time lasts for 8-12 hours.
6. The preparation method according to claim 1, wherein the amine modifier in the step (4) is one of ethylenediamine, hexamethylenediamine, 3-aminopropyl triethoxysilane, polyethyleneimine or tetraethylenepentamine; the organic solvent is one of ethanol, acetonitrile, isopropanol, n-hexane or acetone.
7. The method according to claim 1, wherein the immersing means in the step (5) is one of atmospheric pressure immersion, vacuum immersion or pressure immersion; the auxiliary condition is one of ultrasonic, quartz lamp irradiation or water bath shaking table oscillation; the modification time is 0.5-36 h.
8. The preparation method according to claim 1, wherein the transparent hydrophobic spherical silica aerogel adsorbent prepared in the step (5) is spherical particles with an average particle diameter of 0.5-10 mm, a bulk density of 0.02-0.2 g/cm 3, an apparent density of 0.08-0.8 g/cm 3, a specific surface area of 520.6-1007.1 m 2/g, a water contact angle of 132.0-155.5 degrees, an adsorption amount of CO 2 of 1.64-4.69 mmol/g and an adsorption amount of formaldehyde of 5.85-8.28 mmol/g.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105565843A (en) * | 2015-06-09 | 2016-05-11 | 天津城建大学 | Highly-light-transmitting highly-heat-insulating composite material and preparation method thereof |
| CN108033455A (en) * | 2017-11-30 | 2018-05-15 | 航天材料及工艺研究所 | A kind of preparation method of aerosil |
| CN108383487A (en) * | 2018-03-27 | 2018-08-10 | 陕西科技大学 | A kind of PAN preoxidized fibers felt/silicon dioxide silica aerogel composite material and preparation method thereof |
| CN109354028A (en) * | 2018-11-13 | 2019-02-19 | 江西宏柏新材料股份有限公司 | A method of mixing silicon source copolymerization prepares flexible aeroge compound insulating material |
| CN110339790A (en) * | 2019-07-26 | 2019-10-18 | 南京工业大学 | Spherical amino modified silica aerogel and preparation method thereof |
| CN111164049A (en) * | 2017-10-04 | 2020-05-15 | 日立化成株式会社 | Aerogel and method for producing same |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101187568B1 (en) * | 2010-09-29 | 2012-10-04 | 한국에너지기술연구원 | Preparation method of silica aerogel granules |
| EP3147261B1 (en) * | 2014-05-22 | 2021-01-27 | Panasonic Intellectual Property Management Co., Ltd. | Process for producing silica aerogel |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105565843A (en) * | 2015-06-09 | 2016-05-11 | 天津城建大学 | Highly-light-transmitting highly-heat-insulating composite material and preparation method thereof |
| CN111164049A (en) * | 2017-10-04 | 2020-05-15 | 日立化成株式会社 | Aerogel and method for producing same |
| CN108033455A (en) * | 2017-11-30 | 2018-05-15 | 航天材料及工艺研究所 | A kind of preparation method of aerosil |
| CN108383487A (en) * | 2018-03-27 | 2018-08-10 | 陕西科技大学 | A kind of PAN preoxidized fibers felt/silicon dioxide silica aerogel composite material and preparation method thereof |
| CN109354028A (en) * | 2018-11-13 | 2019-02-19 | 江西宏柏新材料股份有限公司 | A method of mixing silicon source copolymerization prepares flexible aeroge compound insulating material |
| CN110339790A (en) * | 2019-07-26 | 2019-10-18 | 南京工业大学 | Spherical amino modified silica aerogel and preparation method thereof |
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