CN107117855B - 一种聚羧酸系混凝土减水剂及其制备方法 - Google Patents
一种聚羧酸系混凝土减水剂及其制备方法 Download PDFInfo
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- CN107117855B CN107117855B CN201710291993.6A CN201710291993A CN107117855B CN 107117855 B CN107117855 B CN 107117855B CN 201710291993 A CN201710291993 A CN 201710291993A CN 107117855 B CN107117855 B CN 107117855B
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 42
- 239000002253 acid Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000003607 modifier Substances 0.000 claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 12
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 12
- 239000003999 initiator Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000002105 nanoparticle Substances 0.000 claims abstract description 11
- 239000000853 adhesive Substances 0.000 claims abstract description 10
- 230000001070 adhesive effect Effects 0.000 claims abstract description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 9
- 229920001661 Chitosan Polymers 0.000 claims abstract description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 9
- 125000000129 anionic group Chemical group 0.000 claims abstract description 9
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 9
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 8
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims abstract description 8
- RGHNJXZEOKUKBD-SQOUGZDYSA-N Gluconic acid Natural products OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims abstract description 8
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract description 8
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 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 abstract description 8
- 239000000835 fiber Substances 0.000 claims abstract description 8
- 239000000174 gluconic acid Substances 0.000 claims abstract description 8
- 235000012208 gluconic acid Nutrition 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 235000002906 tartaric acid Nutrition 0.000 claims abstract description 8
- 239000011975 tartaric acid Substances 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 10
- 230000001603 reducing effect Effects 0.000 claims description 7
- 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 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 claims description 6
- 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
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 claims description 4
- 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 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- ZJCZFAAXZODMQT-UHFFFAOYSA-N 2-methylpentadecane-2-thiol Chemical compound CCCCCCCCCCCCCC(C)(C)S ZJCZFAAXZODMQT-UHFFFAOYSA-N 0.000 claims description 3
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 3
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- 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 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 3
- 239000012028 Fenton's reagent Substances 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- CTFVTWODMRTVCA-UHFFFAOYSA-N [K+].[Cu+3] Chemical compound [K+].[Cu+3] CTFVTWODMRTVCA-UHFFFAOYSA-N 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 3
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 claims description 3
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 3
- 239000012452 mother liquor Substances 0.000 claims description 3
- 125000005010 perfluoroalkyl group Chemical group 0.000 claims description 3
- ZOCLAPYLSUCOGI-UHFFFAOYSA-M potassium hydrosulfide Chemical compound [SH-].[K+] ZOCLAPYLSUCOGI-UHFFFAOYSA-M 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
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 0.000 claims description 3
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- MGZTXXNFBIUONY-UHFFFAOYSA-N hydrogen peroxide;iron(2+);sulfuric acid Chemical compound [Fe+2].OO.OS(O)(=O)=O MGZTXXNFBIUONY-UHFFFAOYSA-N 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- FPNCFEPWJLGURZ-UHFFFAOYSA-L iron(2+);sulfite Chemical compound [Fe+2].[O-]S([O-])=O FPNCFEPWJLGURZ-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- OKJMLYFJRFYBPS-UHFFFAOYSA-J tetraazanium;cerium(4+);tetrasulfate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[Ce+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OKJMLYFJRFYBPS-UHFFFAOYSA-J 0.000 claims description 2
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 24
- 239000001569 carbon dioxide Substances 0.000 description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 description 12
- 230000000694 effects Effects 0.000 description 4
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- 230000008719 thickening Effects 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 230000000740 bleeding effect Effects 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
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- 125000000524 functional group Chemical group 0.000 description 2
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- 238000005204 segregation Methods 0.000 description 2
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- 238000005303 weighing Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 206010016807 Fluid retention Diseases 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 238000012644 addition polymerization Methods 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
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- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
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- 230000007797 corrosion Effects 0.000 description 1
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- 150000002170 ethers Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- LIRDHUDRLFDYAI-UHFFFAOYSA-H iron(3+);trisulfite Chemical compound [Fe+3].[Fe+3].[O-]S([O-])=O.[O-]S([O-])=O.[O-]S([O-])=O LIRDHUDRLFDYAI-UHFFFAOYSA-H 0.000 description 1
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- 239000002023 wood Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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- 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
- C08J2333/00—Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2335/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical, and containing at least one other carboxyl radical in the molecule, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Derivatives of such polymers
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- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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- C08J2433/00—Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/18—Homopolymers or copolymers of nitriles
- C08J2433/20—Homopolymers or copolymers of acrylonitrile
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- C08J2439/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Derivatives of such polymers
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
本发明公开了一种聚羧酸系混凝土减水剂及其制备方法，该减水剂由以下质量百分比的原料制备而成：聚羧酸系减水剂5‑15％、壳聚糖纤维0.08‑12.6％、聚羧酸保坍剂1‑4％、纳米水性粘合剂4‑8％、阴离子聚丙烯酰胺3‑5％、聚二甲基二烯丙基氯化铵3.7‑8.3％、聚乙二醇丙烯酸酯0.004‑1％、无机纳米粒子1.5‑3.5％、耐化学品改性剂5‑10％、牡蛎壳粉3‑6％、羟基羧酸盐1‑3.5％、酒石酸1‑2％、葡萄糖酸1‑2％、引发剂3‑5％、AS树脂1‑4％，余量水。本发明所得的减水剂可以显著减少和用水，使得混凝土的和易性好，并能有效减少混凝土拌合物的坍落度损失，保持其良好的流动性能。
Description
技术领域
本发明涉及建筑材料领域，具体涉及一种聚羧酸系混凝土减水剂及其制备方法。
背景技术
减水剂在混凝土中的使用，可显著改善混凝土的工作性能、提高混凝土的强度和耐久性。聚羧酸系高性能减水剂是继以木钙为代表的普通减水剂和以萘系为代表的高效减水剂之后发展起来的新一代减水剂，具有低掺量高分散、高减水率及绿色环保等独特优点，是当今世界最前沿、综合性能优异并被广泛应用的一类混凝土减水剂。
近年来，基于混凝土技术的发展、市场竞争、成本控制、以及商品混凝土中胶凝材料的用量减少和品质下降等因素的影响，单一的聚羧酸系减水剂很难满足预拌混凝土的粘聚性和保水性要求，致使混凝土拌合料发生泌水、离析，和易性变差及坍落度损失较大。为保证混凝土正常施工、提高工作效率，则必须复配使用增稠、保坍组份，但研究和实践均发现，聚羧酸系减水剂与部分常用的增稠及保坍组份间的相容性较差，增稠剂使用的效率不高，这为聚羧酸系减水剂的增稠型复配工作带来了很大难度，使生产工艺变得更为复杂；此外，现在市场上聚羧酸系减水剂的合成工艺，主要是由聚氧化烯基醚类不饱和大单体和/或聚氧化烯基酯类不饱和大单体、不饱和羧酸和/或不饱和酸酐，不饱和羧酸衍生物和/或不饱和醚等石油基单体经过加成聚合反应得到的产物，石油资源的日趋枯竭将使得以石油基单体为原料的石化行业难以为继。同时目前市场上所使用的减水剂存在着掺量大，减水性差，增塑效果差的缺点，无法满足市场的要求。
发明内容
为解决上述问题，本发明提供了一种聚羧酸系混凝土减水剂及其制备方法。
为实现上述目的，本发明采取的技术方案为：
一种聚羧酸系混凝土减水剂，由以下质量百分比的原料制备而成：
聚羧酸系减水剂5-15％、壳聚糖纤维0.08-12.6％、聚羧酸保坍剂1-4％、纳米水性粘合剂4-8％、阴离子聚丙烯酰胺3-5％、聚二甲基二烯丙基氯化铵3.7-8.3％、聚乙二醇丙烯酸酯0.004-1％、无机纳米粒子1.5-3.5％、耐化学品改性剂5-10％、牡蛎壳粉3-6％、羟基羧酸盐1-3.5％、酒石酸1-2％、葡萄糖酸1-2％、引发剂3-5％、AS树脂1-4％，余量水。
优选地，所述聚羧酸系减水剂为丙烯酸类、甲基丙烯酸类或马来酸酐类聚羧酸系减水母液。
优选地，所述无机纳米粒子为纳米二氧化硅、纳米蒙脱土中的一种或两种的混合。
优选地，所述耐化学品改性剂为含有全氟烷基的丙烯酸系添加剂，分子量为1000-10000，为液体形态存在。
优选地，所述引发剂为过硫酸铵，过硫酸钾，过硫酸钠，偶氮二异丁腈，过氧化氢，二过碘酸合铜(III)钾，过氧乙酸，亚硫酸铁，巯基乙酸，亚硫酸钠，Fenton试剂，硫化钠，过氧化苯甲酰，硫氢化钠，硫化钾，硫氢化钾，抗坏血酸，硝酸铈铵，硫酸亚铁铵，硫酸亚铁，硫酸铈铵，巯基丙酸，乙二胺，乙二胺四乙酸，N，N，N’，N’-四甲基乙二胺，十二烷基硫醇，十六烷基硫醇中的至少一种。
优选地，所述的AS树脂的重均分子量为3-10W，AN含量为20-35％。
本发明还提供了上述聚羧酸系混凝土减水剂的制备方法，包括如下步骤：
S1、按上述的配方量取各原料；
S2、将量取的壳聚糖纤维、纳米水性粘合剂、阴离子聚丙烯酰胺、聚二甲基二烯丙基氯化铵、聚乙二醇丙烯酸酯、耐化学品改性剂、牡蛎壳粉、羟基羧酸盐、酒石酸、葡萄糖酸、AS树脂置于双螺杆挤出机中，控制螺杆转速为180-600rpm，将液态二氧化碳充入输送泵，加热该二氧化碳至临界温度(31℃)或者更高温度以便将其转化为超临界二氧化碳，然后将超临界二氧化碳在挤出机三-四区和五-八区分别注入，经过熔融挤出，得混合物；
S3、将所得的混合物和无机纳米粒子通过超声波振荡设备分散于所量取的水中，得混合液；
S4、在所得的混合液中加入所称取的引发剂在0-80℃的温度下引发聚合，即得。
优选地，所述超临界二氧化碳流速为1mL/min-50mL/min。
优选地，双螺杆挤出机的螺杆组合中引入拉伸流元件。
优选地，所述双螺杆挤出机包括10个温控区，温控1-2区的温度为100-150℃，温控3-4区的温度为100-150℃，温控5-6区的温度为100-150℃，温控7-8区的温度为100-150℃，温控9-10区的温度为100-150℃，各区的压力为2-15MPa。
本发明具有以下有益效果：
阴离子聚丙烯酰胺、聚乙二醇丙烯酸酯、聚二甲基二烯丙基氯化铵等可聚合交联形成含阳离子、阴离子、非离子基团的网状结构，既可吸附阴离子，又能吸附阳离子，由于其定向的吸附作用大大提高了混凝土的流动性；引用低分子量的AS树脂，进一步增加其流动性，纳米水性粘合剂富含大量羟基和羧基功能基团，添加到混凝土中后其功能基团通过静电吸附作用，能团聚和混凝土微粒，形成具有团粒结构的大粒径混凝土颗粒，有效改良混凝土结构；耐化学品改性剂的添加大大提高了减水剂的防腐性能；本发明对聚合物的结构进行调控，将壳聚糖引入聚合反应合成了聚羧酸系减水剂，所得到的减水剂不仅减水率高，且能够明显改善混凝土易离析、泌水现象，使得混凝土的和易性好，并能有效减少混凝土拌合物的坍落度损失，保持其良好的流动性能，且对混凝土的强度增长效果显著。
具体实施方式
为了使本发明的目的及优点更加清楚明白，以下结合实施例对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
以下实施例中所使用的聚羧酸系减水剂为丙烯酸类、甲基丙烯酸类或马来酸酐类聚羧酸系减水母液，所述无机纳米粒子为纳米二氧化硅、纳米蒙脱土中的一种或两种的混合，所述耐化学品改性剂为含有全氟烷基的丙烯酸系添加剂，分子量为1000-10000，为液体形态存在，所述引发剂为过硫酸铵，过硫酸钾，过硫酸钠，偶氮二异丁腈，过氧化氢，二过碘酸合铜(III)钾，过氧乙酸，亚硫酸铁，巯基乙酸，亚硫酸钠，Fenton试剂，硫化钠，过氧化苯甲酰，硫氢化钠，硫化钾，硫氢化钾，抗坏血酸，硝酸铈铵，硫酸亚铁铵，硫酸亚铁，硫酸铈铵，巯基丙酸，乙二胺，乙二胺四乙酸，N，N，N’，N’-四甲基乙二胺，十二烷基硫醇，十六烷基硫醇中的至少一种，所述的AS树脂的重均分子量为3-10W，AN含量为20-35％。
实施例1
一种聚羧酸系混凝土减水剂，由以下质量百分比的原料制备而成：
聚羧酸系减水剂5％、壳聚糖纤维0.08％、聚羧酸保坍剂1％、纳米水性粘合剂4％、阴离子聚丙烯酰胺3％、聚二甲基二烯丙基氯化铵3.7％、聚乙二醇丙烯酸酯0.004％、无机纳米粒子1.5％、耐化学品改性剂5％、牡蛎壳粉3％、羟基羧酸盐1％、酒石酸1％、葡萄糖酸1％、引发剂3％、AS树脂1％，余量水。
实施例2
一种聚羧酸系混凝土减水剂，由以下质量百分比的原料制备而成：
聚羧酸系减水剂15％、壳聚糖纤维12.6％、聚羧酸保坍剂4％、纳米水性粘合剂8％、阴离子聚丙烯酰胺5％、聚二甲基二烯丙基氯化铵8.3％、聚乙二醇丙烯酸酯1％、无机纳米粒子3.5％、耐化学品改性剂10％、牡蛎壳粉6％、羟基羧酸盐3.5％、酒石酸2％、葡萄糖酸2％、引发剂5％、AS树脂4％，余量水。
实施例3
一种聚羧酸系混凝土减水剂，由以下质量百分比的原料制备而成：
聚羧酸系减水剂10％、壳聚糖纤维6.34％、聚羧酸保坍剂2.5％、纳米水性粘合剂6％、阴离子聚丙烯酰胺4％、聚二甲基二烯丙基氯化铵6％、聚乙二醇丙烯酸酯0.502％、无机纳米粒子2.5％、耐化学品改性剂7.5％、牡蛎壳粉4.5％、羟基羧酸盐2.25％、酒石酸1.5％、葡萄糖酸1.5％、引发剂4％、AS树脂2.5％，余量水
本发明还提供了一种聚羧酸系混凝土减水剂的制备方法，包括如下步骤：
S1、按实施例1-3所述的配方量取各原料；
S2、将量取的壳聚糖纤维、纳米水性粘合剂、阴离子聚丙烯酰胺、聚二甲基二烯丙基氯化铵、聚乙二醇丙烯酸酯、耐化学品改性剂、牡蛎壳粉、羟基羧酸盐、酒石酸、葡萄糖酸、AS树脂置于双螺杆挤出机中，控制螺杆转速为180-600rpm，将液态二氧化碳充入输送泵，加热该二氧化碳至临界温度(31℃)或者更高温度以便将其转化为超临界二氧化碳，然后将超临界二氧化碳在挤出机三-四区和五-八区分别注入，经过熔融挤出，得混合物；所述超临界二氧化碳流速为1mL/min-50mL/min，双螺杆挤出机的螺杆组合中引入拉伸流元件，所述双螺杆挤出机包括10个温控区，温控1-2区的温度为100-150℃，温控3-4区的温度为100-150℃，温控5-6区的温度为100-150℃，温控7-8区的温度为100-150℃，温控9-10区的温度为100-150℃，各区的压力为2-15MPa。
S3、将所得的混合物和无机纳米粒子通过超声波振荡设备分散于所量取的水中，得混合液；
S4、在所得的混合液中加入所称取的引发剂在0-80℃的温度下引发聚合，即得。
本具体实施所得的减水剂掺量为混凝土质量的0.4％-0.8％即可，减水率高达20％-25％，增塑效果好，可明显增大混凝土的坍落度，改善混凝土粘聚性及和易性，坍落度可增加180mm以上。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以作出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。
Claims (6)
1.一种聚羧酸系混凝土减水剂，其特征在于，由以下质量百分比的原料制备而成：
聚羧酸系减水剂5-15％、壳聚糖纤维0.08-12.6％、聚羧酸保坍剂1-4％、纳米水性粘合剂4-8％、阴离子聚丙烯酰胺3-5％、聚二甲基二烯丙基氯化铵3.7-8.3％、聚乙二醇丙烯酸酯0.004-1％、无机纳米粒子1.5-3.5％、耐化学品改性剂5-10％、牡蛎壳粉3-6％、羟基羧酸盐1-3.5％、酒石酸1-2％、葡萄糖酸1-2％、引发剂3-5％、AS树脂1-4％，余量水。
2.如权利要求1所述的一种聚羧酸系混凝土减水剂，其特征在于，所述聚羧酸系减水剂为丙烯酸类、甲基丙烯酸类或马来酸酐类聚羧酸系减水母液。
3.如权利要求1所述的一种聚羧酸系混凝土减水剂，其特征在于，所述无机纳米粒子为纳米二氧化硅、纳米蒙脱土中的一种或两种的混合。
4.如权利要求1所述的一种聚羧酸系混凝土减水剂，其特征在于，所述耐化学品改性剂为含有全氟烷基的丙烯酸系添加剂，分子量为1000-10000，为液体形态存在。
5.如权利要求1所述的一种聚羧酸系混凝土减水剂，其特征在于，所述引发剂为过硫酸铵，过硫酸钾，过硫酸钠，偶氮二异丁腈，过氧化氢，二过碘酸合铜(III)钾，过氧乙酸，亚硫酸铁，巯基乙酸，亚硫酸钠，Fenton试剂，硫化钠，过氧化苯甲酰，硫氢化钠，硫化钾，硫氢化钾，抗坏血酸，硝酸铈铵，硫酸亚铁铵，硫酸亚铁，硫酸铈铵，巯基丙酸，乙二胺，乙二胺四乙酸，N，N，N’，N’-四甲基乙二胺，十二烷基硫醇，十六烷基硫醇中的至少一种。
6.如权利要求1所述的一种聚羧酸系混凝土减水剂，其特征在于，所述的AS树脂的重均分子量为3-10W，AN含量为20-35％。
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