CN110215911A - A kind of preparation method of modified boehmite adsorbed film - Google Patents
A kind of preparation method of modified boehmite adsorbed film Download PDFInfo
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- CN110215911A CN110215911A CN201910433446.6A CN201910433446A CN110215911A CN 110215911 A CN110215911 A CN 110215911A CN 201910433446 A CN201910433446 A CN 201910433446A CN 110215911 A CN110215911 A CN 110215911A
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- Prior art keywords
- boehmite
- water
- esterification
- modified
- film
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- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical class O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910001593 boehmite Inorganic materials 0.000 claims abstract description 63
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 230000032050 esterification Effects 0.000 claims abstract description 28
- 238000005886 esterification reaction Methods 0.000 claims abstract description 28
- 239000003463 adsorbent Substances 0.000 claims abstract description 19
- 239000000178 monomer Substances 0.000 claims abstract description 19
- 150000007524 organic acids Chemical class 0.000 claims abstract description 11
- 229920000642 polymer Polymers 0.000 claims abstract description 10
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 8
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 8
- 239000004088 foaming agent Substances 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000003999 initiator Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000007654 immersion Methods 0.000 claims abstract description 3
- 238000001556 precipitation Methods 0.000 claims abstract description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 11
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical group C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 10
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 10
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 8
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- 235000019394 potassium persulphate Nutrition 0.000 claims description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 3
- 239000004695 Polyether sulfone Substances 0.000 claims description 3
- 229940113088 dimethylacetamide Drugs 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 3
- 229920006393 polyether sulfone Polymers 0.000 claims description 3
- 239000004800 polyvinyl chloride Substances 0.000 claims description 3
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 2
- 229920004890 Triton X-100 Polymers 0.000 claims description 2
- 239000013504 Triton X-100 Substances 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 2
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims description 2
- 229920002492 poly(sulfone) Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 238000010992 reflux Methods 0.000 claims description 2
- PSCXFXNEYIHJST-QPJJXVBHSA-N (e)-4-phenylbut-3-enoic acid Chemical compound OC(=O)C\C=C\C1=CC=CC=C1 PSCXFXNEYIHJST-QPJJXVBHSA-N 0.000 claims 1
- PSCXFXNEYIHJST-UHFFFAOYSA-N trans-styrilacetic acid Natural products OC(=O)CC=CC1=CC=CC=C1 PSCXFXNEYIHJST-UHFFFAOYSA-N 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 7
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 abstract description 5
- 239000003814 drug Substances 0.000 abstract description 5
- 229940079593 drug Drugs 0.000 abstract description 5
- 239000002917 insecticide Substances 0.000 abstract description 5
- 241000894006 Bacteria Species 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 3
- 229920002521 macromolecule Polymers 0.000 abstract description 3
- 241000700605 Viruses Species 0.000 abstract description 2
- 239000000084 colloidal system Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000007857 degradation product Substances 0.000 abstract description 2
- 239000000645 desinfectant Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000000701 coagulant Substances 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 10
- 238000001179 sorption measurement Methods 0.000 description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000009740 moulding (composite fabrication) Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 229920000620 organic polymer Polymers 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- RJKFOVLPORLFTN-LEKSSAKUSA-N Progesterone Chemical compound C1CC2=CC(=O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H](C(=O)C)[C@@]1(C)CC2 RJKFOVLPORLFTN-LEKSSAKUSA-N 0.000 description 2
- -1 Sodium alkyl sulfate Chemical class 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229920001600 hydrophobic polymer Polymers 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 150000005208 1,4-dihydroxybenzenes Chemical class 0.000 description 1
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-OUBTZVSYSA-N Ammonia-15N Chemical compound [15NH3] QGZKDVFQNNGYKY-OUBTZVSYSA-N 0.000 description 1
- QFCQSIFDBNDNBP-UHFFFAOYSA-N C1(=CC=CC=C1)C=CCC(=O)O.C(C)(=O)O Chemical compound C1(=CC=CC=C1)C=CCC(=O)O.C(C)(=O)O QFCQSIFDBNDNBP-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 159000000013 aluminium salts Chemical class 0.000 description 1
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 1
- 229940106691 bisphenol a Drugs 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-M chloroacetate Chemical compound [O-]C(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-M 0.000 description 1
- 229940089960 chloroacetate Drugs 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000006266 etherification reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229960003511 macrogol Drugs 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 229960003387 progesterone Drugs 0.000 description 1
- 239000000186 progesterone Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
-
- 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
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
-
- 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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention provides a kind of preparation methods of modified boehmite adsorbed film, belong to field of compound material.Preparation method of the invention includes three steps: being first esterified with organic acid containing double bonds to boehmite, obtains double bond containing esterification boehmite；Then initiator, monomer, a small amount of crosslinking agent, emulsifier and esterification boehmite are added in water, is graft-polymerized to double bond containing esterification boehmite, prepares boehmite modified adsorbent；Finally match preparation liquid with polymer, boehmite modified adsorbent, pore-foaming agent and solvent, modified boehmite adsorbed film is prepared by immersion precipitation phase inversion process, the film can not only go macromolecular substances, colloid, bacterium and virus in water removal, moreover it is possible to remove insecticide, drug, incretion interferent, phenol, disinfectant and its derivative in water body, oily substance, high polymer coagulant and its degradation product etc..
Description
Technical field
The present invention relates to field of compound material, are related specifically to a kind of preparation method of modified boehmite adsorbed film.
Background technique
Activated alumina is a kind of common adsorbent, and in order to improve its adsorption capacity, Du Wen etc. is modified using copper chloride
Aluminium oxide adsorbs demercuration ability to improve it；Also sodium hydroxide is used to go fluorine ability to alumina modified to improve；Also it adopts
With calcium, magnesium-modified aluminium oxide, to improve the removal ability to fluorine and humic acid；Also its using the modified raising of manganese removes fluorine
Removing solid capacity；Also it uses phosphotungstic acid to be prepared for support type alumina adsorbant using infusion process for modifying agent to remove in wax tailings
Nitride also has double by etherification reaction introducing using coupling agent (silane coupling agent, titanate coupling agent, aluminate coupling agent)
Then key is grafted and is modified to aluminium oxide.
Boehmite (γ-Al00H) contains a large amount of hydroxyl, itself has certain adsorption capacity, in recent years, Many researchers pair
The modification of boehmite has carried out a large amount of research, as Wu Xiu bravely prepares boehmite powder using esterification assisting alcohol-hydrothermal method: should
Application (application number: the 201220319265.4) water for generating esterification, for the hydrolysis of urea, and then in hydrothermal condition
Under, it reacts with aluminium salt, while obtaining esterification product, obtains that granularity is small and uniform boehmite powder；With this
Meanwhile the consumption of water, the balanced sequence of esterification can also be promoted, be conducive to shorten reaction time of esterification, a reaction week
In phase, organic esterified product and inorganic ultrafine powder can be obtained simultaneously, is conducive to the comprehensive utilization of energy, energy-saving effect is bright
It is aobvious；For another example by the activity and chloroacetate reaction of sulfydryl in 5- amido-1,3,4-thiadiazoles -2- mercaptan, prepare end group is beam space
The corrosion inhibiter of carboxylic acid group.Then corrosion inhibiter is bonded by esterification with the hydroxyl in boehmite, is grafted to boehmite
PH sensitivity release type inhibition antirust filler is made in surface.
Boehmite is hydroaropic substance, to insecticide, drug, incretion interferent, phenol, chloroform and the derivative in water body
The adsorption capacities such as object, oily substance are weak, and hydrophobic organic polymer has very strong adsorption capacity, but its to these substances
It is difficult to soak in water；Therefore directly add boehmite in film then adsorption effect is poor, and directly add hydrophobic organic polymer
Object particle, hydrophobic polymer particle, which cannot be spontaneously wet out by water and then reduce contact area, reduces adsorption capacity, and its hydrophobicity
It also will affect the strainability and stain resistance of film.By the way that hydrophilic boehmite and hydrophobic organic polymer are grafted to together
The particle of preparation can be quickly spontaneously wet out by water, to insecticide, drug, incretion interferent, phenol, chloroform and the derivative in water body
The existing very strong adsorption capacity of object, oily substance, also there is certain hydrophily；It, which is added in film, can overcome addition boehmite
Or the shortcomings that particulate hydrophobic polymer, has good adsorption capacity concurrently in the case where so that film is had good strainability.
Summary of the invention
The purpose of the present invention is background technique propose aiming at the problem that, a kind of system for the modified boehmite adsorbed film designed
Boehmite and organic acid reaction containing double bond are obtained being esterified boehmite containing double bond, are then added and draw in water by Preparation Method, this method
Agent, monomer, a small amount of crosslinking agent, emulsifier and esterification boehmite are sent out, is graft-polymerized, prepares to double bond containing esterification boehmite
Boehmite modified adsorbent；Finally match preparation liquid with polymer, boehmite modified adsorbent, pore-foaming agent and solvent, passes through submergence
It precipitates phase inversion and prepares modified boehmite adsorbed film, which can not only go macromolecular substances, colloid, bacterium and disease in water removal
Poison, moreover it is possible to remove insecticide, drug, incretion interferent, phenol, disinfectant and its derivative, oily substance, the height in water body
Molecular flocculant and its degradation product etc..
Inventor passes through a large number of experiments and unremitting effort, is finally obtained following scheme:
A kind of preparation method of modified boehmite adsorbed film, the preparation method include the following steps:
(1) boehmite be first added to the water or the water containing a certain amount of hydroquinone in or be added dimethylbenzene in carry out at dispersion
Then reason is added double bond containing organic acid and carries out esterification, obtains double bond containing esterification boehmite, esterification condition
Are as follows: aqueous solution is stirred to react 10-72 hours or (138-145 DEG C) reflux 10-72 hours in dimethylbenzene at 70-100 DEG C of temperature；
The molar ratio of the boehmite and the organic acid containing double bond is 1:1-1:4；
The double bond containing organic acid is acrylic acid, methacrylic acid, butene dioic acid, styrene sulfonic acid, trans--styrene
Any one of acetic acid (4- phenyl -3-butenoic acid)；
Concentration of the boehmite in water or in the water containing a certain amount of hydroquinone or in dimethylbenzene is 1-8wt%；
(2) initiator, monomer, crosslinking agent, emulsifier and esterification boehmite are added in water, obtains mixed aqueous solution,
It is graft-polymerized under nitrogen protection, stirring to double bond containing esterification boehmite, reaction temperature is 60-80 DEG C, reaction time
It 3-15 hours, then arrives by being centrifuged, being filtered, washed, being dried in vacuo as boehmite modified adsorbent；
Monomer concentration is 2-10wt% in the aqueous solution, and initiator additive amount is the 0.5-2wt% of monomer, and crosslinking agent is used
Amount is the 1-5wt% of monomer, and content of the emulsifier in mixed aqueous solution is 0.05-2wt%, is esterified the matter of boehmite and monomer
Amount is than being 1:2-1:10；
The initiator is any one of potassium peroxydisulfate, sodium peroxydisulfate and ammonium persulfate；
The monomer is methyl methacrylate, butyl methacrylate, lauryl methacrylate, one in styrene
Kind is a variety of；
The crosslinking agent is divinylbenzene, butadiene is any one or more of；
The emulsifier is one of span80, lauryl sodium sulfate, Triton X-100 or a variety of；
(3) polymer, boehmite modified adsorbent, solvent, pore-foaming agent are mixed, constant temperature stirring 24 is small at 50-70 DEG C
Shi Peicheng film making solution, is film-made using immersion precipitation phase inversion process, the film of preparation be placed in pure water impregnate 24 hours or more to get
To containing modified boehmite adsorbed film, wherein polymer content is 16-24wt% in film making solution, boehmite modified adsorbent is
0.5-5wt%, pore-foaming agent 1-8wt%, solvent 63-82.5wt%；
The polymer is any one of polysulfones, polyether sulfone, polyacrylonitrile, polyvinyl chloride and Kynoar；
The solvent is any one of dimethylformamide, dimethyl acetamide, dimethyl sulfoxide, N-Methyl pyrrolidone
Or it is a variety of；
The pore-foaming agent is any one of polyethylene glycol, polyvinylpyrrolidone, lithium chloride.
The present invention is as follows using the principle of boehmite and the organic acid reaction containing double bond: contain great amount of hydroxy group on boehmite, with
Carboxyl in organic acid containing double bond reacts, and dehydration obtains double bond containing ester.
Compared with prior art, advantages of the present invention are as follows:
1, by the esterification of boehmite and the organic acid containing double bond, double bond containing active monomer is secured by covalent bond
Ground is incorporated on boehmite, and then can easily carry out subsequent graft modification, to overcome the profit of hydrophobic adsorbent
The problems such as wet problem or the water solubility of hydrophilic adsorbent.
2, a kind of modified boehmite adsorbed film prepared by the present invention not only has filtering function, can remove the glue in water body
Body, macromolecular substances, bacterium and virus, and can also insecticide, drug, incretion interferent, benzene in quick adsorption water body
Phenol, chloroform and derivative, oily substance etc..
Detailed description of the invention
Fig. 1 is the schematic diagram that boehmite is reacted with acrylic acid.
Specific embodiment
Below in conjunction with attached drawing, embodiments of the present invention is further illustrated, to make the purpose of the present invention, technical solution and excellent
Point is clearer, below technical solution in the present invention be clearly and completely described, it is clear that described embodiment is this
Invention a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art exist
Every other embodiment obtained under the premise of creative work is not made, shall fall within the protection scope of the present invention.
Embodiment 1
A kind of preparation method of modified boehmite adsorbed film, the preparation method include the following steps:
(1) 50 gram of boehmite (0.83mol), which is added in 800 milliliters of distilled water, disperses, and is ultrasonically treated, 5 minutes
Afterwards be added 3 grams of hydroquinones, be then slowly added to methacrylic acid (154g, 1.8mol) at room temperature, 70 DEG C stirring under into
Row reaction in 20 hours, solid matter with deionized water washing, finally in a vacuum 50 DEG C drying 20 hours i.e. obtain esterification suddenly
Nurse stone；
(2) add 30g monomer in 450 milliliters of water (monomer is methyl methacrylate and styrene is 1:1 in mass ratio
Mix), 8g span80,1.5g divinylbenzene, 10g esterification boehmite and 0.20g potassium peroxydisulfate, logical nitrogen 10 divides
Clock, stirring, reacts 12 hours at 65 DEG C, and then centrifugation, filtering are successively washed with water, acetone and hexane, dry at 50 DEG C
Obtain boehmite modified adsorbent.
(3) mixed with 20g polyether sulfone, 1g boehmite modified adsorbent, 1g polyvinylpyrrolidone and 78g dimethyl acetamide
It closes, in 60 DEG C of stirrings, 24 hours wiring solution-formings, is film-made by gel media of water, evaporation time is 30 seconds, and film is put to be impregnated in water
24 hours, the adsorbed film containing modified boehmite is obtained, the performance of film is shown in Table 1.
Embodiment 2
A kind of preparation method of modified boehmite adsorbed film, the preparation method include the following steps:
(1) it disperses 10.0g boehmite in 250mL dimethylbenzene, adds 49g acrylic acid, mixture 138- in dimethylbenzene
145 DEG C are flowed back 72 hours, and vacuum distillation removal dimethylbenzene washs solid removal impurity with ether, obtain white esterification after dry
Boehmite powder.
(2) add 50g monomer (butyl methacrylate is 1:2 with styrene mass ratio), 0.25g 12 in 450 milliliters of water
Sodium alkyl sulfate, 1.0g divinylbenzene and 1.0g butadiene, the boehmite of 5g esterification and the stirring of 0.50g potassium peroxydisulfate, 80
It is reacted 5 hours at DEG C, centrifugal filtration, is then successively washed with water, acetone and petroleum ether, is dried to obtain boehmite at 80 DEG C
Modified adsorbent.
(3) 24g polyvinyl chloride, 5g boehmite modified adsorbent, 8g Macrogol 600 and 73g N-Methyl pyrrolidone are used
Mixing is film-made in 60 DEG C of stirrings, 24 hours wiring solution-formings by gel media of water, and evaporation time is 10 seconds, and film is put to be soaked in water
Bubble 26 hours obtains the adsorbed film containing modified boehmite.
Embodiment 3
A kind of preparation method of modified boehmite adsorbed film, the preparation method include the following steps:
(1) take 6.0g business boehmite, after adding 250mL water dispersion, then plus 11.6g butene dioic acid, agitating and heating is in diformazan
It flows back 24 hours for 138-145 DEG C in benzene, filtering, ethanol washing is dried to obtain esterification boehmite at 80 DEG C.
(2) add 20g monomer in 450 milliliters of water (monomer is butyl methacrylate and styrene is 1:1 in mass ratio
Mix), 0.10g lauryl sodium sulfate and 3g span80,0.5g divinylbenzene, 10g esterification boehmite and
0.20g potassium peroxydisulfate leads to nitrogen 15 minutes, and stirring is reacted 5 hours, centrifugal filtration at 72 DEG C, is then successively washed with water, third
Ketone and petroleum ether are dried to obtain boehmite modified adsorbent at 80 DEG C.
(3) 16g polyacrylonitrile, 0.5g boehmite modified adsorbent, 1g polyvinylpyrrolidone and 82.5g dimethyl sulfoxide are used
Mixing is film-made in 60 DEG C of stirrings, 24 hours wiring solution-formings by gel media of water, and evaporation time is 30 seconds, and film is put to be soaked in water
Bubble 24 hours obtains the adsorbed film containing modified boehmite.
The sample that we prepare embodiment 1, is determined its performance, is specifically shown in Table 1.
The performance of the modified adsorbed film of table 1, boehmite
Note: 1. " boehmite films " and " polymer microballoon film " are comparative film.
2. the feeding liquid concentration of nitrobenzene, progesterone and bisphenol-A be 20ppm, 25 DEG C of temperature.
Claims (1)
1. a kind of preparation method containing modified boehmite adsorbed film, it is characterised in that: the preparation method the following steps are included:
(1) boehmite be first added to the water or the water containing a certain amount of hydroquinone in or be added dimethylbenzene in carry out decentralized processing, so
After double bond containing organic acid be added carry out esterification, obtain double bond containing esterification boehmite, esterification condition are as follows: temperature
Be stirred to react at 70-100 DEG C 10-72 hours or in dimethylbenzene, 138-145 DEG C reflux 10-72 hours；
The molar ratio of the boehmite and the organic acid containing double bond is 1:1-1:4；
The double bond containing organic acid is acrylic acid, methacrylic acid, butene dioic acid, styrene sulfonic acid, trans--phenylethyl acetate
Any one of (4- phenyl -3-butenoic acid)；
Concentration of the boehmite in water or in the water containing a certain amount of hydroquinone or in dimethylbenzene is 1-8wt%；
(2) initiator, monomer, crosslinking agent, emulsifier and esterification boehmite are added in water, mixed aqueous solution is obtained, in nitrogen
It is graft-polymerized under protection, stirring to double bond containing esterification boehmite, reaction temperature is 60-80 DEG C, reaction time 3-15
Hour, then arrive by being centrifuged, being filtered, washed, being dried in vacuo as boehmite modified adsorbent；
Monomer concentration is 2-10wt% in the aqueous solution, and initiator additive amount is the 0.5-2wt% of monomer, and dosage of crosslinking agent is single
The 1-5wt% of body, content of the emulsifier in mixed aqueous solution are 0.05-2wt%, and the mass ratio for being esterified boehmite and monomer is 1:
2-1:10；
The initiator is any one of potassium peroxydisulfate, sodium peroxydisulfate and ammonium persulfate；
The monomer be one of methyl methacrylate, butyl methacrylate, lauryl methacrylate, styrene or
It is a variety of；
The crosslinking agent is divinylbenzene, butadiene is any one or more of；
The emulsifier is one of span80, lauryl sodium sulfate, Triton X-100 or a variety of；
(3) polymer, boehmite modified adsorbent, solvent, pore-foaming agent are mixed, constant temperature stirs 24 hours and matches at 50-70 DEG C
It at film making solution, is film-made using immersion precipitation phase inversion process, the film of preparation, which is placed in pure water, impregnates 24 hours or more to get to containing
Modified boehmite adsorbed film, wherein polymer content is 16-24wt% in film making solution, boehmite modified adsorbent is 0.5-
5wt%, pore-foaming agent 1-8wt%, solvent 63-82.5wt%；
The polymer is any one of polysulfones, polyether sulfone, polyacrylonitrile, polyvinyl chloride and Kynoar；
The solvent is dimethylformamide, in dimethyl acetamide, dimethyl sulfoxide, N-Methyl pyrrolidone
It is any one or more；
The pore-foaming agent is any one of polyethylene glycol, polyvinylpyrrolidone, lithium chloride.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112999896A (en) * | 2021-03-11 | 2021-06-22 | 上海洁晟环保科技有限公司 | Boehmite modified adsorption film and preparation method and application thereof |
| CN115605551A (en) * | 2020-03-10 | 2023-01-13 | 萨索尔（美国）公司（Us） | Alumina modified with short-chain carboxylic acid for use as coating and method for producing the same |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090312494A1 (en) * | 2005-10-14 | 2009-12-17 | William Bett | Method for preparing a grafted copolymer by polyunsaturated fatty acids, copolymer grafted by polyunsaturated fatty acids obtainable by said method and uses thereof |
| CN102583469A (en) * | 2012-03-09 | 2012-07-18 | 广州慧谷化学有限公司 | Industrial production method for superfine high-purity alpha-alumina |
| CN104043434A (en) * | 2014-07-03 | 2014-09-17 | 江苏大学 | Preparation method for cellulose hollow magnetic imprinted composite microsphere adsorbent |
| CN104226274A (en) * | 2014-07-08 | 2014-12-24 | 兰州大学 | Adsorbing agent for removing petroleum type pollutants in environmental water sample and preparation method of adsorbing agent |
| CN105664882A (en) * | 2016-04-14 | 2016-06-15 | 福州大学 | Cellulose-based phenolic compound molecularly-imprinted adsorbing agent and preparation method thereof |
-
2019
- 2019-05-22 CN CN201910433446.6A patent/CN110215911A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090312494A1 (en) * | 2005-10-14 | 2009-12-17 | William Bett | Method for preparing a grafted copolymer by polyunsaturated fatty acids, copolymer grafted by polyunsaturated fatty acids obtainable by said method and uses thereof |
| CN102583469A (en) * | 2012-03-09 | 2012-07-18 | 广州慧谷化学有限公司 | Industrial production method for superfine high-purity alpha-alumina |
| CN104043434A (en) * | 2014-07-03 | 2014-09-17 | 江苏大学 | Preparation method for cellulose hollow magnetic imprinted composite microsphere adsorbent |
| CN104226274A (en) * | 2014-07-08 | 2014-12-24 | 兰州大学 | Adsorbing agent for removing petroleum type pollutants in environmental water sample and preparation method of adsorbing agent |
| CN105664882A (en) * | 2016-04-14 | 2016-06-15 | 福州大学 | Cellulose-based phenolic compound molecularly-imprinted adsorbing agent and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| PARISA DARAEI ET AL.: "PAA grafting onto new acrylate-alumoxane/PES mixed matrix nano-enhanced membrane: Preparation, characterization and performance in dye removal", 《CHEMICAL ENGINEERING JOURNAL》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115605551A (en) * | 2020-03-10 | 2023-01-13 | 萨索尔（美国）公司（Us） | Alumina modified with short-chain carboxylic acid for use as coating and method for producing the same |
| CN112999896A (en) * | 2021-03-11 | 2021-06-22 | 上海洁晟环保科技有限公司 | Boehmite modified adsorption film and preparation method and application thereof |
| CN112999896B (en) * | 2021-03-11 | 2023-12-22 | 西西埃热能(南京)有限公司 | Boehmite modified adsorption film and preparation method and application thereof |
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