CN116178610A - Preparation method of super absorbent resin - Google Patents
Preparation method of super absorbent resin Download PDFInfo
- Publication number
- CN116178610A CN116178610A CN202211659877.2A CN202211659877A CN116178610A CN 116178610 A CN116178610 A CN 116178610A CN 202211659877 A CN202211659877 A CN 202211659877A CN 116178610 A CN116178610 A CN 116178610A
- Authority
- CN
- China
- Prior art keywords
- preparation
- acrylic acid
- mass
- neutralization
- acrylamide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002250 absorbent Substances 0.000 title claims abstract description 14
- 230000002745 absorbent Effects 0.000 title claims abstract description 14
- 239000011347 resin Substances 0.000 title claims abstract description 14
- 229920005989 resin Polymers 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000003516 soil conditioner Substances 0.000 claims abstract description 8
- 238000006386 neutralization reaction Methods 0.000 claims description 40
- 239000002245 particle Substances 0.000 claims description 35
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 27
- 239000011259 mixed solution Substances 0.000 claims description 25
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 23
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 22
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 20
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 18
- 239000007863 gel particle Substances 0.000 claims description 16
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 239000012752 auxiliary agent Substances 0.000 claims description 12
- 238000005520 cutting process Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 230000000977 initiatory effect Effects 0.000 claims description 11
- 239000012764 mineral filler Substances 0.000 claims description 11
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 claims description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 10
- -1 alkyl phosphate Chemical compound 0.000 claims description 10
- 125000004386 diacrylate group Chemical group 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000001125 extrusion Methods 0.000 claims description 10
- 229920001223 polyethylene glycol Polymers 0.000 claims description 10
- 238000006116 polymerization reaction Methods 0.000 claims description 10
- 235000010265 sodium sulphite Nutrition 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 9
- 229960004063 propylene glycol Drugs 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 7
- 229940001584 sodium metabisulfite Drugs 0.000 claims description 7
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
- 239000003431 cross linking reagent Substances 0.000 claims description 6
- 239000012966 redox initiator Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- PUGOMSLRUSTQGV-UHFFFAOYSA-N 2,3-di(prop-2-enoyloxy)propyl prop-2-enoate Chemical class C=CC(=O)OCC(OC(=O)C=C)COC(=O)C=C PUGOMSLRUSTQGV-UHFFFAOYSA-N 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 239000003999 initiator Substances 0.000 claims description 4
- 238000004381 surface treatment Methods 0.000 claims description 4
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 4
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 3
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 229960000892 attapulgite Drugs 0.000 claims description 3
- 239000000440 bentonite Substances 0.000 claims description 3
- 229910000278 bentonite Inorganic materials 0.000 claims description 3
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052625 palygorskite Inorganic materials 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 3
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 3
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 2
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 claims description 2
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 claims description 2
- SGJUFIMCHSLMRJ-UHFFFAOYSA-N 2-hydroperoxypropane Chemical compound CC(C)OO SGJUFIMCHSLMRJ-UHFFFAOYSA-N 0.000 claims description 2
- FYRWKWGEFZTOQI-UHFFFAOYSA-N 3-prop-2-enoxy-2,2-bis(prop-2-enoxymethyl)propan-1-ol Chemical compound C=CCOCC(CO)(COCC=C)COCC=C FYRWKWGEFZTOQI-UHFFFAOYSA-N 0.000 claims description 2
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 2
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 2
- 239000004641 Diallyl-phthalate Substances 0.000 claims description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 2
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- 229910021536 Zeolite Inorganic materials 0.000 claims description 2
- GUCYFKSBFREPBC-UHFFFAOYSA-N [phenyl-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C)C=C(C)C=C1C GUCYFKSBFREPBC-UHFFFAOYSA-N 0.000 claims description 2
- QUDWYFHPNIMBFC-UHFFFAOYSA-N bis(prop-2-enyl) benzene-1,2-dicarboxylate Chemical compound C=CCOC(=O)C1=CC=CC=C1C(=O)OCC=C QUDWYFHPNIMBFC-UHFFFAOYSA-N 0.000 claims description 2
- MQDJYUACMFCOFT-UHFFFAOYSA-N bis[2-(1-hydroxycyclohexyl)phenyl]methanone Chemical compound C=1C=CC=C(C(=O)C=2C(=CC=CC=2)C2(O)CCCCC2)C=1C1(O)CCCCC1 MQDJYUACMFCOFT-UHFFFAOYSA-N 0.000 claims description 2
- 239000002734 clay mineral Substances 0.000 claims description 2
- YQHLDYVWEZKEOX-UHFFFAOYSA-N cumene hydroperoxide Chemical compound OOC(C)(C)C1=CC=CC=C1 YQHLDYVWEZKEOX-UHFFFAOYSA-N 0.000 claims description 2
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 2
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 VFHVQBAGLAREND-UHFFFAOYSA-N 0.000 claims description 2
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 2
- 229910001701 hydrotalcite Inorganic materials 0.000 claims description 2
- 229960001545 hydrotalcite Drugs 0.000 claims description 2
- 238000005286 illumination Methods 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- UHGIMQLJWRAPLT-UHFFFAOYSA-N octadecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCCCCCCCOP(O)(O)=O UHGIMQLJWRAPLT-UHFFFAOYSA-N 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical compound CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims description 2
- 235000013772 propylene glycol Nutrition 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims description 2
- 239000010457 zeolite Substances 0.000 claims description 2
- DDONFLBXWPGDQO-UHFFFAOYSA-N acetic acid;2-tert-butylperoxy-2-methylpropane Chemical compound CC(O)=O.CC(C)(C)OOC(C)(C)C DDONFLBXWPGDQO-UHFFFAOYSA-N 0.000 claims 1
- KOMDZQSPRDYARS-UHFFFAOYSA-N cyclopenta-1,3-diene titanium Chemical compound [Ti].C1C=CC=C1.C1C=CC=C1 KOMDZQSPRDYARS-UHFFFAOYSA-N 0.000 claims 1
- WMOVHXAZOJBABW-UHFFFAOYSA-N tert-butyl acetate Chemical compound CC(=O)OC(C)(C)C WMOVHXAZOJBABW-UHFFFAOYSA-N 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 19
- 150000003839 salts Chemical class 0.000 abstract description 5
- 229920000642 polymer Polymers 0.000 abstract description 4
- 125000003368 amide group Chemical group 0.000 abstract description 2
- 125000002843 carboxylic acid group Chemical group 0.000 abstract description 2
- 229920001577 copolymer Polymers 0.000 abstract description 2
- 238000007334 copolymerization reaction Methods 0.000 abstract description 2
- 239000000178 monomer Substances 0.000 abstract description 2
- 150000003254 radicals Chemical class 0.000 abstract description 2
- 241001122767 Theaceae Species 0.000 description 26
- 239000002689 soil Substances 0.000 description 19
- 229920000247 superabsorbent polymer Polymers 0.000 description 14
- 239000000243 solution Substances 0.000 description 13
- 238000004132 cross linking Methods 0.000 description 12
- 239000004583 superabsorbent polymers (SAPs) Substances 0.000 description 12
- KWVGIHKZDCUPEU-UHFFFAOYSA-N 2,2-dimethoxy-2-phenylacetophenone Chemical compound C=1C=CC=CC=1C(OC)(OC)C(=O)C1=CC=CC=C1 KWVGIHKZDCUPEU-UHFFFAOYSA-N 0.000 description 6
- 239000012467 final product Substances 0.000 description 6
- 239000005457 ice water Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 5
- 239000002504 physiological saline solution Substances 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- 239000002364 soil amendment Substances 0.000 description 5
- 238000005303 weighing Methods 0.000 description 4
- 229920002125 Sokalan® Polymers 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000010413 gardening Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000004584 polyacrylic acid Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000008213 purified water Substances 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000004745 nonwoven fabric Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- PEXNXOXCZLFQAO-ODZAUARKSA-N (z)-but-2-enedioic acid;ethenyl acetate Chemical compound CC(=O)OC=C.OC(=O)\C=C/C(O)=O PEXNXOXCZLFQAO-ODZAUARKSA-N 0.000 description 1
- XYFRHHAYSXIKGH-UHFFFAOYSA-N 3-(5-methoxy-2-methoxycarbonyl-1h-indol-3-yl)prop-2-enoic acid Chemical compound C1=C(OC)C=C2C(C=CC(O)=O)=C(C(=O)OC)NC2=C1 XYFRHHAYSXIKGH-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- PESYEWKSBIWTAK-UHFFFAOYSA-N cyclopenta-1,3-diene;titanium(2+) Chemical compound [Ti+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 PESYEWKSBIWTAK-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 230000015784 hyperosmotic salinity response Effects 0.000 description 1
- 239000003621 irrigation water Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- GYVGXEWAOAAJEU-UHFFFAOYSA-N n,n,4-trimethylaniline Chemical compound CN(C)C1=CC=C(C)C=C1 GYVGXEWAOAAJEU-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 1
- 229910000342 sodium bisulfate Inorganic materials 0.000 description 1
- 239000004289 sodium hydrogen sulphite Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- KXYJPVZMZBJJBZ-UHFFFAOYSA-N tert-butyl 2-ethylbutaneperoxoate Chemical compound CCC(CC)C(=O)OOC(C)(C)C KXYJPVZMZBJJBZ-UHFFFAOYSA-N 0.000 description 1
- 230000005068 transpiration Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention provides a preparation method of a super absorbent resin for a soil conditioner, which has high absorption rate, good water retention performance, anti-caking and excellent salt resistance. Two different functional monomers are adopted, and the binary copolymerized super absorbent resin is prepared through free radical copolymerization, and multiple groups such as carboxylic acid groups, amide groups and the like in the copolymer are mutually cooperated, so that the water absorption and water retention properties of the polymer are improved.
Description
Technical Field
The invention belongs to the field of functional polymer materials, and particularly relates to a preparation method of a super absorbent resin for a soil conditioner.
Background
The soil conditioner has the functions of preserving soil moisture and increasing temperature, can effectively improve the soil moisture content, increase the soil temperature of a cultivation layer and increase the soil humidity, and can also improve the soil structure, coordinate the relationship among soil water, fertilizer, gas, heat and organisms, prevent water and soil loss, enhance the seepage prevention capability of channels, inhibit the secondary salinization of the soil and improve the development and utilization of sandy barren lands. The soil conditioner forms large and water-stable aggregates by binding a plurality of small soil particles, and is widely applied to the fields of preventing soil from erosion, reducing soil water evaporation or excessive transpiration, saving irrigation water, promoting healthy growth of plants and the like.
The traditional soil improvement method adopts natural soil improvement agents, such as adding sand soil into clay, adding loam into sand soil and the like. At present, organic extracts, natural minerals or artificial high molecular polymers are mostly adopted to synthesize soil amendments. The synthetic polymers mainly include polyacrylic acid, vinyl acetate maleic acid, polyvinyl alcohol, etc. The soil structure modifier used internationally at present is mainly polyacrylic acid, gypsum as a byproduct of sulfur removal in coal-fired power plants, and the like.
The polyacrylic acid (salt) type super absorbent resin (SAP) is a polymer which contains a strong hydrophilic group and is insoluble in water, but can absorb water of which the dead weight is tens, hundreds or thousands times. Has the advantages of excellent water absorption and water retention performance, simple and mature production process, stable product performance, easy storage and the like. SAP (super absorbent polymers) is an indispensable functional material in the fields of sanitary products, agriculture and forestry, gardening, building industry, petroleum exploitation and the like.
China is a large population country and a large agricultural country, but in recent years, the soil quality problem is continuously remarkable due to the reasons of excessive use of fertilizers, overload cultivation and the like, so that the crop yield, the quality and the food taste are reduced to different degrees. Soil amendments are receiving increasing attention. Therefore, the SAP has good market prospect in the agricultural fields such as soil amendment, agriculture, forestry, gardening water retention agent, seedling cultivation and transplanting and the like.
Because of the wide range of operators in the field of China, the climate environment and the soil structure of different regions have obvious differences, such as northern arid, semiarid and areas with insufficient accumulated temperature in the growing period of crops, especially the severe soil environments of arid lands, hilly lands, saline-alkali lands and the like with serious water deficiency. There is therefore a differential need for SAP for soil amendments. At present, the special SAP for the commercial soil conditioner is less, and the existing product generally has the defects of low absorption rate, poor water retention performance, poor salt tolerance and the like, and has adverse effects in practical application.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the preparation method of the SAP for the soil conditioner, which has the advantages of high absorption rate, good water retention performance, caking resistance and excellent salt resistance.
The preparation method of the super absorbent resin for the soil conditioner comprises the following steps:
(1) Mixing refined acrylic acid, acrylamide and deionized water according to the mass ratio of 1 (0.08-1.4) to 1.8-3.5, uniformly stirring, and adding potassium hydroxide accounting for 0.62-0.7 weight part of the refined acrylic acid for neutralization to obtain a neutralization mixed solution with the neutralization degree of 0-80%;
the mass concentration of the refined acrylic acid is 25% -35%;
(2) Adding a cross-linking agent and a composite initiator into the neutralization mixed solution;
the cross-linking agent is selected from one or more of N, N' -methylene bisacrylamide, ethylene glycol dimethacrylate, alkyl phosphate, octadecyl phosphate monoester, pentaerythritol triallyl ether, diallyl phthalate, polyethylene glycol (300) diacrylate, polyethylene glycol (400) diacrylate, polyethylene glycol (600) diacrylate, polyethylene glycol (800) diacrylate, trimethylolpropane triacrylate and triethoxylated glycerol triacrylate, and the addition mass of the cross-linking agent accounts for 0.10-0.60% of the total amount of acrylic acid and acrylamide;
the composite initiator consists of a redox initiator and a photoinitiator, wherein the redox initiator is selected from one or two of sodium persulfate, potassium persulfate, ammonium persulfate, dibenzoyl peroxide, cumyl hydroperoxide, isopropyl hydroperoxide, tert-butyl hydroperoxide, isobutyl methyl ketone peroxide, methyl ethyl ketone peroxide, benzoyl peroxide, hydrogen peroxide, tert-butyl peroxydiethylacetate, tert-butyl peroxyacetate, tert-butyl peroxybenzoate, sodium sulfite, sodium metabisulfite, sodium bisulfate, dimethylaniline, N-dimethyl-p-toluidine, sodium bisulphite and sodium metabisulfite, and the addition amount of the redox initiator accounts for 0.01-1.00% of the total amount of acrylic acid and acrylamide;
the photoinitiator is selected from one or two of bis (1- (2, 4-difluorophenyl) -3-pyrrolyl) titanocene, diphenyl- (2, 4, 6-trimethylbenzoyl) phosphorus oxide, 1-hydroxycyclohexyl phenyl ketone, 2-dimethoxy-2-phenylacetophenone, phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, 2-phenylbenzyl-2-dimethylamine-1- (4-morpholinophenyl) butanone, 2-hydroxy-methylphenyl propane-1-ketone and 2-methyl-l- (4-methylthiophenyl) -2-morpholinyl-l-acetone, and the addition amount of the photoinitiator accounts for 0.005% -0.03% of the total amount of acrylic acid and acrylamide;
(3) Adding modified mineral filler into the neutralization mixed solution, stirring and mixing uniformly, initiating polymerization reaction under UV light irradiation, wherein the initial reaction temperature is 5-15 ℃, initiating by ultraviolet light, heating is not needed, the reaction time is 5-45 min, and the temperature rise is 60-70 ℃ to indicate that the reaction is complete, so as to obtain gel;
the mineral filler is one or more clay mineral substances such as bentonite, kaolin, attapulgite, mica, diatomite, hydrotalcite, zeolite and the like, and the addition amount of the mineral filler is 0.1-10% of the total amount of acrylic acid and acrylamide;
the polymerization initiation mode is UV photoinitiation, the wavelength of UV light is 140-360 nm, and the illumination time is 1-40 min;
(4) Extruding and granulating the gel for multiple times by an extruding and granulating machine, and uniformly adding a gel cutting auxiliary agent into the extruding machine in the extruding process to obtain gel particles;
the granulating mode is one of single-screw extrusion granulating and double-screw extrusion granulating, the gel cutting auxiliary agent is one or more of sodium stearate, sucrose ester, sodium sulfite and sodium metabisulfite, and the added mass of the gel cutting auxiliary agent accounts for 0.01-3% of the total amount of acrylic acid and acrylamide;
(5) Drying the prepared gel particles at 90-180 ℃ for 15-120 min, and crushing and screening to obtain primary basic particles with the particle size of 5-10 meshes;
(6) Spraying surface treatment liquid on the surfaces of the primary basic particles, and carrying out heat treatment to obtain the super absorbent resin particles, wherein the heat treatment temperature is 70-180 ℃ and the time is 10-30 min;
the surface treatment liquid is formed by mixing 1, 2-propanediol, ethylene glycol diglycidyl ether and sulfate, wherein the mass of the propanediol accounts for 0.02-3% of the total mass of the primary base particles, the mass of the ethylene glycol diglycidyl ether accounts for 0.002-0.4% of the total mass of the primary base particles, and the mass of the sulfate accounts for 0.1-4.0% of the total mass of the primary base particles. The sulfate is one or two of aluminum sulfate, sodium sulfate and sodium sulfite.
The invention has the following beneficial technical effects:
(1) Two different functional monomers are adopted, and a binary copolymerized super absorbent resin is prepared through a free radical copolymerization reaction, and a plurality of groups such as carboxylic acid groups, amide groups and the like in the copolymer are mutually cooperated, so that the water absorption and water retention properties of the polymer are improved;
(2) Inorganic mineral filler is adopted, inorganic components are introduced into a three-dimensional network of the super absorbent polymer, so that the liquid absorption rate and liquid absorption rate of the super absorbent polymer are improved, the properties such as salt resistance, gel strength, thermal stability and repeated use are improved, and meanwhile, the production cost is reduced;
(3) The UV photoinitiation process is adopted, so that the production efficiency is high, the energy consumption is low, and the continuous production can be realized.
The specific embodiment is as follows:
example 1
(1) 82g of refined acrylic acid is diluted by 273g of water, and 51g of potassium hydroxide is added into an ice water bath for neutralization to prepare a neutralization solution; adding 103g of acrylamide into the neutralization solution to obtain a neutralization mixed solution;
(2) Adding 0.36g of polyethylene glycol (600) diacrylate, 0.05g of 2, 2-dimethoxy-2-phenylacetophenone and 0.78g of ammonium persulfate into the neutralization mixed solution;
(3) Adding 0.2g of diatomite serving as an inert mineral filler into the mixed solution, stirring and uniformly mixing, initiating a polymerization reaction under the irradiation of UV light at the initial temperature of 10 ℃, wherein the wavelength of the UV light is 140-360 nm, and the reaction time is 30min to obtain gel;
(4) Granulating by adopting a single screw extruder, and uniformly adding a gel cutting auxiliary agent and 5.09g of sodium sulfite into the extruder in the extrusion process to obtain gel particles;
(5) Drying the prepared gel particles at 180 ℃ for 60min, and then crushing to obtain 100g of primary basic particles, wherein the average particle size is controlled to be 5-10 meshes;
(6) Uniformly mixing 1.3g of 1,2 propylene glycol, 0.06g of ethylene glycol diglycidyl ether, 2.9g of sulfate and 7.2g of deionized water to obtain a surface cross-linking liquid, uniformly spraying the surface cross-linking liquid on the surfaces of the primary basic particles obtained in the step (5), and carrying out heat treatment at 160 ℃ to obtain a final product.
Example 2
(1) Adding 150g of water into 82g of refined acrylic acid to dilute, and adding 51g of potassium hydroxide into an ice water bath to neutralize so as to obtain a neutralization solution; adding 7.0g of acrylamide into the neutralization solution to obtain a neutralization mixed solution;
(2) Adding 0.10g of triethoxylated glycerol triacrylate, 0.005g of 2, 2-dimethoxy-2-phenylacetophenone and 0.01g of ammonium persulfate into the neutralization mixed solution;
(3) Adding 0.1g of kaolin serving as an inert mineral filler into the mixed solution, stirring and uniformly mixing, initiating polymerization reaction under the irradiation of UV light at an initial temperature of 15 ℃, wherein the wavelength of the UV light is 140-360 nm, and the reaction time is 35min to obtain gel;
(4) Granulating by adopting a single screw extruder, and uniformly adding a gel cutting auxiliary agent and 0.01g of sodium stearate into the extruder in the extrusion process to obtain gel particles;
(5) Drying the prepared gel particles at 180 ℃ for 60min, and then crushing to obtain primary basic particles, wherein the average particle size is controlled to be 5-10 meshes;
(6) Uniformly mixing 1.4g of 1,2 propylene glycol, 0.05g of ethylene glycol diglycidyl ether, 2.5g of sulfate and 8.0g of deionized water to obtain a surface cross-linking liquid, uniformly spraying the surface cross-linking liquid on the surfaces of the primary basic particles obtained in the step (5), and carrying out heat treatment at 160 ℃ to obtain a final product.
Example 3
(1) 82g of refined acrylic acid is diluted by 273g of water, and 51g of potassium hydroxide is added into an ice water bath for neutralization to prepare a neutralization solution; adding 103g of acrylamide into the neutralization solution to obtain a neutralization mixed solution;
(2) 1.11g of N, N' -methylenebisacrylamide, 0.05g of 2, 2-dimethoxy-2-phenylacetophenone and 1.85g of N, N-dimethyl-p-toluidine are added into the neutralization mixed solution;
(3) Adding 18.5g of inert mineral filler attapulgite into the mixed solution, stirring and mixing uniformly, initiating polymerization reaction under the irradiation of UV light at an initial temperature of 5 ℃, wherein the wavelength of the UV light is 140-360 nm, and the reaction time is 30min to obtain gel;
(4) Granulating by adopting a single screw extruder, and uniformly adding a gel cutting auxiliary agent and 5.55g of sodium sulfite into the extruder in the extrusion process to obtain gel particles;
(5) Drying the prepared gel particles at 180 ℃ for 60min, and then crushing to obtain primary basic particles, wherein the average particle size is controlled to be 5-10 meshes;
(6) Uniformly mixing 1.4g of 1,2 propylene glycol, 0.07g of ethylene glycol diglycidyl ether, 2.8g of aluminum sulfate and 8.0g of deionized water to obtain a surface cross-linking liquid, uniformly spraying the surface cross-linking liquid on the surfaces of the primary basic particles obtained in the step (5), and performing heat treatment at 160 ℃ to obtain a final product.
Example 4
(1) 82g of refined acrylic acid is diluted by 273g of water, and 51g of potassium hydroxide is added into an ice water bath for neutralization to prepare a neutralization solution; adding 103g of acrylamide into the neutralization solution to obtain a neutralization mixed solution;
(2) Adding 0.35g of trimethylolpropane triacrylate, 0.04g of 2, 2-dimethoxy-2-phenylacetophenone and 0.70g of potassium persulfate into the neutralization mixed solution;
(3) Adding 10.0g of inert mineral filler bentonite into the mixed solution, stirring and mixing uniformly, initiating polymerization reaction under the irradiation of UV light at the initial temperature of 10 ℃, wherein the wavelength of the UV light is 140-360 nm, and the reaction time is 30min to obtain gel;
(4) Granulating by adopting a single screw extruder, and uniformly adding a gel cutting auxiliary agent and 4.8g of sodium metabisulfite into the extruder in the extrusion process to obtain gel particles;
(5) Drying the prepared gel particles at 180 ℃ for 60min, and then crushing to obtain primary basic particles, wherein the average particle size is controlled to be 5-10 meshes;
(6) Uniformly mixing 1.4g of 1,2 propylene glycol, 0.06g of ethylene glycol diglycidyl ether, 2.7g of aluminum sulfate and 7.2g of deionized water to obtain a surface cross-linking liquid, uniformly spraying the surface cross-linking liquid on the surfaces of the primary basic particles obtained in the step (5), and carrying out heat treatment at 160 ℃ to obtain a final product.
Comparative example 1
(1) 82g of refined acrylic acid is diluted by 273g of water, and 51g of potassium hydroxide is added into an ice water bath for neutralization to prepare a neutralization solution; adding 103g of acrylamide into the neutralization solution to obtain a neutralization mixed solution;
(2) Adding 0.38g of triethoxylated glycerol triacrylate, 0.04g of 2, 2-dimethoxy-2-phenylacetophenone and 0.82g of ammonium persulfate into the neutralization mixed solution;
(3) Stirring and mixing the mixed solution uniformly, initiating polymerization reaction under the irradiation of UV light, wherein the wavelength of the UV light is 140-360 nm, and the irradiation time is 35min, so as to obtain gel;
(4) Granulating by adopting a single screw extruder, and uniformly adding a gel cutting auxiliary agent and 4.8g of sodium sulfite into the extruder in the extrusion process to obtain gel particles;
(5) Drying the prepared gel particles at 180 ℃ for 60min, and then crushing to obtain primary basic particles, wherein the average particle size is controlled to be 5-10 meshes;
(6) Uniformly mixing 1.4g of 1,2 propylene glycol, 0.05g of ethylene glycol diglycidyl ether, 2.5g of sulfate and 8.0g of deionized water to obtain a surface cross-linking liquid, uniformly spraying the surface cross-linking liquid on the surfaces of the primary basic particles obtained in the step (5), and carrying out heat treatment at 160 ℃ to obtain a final product.
Comparative example 2
(1) 82g of refined acrylic acid is diluted by 273g of water, and 51g of potassium hydroxide is added into an ice water bath for neutralization to prepare a neutralization solution; adding 103g of acrylamide into the neutralization solution to obtain a neutralization mixed solution;
(2) Adding 0.36g of polyethylene glycol (600) diacrylate, 0.05g of 2, 2-dimethoxy-2-phenylacetophenone and 0.78g of ammonium persulfate into the neutralization mixed solution;
(3) Stirring and mixing the mixed solution uniformly, initiating polymerization reaction under the irradiation of UV light, wherein the wavelength of the UV light is 140-360 nm, and the irradiation time is 30min, so as to obtain gel;
(4) Granulating by adopting a single screw extruder, and uniformly adding a gel cutting auxiliary agent and 5.09g of sodium sulfite into the extruder in the extrusion process to obtain gel particles;
(5) Drying the prepared gel particles at 180 ℃ for 60min, and then crushing to obtain primary basic particles, wherein the average particle size is controlled to be 5-10 meshes;
(6) Uniformly mixing 1.3g of 1,2 propylene glycol, 0.06g of ethylene glycol diglycidyl ether, 2.9g of sulfate and 7.2g of deionized water to obtain a surface cross-linking liquid, uniformly spraying the surface cross-linking liquid on the surfaces of the primary basic particles obtained in the step (5), and carrying out heat treatment at 160 ℃ to obtain a final product.
Experimental example 1 deionized Water double absorption/physiological saline double absorption/tap Water double absorption test
Determination of absorption Rate of physiological saline
1. Principle of the method
A quantity of the sample was weighed and placed in a tea bag. And (3) placing the tea bag into liquid to absorb liquid for 30min, suspending for 10min, draining off excessive liquid, weighing, calculating, and determining the water absorption rate.
2. Reagents and materials
1) Physiological saline: sodium chloride solution with mass fraction of 0.9%;
2) Square plastic basin: about 5cm-15cm deep, sufficient to hold several bags;
3) Weigh the paper.
3. Apparatus and device
1) An electronic balance: the sensing amount is 0.001g;
2) And (3) a heat sealing machine: a sealable nonwoven fabric;
3) And (3) a timer: accurate to 1s.
4. Analytical procedure
1) Folding the non-woven fabric, and heat-sealing the two sides for 3-5 mm to prepare the tea bag. Characteristics of the tea bag:
2) 0.2g of the sample was weighed out to the nearest 0.005g. And pouring all the samples into the bottom of the tea bag, and sealing the tea bag when all the samples attached to the inner side of the tea bag are poured into the bottom of the tea bag. Weighing: the mass of the tea bag containing the SAP powder is mw1.
3) Another tea bag was prepared in the same manner as 4.2.2.4.2 and weighed: the mass of the tea bag containing the SAP powder is mw2. If the envelope takes more than 5 minutes before the test, the envelope should be kept in a desiccator.
4) Two blank tea bags were prepared and tested with the sample tea bag containing SAP powder. As long as the bag material and closure conditions have not changed, historical data may be considered for use. In which case the blank bag is no longer tested.
5) The tea bag is placed on the surface of the physiological saline. The tea bag was allowed to wet on the saline surface for 1 minute and pushed under the liquid surface. The tea bag is adjusted to expel entrained air bubbles. The soaking time is 30min.
6) After 30min, the tea bag filled with the sample and the blank tea bag are gently lifted up, hung by a clamp, and dripped for 10min in a static state. When a plurality of tea bags are hung at the same time, attention is paid to the fact that the tea bags should not be contacted with each other.
7) After 10min, each bag was weighed and the mass of two tea bags was recorded as mb1 and mb2.
8) And (3) calculating: the physiological saline absorption times are as follows: the arithmetic mean of mb1-mw1 and mb2-mw 2.
The deionized water and purified water are sucked in the same way, and the normal saline is replaced by the deionized water and the purified water. Deionized water and purified water have high absorption power, and the big tea bag is replaced, and the size of the tea bag is 100mm multiplied by 125mm.
Experimental example 2 centrifugal Water Retention test
1. Test instrument: centrifuge: FL-2 type, 200mm diameter, rotational speed 1500r/min (which may generate a centrifugal force of about 250 g).
2. The centrifugal water retention capacity test method has the same steps as those of the normal saline absorption test method 1-6 in the first 1-6 steps.
7) The tea bag containing the sample was placed in a centrifuge bowl and centrifuged at 250g for 3min.
8) And after the dehydration is finished for 3min, waiting for the centrifugal disc to stop thoroughly, opening the centrifugal cover and taking out the tea bag.
9) After removal of the tea bags, the bags were weighed and the two bags were recorded as having a mass of mb1 and mb2
10 Calculation: the centrifugal water retention capacity is as follows: the arithmetic mean of mb1-mw1 and mb2-mw 2.
Experimental example 3 anti-caking test
Instrument: constant temperature and humidity box, electronic balance, culture dish and 5-mesh screen
The testing steps are as follows:
(1) Weighing 10g of a sample, and spreading the sample in a culture dish;
(2) Placing the mixture into a constant temperature and humidity box, and setting the humidity to be 70%;
(3) Taking out the sample after 30min, sieving out agglomeration and adhesion large particles (more than 5 meshes) after moisture absorption;
(4) Weighing more than 5 meshes of weight mb;
(5) Calculate mb/10 x 100% as hygroscopic blocking rate:
the moisture absorption and adhesion rate is less than or equal to 20 percent, and the caking resistance is good; 20-40% is anti-caking general; and the caking resistance is poor at more than or equal to 40 percent.
The performance indexes of the super absorbent resin prepared by the embodiment of the invention are as follows:
therefore, the super absorbent resin prepared by the method has the characteristics of high absorption rate, good water retention performance, excellent anti-caking and salt resistance, safety, environmental protection and the like, and is suitable for the fields of agricultural SAP (super absorbent polymers) such as soil amendments, agriculture, forestry, gardening water retention agents, seedling cultivation and transplanting and the like.
Claims (10)
1. The preparation method of the super absorbent resin is characterized by comprising the following steps of:
(1) Mixing refined acrylic acid, acrylamide and deionized water, uniformly stirring, and adding potassium hydroxide for neutralization to obtain a neutralization mixed solution;
(2) Adding a cross-linking agent and a composite initiator into the neutralization mixed solution;
(3) Adding modified mineral filler into the neutralization mixed solution, stirring and mixing uniformly, and initiating polymerization reaction under UV light irradiation to obtain gel;
(4) Extruding and granulating the gel for multiple times by an extruding and granulating machine, and uniformly adding a gel cutting auxiliary agent into the extruding machine in the extruding process to obtain gel particles;
(5) Drying the prepared gel particles, and crushing and screening to obtain primary base particles;
(6) Spraying surface treatment liquid on the surfaces of the primary basic particles, and performing heat treatment to obtain the super absorbent resin particles.
2. The preparation method of claim 1, wherein in the step (1), the mass ratio of the refined acrylic acid, the acrylamide and the deionized water is 1:0.08-1.4:1.8-3.5, and the mass concentration of the refined acrylic acid is 25% -35%; the mass ratio of the potassium hydroxide to the refined acrylic acid is 0.62-0.7:1, wherein the neutralization degree of the neutralization mixed solution is 0-80%.
3. The preparation method of claim 1, wherein the cross-linking agent in the step (2) is selected from one or more of N, N' -methylenebisacrylamide, ethylene glycol dimethacrylate, alkyl phosphate, octadecyl phosphate monoester, pentaerythritol triallyl ether, diallyl phthalate, polyethylene glycol (300) diacrylate, polyethylene glycol (400) diacrylate, polyethylene glycol (600) diacrylate, polyethylene glycol (800) diacrylate, trimethylolpropane triacrylate and triethoxylated glycerol triacrylate, and the mass of the cross-linking agent accounts for 0.10% -0.60% of the total amount of acrylic acid and acrylamide.
4. The preparation method according to claim 1, wherein the composite initiator in the step (2) consists of a redox initiator and a photoinitiator, wherein the redox initiator is selected from one or two of sodium persulfate, potassium persulfate, ammonium persulfate, dibenzoyl peroxide, cumyl hydroperoxide, isopropyl hydroperoxide, tert-butyl hydroperoxide, isobutyl methyl ketone peroxide, methyl ethyl ketone peroxide, benzoyl peroxide, hydrogen peroxide, diethyl acetate tert-butyl peroxide, tert-butyl acetate, tert-butyl peroxybenzoate, sodium sulfite, sodium metabisulfite, sodium bisulfite, dimethylaniline, N-dimethyl-p-toluidine, sodium bisulfite, sodium metabisulfite, and the photoinitiator is selected from bis (1- (2, 4-difluorophenyl) -3-pyrrolyl) titanocene, diphenyl- (2, 4, 6-trimethylbenzoyl) phosphorus oxide, 1-hydroxycyclohexyl phenyl ketone, 2-dimethoxy-2-phenyl acetophenone, phenyl bis (2, 4, 6-trimethylbenzoyl) phosphine oxide, 2-phenylbenzyl-2-dimethyl-1- (4-methylbenzyl) -2-hydroxy-phenyl) -2-methyl-butanone, 2-phenyl-2-methyl-butanone, and 2-phenyl-2-morpholinone.
5. The method according to claim 4, wherein the redox initiator is added in an amount of 0.01 to 1.00% based on the total amount of acrylic acid and acrylamide, and the photoinitiator is added in an amount of 0.005 to 0.03% based on the total amount of acrylic acid and acrylamide.
6. The preparation method of claim 1, wherein the mineral filler in the step (3) is one or more clay minerals selected from bentonite, kaolin, attapulgite, mica, diatomite, hydrotalcite, zeolite and the like, and the addition amount of the mineral filler is 0.1% -10% of the total amount of acrylic acid and acrylamide; the polymerization initiation mode is UV photoinitiation, the wavelength of UV light is 140-360 nm, the initial reaction temperature is 5-15 ℃, and the illumination time is 1-40 min.
7. The preparation method of claim 1, wherein the granulating mode in the step (4) is one of single-screw extrusion granulating and double-screw extrusion granulating, the gum cutting auxiliary agent is one or more of sodium stearate, sucrose ester, sodium sulfite and sodium metabisulfite, and the addition mass of the gum cutting auxiliary agent accounts for 0.01-3% of the total amount of acrylic acid and acrylamide.
8. The preparation method according to claim 1, wherein in the step (5), the drying temperature is 90-180 ℃, the drying time is 15-120 min, and primary base particles with the particle size of 5-10 meshes are obtained after crushing and screening.
9. The preparation method according to claim 1, wherein the heat treatment temperature in the step (6) is 70-180 ℃ and the time is 10-30 min, the surface treatment liquid is formed by mixing 1, 2-propanediol, ethylene glycol diglycidyl ether and sulfate, wherein the mass of the propanediol accounts for 0.02-3% of the total mass of primary base particles, the mass of the ethylene glycol diglycidyl ether accounts for 0.002-0.4% of the total mass of primary base particles, the sulfate is one or two of aluminum sulfate, sodium sulfate and sodium sulfite, and the mass of the sulfate accounts for 0.1-4.0% of the total mass of primary base particles.
10. Use of the super absorbent resin obtained by the preparation method according to any one of claims 1 to 9 in the preparation of a soil conditioner.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106750475A (en) * | 2017-02-27 | 2017-05-31 | 江苏虹创新材料有限公司 | It is a kind of to resist the preparation method for returning the super absorbent resin for oozing performance with height |
| CN108047477A (en) * | 2017-12-20 | 2018-05-18 | 江苏斯尔邦石化有限公司 | A kind of preparation method of super absorbent resin |
| CN110590983A (en) * | 2019-01-31 | 2019-12-20 | 江苏斯尔邦石化有限公司 | Method for preparing water-absorbent resin by multistage initiation polymerization |
| CN110746541A (en) * | 2019-11-05 | 2020-02-04 | 深圳市乐闵科技有限公司 | High-salt-tolerance super absorbent resin and preparation method and application thereof |
| CN111087558A (en) * | 2019-12-16 | 2020-05-01 | 浙江卫星新材料科技有限公司 | Modified acrylic-based high-strength salt-resistant high-absorptivity resin and preparation method thereof |
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2022
- 2022-12-22 CN CN202211659877.2A patent/CN116178610A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106750475A (en) * | 2017-02-27 | 2017-05-31 | 江苏虹创新材料有限公司 | It is a kind of to resist the preparation method for returning the super absorbent resin for oozing performance with height |
| CN108047477A (en) * | 2017-12-20 | 2018-05-18 | 江苏斯尔邦石化有限公司 | A kind of preparation method of super absorbent resin |
| CN110590983A (en) * | 2019-01-31 | 2019-12-20 | 江苏斯尔邦石化有限公司 | Method for preparing water-absorbent resin by multistage initiation polymerization |
| CN110746541A (en) * | 2019-11-05 | 2020-02-04 | 深圳市乐闵科技有限公司 | High-salt-tolerance super absorbent resin and preparation method and application thereof |
| CN111087558A (en) * | 2019-12-16 | 2020-05-01 | 浙江卫星新材料科技有限公司 | Modified acrylic-based high-strength salt-resistant high-absorptivity resin and preparation method thereof |
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