CN115286742B - Water-in-water type retention and drainage aid and preparation method thereof - Google Patents
Water-in-water type retention and drainage aid and preparation method thereof Download PDFInfo
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- CN115286742B CN115286742B CN202211065449.7A CN202211065449A CN115286742B CN 115286742 B CN115286742 B CN 115286742B CN 202211065449 A CN202211065449 A CN 202211065449A CN 115286742 B CN115286742 B CN 115286742B
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- Prior art keywords
- water
- reaction
- boric acid
- monomer
- retention
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 230000014759 maintenance of location Effects 0.000 title abstract description 57
- 239000000178 monomer Substances 0.000 claims abstract description 101
- 238000006243 chemical reaction Methods 0.000 claims abstract description 71
- 239000004327 boric acid Substances 0.000 claims abstract description 59
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 55
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 48
- 125000002091 cationic group Chemical group 0.000 claims abstract description 43
- 239000012966 redox initiator Substances 0.000 claims abstract description 29
- 239000008139 complexing agent Substances 0.000 claims abstract description 26
- 239000003999 initiator Substances 0.000 claims abstract description 26
- 229910052751 metal Inorganic materials 0.000 claims abstract description 25
- 239000002184 metal Substances 0.000 claims abstract description 25
- AJSTXXYNEIHPMD-UHFFFAOYSA-N triethyl borate Chemical compound CCOB(OCC)OCC AJSTXXYNEIHPMD-UHFFFAOYSA-N 0.000 claims abstract description 23
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 18
- 150000003973 alkyl amines Chemical class 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000006467 substitution reaction Methods 0.000 claims abstract description 8
- 238000006116 polymerization reaction Methods 0.000 claims description 35
- 239000002904 solvent Substances 0.000 claims description 33
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 17
- 239000003112 inhibitor Substances 0.000 claims description 16
- 150000001350 alkyl halides Chemical class 0.000 claims description 14
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- 125000005619 boric acid group Chemical group 0.000 claims description 11
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 8
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- ZGCZDEVLEULNLJ-UHFFFAOYSA-M benzyl-dimethyl-(2-prop-2-enoyloxyethyl)azanium;chloride Chemical compound [Cl-].C=CC(=O)OCC[N+](C)(C)CC1=CC=CC=C1 ZGCZDEVLEULNLJ-UHFFFAOYSA-M 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 235000002639 sodium chloride Nutrition 0.000 claims description 6
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 6
- RRHXZLALVWBDKH-UHFFFAOYSA-M trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)C RRHXZLALVWBDKH-UHFFFAOYSA-M 0.000 claims description 6
- DPBJAVGHACCNRL-UHFFFAOYSA-N 2-(dimethylamino)ethyl prop-2-enoate Chemical compound CN(C)CCOC(=O)C=C DPBJAVGHACCNRL-UHFFFAOYSA-N 0.000 claims description 5
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 5
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 5
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 5
- 229940101006 anhydrous sodium sulfite Drugs 0.000 claims description 5
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 5
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 5
- 229950000688 phenothiazine Drugs 0.000 claims description 5
- 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
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 5
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 5
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 5
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 5
- PBLNBZIONSLZBU-UHFFFAOYSA-N 1-bromododecane Chemical compound CCCCCCCCCCCCBr PBLNBZIONSLZBU-UHFFFAOYSA-N 0.000 claims description 4
- HNTGIJLWHDPAFN-UHFFFAOYSA-N 1-bromohexadecane Chemical compound CCCCCCCCCCCCCCCCBr HNTGIJLWHDPAFN-UHFFFAOYSA-N 0.000 claims description 4
- KOFZTCSTGIWCQG-UHFFFAOYSA-N 1-bromotetradecane Chemical compound CCCCCCCCCCCCCCBr KOFZTCSTGIWCQG-UHFFFAOYSA-N 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 4
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 4
- 239000003638 chemical reducing agent Substances 0.000 claims description 4
- -1 dihydroxyethyl alkylamine Chemical class 0.000 claims description 4
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical group CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- DFENKTCEEGOWLB-UHFFFAOYSA-N n,n-bis(methylamino)-2-methylidenepentanamide Chemical compound CCCC(=C)C(=O)N(NC)NC DFENKTCEEGOWLB-UHFFFAOYSA-N 0.000 claims description 4
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 239000004289 sodium hydrogen sulphite Substances 0.000 claims description 4
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical group CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 claims description 4
- FZGFBJMPSHGTRQ-UHFFFAOYSA-M trimethyl(2-prop-2-enoyloxyethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCOC(=O)C=C FZGFBJMPSHGTRQ-UHFFFAOYSA-M 0.000 claims description 4
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims description 3
- HFNVACONKMSOTH-UHFFFAOYSA-K [Na+].[Na+].[Na+].OC(=O)CN(CCN(CC(O)=O)CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O Chemical compound [Na+].[Na+].[Na+].OC(=O)CN(CCN(CC(O)=O)CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O HFNVACONKMSOTH-UHFFFAOYSA-K 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- GQOKIYDTHHZSCJ-UHFFFAOYSA-M dimethyl-bis(prop-2-enyl)azanium;chloride Chemical compound [Cl-].C=CC[N+](C)(C)CC=C GQOKIYDTHHZSCJ-UHFFFAOYSA-M 0.000 claims description 3
- 125000001484 phenothiazinyl group Chemical group C1(=CC=CC=2SC3=CC=CC=C3NC12)* 0.000 claims description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
- XOJITQHBMRQMRX-UHFFFAOYSA-M sodium;ethane-1,2-diamine;2-oxido-1,3,2$l^{5}-dioxaphosphepane 2-oxide Chemical compound [Na+].NCCN.[O-]P1(=O)OCCCCO1 XOJITQHBMRQMRX-UHFFFAOYSA-M 0.000 claims description 3
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 claims description 2
- SNRUBQQJIBEYMU-NJFSPNSNSA-N dodecane Chemical group CCCCCCCCCCC[14CH3] SNRUBQQJIBEYMU-NJFSPNSNSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 4
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 17
- 229920000642 polymer Polymers 0.000 description 29
- 239000000835 fiber Substances 0.000 description 20
- 239000000243 solution Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 14
- 238000003756 stirring Methods 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 238000010992 reflux Methods 0.000 description 12
- 229940043237 diethanolamine Drugs 0.000 description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 238000010008 shearing Methods 0.000 description 8
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- LTJBQXYUTWVQDR-UHFFFAOYSA-N N,N-dihydroxyoctadecan-3-amine Chemical compound ON(O)C(CCCCCCCCCCCCCCC)CC LTJBQXYUTWVQDR-UHFFFAOYSA-N 0.000 description 5
- 238000004821 distillation Methods 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000011592 zinc chloride Substances 0.000 description 4
- 235000005074 zinc chloride Nutrition 0.000 description 4
- 229920001131 Pulp (paper) Polymers 0.000 description 3
- 230000002411 adverse Effects 0.000 description 3
- 239000012752 auxiliary agent Substances 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- WJFKNYWRSNBZNX-UHFFFAOYSA-N 10H-phenothiazine Chemical compound C1=CC=C2NC3=CC=CC=C3SC2=C1 WJFKNYWRSNBZNX-UHFFFAOYSA-N 0.000 description 2
- UWNADWZGEHDQAB-UHFFFAOYSA-N 2,5-dimethylhexane Chemical group CC(C)CCC(C)C UWNADWZGEHDQAB-UHFFFAOYSA-N 0.000 description 2
- SIAVMDKGVRXFAX-UHFFFAOYSA-N 4-carboxyphenylboronic acid Chemical group OB(O)C1=CC=C(C(O)=O)C=C1 SIAVMDKGVRXFAX-UHFFFAOYSA-N 0.000 description 2
- HOIZOTWLTZEHOO-UHFFFAOYSA-N CCCCCCCCCCCCCC(CC)N(O)O Chemical compound CCCCCCCCCCCCCC(CC)N(O)O HOIZOTWLTZEHOO-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- OBRIKKLMNAKCPQ-UHFFFAOYSA-N n,n-dihydroxytetradecan-3-amine Chemical compound CCCCCCCCCCCC(CC)N(O)O OBRIKKLMNAKCPQ-UHFFFAOYSA-N 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920002401 polyacrylamide Polymers 0.000 description 2
- 238000010526 radical polymerization reaction Methods 0.000 description 2
- 239000001488 sodium phosphate Substances 0.000 description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 2
- HMLSBRLVTDLLOI-UHFFFAOYSA-N 1-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)C(C)OC(=O)C(C)=C HMLSBRLVTDLLOI-UHFFFAOYSA-N 0.000 description 1
- QKDFWYFCMLUTQD-UHFFFAOYSA-N 17-bromo-N,N-dimethylheptadecan-1-amine Chemical compound BrCCCCCCCCCCCCCCCCCN(C)C QKDFWYFCMLUTQD-UHFFFAOYSA-N 0.000 description 1
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 description 1
- 241000251468 Actinopterygii Species 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 229920002907 Guar gum Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- ZXBLVTLRLTWNRE-UHFFFAOYSA-N [3-(prop-2-enoylamino)phenoxy]boronic acid Chemical group OB(O)Oc1cccc(NC(=O)C=C)c1 ZXBLVTLRLTWNRE-UHFFFAOYSA-N 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 150000001409 amidines Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- CRGOPMLUWCMMCK-UHFFFAOYSA-M benzyl-dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)CC1=CC=CC=C1 CRGOPMLUWCMMCK-UHFFFAOYSA-M 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000013051 drainage agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000000665 guar gum Substances 0.000 description 1
- 235000010417 guar gum Nutrition 0.000 description 1
- 229960002154 guar gum Drugs 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- MCLZMWVEJOJWRA-UHFFFAOYSA-I pentasodium;pentaacetate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O MCLZMWVEJOJWRA-UHFFFAOYSA-I 0.000 description 1
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000007762 w/o emulsion Substances 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
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic System
- C07F5/02—Boron compounds
- C07F5/04—Esters of boric acids
-
- 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
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/10—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of amides or imides
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/06—Paper forming aids
- D21H21/10—Retention agents or drainage improvers
Abstract
The invention provides a water-in-water type retention and drainage aid and a preparation method thereof, wherein the method comprises the following steps: (1) Uniformly mixing a first cationic monomer with water, introducing nitrogen, and then adding an azo initiator, a metal complexing agent and a redox initiator for reaction to obtain a prepolymer; (2) Adding boric acid monomer, inorganic salt, acrylamide, second cationic monomer and prepolymer into water, uniformly mixing, introducing nitrogen, and then adding azo initiator, metal complexing agent and redox initiator for reaction to obtain the water-in-water retention and drainage aid; the boric acid monomer is prepared by substitution reaction, and the raw materials for preparing the boric acid monomer comprise N, N-dihydroxyethyl alkylamine, triethyl borate and N-methylolacrylamide. The retention and drainage aid prepared by the method has the advantages of stable performance, good retention and drainage aid effect, good solubility and no pollution.
Description
Technical Field
The invention relates to the technical field of papermaking additives, in particular to a water-in-water type retention and drainage aid and a preparation method thereof.
Background
The retention and drainage aid is a common papermaking auxiliary agent, and after the papermaking retention and drainage aid is added in the papermaking process, the retention time and the retention amount of paper pulp on a net are greatly increased, and the retention and drainage aid has excellent retention effect on fillers and fine fibers and has obvious pulp retention effect; therefore, the retention and drainage aid can save paper pulp, quicken water filtration, reduce energy consumption, increase yield and save production cost.
The common retention and drainage aids are mainly inorganic and organic high molecular substances; wherein, organic polymer class helps stays filter aid because of it has the molecular weight great, and the quantity is few, and flocculation speed is fast, and pH application scope is wider, receives salt and external environment to influence little, and treatment effect is good grade advantage, has received wide attention and application in the papermaking field, and common organic polymer class helps stays filter aid includes: starch and modified starch, sodium carboxymethyl cellulose, chitosan series, guar gum series, polyacrylamide series, polyethylenimine, polydiallyl dimethyl ammonium chloride, polyethylene oxide, etc.; however, the existing retention and drainage aids still have the problems of poor solubility, unstable product performance and poor retention and drainage effects in the application process, so that a retention and drainage aid with good solubility, stable performance and good retention and drainage effects needs to be studied.
Disclosure of Invention
The invention provides a water-in-water type retention and drainage aid and a preparation method thereof, and the prepared retention and drainage aid has the advantages of stable performance, good retention and drainage aid effect, good solubility and no pollution.
In a first aspect, the present invention provides a method for preparing a water-in-water retention and drainage aid, the method comprising the steps of:
(1) Uniformly mixing a first cationic monomer with water, introducing nitrogen, and then adding an azo initiator, a metal complexing agent and a redox initiator for reaction to obtain a prepolymer;
(2) Adding boric acid monomer, inorganic salt, acrylamide, second cationic monomer and prepolymer into water, uniformly mixing, introducing nitrogen, and then adding azo initiator, metal complexing agent and redox initiator for reaction to obtain the water-in-water retention and drainage aid;
the boric acid monomer is prepared by substitution reaction, and the raw materials for preparing the boric acid monomer comprise N, N-dihydroxyethyl alkylamine, triethyl borate and N-methylolacrylamide.
Preferably, the preparation method of the boric acid monomer comprises the following steps:
(21) Adding haloalkane and diethanolamine into a first solvent, uniformly mixing and reacting to obtain N, N dihydroxyethyl alkylamine;
(22) Adding the N, N dihydroxyethyl alkylamine and triethyl borate into a second solvent, uniformly mixing and reacting to obtain a reaction product, and adding N-methylol acrylamide and a polymerization inhibitor into the reaction product for continuous reaction to obtain a monomer containing boric acid groups;
more preferably, the first solvent is dimethylformamide; the second solvent is benzene or toluene; the polymerization inhibitor is phenothiazine or hydroquinone.
Preferably, in the step (21), the haloalkane and the diethanolamine are reacted at a temperature of 85-95 ℃ for a time of 5-7 hours;
in the step (22), the temperature of the reaction is 55-65 ℃, and the time of the reaction is 1-1.5 h.
Preferably, the alkyl halide is at least one of bromododecane, bromotetradecane, bromohexadecane or bromohexadecyl trimethylamine;
in step (21), the ratio of the amounts of the substances of the haloalkane, diethanolamine and first solvent is 1: (1.2-1.5): (25-28);
in step (22), the ratio of the amounts of the substances of N, N-dihydroxyethyl alkylamine, triethyl borate and N-methylolacrylamide is 1: (0.2-0.5): (0.2 to 0.5);
the ratio of the amounts of the substances of triethyl borate, the second solvent and the polymerization inhibitor is 1: (30-50): (0.005-0.01).
Preferably, the first cationic monomer is at least one of acrylic acid-N, N-dimethylamino ethyl ester, methacrylic acid-N, N-dimethylamino ethyl ester or N, N-dimethylamino propyl acrylamide;
the second cationic monomer is at least one of acryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride, dimethyl diallyl ammonium chloride, acryloyloxyethyl dimethyl benzyl ammonium chloride or methacryloyloxyethyl dimethyl benzyl ammonium chloride;
the inorganic salt is at least one of anhydrous sodium sulfate, ammonium sulfate or sodium chloride.
Preferably, the azo initiator is at least one of azobisisobutyronitrile, azobisisobutylamidine hydrochloride or azobisiso Ding Mi hydrochloride;
the metal complexing agent is at least one of disodium ethylenediamine tetraacetate, trisodium diethylenetriamine pentaacetate, sodium ethylenediamine tetramethylene phosphate or sodium citrate;
the oxidant in the redox initiator is at least one of hydrogen peroxide, di-tert-butyl peroxide, tert-butyl hydroperoxide, potassium persulfate or ammonium persulfate, and the reducing agent in the redox initiator is at least one of anhydrous sodium sulfite, sodium bisulphite or sodium thiosulfate.
Preferably, in step (1), the mass ratio of the first cationic monomer to water is 1: (5-8);
the mass ratio of the first cationic monomer to the azo initiator to the metal complexing agent to the redox initiator is 1: (0.001-0.005): (0.0005-0.001): (0.005-0.01).
Preferably, in step (2), the mass ratio of boric acid monomer, inorganic salt, acrylamide, second cationic monomer, prepolymer and water is (0.03 to 0.05): (0.1-0.3): (0.05-0.1): (0.06-0.1): (0.05-0.1): (0.5-0.8).
Preferably, in the step (2), the mass ratio of the boric acid monomer, azo-based initiator, metal complexing agent and redox initiator is (0.03 to 0.05): (0.0003 to 0.0005): (0.00001-0.00003): (0.0001-0.0005).
Preferably, in the step (1) and the step (2), before introducing nitrogen, the method further comprises adding a pH regulator to the uniformly mixed solution to regulate the pH to 4.2-4.6, and preferably, in the step (1), regulating the pH to 4.4-4.6;
the pH regulator is at least one of acetic acid, hydrochloric acid, 2-acrylamide-2-methylpropanesulfonic acid or citric acid.
Preferably, in the step (1), the temperature of the reaction is 60-65 ℃, and the time of the reaction is 3-5 hours;
in the step (2), the temperature of the reaction is 50-60 ℃, and the time of the reaction is 3-5 h.
Preferably, the nitrogen introducing time is 30-35 min.
In a second aspect, the present invention provides a water-in-water retention and drainage aid, prepared by the preparation method according to any one of the first aspects.
Compared with the prior art, the invention has at least the following beneficial effects:
in the invention, boric acid monomers are introduced in the water-in-water polymerization process, and are of long-chain structures, and contain double bonds capable of participating in reaction, so that the boric acid monomers and other monomers can form water-in-water polymer emulsion through free radical polymerization, in the application process, boric acid groups in the polymer can form boric acid ester bonds with hydroxyl groups in slurry fibers, so that a micro-crosslinking structure is formed, the adhesion capacity to fine fibers can be remarkably enhanced, meanwhile, the formed polymer is of a macromolecular long-chain structure, and boric acid ester bonds formed by boric acid groups and hydroxyl groups in the fibers have reversible fracture properties, so that the polymer in the invention not only has excellent shearing resistance, but also has good self-healing capacity even if the polymer breaks under a high shearing environment, and further improves the retention and drainage aid effects of polymer assistants; the retention and drainage aid in the invention is water-in-water emulsion, which not only can effectively improve the retention rate of fine fibers, but also has the advantages of high dissolution speed, low cost, environmental friendliness and the like.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by persons of ordinary skill in the art without making creative efforts based on the embodiments of the present invention are all within the scope of protection of the present invention.
The invention provides a preparation method of a water-in-water type retention and drainage aid, which comprises the following steps:
(1) Uniformly mixing a first cationic monomer with water, introducing nitrogen, and then adding an azo initiator, a metal complexing agent and a redox initiator for reaction to obtain a prepolymer;
(2) Adding boric acid monomer, inorganic salt, acrylamide, second cationic monomer and prepolymer into water, uniformly mixing, introducing nitrogen, and then adding azo initiator, metal complexing agent and redox initiator for reaction to obtain the water-in-water retention and drainage aid;
the preparation method comprises the steps of firstly preparing a prepolymer by adopting a first cationic monomer, wherein the prepolymer not only can play a role in dispersion in the subsequent water-in-water polymerization process, but also can play a role in cationic charge and anionic charge in fibers, so that the retention rate of the fine fibers is improved; the boric acid monomer is of a long-chain structure and contains boric acid groups and a double bond structure capable of participating in reaction, the existence of the double bond structure can enable the boric acid monomer, acrylamide, inorganic salt, second cationic monomer and prepolymer to undergo free radical polymerization reaction, so that the boric acid monomer is introduced into the polymer to form a polymer structure of a macromolecular long chain, the boric acid groups in the polymer can interact with hydroxyl groups in papermaking pulp fibers to form boric acid ester bonds, and the boric acid groups and the fibers form a micro-crosslinking structure, so that the adhesion capacity to fine fibers can be remarkably improved, the retention and drainage aid performance is enhanced, and meanwhile, the boric acid ester bonds formed by the boric acid groups and the hydroxyl groups in the fibers are dynamic covalent bonds, not only have the stability of covalent bonds, but also have the reversibility of non-covalent bonds, so that the polymer of the invention not only has excellent shearing resistance, but also has good self-healing capacity even if the polymer breaks under a high shearing environment, and further improves the retention and drainage aid effect of the polymer auxiliary agent; the invention also introduces a second cationic monomer in the polymerization process, and positive charges in the cationic monomer can further adsorb negative charges in the fiber, thereby further improving the adhesion of the polymer auxiliary agent to the fine fiber and further improving the retention rate of the fiber;
the boric acid monomer is prepared by substitution reaction, and the raw materials for preparing the boric acid monomer comprise N, N-dihydroxyethyl alkylamine, triethyl borate and N-methylolacrylamide; the invention adopts N, N-dihydroxyethyl alkylamine, triethyl borate and N-methylol acrylamide to prepare boric acid monomer through polymerization reaction, and the structural formula is as follows:
wherein R is dodecane, tetradecane or hexadecane; according to the structural formula, the boric acid monomer prepared by the method is of a long-chain structure, contains boric acid groups and double bond structures capable of participating in the reaction, so that the boric acid monomer can participate in the water-in-water polymerization reaction, the polymer auxiliary contains the boric acid groups and the long-chain structure, and further the retention and drainage effects and the shearing resistance of the polymer auxiliary are improved.
According to some preferred embodiments, the specific preparation method of the boric acid monomer comprises the following steps:
(21) Firstly, synthesizing N, N-dihydroxyethyl alkylamine, adding haloalkane and diethanolamine into a first solvent, uniformly mixing and reacting to obtain N, N-dihydroxyethyl alkylamine; when preparing N, N-dihydroxyethyl alkylamine, adding haloalkane, diethanolamine and a first solvent into a four-mouth flask provided with an electric stirring device and a condenser tube, controlling the reaction temperature through a water bath to perform a reaction, adding a proper amount of catalyst which can be sodium carbonate in the reaction process to improve the reaction rate, and distilling under reduced pressure at 160-180 ℃ after the reaction to remove unreacted raw materials and the solvent to obtain the product N, N-dihydroxyethyl alkylamine;
(22) Adding the N, N-dihydroxyethyl alkylamine and triethyl borate into a second solvent, uniformly mixing and reacting to obtain a reaction product, and adding N-methylol acrylamide and a polymerization inhibitor into the reaction product for continuous reaction to obtain the boric acid monomer;
according to some preferred embodiments, the first solvent is dimethylformamide; the second solvent is benzene or toluene; the polymerization inhibitor is phenothiazine or hydroquinone; in step (21), the temperature of the reaction is 85 to 95 ℃ (e.g., may be 85 ℃, 88 ℃, 90 ℃, 92 ℃ or 95 ℃), and the time of the reaction is 5 to 7 hours (e.g., may be 5 hours, 6 hours or 7 hours); in step (22), the temperature of the reaction is 55 to 65 ℃ (for example, may be 55 ℃, 58 ℃, 60 ℃, 62 ℃ or 65 ℃), and the reaction is 2 to 3 hours (for example, may be 2 hours, 2.2 hours, 2.5 hours, 2.7 hours, 2.8 hours or 3 hours); in the invention, when boric acid monomer is prepared, N-dihydroxyethyl alkylamine, triethyl borate and solvent are specifically added into a four-neck flask provided with an electric stirring device, an oil-water separator and a vacuum pressure reducing device, the oil-water separator is preloaded with zinc chloride solid so as to remove ethanol generated by the reaction through reduced pressure reflux, the reaction temperature is controlled through a water bath, the vacuum degree is controlled to be 0.04MPa, normal reflux is ensured, after 1-1.5 h of reaction, N-methylolacrylamide and a polymerization inhibitor are added into the reaction device, the reaction is continued for 1-1.5 h at the same temperature, after stopping the reaction, the solvent is removed through reduced pressure distillation, then the reaction solution is poured into acetone, the homopolymerized product insoluble in the acetone is filtered and removed, and finally the acetone is removed through reduced pressure distillation, so that boric acid monomer is obtained.
According to some preferred embodiments, the alkyl halide is at least one of bromododecane, bromotetradecane, or bromohexadecane; at least one kind is a mixture obtained by mixing any one or more kinds of materials in any proportion; in the present invention, the ratio of the amounts of the substances of the haloalkane, diethanolamine and the first solvent is 1: (1.2-1.5): (25-28) (e.g., may be 1:1.2:25, 1:1.3:26, 1:1.4:27, 1:1.5:28); the ratio of the amounts of the substances of N, N-dihydroxyethyl alkylamine, triethylborate and N-methylolacrylamide is 1: (0.2-0.5): (0.2-0.5) (e.g., may be 1:0.2:0.2, 1:0.4:0.2, 1:0.5:0.2, 1:0.2:0.3, 1:0.3:0.4, or 1:0.4:0.5); the ratio of the amounts of the substances of triethyl borate, solvent and polymerization inhibitor is 1: (30-50): (0.005-0.01) (e.g., may be 1:30:0.005, 1:40:0.006, 1:50:0.008, 1:30:0.01, 1:40:0.01, or 1:50:0.01); in the invention, N-dihydroxyethyl alkylamine, triethyl borate and N-methylol acrylamide are used as reaction raw materials, firstly N, N-dihydroxyethyl hexadecylamine and triethyl borate can be connected together through substitution reaction, ethanol is generated when the N, N-dihydroxyethyl hexadecylamine and the triethyl borate are subjected to substitution reaction, so that the generated ethanol can be removed through reduced pressure reflux in the reaction process, then N-methylol acrylamide with double bonds and a polymerization inhibitor are added into a reaction system to continue reaction, hydroxyl in the N-methylol acrylamide can be subjected to substitution reaction with ethyl branched on the triethyl borate, so that the hydroxyl in the N-methylol acrylamide can be connected together, and the polymerization inhibitor can prevent the N-methylol acrylamide from self-polymerizing.
According to some preferred embodiments, the first cationic monomer is at least one of N, N-dimethylaminoethyl acrylate, N-dimethylaminoethyl methacrylate or N, N-dimethylaminopropyl acrylamide; the second cationic monomer is at least one of acryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride, dimethyl diallyl ammonium chloride, acryloyloxyethyl dimethyl benzyl ammonium chloride or methacryloyloxyethyl dimethyl benzyl ammonium chloride; the inorganic salt is at least one of anhydrous sodium sulfate, ammonium sulfate or sodium chloride; firstly, an azo initiator, a metal complexing agent and a redox initiator are adopted to react with a first cationic monomer to form a prepolymer, then the prepolymer and other monomers are subjected to water-in-water polymerization, and the prepolymer not only can play a good dispersing role in the subsequent water-in-water polymerization process, but also can provide a part of positive charges, so that the finally formed polymer can adsorb fine fibers; meanwhile, a second cationic monomer is further introduced in the water-in-water polymerization process, so that the positive charge density in the polymer is further increased, and the electrostatic attraction between the polymer and the surface of the fine fiber particles is increased, so that the retention and filtration effects of the polymer are further enhanced.
According to some preferred embodiments, the azo-based initiator is at least one of azobisisobutyronitrile, azobisisobutylamidine hydrochloride or azobisisob Ding Mi hydrochloride;
the metal complexing agent is at least one of disodium ethylenediamine tetraacetate, trisodium diethylenetriamine pentaacetate, sodium ethylenediamine tetramethylene phosphate or sodium citrate;
the oxidant in the redox initiator is at least one of hydrogen peroxide, di-tert-butyl peroxide, tert-butyl hydroperoxide, potassium persulfate or ammonium persulfate, and the reducing agent in the redox initiator is at least one of anhydrous sodium sulfite, sodium bisulphite or sodium thiosulfate; in the invention, the mass ratio of the oxidant to the reducer in the redox initiator is 1: (1.5-2).
According to some preferred embodiments, in step (1), the ratio of the mass of the first cationic monomer to the mass of water is 1: (5-8) (e.g., may be 1:5, 1:6, 1:7, or 1:8); the mass ratio of the first cationic monomer to the azo initiator to the metal complexing agent to the redox initiator is 1: (0.001-0.005): (0.0005-0.001): (0.005-0.01) (e.g., 1:0.001:0.0005:0.005, 1:0.002:0.0006:0.006, 1:0.003:0.0007:0.007, 1:0.004:0.0008, 0.0008, 1:0.005:0.0009:0.0009, or 1:0.005:0.001:0.001); in the invention, the mass ratio of the first cationic monomer to the water is preferably in the above range, so that the prepared prepolymer is more beneficial to playing a dispersing role in the subsequent water-in-water polymerization, and if the addition amount of the first cationic monomer is too small, the collision probability among molecules is reduced, the molecular chain of the formed polymer is shortened, and the dispersing performance of the prepolymer is further adversely affected.
According to some preferred embodiments, in step (2), the ratio of the mass of boric acid monomer, inorganic salt, acrylamide, second cationic monomer, prepolymer and water is (0.03-0.05): (0.1-0.3): (0.05-0.1): (0.06-0.1): (0.05-0.1): (0.5-0.8) (e.g., may be 0.03:0.1:0.05:0.06:0.05:0.5, 0.03:0.2:0.06:0.05:0.6, 0.03:0.3:0.08:0.06:0.05:0.7, 0.04:0.2:0.08:0.06:0.08:0.5, 0.05:0.1:0.05:0.05:0.05:0.5, 0.05:0.2:0.08:0.09:0.08:0.8, or 0.05:0.3:0.1:0.1:0.1:0.8); in the water-in-water polymerization process, the mass ratio of the substances is preferably within the range, so that the polymer formed by water-in-water polymerization can be ensured to have higher solubility, and better retention and filtration effects and shearing resistance can be achieved; the double bond structure in the boric acid monomer can participate in the polymerization reaction, so that the formed polymer is of a macromolecular long-chain structure, if the addition amount of the boric acid monomer is too small, the content of boric acid groups in the formed polymer is reduced, and then the bonding sites of the polymer and hydroxyl groups in the fiber are reduced, so that the performance of the polymer for adhering the fine fiber is adversely affected; if the adding amount of the boric acid monomer is too large, the crosslinking degree is too high, so that the uniformity of the paper is uneven, the strength is reduced, and the local filtering assisting effect is poor; a certain amount of inorganic salt is added in the water-in-water polymerization, so that the polymer can be separated out from the water solution, and the water-in-water polymerization efficiency is effectively improved; if the amount of the inorganic salt added is too small, the solubility of the polymer in water is not favorably lowered, the polymer is dissolved in water, the rate of polymerization in water is lowered, and if the amount of the inorganic salt added is too large, the rate of polymerization in water can be increased to some extent, but the solubility of the finally formed polymer is deteriorated, which is not favorable for field application.
According to some preferred embodiments, the mass ratio of boric acid monomer, azo-based initiator, metal complexing agent and redox initiator is (0.03-0.05): (0.0003 to 0.0005): (0.00001-0.00003): (0.0001-0.0005) (e.g., can be 0.03:0.00003:0.00001:0.001, 0.04:0.00004:0.00002:0.002, 0.05:0.00005:0.00003:0.003, 0.05:0.00005:0.00004:0.004, 0.05:0.00005:0.00005:0.005).
According to some preferred embodiments, in step (1) and step (2), before introducing nitrogen, the method further comprises adding a pH regulator to the mixed solution to adjust the pH to 4.2-4.6 (for example, 4.2, 4.3, 4.4, 4.5 or 4.6), preferably, in step (1), the pH is adjusted to 4.4-4.6 (for example, 4.4, 4.5 or 4.6); before azo initiators, metal complexing agents and redox initiators are added in the step (1) and the step (2) to react, a proper amount of pH regulator can be added into the mixed solution to regulate the pH value of the solution, so that the subsequent reaction process is more favorably ensured to be carried out at a proper speed; the pH regulator in the invention can be at least one of acetic acid, hydrochloric acid, 2-acrylamide-2-methylpropanesulfonic acid or citric acid.
According to some preferred embodiments, in step (1), the temperature of the reaction is 60-65 ℃ (e.g. may be 60 ℃, 61 ℃, 62 ℃, 63 ℃, 64 ℃ or 65 ℃), the time of the reaction is 3-5 h (e.g. may be 3h, 3.5h, 4h, 4.5h or 5 h);
in step (2), the temperature of the reaction is 50 to 60 ℃ (for example, may be 50 ℃, 52 ℃, 54 ℃, 56 ℃, 58 ℃ or 60 ℃), and the time of the reaction is 3 to 5 hours (for example, may be 3 hours, 3.5 hours, 4 hours, 4.5 hours or 5 hours); meanwhile, in the invention, the reaction substances can be uniformly mixed at the rotating speed of 300-500 r/min after being mixed.
According to some preferred embodiments, the nitrogen pass time is 30-35 min (e.g., may be 30min, 31min, 32min, 33min, 34min, or 35 min); in the invention, because oxygen is taken as a polymerization inhibitor to have adverse effect on the polymerization reaction, before the initiator and the complexing agent are added to initiate the reaction, nitrogen is firstly introduced into the reaction system for a period of time, and the oxygen in the reaction system is removed to ensure that the polymerization reaction is normally carried out.
The invention also provides a water-in-water type retention and drainage aid, which is prepared by adopting the preparation method provided by the invention.
The retention and drainage aid prepared by the invention is water-in-water type, water is used as a medium for polymerization reaction in the preparation process, so that the cost is low, the influence of an organic solvent on environmental pollution can be eliminated, and compared with the dry powder retention and drainage aid in the prior art, the retention and drainage aid prepared by the invention has the advantages of high dissolution speed, good retention and drainage aid effect, excellent shearing resistance and environmental friendliness, and the problems of low dissolution speed, easiness in fish eyes generation and the like of polyacrylamide retention and drainage aid particles in the prior art can be solved; and the defect that the cost is high and the environment is polluted by adopting the water-in-oil emulsion.
In order to more clearly illustrate the technical scheme and advantages of the present invention, a water-in-water type retention and drainage agent and a preparation method thereof are described in detail below through several examples.
Example 1:
(1) 100g of a first cationic monomer (acrylic acid-N, N-dimethylaminoethyl ester) and 600g of deionized water are added into a reaction kettle provided with a stirrer, a thermometer and a nitrogen introducing pipe, uniformly mixed at a rotating speed of 300r/min, the pH value of the solution is regulated to 4.5, after nitrogen introduction for 30min, 0.2g of azo initiator (azodiisobutyronitrile), 0.05g of metal complexing agent (disodium ethylenediamine tetraacetate) and 0.6g of redox initiator (0.2 g of potassium persulfate and 0.4g of sodium bisulfite) are added, and reaction is carried out for 3.5h at 60 ℃ to obtain a prepolymer;
(2) Preparation of boric acid monomer:
(21) Adding 30.5g of haloalkane (bromohexadecane) and 12.6g of diethanol amine into 200g of first solvent (dimethylformamide), adding into a four-mouth flask with an electric stirring device and a condenser tube, uniformly mixing, adding 5g of catalyst (sodium carbonate), controlling the reaction temperature to 90 ℃ in a water bath, reacting for 6 hours, and distilling under reduced pressure to remove unreacted raw materials and solvent to obtain N, N-dihydroxyethyl hexadecylamine;
(22) Adding 32.9g of N, N-dihydroxyethyl hexadecylamine, 7.3g of triethyl borate and 156g of solvent (benzene) into a four-neck flask provided with an electric stirring device, an oil-water separator and a vacuum pressure reducing device, wherein the oil-water separator is preloaded with zinc chloride solid so as to remove ethanol generated by the reaction through reduced pressure reflux, the water bath temperature is controlled to be 60 ℃, the vacuum degree is 0.04MP, normal reflux is ensured, after stirring and reacting for 1h at 300r/min, 5g of N-methylolacrylamide and 0.06g of polymerization inhibitor (phenothiazine) are added, after continuing the reflux and reacting for 1.5h, stopping the reaction, and removing the solvent through reduced pressure distillation, thus obtaining boric acid monomer;
50g of boric acid monomer, 300g of inorganic salt (ammonium sulfate), 100g of acrylamide, 100g of second cationic monomer (methacryloxyethyl trimethyl ammonium chloride) and 100g of prepolymer are added into 500g of deionized water, uniformly mixed at the rotating speed of 300r/min, the pH value of the solution is regulated to 4.3, after 30min of nitrogen is introduced, 0.4g of azo initiator (azodiisobutyronitrile), 0.02g of metal complexing agent (disodium ethylenediamine tetraacetate) and 0.3g of redox initiator (0.1 g of potassium persulfate and 0.2g of sodium bisulphite) are added, and the reaction is carried out for 4h at 55 ℃ to obtain the water-in-water retention and drainage aid.
Example 2:
(1) 100g of a first cationic monomer (acrylic acid-N, N-dimethylaminoethyl ester) and 600g of deionized water are added into a reaction kettle provided with a stirrer, a thermometer and a nitrogen introducing pipe, uniformly mixed at a rotating speed of 350r/min, the pH value of the solution is regulated to 4.4, after nitrogen introduction for 32min, 0.2g of azo initiator (azo diisobutylamidine hydrochloride), 0.05g of metal complexing agent (diethyl triamine pentaacetic acid trisodium salt) and 0.6g of redox initiator (0.2 g of hydrogen peroxide and 0.4g of sodium thiosulfate) are added, and reaction is carried out for 3 hours at 62 ℃ to obtain a prepolymer;
(2) Preparation of boric acid monomer:
(21) Adding 27.7g of haloalkane (bromotetradecane) and 12.6g of diethanol amine into 200g of a first solvent (dimethylformamide), adding into a four-neck flask provided with an electric stirring device and a condenser tube, uniformly mixing, adding 5g of catalyst (and sodium carbonate), controlling the reaction temperature to 90 ℃ in a water bath, reacting for 6 hours, and distilling under reduced pressure to remove unreacted raw materials and solvent to obtain N, N-dihydroxyethyltetradecylamine;
(22) Adding 30.1g of N, N-dihydroxyethyl tetradecylamine, 7.3g of triethyl borate and 156g of solvent (benzene) into a four-neck flask provided with an electric stirring device, an oil-water separator and a vacuum pressure reducing device, wherein the oil-water separator is preloaded with zinc chloride solid so as to remove ethanol generated by the reaction through reduced pressure reflux, the water bath temperature is controlled to be 60 ℃, the vacuum degree is 0.04MP, normal reflux is ensured, after stirring and reacting for 1h at 300r/min, 5g of N-methylolacrylamide and 0.06g of polymerization inhibitor (phenothiazine) are added, after continuing the reflux and reacting for 1.5h, stopping the reaction, and removing the solvent through reduced pressure distillation, thereby obtaining boric acid monomer;
adding 40g of boric acid monomer, 200g of inorganic salt (anhydrous sodium sulfate), 75g of acrylamide, 80g of second cationic monomer (acryloyloxyethyl trimethyl ammonium chloride) and 75g of prepolymer into 700g of deionized water, uniformly mixing at the rotating speed of 350r/min, regulating the pH value of the solution to 4.5, introducing nitrogen for 32min, adding 0.4g of azo initiator (azo diisobutyl amidine hydrochloride), 0.02g of metal complexing agent (diethyl triamine penta sodium acetate) and 0.3g of redox initiator (0.1 g of hydrogen peroxide and 0.2g of sodium thiosulfate), and reacting for 3.5h at 58 ℃ to obtain the water-in-water retention and drainage aid.
Example 3:
(1) 100g of a first cationic monomer (N, N-dimethylaminopropyl acrylamide) and 600g of deionized water are added into a reaction kettle provided with a stirrer, a thermometer and a nitrogen introducing pipe, uniformly mixed at a rotating speed of 330r/min, the pH value of the solution is regulated to 4.6, after nitrogen introduction for 35min, 0.2g of azo initiator (azo diiso Ding Mi hydrochloride), 0.05g of metal complexing agent (ethylenediamine tetramethylene sodium phosphate) and 0.6g of redox initiator (0.2 g of di-tert-butyl peroxide and 0.4g of anhydrous sodium sulfite) are added, and reaction is carried out for 5h at 60 ℃ to obtain a prepolymer;
(2) Preparation of boric acid monomer:
(21) Adding 24.9g of haloalkane (bromododecane) and 12.6g of diethanol amine into 200g of a first solvent (dimethylformamide), adding into a four-mouth flask provided with an electric stirring device and a condenser tube, uniformly mixing, adding 5g of catalyst (sodium carbonate), controlling the reaction temperature to 90 ℃ in a water bath, reacting for 6 hours, and distilling under reduced pressure to remove unreacted raw materials and the solvent to obtain N, N-dihydroxyethyl dodecylamine;
(22) Adding 27.3g of N, N-dihydroxyethyl dodecylamine into a four-neck flask provided with an electric stirring device, an oil-water separator and a vacuum pressure reducing device, wherein the oil-water separator is preloaded with zinc chloride solid so as to remove ethanol generated by the reaction through reduced pressure reflux, the water bath temperature is controlled to be 60 ℃, the vacuum degree is 0.04MP, normal reflux is ensured, after stirring and reacting for 1h at 300r/min, 5g of N-methylolacrylamide and 0.033g of polymerization inhibitor (hydroquinone) are added, after continuing the reflux and reacting for 1.5h, stopping the reaction, and the solvent is removed through reduced pressure distillation, thus obtaining boric acid monomers;
30g of boric acid monomer, 100g of inorganic salt (sodium chloride), 50g of acrylamide, 60g of second cationic monomer (methacryloxyethyl dimethyl benzyl ammonium chloride) and 50g of prepolymer are added into 800g of deionized water, uniformly mixed at the rotating speed of 330r/min, the pH value of the solution is regulated to 4.6, after nitrogen is introduced for 35min, 0.4g of azo initiator (azo diiso Ding Mi hydrochloride), 0.02g of metal complexing agent (ethylenediamine tetramethylene sodium phosphate) and 0.3g of redox initiator (0.1 g of di-tert-butyl peroxide and 0.02g of anhydrous sodium sulfite) are added, and the reaction is carried out for 3h at 60 ℃ to obtain the water-in-water retention and drainage aid.
Example 4:
example 4 is substantially the same as example 1 except that: in the step (1), in the preparation of the prepolymer, the first cationic monomer is methacryloyloxyethyl trimethyl ammonium chloride.
Example 5:
example 5 is substantially the same as example 1 except that: in the step (1), in the process of preparing the prepolymer, the first cationic monomer is methacryloyloxyethyl trimethyl ammonium chloride; the second cationic monomer in the step (2) is acrylic acid-N, N-dimethylaminoethyl ester.
Example 6:
example 6 is substantially the same as example 1 except that: in the step (1), the addition amount of the first cationic monomer was 120g.
Example 7:
example 7 is substantially the same as example 1 except that: in the step (2), the addition amount of the boric acid monomer was 20g.
Example 8:
example 8 is substantially the same as example 1 except that: in the step (2), the addition amount of the boric acid monomer was 60g.
Example 9:
example 9 is substantially the same as example 1 except that: in the step (2), the amount of the prepolymer added was 40g.
Example 10:
example 10 is substantially the same as example 1 except that: in the step (2), the amount of the prepolymer added was 110g.
Example 11:
example 11 is substantially the same as example 1 except that: in the step (2), the amount of the inorganic salt added was 90g.
Example 12:
example 12 is substantially the same as example 1 except that: when preparing the boric acid monomer, the amount of triethyl borate added was 292g.
Example 13:
example 13 is substantially the same as example 1 except that: when boric acid monomer was prepared, the amount of triethyl borate added was 146g.
Example 14:
example 14 is substantially the same as example 1 except that: in the preparation of the boric acid monomer, N, N-dihydroxyethyl alkylamine (N, N-dihydroxyethyl hexadecylamine) was added in an amount of 493.5.
Example 15:
example 16 is substantially the same as example 1 except that: the amount of N-methylolacrylamide added in the preparation of the boric acid monomer was 173.3g.
Example 16:
example 16 is substantially the same as example 1 except that: the amount of N-methylolacrylamide added in the preparation of the boric acid monomer was 86.7g.
Comparative example 1:
comparative example 1 is substantially the same as example 1 except that: in step (2), no boric acid monomer is added.
Comparative example 2:
comparative example 2 is substantially the same as example 1 except that: in step (2), the second cationic monomer is not added.
Comparative example 3:
comparative example 3 is substantially the same as example 1 except that: in step (2), the boric acid monomer is replaced with p-carboxyphenylboronic acid.
Comparative example 4:
comparative example 4 is substantially the same as example 1 except that: in step (2), the boric acid monomer is replaced with 3-acrylamidophenylboric acid.
Comparative example 5:
comparative example 5 was prepared as follows: 10g of polyvinyl amine and 1000mL of water are stirred and mixed at the normal temperature (25 ℃) at 300 r/min; then 10g of p-carboxyphenylboronic acid was added, stirred for 50min, then heated to 40℃and 0.1M diluted hydrochloric acid was added to adjust the pH of the solution to 6.0, 10g of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride was slowly added under nitrogen protection, stirred for 3h and then cooled to room temperature (25 ℃): collecting the reaction solution, separating in a regenerated cellulose dialysis membrane (with molecular weight cut-off of 1.2 ten thousand) for 3 days, and drying the solution at-45deg.C under vacuum degree of 8Pa to obtain the retention and filter aid.
The retention and drainage aids prepared in examples 1 to 16 and comparative examples 1 to 5 were subjected to performance testing by the following specific test methods:
(1) Retention and drainage aid performance test: setting the basis weight of paper to be 60 g/square meter, the filling amount of talcum powder to be 15wt%, and the mass of single handsheet to be 1.884g, wherein 1.6014g of absolute dry pulp and 0.2826g of talcum powder are contained; accurately weighing 1.6014g of absolute dry pulp and 0.2826g of talcum powder, wherein the absolute dry weight of the paper material is the sum of the mass of the absolute dry pulp and the mass of the talcum powder; putting the mixture into a 1000mL beaker, adding water, uniformly dispersing the mixture by using a stirrer, adding 0.06 percent (based on absolute dry pulp) of reagent (namely, the retention and drainage aid prepared in the examples and the comparative examples) into the dispersed pulp, continuously stirring the mixture for 5 minutes, then carrying out sheet making on a sheet making machine, and drying the handsheet at a constant temperature of 105 ℃;
drying the handsheet in a forced air drying oven at 105 ℃ for 5 hours, weighing the dried handsheet weight to be the absolute dry weight of the paper sheet, and calculating the retention rate of the paper stock by using the following formula; retention%paper =sheet absolute dry weight%100%/sheet absolute dry weight;
accurately weighing 2g of absolute dry pulp, adding water, uniformly dispersing by using a stirrer, then adding 0.06% (based on absolute dry pulp) of a reagent (namely, the retention and drainage aid prepared in the examples and the comparative examples), stirring for 5 minutes, finally accurately preparing 1000mL of pulp, and measuring the beating degree to obtain the filtration-assisting performance;
(2) Shear resistance test: the retention and drainage aids prepared in examples 1 to 16 and comparative examples 1 to 5 were subjected to shear at 30℃and 511r/s for 120min, and then subjected to retention and drainage aid performance test according to step (1), and the data before and after shear were compared to determine the shear resistance.
TABLE 1
As can be seen from Table 1, after the retention and drainage aid prepared in the embodiment of the invention is added into paper pulp for papermaking, the retention rate of fibers at the net part in the papermaking process can be effectively improved, the loss of fine fibers and fillers in the papermaking process is avoided, and after the retention and drainage aid in the embodiment of the invention is sheared for 120min, the retention and drainage aid still has a good retention and drainage aid effect, which indicates that the retention and drainage aid in the embodiment of the invention has excellent shearing resistance and stable retention and drainage aid effect, and in addition, the retention and drainage aid in the invention is water-in-water type, and has the advantages of higher dissolution speed and no pollution.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (12)
1. A method for preparing a water-in-water retention and drainage aid, which is characterized by comprising the following steps:
(1) Uniformly mixing a first cationic monomer with water, introducing nitrogen, and then adding an azo initiator, a metal complexing agent and a redox initiator for reaction to obtain a prepolymer; the first cationic monomer is at least one of acrylic acid-N, N-dimethylaminoethyl ester, methacrylic acid-N, N-dimethylaminoethyl ester or N, N-dimethylaminopropyl acrylamide;
(2) Adding boric acid monomer, inorganic salt, acrylamide, second cationic monomer and prepolymer into water, uniformly mixing, introducing nitrogen, and then adding azo initiator, metal complexing agent and redox initiator for reaction to obtain the water-in-water retention and drainage aid; the second cationic monomer is at least one of acryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride, dimethyl diallyl ammonium chloride, acryloyloxyethyl dimethyl benzyl ammonium chloride or methacryloyloxyethyl dimethyl benzyl ammonium chloride;
the boric acid monomer is prepared by substitution reaction, and the raw materials for preparing the boric acid monomer comprise N, N-dihydroxyethyl alkylamine, triethyl borate and N-methylolacrylamide;
boric acid monomer with the following structural formula:
wherein R is dodecane, tetradecane or hexadecane.
2. The method of manufacturing according to claim 1, wherein:
the preparation method of the boric acid monomer comprises the following steps:
(21) Adding haloalkane and diethanolamine into a first solvent, uniformly mixing and reacting to obtain N, N dihydroxyethyl alkylamine;
(22) Adding the N, N-dihydroxyethyl alkylamine and triethyl borate into a second solvent, uniformly mixing and reacting to obtain a reaction product, and adding N-methylol acrylamide and a polymerization inhibitor into the reaction product for continuous reaction to obtain a monomer containing boric acid groups.
3. The preparation method according to claim 2, wherein:
the first solvent is dimethylformamide; the second solvent is benzene or toluene; the polymerization inhibitor is phenothiazine or hydroquinone.
4. The preparation method according to claim 2, wherein:
in the step (21), the reaction temperature is 85-95 ℃, and the reaction time is 5-7 hours;
in the step (22), the reaction temperature is 55-65 ℃, and the reaction time is 1-1.5 h.
5. The preparation method according to claim 2, wherein:
the alkyl halide is at least one of bromododecane, bromotetradecane or bromohexadecane;
in step (21), the ratio of the amounts of the substances of the haloalkane, diethanolamine and first solvent is 1: (1.2 to 1.5): (25-28);
in step (22), the ratio of the amounts of the substances of N, N-dihydroxyethyl alkylamine, triethyl borate and N-methylolacrylamide is 1: (0.2 to 0.5): (0.2 to 0.5);
the ratio of the amounts of the substances of triethyl borate, the second solvent and the polymerization inhibitor is 1: (30-50): (0.005-0.01).
6. The method of manufacturing according to claim 1, wherein:
the inorganic salt is at least one of anhydrous sodium sulfate, ammonium sulfate or sodium chloride.
7. The method of manufacturing according to claim 1, wherein:
the azo initiator is at least one of azodiisobutyronitrile, azodiisobutylamidine hydrochloride or azodiiso Ding Mi hydrochloride;
the metal complexing agent is at least one of disodium ethylenediamine tetraacetate, trisodium diethylenetriamine pentaacetate, sodium ethylenediamine tetramethylene phosphate or sodium citrate;
the oxidant in the redox initiator is at least one of hydrogen peroxide, di-tert-butyl peroxide, tert-butyl hydroperoxide, potassium persulfate or ammonium persulfate, and the reducing agent in the redox initiator is at least one of anhydrous sodium sulfite, sodium bisulphite or sodium thiosulfate.
8. The method of claim 1, wherein in step (1):
the mass ratio of the first cationic monomer to water is 1: (5-8);
the mass ratio of the first cationic monomer to the azo initiator to the metal complexing agent to the redox initiator is 1: (0.001 to 0.005): (0.0005 to 0.001): (0.005-0.01).
9. The method of claim 1, wherein in step (2):
the mass ratio of boric acid monomer, inorganic salt, acrylamide, second cationic monomer, prepolymer and water is (0.03-0.05): (0.1 to 0.3): (0.05-0.1): (0.06-0.1): (0.05-0.1): (0.5 to 0.8); and/or
The mass ratio of the boric acid monomer, the azo initiator, the metal complexing agent and the redox initiator is (0.03-0.05): (0.0003 to 0.0005): (0.00001 to 0.00003): (0.0001 to 0.0005).
10. The preparation method according to claim 1, wherein,
in the step (1) and the step (2), before introducing nitrogen, adding a pH regulator into the uniformly mixed solution to regulate the pH to 4.2-4.6, and in the step (1), regulating the pH to 4.4-4.6;
the pH regulator is at least one of acetic acid, hydrochloric acid, 2-acrylamide-2-methylpropanesulfonic acid or citric acid.
11. The preparation method according to claim 1, wherein,
in the step (1), the reaction temperature is 60-65 ℃, and the reaction time is 3-5 h;
in the step (2), the reaction temperature is 50-60 ℃, and the reaction time is 3-5 h; and/or
The nitrogen introducing time is 30-35 min.
12. A water-in-water retention and drainage aid prepared by the method of any one of claims 1 to 11.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002249995A (en) * | 2001-02-21 | 2002-09-06 | Kurita Water Ind Ltd | Fixing agent for anionic rosin emulsion sizing agent and fixing method |
| CN103467642A (en) * | 2013-09-17 | 2013-12-25 | 凯瑞化工股份有限公司 | Preparation method of ethylene glycol dealdehyding resin |
| CN103772606A (en) * | 2014-01-24 | 2014-05-07 | 安徽天润化学工业股份有限公司 | Preparation method of polyacrylamide for retention and drainage of papermaking |
| CN107556432A (en) * | 2017-10-11 | 2018-01-09 | 青岛科技大学 | A kind of method added molecular weight regulator and prepare paper grade (stock) cationic retention aid filter aid |
| CN108659164A (en) * | 2018-04-28 | 2018-10-16 | 东营市诺尔化工有限责任公司 | A kind of ultra-high molecular weight cationic polyacrylamide and its preparation method and application |
| CN108690171A (en) * | 2018-06-05 | 2018-10-23 | 东营市诺尔化工有限责任公司 | A kind of water in water CPAM lotion and its preparation method and application |
| CN113087858A (en) * | 2021-05-12 | 2021-07-09 | 北京金隅水泥节能科技有限公司 | Shrinkage-reducing polycarboxylate superplasticizer and preparation method thereof |
| CN114940727A (en) * | 2022-07-22 | 2022-08-26 | 山东诺尔生物科技有限公司 | Water-in-water filtrate reducer and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6942142B2 (en) * | 2015-12-14 | 2021-09-29 | エコラブ ユーエスエイ インク | Boronic acid-containing polymer for papermaking process |
-
2022
- 2022-08-31 CN CN202211065449.7A patent/CN115286742B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002249995A (en) * | 2001-02-21 | 2002-09-06 | Kurita Water Ind Ltd | Fixing agent for anionic rosin emulsion sizing agent and fixing method |
| CN103467642A (en) * | 2013-09-17 | 2013-12-25 | 凯瑞化工股份有限公司 | Preparation method of ethylene glycol dealdehyding resin |
| CN103772606A (en) * | 2014-01-24 | 2014-05-07 | 安徽天润化学工业股份有限公司 | Preparation method of polyacrylamide for retention and drainage of papermaking |
| CN107556432A (en) * | 2017-10-11 | 2018-01-09 | 青岛科技大学 | A kind of method added molecular weight regulator and prepare paper grade (stock) cationic retention aid filter aid |
| CN108659164A (en) * | 2018-04-28 | 2018-10-16 | 东营市诺尔化工有限责任公司 | A kind of ultra-high molecular weight cationic polyacrylamide and its preparation method and application |
| CN108690171A (en) * | 2018-06-05 | 2018-10-23 | 东营市诺尔化工有限责任公司 | A kind of water in water CPAM lotion and its preparation method and application |
| CN113087858A (en) * | 2021-05-12 | 2021-07-09 | 北京金隅水泥节能科技有限公司 | Shrinkage-reducing polycarboxylate superplasticizer and preparation method thereof |
| CN114940727A (en) * | 2022-07-22 | 2022-08-26 | 山东诺尔生物科技有限公司 | Water-in-water filtrate reducer and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| The Surface Activity of Borate Surfmers with Different Hydrophobic Chain Length and Their Mixing Effect with Hexadecyl Trimethyl Ammonium Bromide;Zhengyong Liang，等;journal of surfactants and detergents;第15卷(第2期);217-222 * |
| 可聚硼酸酯表面活性剂的表面化学性质及与LAS相互作用;王海鹰，等;物理化学学报;第02卷;253-257 * |
| 新型聚合硼酸酯表面活性剂PBE的合成及其性能;王海鹰;李斌栋;林卫娜;吕春绪;;应用化学(第03期);253-257 * |
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