CN112979214B - Polyether water-retaining agent, preparation method thereof and cement-based building material - Google Patents
Polyether water-retaining agent, preparation method thereof and cement-based building material Download PDFInfo
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- CN112979214B CN112979214B CN202110200256.7A CN202110200256A CN112979214B CN 112979214 B CN112979214 B CN 112979214B CN 202110200256 A CN202110200256 A CN 202110200256A CN 112979214 B CN112979214 B CN 112979214B
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- polyether
- unsaturated
- water
- retaining agent
- agent
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- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 79
- 229920000570 polyether Polymers 0.000 title claims abstract description 79
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 65
- 239000004568 cement Substances 0.000 title claims abstract description 17
- 239000004566 building material Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 150000001408 amides Chemical class 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims abstract description 11
- RGHNJXZEOKUKBD-SQOUGZDYSA-M D-gluconate Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O RGHNJXZEOKUKBD-SQOUGZDYSA-M 0.000 claims abstract description 11
- 229940050410 gluconate Drugs 0.000 claims abstract description 11
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 11
- 239000006172 buffering agent Substances 0.000 claims abstract description 9
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- 239000010703 silicon Substances 0.000 claims abstract description 9
- 239000000872 buffer Substances 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- 229920000642 polymer Polymers 0.000 claims abstract description 3
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 19
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000003638 chemical reducing agent Substances 0.000 claims description 13
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 150000003871 sulfonates Chemical class 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 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 10
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 9
- 239000004576 sand Substances 0.000 claims description 9
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 8
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 8
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 6
- JHUFGBSGINLPOW-UHFFFAOYSA-N 3-chloro-4-(trifluoromethoxy)benzoyl cyanide Chemical group FC(F)(F)OC1=CC=C(C(=O)C#N)C=C1Cl JHUFGBSGINLPOW-UHFFFAOYSA-N 0.000 claims description 5
- 235000010323 ascorbic acid Nutrition 0.000 claims description 5
- 229960005070 ascorbic acid Drugs 0.000 claims description 5
- 239000011668 ascorbic acid Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- 239000001530 fumaric acid Substances 0.000 claims description 4
- SNVLJLYUUXKWOJ-UHFFFAOYSA-N methylidenecarbene Chemical compound C=[C] SNVLJLYUUXKWOJ-UHFFFAOYSA-N 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims description 4
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 claims description 4
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 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
- GTZCVFVGUGFEME-HNQUOIGGSA-N trans-aconitic acid Chemical compound OC(=O)C\C(C(O)=O)=C/C(O)=O GTZCVFVGUGFEME-HNQUOIGGSA-N 0.000 claims description 3
- GTZCVFVGUGFEME-UHFFFAOYSA-N trans-aconitic acid Natural products OC(=O)CC(C(O)=O)=CC(O)=O GTZCVFVGUGFEME-UHFFFAOYSA-N 0.000 claims description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- GCSJLQSCSDMKTP-UHFFFAOYSA-N ethenyl(trimethyl)silane Chemical compound C[Si](C)(C)C=C GCSJLQSCSDMKTP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 2
- 239000004567 concrete Substances 0.000 abstract description 26
- 238000005204 segregation Methods 0.000 abstract description 15
- 239000000178 monomer Substances 0.000 abstract description 11
- 239000002253 acid Substances 0.000 abstract description 4
- 125000001273 sulfonato group Chemical class [O-]S(*)(=O)=O 0.000 abstract 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 1
- 150000001735 carboxylic acids Chemical class 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 238000012360 testing method Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 description 5
- 230000000740 bleeding effect Effects 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 239000000176 sodium gluconate Substances 0.000 description 5
- 235000012207 sodium gluconate Nutrition 0.000 description 5
- 229940005574 sodium gluconate Drugs 0.000 description 5
- 239000000654 additive Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 2
- 239000010881 fly ash Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- 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 description 2
- 239000004575 stone Substances 0.000 description 2
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 description 1
- PQUXFUBNSYCQAL-UHFFFAOYSA-N 1-(2,3-difluorophenyl)ethanone Chemical compound CC(=O)C1=CC=CC(F)=C1F PQUXFUBNSYCQAL-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical class [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- HLCFGWHYROZGBI-JJKGCWMISA-M Potassium gluconate Chemical compound [K+].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O HLCFGWHYROZGBI-JJKGCWMISA-M 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229940069428 antacid Drugs 0.000 description 1
- 239000003159 antacid agent Substances 0.000 description 1
- 230000001458 anti-acid effect Effects 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 229920003086 cellulose ether Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- HNEGQIOMVPPMNR-IHWYPQMZSA-N citraconic acid Chemical compound OC(=O)C(/C)=C\C(O)=O HNEGQIOMVPPMNR-IHWYPQMZSA-N 0.000 description 1
- 229940018557 citraconic acid Drugs 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- KZCOBXFFBQJQHH-UHFFFAOYSA-N octane-1-thiol Chemical compound CCCCCCCCS KZCOBXFFBQJQHH-UHFFFAOYSA-N 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000002986 polymer concrete Substances 0.000 description 1
- 239000001508 potassium citrate Substances 0.000 description 1
- 229960002635 potassium citrate Drugs 0.000 description 1
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 1
- 235000011082 potassium citrates Nutrition 0.000 description 1
- 239000004224 potassium gluconate Substances 0.000 description 1
- 229960003189 potassium gluconate Drugs 0.000 description 1
- 235000013926 potassium gluconate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 239000011376 self-consolidating concrete Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229940047670 sodium acrylate Drugs 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 150000000000 tetracarboxylic acids Chemical class 0.000 description 1
- 150000003627 tricarboxylic acid derivatives Chemical class 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- 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
- C04B2103/46—Water-loss or fluid-loss reducers, hygroscopic or hydrophilic agents, water retention agents
- C04B2103/465—Water-sorbing agents, hygroscopic or hydrophilic agents
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention belongs to the field of building materials, and relates to a polyether water-retaining agent, a preparation method thereof and a cement-based building material containing the polyether water-retaining agent. The polymer contained in the polyether type water-retaining agent comprises unsaturated polyether structural units, unsaturated amide structural units, polyfunctional unsaturated carboxylic acid structural units, organic silicon structural units and unsaturated sulfonate structural units with specific content; in the synthesis process of the polyether water-retaining agent, gluconate and/or citrate are/is added to stabilize the pH value of a polymerization system, and the buffer is gluconate and/or citrate. According to the invention, in a system which takes unsaturated polyether and unsaturated amide as main polymerization monomers and takes organosilicon and unsaturated sulfonate as auxiliary polymerization monomers, a polycarboxylic acid monomer is introduced, and meanwhile, gluconate and/or citrate is added into the polymerization system as a buffering agent, so that the water retention and segregation resistance of concrete is improved.
Description
Technical Field
The invention belongs to the field of building materials, and particularly relates to a polyether water-retaining agent, a preparation method thereof and a cement-based building material containing the polyether water-retaining agent.
Background
With the development of building science, commercial concrete increasingly requires high slump and high fluidity in order to improve the construction performance and efficiency, and is particularly significant in underwater pile concrete, self-compacting concrete, high-rise pumping concrete and the like. However, the fluidity and cohesiveness of concrete are often incompatible, i.e., it is difficult to maintain high cohesiveness in concrete in a large flow regime. Thus, the concrete with high fluidity is easy to generate bleeding and segregation phenomena. In addition, with the gradual exhaustion of river sand resources and mineral resources in China, the large fluctuation of the grading, fineness and the like of river sand, the large-scale use of common machine-made sand with poor grain type, the fluctuation of the water retention property of cement, and the continuous popularization of the polycarboxylic acid type water reducing agent with high water reduction but higher sensitivity, the quality control of the ready-mixed concrete faces increasingly serious challenges.
In order to solve the problem of concrete workability, biological additives such as xanthan gum, cellulose ether, dextrin and the like are generally added to adjust the workability of the concrete. However, the above-mentioned bio-additives have problems of solubility and storage stability, etc., so that their use is greatly restricted.
In addition, some polymer concrete segregation resisting agents have been developed in the year. For example, CN103539889A discloses a concrete segregation reducing agent, which is prepared by copolymerizing a monomer a and a monomer B, wherein the monomer a is at least one selected from acrylamide, N-methylolacrylamide, acrylic acid and methacrylic acid, and the monomer B is at least one selected from hydroxyethyl acrylate, hydroxyethyl methacrylate, maleic anhydride, fumaric acid, polyethylene glycol maleate, citraconic acid, antacid, itaconic acid, sodium methallylate, sodium acrylate sulfonate and 2-acrylamide-2 methylpropanesulfonic acid. Although the anti-segregation agent can obtain an obvious anti-segregation effect when the dosage of the anti-segregation agent accounts for 0.01-0.01% of the concrete gel material, the anti-segregation agent needs to be synthesized under the conditions of high temperature and air isolation, the acting force of the anti-segregation agent with materials such as cement, sand and stone is poor, the bleeding segregation phenomenon can be effectively improved only by using a higher dosage, the acting time is shorter, and the effect of improving the bleeding segregation of concrete still needs to be improved.
Disclosure of Invention
The invention aims to overcome the problem that the existing high-fluidity concrete is easy to generate bleeding segregation phenomenon, and provides a novel polyether water-retaining agent, a preparation method thereof and a cement-based building material containing the polyether water-retaining agent.
The inventor of the invention finds out after intensive research that aiming at a polyether water retention agent which takes a polyether macromonomer and unsaturated amide as main polymerization monomers, polyfunctional unsaturated carboxylic acid with dicarboxylic acid, tricarboxylic acid or tetracarboxylic acid is introduced into a macromolecular chain of the polyether water retention agent, the acting force of an additive and the surface of cement can be improved through chelating chemical action with metal ions, and further the water retention and segregation resistance of concrete is improved, but the chelating action of the polyfunctional unsaturated carboxylic acid and the metal ions is easily influenced by pH value fluctuation, and the addition of gluconate and/or citrate as a buffering agent in the polymerization reaction process can obviously reduce the change of the pH value in a system, so that the chelating process is smoothly carried out, and the water retention and segregation resistance of the obtained concrete is very excellent. Based on this, the present invention has been completed.
Specifically, the invention provides a polyether water-retaining agent, wherein a polymer contained in the polyether water-retaining agent comprises a structural unit derived from unsaturated polyether, a structural unit derived from unsaturated amide, a structural unit derived from polyfunctional unsaturated carboxylic acid, a structural unit derived from organosilicon and a structural unit derived from unsaturated sulfonate in a weight ratio of 100 (55.5-85.5): 7.4-37): 3.7-5.2: 1.8-3.7; (ii) the structural units derived from a polyfunctional unsaturated carboxylic acid have a carboxylic acid functionality of at least 2; a buffering agent is added to stabilize the pH value of a polymerization system in the synthesis process of the polyether water-retaining agent, wherein the buffering agent is gluconate and/or citrate; the pH value of the polyether water-retaining agent is 5-6.
In the polyether water-retaining agent provided by the invention, the content of the structural unit derived from unsaturated polyether is 100 parts by weight; the content of the structural unit derived from the unsaturated amide is 55.5 to 85.5 parts by weight, specifically 55.5, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 85.5 parts by weight and the like; the content of the structural unit derived from the polyfunctional unsaturated carboxylic acid is 7.4 to 37 parts by weight, specifically 7.5, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37 parts by weight and the like; the structural unit derived from the silicone is contained in an amount of 3.7 to 5.2 parts by weight, and for example, may be 3.7, 3.8, 3.9, 4.0, 4.1, 4.2, 4.3, 4.4, 4.5, 4.6, 4.7, 4.8, 4.9, 5.0, 5.1, 5.2 parts by weight, or the like; the content of the structural unit derived from the unsaturated sulfonate is 1.8 to 3.7 parts by weight, and for example, may be 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3.0, 3.1, 3.2, 3.3, 3.4, 3.5, 3.6, 3.7 parts by weight, and the like.
In the present invention, the buffer is gluconate and/or citrate. The gluconate may be, for example, potassium gluconate or sodium gluconate. The citrate may be, for example, potassium citrate, sodium citrate, or the like.
In a preferred embodiment of the present invention, the weight ratio of the structural unit derived from the unsaturated polyether to the buffer is 100 (3-7.4), and for example, may be 100:3, 100:4, 100:5, 100:6, 100:7, 100:7.4, and the like.
In a preferred embodiment of the invention, the solid content of the polyether water retention agent is 8-15%.
In a preferred embodiment of the invention, the unsaturated polyether is TPEG and/or HPEG, TPEG having the formula CH2＝C(CH3)CH2CH2O(CH2CH2O)nH, HPEG molecular formula is CH2＝C(CH3)CH2O(CH2CH2O)nH and n are positive integers. In addition, the number average molecular weight of the unsaturated polyether is preferably 2300 to 2500.
In a preferred embodiment of the present invention, the polyfunctional unsaturated carboxylic acid is at least one selected from the group consisting of maleic anhydride, fumaric acid and trans-aconitic acid.
In a preferred embodiment of the invention, the unsaturated amide is acrylamide and/or methacrylamide.
In a preferred embodiment of the invention, the silicone is vinyltrimethylsilane and/or gamma-methacryloxypropyltrimethoxysilane.
In a preferred embodiment of the invention, the unsaturated sulfonate is sodium allyl sulfonate and/or sodium vinyl sulfonate.
The invention also provides a preparation method of the polyether water-retaining agent, which comprises the following steps: under the stirring condition, adding unsaturated polyether, unsaturated amide, polyfunctional unsaturated carboxylic acid, organic silicon, a buffering agent and water into a reaction kettle, uniformly mixing, adding an oxidant once again, dropwise adding a mixed aqueous solution of unsaturated sulfonate and a reducing agent, controlling the dropping within 1-4 h, stirring and reacting at room temperature for 1-5 h after the dropping is finished, and then adjusting the pH value of the obtained reaction product to 5-6; the weight ratio of the unsaturated polyether, the unsaturated amide, the polyfunctional group unsaturated carboxylic acid, the organic silicon and the unsaturated sulfonate is 100 (55.5-85.5): (7.4-37): (3.7-5.2): 1.8-3.7); the buffer is gluconate and/or citrate.
In the preparation process of the polyether water-retaining agent provided by the invention, the using amount of the unsaturated polyether is 100 parts by weight; the amount of the unsaturated amide is 55.5 to 85.5 parts by weight, specifically 55.5, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 85.5 parts by weight, or the like; the polyfunctional unsaturated carboxylic acid is used in an amount of 7.4 to 37 parts by weight, specifically 7.5, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37 parts by weight, and the like; the amount of the silicone is 3.7 to 5.2 parts by weight, for example, 3.7, 3.8, 3.9, 4.0, 4.1, 4.2, 4.3, 4.4, 4.5, 4.6, 4.7, 4.8, 4.9, 5.0, 5.1, 5.2 parts by weight, etc.; the amount of the unsaturated sulfonate to be used is 1.8 to 3.7 parts by weight, and may be, for example, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3.0, 3.1, 3.2, 3.3, 3.4, 3.5, 3.6, 3.7 parts by weight or the like.
In a preferred embodiment of the present invention, the weight ratio of the unsaturated polyether to the buffer is 100 (3 to 7.4), and may be, for example, 100:3, 100:4, 100:5, 100:6, 100:7, 100:7.4, or the like.
In a preferred embodiment of the present invention, the weight ratio of the oxidizing agent to the unsaturated polyether is (3 to 5):100, and may be, for example, 3.0:100, 3.1:100, 3.2:100, 3.3:100, 3.4:100, 3.5:100, 3.6:100, 3.7:100, 3.8:100, 3.9:100, 4.0:100, 4.1:100, 4.2:100, 4.3:100, 4.4:100, 4.5:100, 4.6:100, 4.7:100, 4.8:100, 4.9:100, 5.0:100, or the like.
In a preferred embodiment of the present invention, the weight ratio of the reducing agent to the unsaturated polyether is (1.5 to 2.2):100, and may be, for example, 1.5:100, 1.6:100, 1.7:100, 1.8:100, 1.9:100, 2.0:100, 2.1:100, 2.2:100, or the like.
In a preferred embodiment of the invention, the polyether water-retaining agent is prepared from the following raw materials in parts by weight:
and determining the use amount of the sodium hydroxide and/or potassium hydroxide aqueous solution according to the final pH value, and adjusting the final pH value to 5-6.
In a preferred embodiment of the present invention, the oxidizing agent is selected from at least one of hydrogen peroxide, potassium persulfate, and ammonium persulfate.
In a preferred embodiment of the present invention, the reducing agent is selected from at least one of ascorbic acid, sodium formaldehyde sulfoxylate and sodium bisulfite.
In addition, the invention also provides a cement-based building material which contains sand, cement, an admixture, a water reducing agent, a water retaining agent and water, wherein the water retaining agent is the polyether water retaining agent.
According to the invention, unsaturated polyether, unsaturated amide, polyfunctional unsaturated carboxylic acid, organic silicon and unsaturated sulfonate with specific dosage are used in a matching way, in a system taking unsaturated polyether and unsaturated amide as main polymerization monomers and taking organic silicon and unsaturated sulfonate as auxiliary polymerization monomers, polycarboxylic acid monomers are introduced, and gluconate and/or citrate is added into the polymerization system as a buffering agent, so that the obtained polyether water retention agent can stably generate chelation with metal ions, the acting force of an additive and the cement surface is improved, and the water retention and segregation resistance of concrete is improved.
Drawings
FIG. 1 is an infrared spectrum of a polyether water-retaining agent obtained in example 1.
Detailed Description
The present invention will be described in detail below by way of examples. The examples of embodiments are intended to be illustrative of the invention and are not to be construed as limiting the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
In the following examples and comparative examples, the parts of the raw materials are parts by weight.
Example 1
100 parts of TPEG (number average molecular weight 2400, the same below), 62.5 parts of acrylamide, 8.4 parts of maleic anhydride, 4.2 parts of gamma-methacryloxypropyltrimethoxysilane, 4.2 parts of sodium gluconate, and 729 parts of deionized water were added to the reaction kettle. After stirring for 10min, 3.6 parts of ammonium persulfate were added in one portion. Then, a mixed aqueous solution containing 1.8 parts of ascorbic acid and 2.1 parts of sodium allylsulfonate was added dropwise under stirring, and the addition was carried out for 4 hours. After the dripping is finished, stirring and reacting are continued for 2 hours. After the reaction is finished, adding the aqueous solution of sodium hydroxide into a reaction kettle, and adjusting the final pH value to 5-6 to obtain the polyether water-retaining agent with the solid content of 15%. The sample was recorded as G1. The infrared spectrum of the polyether water-retaining agent G1 (which IS separated, purified and scanned by adopting ATR accessory of Nigao force IS 5) IS shown in figure 1, and can be seen from figure 1, 3338cm-1And 3198cm-1Shows an absorption peak of N-H bond on the amide, 1778cm-1The absorption peak of carbonyl group of maleic anhydride was 1659cm-1The absorption peak of the amide at carbonyl group was 1098cm-1The peak of contraction vibration of ether bond on TPEG appeared. It can be demonstrated that acrylamide, maleic anhydride and polyether macromonomer undergo radical copolymerization.
Example 2
100 parts of TPEG, 55.5 parts of acrylamide, 7.4 parts of fumaric acid, 3.7 parts of vinyltrimethoxysilane, 3.7 parts of sodium citrate and 1440 parts of deionized water are added into the reaction kettle. After stirring for 10min, 3.0 parts of potassium persulfate was added in one portion. Then, a mixed aqueous solution containing 1.5 parts of ascorbic acid and 1.9 parts of sodium vinylsulfonate was added dropwise under stirring, and the addition was completed within 1 hour. After the dripping is finished, stirring and reacting are continued for 2 hours. After the reaction is finished, adding a sodium hydroxide aqueous solution into the reaction kettle, and adjusting the final pH value to 5-6 to obtain the polyether water-retaining agent with the solid content of 10%. The sample was recorded as G2.
Example 3
100 parts of TPEG, 55.5 parts of acrylamide, 37 parts of maleic anhydride, 3.7 parts of gamma-methacryloxypropyltrimethoxysilane, 7.4 parts of sodium gluconate and 1410 parts of deionized water were added to the reaction kettle. After stirring for 10min, 3.0 parts of ammonium persulfate was added at once. Then, a mixed aqueous solution containing 2.2 parts of ascorbic acid and 3.7 parts of sodium allylsulfonate was added dropwise under stirring, and the addition was carried out for 3 hours. After the dripping is finished, stirring and reacting are continued for 2 hours. And after the reaction is finished, adding a sodium hydroxide aqueous solution into the reaction kettle, and adjusting the final pH value to 5-6 to obtain the polyether water-retaining agent with the solid content of 10%. The sample was recorded as G3.
Example 4
100 parts of HPEG, 82.5 parts of methacrylamide, 18.5 parts of trans-aconitic acid, 5.2 parts of gamma-methacryloxypropyltrimethoxysilane, 3 parts of sodium gluconate and 1800 parts of deionized water are added into a reaction kettle. After stirring for 10min, 5.0 parts of ammonium persulfate was added at once. Then, under the condition of continuous stirring, a mixed aqueous solution containing 2.2 parts of sodium formaldehyde sulfoxylate and 1.8 parts of sodium vinylsulfonate is dropwise added, and the dropping is controlled to be finished within 3 hours. After the dripping is finished, stirring and reacting are continued for 2 hours. And after the reaction is finished, adding a sodium hydroxide aqueous solution into the reaction kettle, and adjusting the final pH value to 5-6 to obtain the polyether water-retaining agent with the solid content of 8%. The sample was recorded as G4.
Comparative example 1
104.8 parts of TPEG, 71.4 parts of acrylamide, 4.8 parts of sodium allylsulfonate, 3.8 parts of gamma-methacryloxypropyltrimethoxysilane and 1440 parts of deionized water were added to the reaction kettle. After stirring for 10min, 2.9 parts of ammonium persulfate was added at once. Then, under the condition of continuous stirring, 1.9 parts of sodium formaldehyde sulfoxylate, 23.8 parts of acrylic acid and 0.5 part of octyl mercaptan solution are dropwise added, and the dropwise addition is controlled to be finished within 4 hours. After the dripping is finished, stirring and reacting are continued for 2 hours. And after the reaction is finished, adding sodium hydroxide into the reaction kettle, and adjusting the final pH value to 5-6 to obtain the reference polyether type water-retaining agent with the solid content of 10%. The sample was recorded as DG 1.
Comparative example 2
A polyether water-retaining agent was prepared by following the procedure of example 3 except that maleic anhydride was replaced with the same parts by weight of acrylic acid and the other conditions were the same as in example 3 to obtain a reference polyether water-retaining agent having a solid content of 10%. The sample was recorded as DG 2.
Comparative example 3
A polyether water-retaining agent was prepared by following the procedure of example 3 except that sodium gluconate was replaced with the same part by weight of water and the remaining conditions were the same as in example 3 to obtain a reference polyether water-retaining agent having a solid content of 10%. The sample was recorded as DG 3.
Comparative example 4
A polyether water-retaining agent was prepared by following the procedure of example 3 except that acrylamide was replaced with the same parts by weight of TPEG, and the remaining conditions were the same as in example 3, to obtain a reference polyether water-retaining agent having a solid content of 10%. The sample was recorded as DG 4.
Test effects
(1) And (3) mortar test:
referring to GB50119-2013 about a rapid test method for concrete admixture compatibility, mortar tests are carried out on polyether water-retaining agents G1-G4 obtained in examples 1-4 and reference polyether water-retaining agents DG 1-DG 4 obtained in comparative examples 1-4. The mixing proportion of the mortar is as follows: P.O42.5 cement, 400 g; 119g of fly ash, grade II; mineral powder, S95, 136 g; sand, ISO, 1350 g; water, 215 g; the water reducing agent is a commercially available high water reducing type polycarboxylate water reducing agent, and the folded solid content is 0.066%; the water-retaining agent has a folding solid content of 0.006%. The results of the experiment are shown in table 1.
TABLE 1 mortar test data
(2) Concrete test:
the workability test and bleeding test of the mixture were carried out according to GB/T50080-2002 Standard test methods for Performance of ordinary concrete mixtures. The strength grade of the test concrete is C30 concrete: c30 concrete, the total amount of cementing material is 340kg/m3The cement is P.O.42.5 cement, the fly ash is II-grade ash, the fineness modulus of sand is 2.7, the coarse aggregate is crushed stone with the thickness of 5-25 mm, the water-cement ratio is 0.51, the sand rate is 45.5%, a commercial retarding polycarboxylic acid high-performance water reducing agent (the folding and fixing mixing amount is 0.16-0.18%) and the folding and fixing mixing amount of a water-retaining agent is 0.006%.
Table 2 concrete test data
As can be seen from the results in tables 1 and 2, the polyether water retention agent provided by the invention not only can effectively control the post-bleeding phenomenon of mortar and concrete, but also can improve the workability of concrete with high fluidity, and achieve the effects of water retention and viscosity increase. In addition, the preparation method of the polyether water-retaining agent provided by the invention is efficient, does not need a heat source, is simple in process and is suitable for a large-scale industrial production method.
Although embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are exemplary and not to be construed as limiting the present invention, and that those skilled in the art may make variations, modifications, substitutions and alterations within the scope of the present invention without departing from the spirit and scope of the present invention.
Claims (10)
1. The polyether water-retaining agent is characterized in that a polymer contained in the polyether water-retaining agent comprises a structural unit derived from unsaturated polyether, a structural unit derived from unsaturated amide, a structural unit derived from polyfunctional unsaturated carboxylic acid, a structural unit derived from organic silicon and a structural unit derived from unsaturated sulfonate in a weight ratio of 100 (55.5-85.5) to (7.4-37) to (3.7-5.2) to (1.8-3.7); (ii) the structural units derived from a polyfunctional unsaturated carboxylic acid have a carboxylic acid functionality of at least 2; a buffering agent is added to stabilize the pH value of a polymerization system in the synthesis process of the polyether water-retaining agent, wherein the buffering agent is gluconate and/or citrate; the pH value of the polyether water-retaining agent is 5-6.
2. The polyether water-retaining agent as claimed in claim 1, wherein the weight ratio of the structural unit derived from unsaturated polyether to the buffer is 100 (3-7.4).
3. The polyether water-retaining agent as claimed in claim 1, wherein the solid content of the polyether water-retaining agent is 8-15%.
4. The polyether water-retaining agent of claim 1, wherein the polyfunctional unsaturated carboxylic acid is at least one selected from the group consisting of maleic anhydride, fumaric acid and trans-aconitic acid.
5. The polyether water-retaining agent as claimed in any one of claims 1 to 4, wherein the unsaturated polyether is TPEG and/or HPEG, and the molecular formula of TPEG is CH2＝C(CH3)CH2CH2O(CH2CH2O)nH, HPEG molecular formula is CH2＝C(CH3)CH2O(CH2CH2O)nH and n are positive integers; the number average molecular weight of the unsaturated polyether is 2300-2500;
the unsaturated amide is acrylamide and/or methacrylamide;
the organic silicon is vinyl trimethylsilane and/or gamma-methacryloxypropyl trimethoxysilane;
the unsaturated sulfonate is sodium allyl sulfonate and/or sodium vinyl sulfonate.
6. A method for preparing the polyether water-retaining agent of any one of claims 1 to 5, wherein the method comprises the following steps: under the stirring condition, adding unsaturated polyether, unsaturated amide, polyfunctional unsaturated carboxylic acid, organic silicon, a buffering agent and water into a reaction kettle, uniformly mixing, adding an oxidant once again, dropwise adding a mixed aqueous solution of unsaturated sulfonate and a reducing agent, controlling the dropping within 1-4 h, stirring and reacting at room temperature for 1-5 h after the dropping is finished, and then adjusting the pH value of the obtained reaction product to 5-6; the weight ratio of the unsaturated polyether, the unsaturated amide, the polyfunctional group unsaturated carboxylic acid, the organic silicon and the unsaturated sulfonate is 100 (55.5-85.5): (7.4-37): (3.7-5.2): 1.8-3.7); the buffer is gluconate and/or citrate.
7. The preparation method of the polyether water-retaining agent as claimed in claim 6, wherein the weight ratio of the unsaturated polyether to the buffer is 100 (3-7.4).
8. The method for preparing polyether water-retaining agent as claimed in claim 6, wherein the weight ratio of the oxidant, the reducing agent and the unsaturated polyether is (3-5): 1.5-2.2): 100.
9. The method for preparing polyether water-retaining agent according to claim 6,
the oxidant is at least one of hydrogen peroxide, potassium persulfate and ammonium persulfate;
the reducing agent is selected from at least one of ascorbic acid, sodium formaldehyde sulfoxylate and sodium bisulfite.
10. A cement-based building material, which contains sand, cement, an admixture, a water reducing agent, a water retaining agent and water, wherein the water retaining agent is the polyether water retaining agent of any one of claims 1 to 5.
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