CN114014995A - A kind of cross-linked polyether concrete water-retaining agent and preparation method thereof - Google Patents
A kind of cross-linked polyether concrete water-retaining agent and preparation method thereof Download PDFInfo
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- CN114014995A CN114014995A CN202111423028.2A CN202111423028A CN114014995A CN 114014995 A CN114014995 A CN 114014995A CN 202111423028 A CN202111423028 A CN 202111423028A CN 114014995 A CN114014995 A CN 114014995A
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- 239000004567 concrete Substances 0.000 title claims abstract description 74
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 47
- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 31
- 229920000570 polyether Polymers 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000178 monomer Substances 0.000 claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000004132 cross linking Methods 0.000 claims abstract description 34
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 23
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims abstract description 22
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 22
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 22
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 22
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 21
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims abstract description 17
- 150000001408 amides Chemical class 0.000 claims abstract description 16
- 125000002091 cationic group Chemical group 0.000 claims abstract description 16
- 239000007800 oxidant agent Substances 0.000 claims abstract description 15
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 14
- 230000001590 oxidative effect Effects 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 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 16
- 238000002156 mixing Methods 0.000 claims description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 10
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 10
- 238000006136 alcoholysis reaction Methods 0.000 claims description 10
- 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 10
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 8
- 229930003268 Vitamin C Natural products 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- 235000019154 vitamin C Nutrition 0.000 claims description 8
- 239000011718 vitamin C Substances 0.000 claims description 8
- 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 4
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 3
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 3
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- JCRDPEHHTDKTGB-UHFFFAOYSA-N dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound Cl.CN(C)CCOC(=O)C(C)=C JCRDPEHHTDKTGB-UHFFFAOYSA-N 0.000 claims description 2
- 239000012948 isocyanate Substances 0.000 claims description 2
- 150000002513 isocyanates Chemical class 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 2
- 235000010265 sodium sulphite Nutrition 0.000 claims description 2
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 2
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 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 2
- 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 2
- OEIXGLMQZVLOQX-UHFFFAOYSA-N trimethyl-[3-(prop-2-enoylamino)propyl]azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CCCNC(=O)C=C OEIXGLMQZVLOQX-UHFFFAOYSA-N 0.000 claims description 2
- CZFMLDUNXATLOW-XKZIYDEJSA-N (5z)-5-[[3-(2-hydroxyethoxymethyl)thiophen-2-yl]methylidene]-10-methoxy-2,2,4-trimethyl-1h-chromeno[3,4-f]quinolin-9-ol Chemical compound C1=CC=2NC(C)(C)C=C(C)C=2C2=C1C=1C(OC)=C(O)C=CC=1O\C2=C/C=1SC=CC=1COCCO CZFMLDUNXATLOW-XKZIYDEJSA-N 0.000 claims 1
- SEGBQNJGOCXIGC-FHERZECASA-N benzyl n-[(2s)-1-[(4-hydroxyoxolan-3-yl)amino]-4-methyl-1-oxopentan-2-yl]carbamate Chemical compound N([C@@H](CC(C)C)C(=O)NC1C(COC1)O)C(=O)OCC1=CC=CC=C1 SEGBQNJGOCXIGC-FHERZECASA-N 0.000 claims 1
- 230000000740 bleeding effect Effects 0.000 abstract description 14
- 238000005204 segregation Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 description 18
- 239000012153 distilled water Substances 0.000 description 12
- 238000005303 weighing Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 4
- 239000004568 cement Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229920005646 polycarboxylate Polymers 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000010881 fly ash Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 206010016807 Fluid retention Diseases 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 description 1
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000000963 oxybis(methylene) group Chemical group [H]C([H])(*)OC([H])([H])* 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
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Classifications
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- 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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- 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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a cross-linking polyether concrete water-retaining agent, which comprises the following raw materials in parts by weight: 50-80 parts of allyl polyoxyethylene ether, 20-40 parts of polyvinyl alcohol, 10-20 parts of unsaturated amide monomer, 1-10 parts of unsaturated carboxylic acid monomer, 3-6 parts of unsaturated cationic monomer, 3-10 parts of cross-linking agent, 0.1-3 parts of oxidant, 1-3 parts of reducing agent and 800-900 parts of water. The invention also discloses a preparation method of the crosslinking polyether concrete water-retaining agent. The water-retaining agent prepared by the invention has higher water-retaining property, can effectively improve the cohesiveness and the wrapping property of concrete, and inhibits the segregation and bleeding of the concrete.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to a cross-linking polyether concrete water-retaining agent and a preparation method thereof.
Background
In recent years, with the shortage of river sand and the shortage of sandstone resources, the machine-made sandstone is used on a large scale in the production process of concrete, but the use of the machine-made sandstone with a large amount of grading and poor grain type often causes the phenomena of concrete segregation and bleeding. Meanwhile, the polycarboxylic acid high-performance water reducing agent is a concrete fluidity adjusting additive which is widely applied, and the polycarboxylic acid water reducing agent gradually exposes some inherent problems and defects, is sensitive to mixing amount, temperature and ground material change, and often causes the concrete slump loss to be too fast or the concrete to be greatly bleeding due to hysteresis, so that the quality of the concrete is difficult to ensure.
In the prior art, common engineering application can frequently compound different varieties of polycarboxylic acid water reducing agents with various chemical admixtures for adjusting viscosity, but the addition of a viscosity adjusting agent can affect the fluidity of concrete. Therefore, the concrete water-retaining agent which is simple to produce, green, environment-friendly and excellent in performance is provided in order to reduce the sensitivity of the polycarboxylate water-reducing agent to materials, improve the cohesiveness of concrete and reduce the segregation and bleeding of the concrete.
Disclosure of Invention
The invention aims to provide a cross-linking polyether concrete water-retaining agent and a preparation method thereof, which are used for solving the problems that a polycarboxylate water-reducing agent in the prior art is high in material sensitivity and concrete is easy to segregate and bleed.
In order to achieve the above purpose, an embodiment of the present invention provides a cross-linking polyether type concrete water-retaining agent, which comprises the following raw materials in parts by weight:
50-80 parts of allyl polyoxyethylene ether, 20-40 parts of polyvinyl alcohol,
10 to 20 parts of unsaturated amide monomer, 1 to 10 parts of unsaturated carboxylic acid monomer,
3 to 6 parts of unsaturated cationic monomer, 3 to 10 parts of cross-linking agent,
0.1-3 parts of oxidant, 1-3 parts of reducer and 800-900 parts of water.
In one preferable scheme of the invention, the cross-linked polyether concrete water-retaining agent comprises the following raw materials in parts by weight:
52-76 parts of allyl polyoxyethylene ether, 23-35 parts of polyvinyl alcohol,
11 to 19 parts of unsaturated amide monomer, 3 to 9 parts of unsaturated carboxylic acid monomer,
3 to 6 parts of unsaturated cationic monomer, 4 to 10 parts of cross-linking agent,
0.3 to 3 portions of oxidant, 1 to 3 portions of reducer and 810 to 900 portions of water.
In one preferable scheme of the invention, the cross-linked polyether concrete water-retaining agent comprises the following raw materials in parts by weight:
55-73 parts of allyl polyoxyethylene ether, 26-32 parts of polyvinyl alcohol,
13 to 18 parts of unsaturated amide monomer, 5 to 8 parts of unsaturated carboxylic acid monomer,
3 to 5 parts of unsaturated cationic monomer, 4 to 8 parts of cross-linking agent,
0.5-2.6 parts of oxidant, 1-3 parts of reducer and 815-880 parts of water.
In one of the preferred embodiments of the present invention, the molecular weight of the allyl polyoxyethylene ether may be 1000, 1200, and 2400.
In a preferred embodiment of the present invention, the polyvinyl alcohol has the formula [ C2H4O]nWherein n is an integer and the alcoholysis degree is 75-90%.
In a preferred embodiment of the present invention, the unsaturated amide monomer is any one of acrylamide, 2-acrylamido-2-methylpropanesulfonic acid, and N-isopropylacrylamide; the unsaturated carboxylic acid monomer is any one of acrylic acid, methacrylic acid and maleic anhydride.
In a preferred embodiment of the present invention, the unsaturated cationic monomer is any one of acryloyloxyethyltrimethyl ammonium chloride, methacryloyloxyethyltrimethyl ammonium chloride, dimethyldiallylammonium chloride, (3-acrylamidopropyl) trimethyl ammonium chloride, and dimethylaminoethyl methacrylate hydrochloride.
In one preferable embodiment of the present invention, the crosslinking agent is any one of NN-methylene bisacrylamide, isocyanate, and ethylene glycol dimethacrylate; the oxidant is any one of ammonium persulfate, potassium persulfate and hydrogen peroxide; the reducing agent is any one of vitamin C, sodium sulfite, sodium bisulfite, sodium hypophosphite and sodium thiosulfate.
Based on the cross-linking polyether concrete water-retaining agent provided by the invention, the invention also discloses a preparation method of the cross-linking polyether concrete water-retaining agent, which comprises the following steps:
step (1): putting allyl polyoxyethylene ether, polyvinyl alcohol and unsaturated amide monomer into a round-bottom flask provided with a thermometer and a stirrer according to parts by weight, adding water, and stirring to prepare a uniform aqueous solution A;
step (2): adding water into an unsaturated carboxylic acid monomer and an unsaturated cationic monomer according to the weight parts, and uniformly mixing to prepare an aqueous solution B;
and (3): adding water into a reducing agent according to the parts by weight, and uniformly mixing to prepare an aqueous solution C;
and (4): and adding an oxidant into the aqueous solution A in the flask, simultaneously dropwise adding the aqueous solution B and the aqueous solution C into the flask, stirring after dropwise adding is finished, and adjusting the pH value by using a sodium hydroxide aqueous solution after stirring is finished to obtain the cross-linking water-retaining agent.
In one preferable embodiment of the invention, the specification of the round-bottom flask in the step (1) is 1L; the dripping time in the step (4) is 1-3 h, and the pH is adjusted to 5-6.
The invention has the beneficial effects that: the allyl polyoxyethylene ether, the polyvinyl alcohol, the unsaturated amide monomer and the unsaturated carboxylic acid monomer in the concrete water-retaining agent have stronger hydrophilic groups, and form a strong water-absorbing net structure through copolymerization and crosslinking, so that the loss of free water in concrete is effectively inhibited, meanwhile, the aggregate particles are suspended, the sedimentation is prevented, and the reaction formula is shown in figure 1. Allyl polyoxyethylene ether, polyvinyl alcohol long-chain monomer, cationic monomer and the like can effectively reduce competitive adsorption of the water-retaining agent on positively charged cement particle surfaces and the polycarboxylate water reducer through steric hindrance and electrostatic repulsion, the fluidity of concrete is ensured, and the water-retaining agent has better adaptability with the polycarboxylate water reducer.
Drawings
FIG. 1 is a reaction formula diagram of a network structure formed by copolymerization and crosslinking of allyl polyoxyethylene ether, polyvinyl alcohol, an unsaturated amide monomer and an unsaturated carboxylic acid monomer;
Detailed Description
Example 1
A cross-linking polyether concrete water-retaining agent comprises the following raw materials in parts by weight: 51.6 parts of allyl polyoxyethylene ether, 24.2 parts of polyvinyl alcohol (with alcoholysis degree of 75%), 16.8 parts of unsaturated amide monomer acrylamide, 6.4 parts of unsaturated carboxylic acid monomer acrylic acid, 4.5 parts of unsaturated cationic monomer dimethyl diallyl ammonium chloride, 4.2 parts of crosslinking agent NN-methylene bisacrylamide, 1.5 parts of oxidant ammonium persulfate, 1.2 parts of reducing agent vitamin C and 890 parts of water.
A preparation method of a cross-linking polyether concrete water-retaining agent comprises the following steps:
step (1): weighing 51.6 parts of allyl polyoxyethylene ether (APEG-2000), 24.2 parts of polyvinyl alcohol (alcoholysis degree of 75), 16.8 parts of acrylamide and 4.2 parts of NN-methylene bisacrylamide, putting the mixture into a 1L round bottom flask provided with a thermometer and a stirrer, adding 750 parts of distilled water, and stirring to prepare a uniform aqueous solution A;
step (2): uniformly mixing 6.4 parts of acrylic acid, 4.5 parts of dimethyl diallyl ammonium chloride and 70 parts of distilled water to prepare an aqueous solution B;
and (3): uniformly mixing 1 part of vitamin C and 70 parts of distilled water to prepare an aqueous solution C;
and (4): adding 1.5 parts of ammonium persulfate into the aqueous solution A in the flask, simultaneously dropwise adding the aqueous solution B and the aqueous solution C into the flask at the same speed within 2h, continuously stirring for 1h after dropwise adding is finished, and adjusting the pH to 5-6 by using an aqueous sodium hydroxide solution to obtain a cross-linking type water-retaining agent, which is marked as S1.
Example 2
A cross-linking polyether concrete water-retaining agent comprises the following raw materials in parts by weight: 58 parts of allyl polyoxyethylene ether, 21 parts of polyvinyl alcohol (the alcoholysis degree is 75%), 14.5 parts of unsaturated amide monomer acrylamide, 3.6 parts of unsaturated carboxylic acid monomer acrylic acid, 6 parts of unsaturated cationic monomer dimethyl diallyl ammonium chloride, 5 parts of crosslinking agent NN-methylene bisacrylamide, 0.4 part of oxidant hydrogen peroxide, 1.2 parts of reducing agent vitamin C and 890 parts of water.
A preparation method of a cross-linking polyether concrete water-retaining agent comprises the following steps:
step (1): weighing 58 parts of allyl polyoxyethylene ether (APEG-2000), 21 parts of polyvinyl alcohol (alcoholysis degree of 75), 14.5 parts of acrylamide and 5 parts of NN-methylene bisacrylamide, putting the materials into a 1L round-bottom flask provided with a thermometer and a stirrer, adding 750 parts of distilled water, and stirring to prepare a uniform aqueous solution A;
step (2): uniformly mixing 3.6 parts of acrylic acid, 6 parts of dimethyl diallyl ammonium chloride and 70 parts of distilled water to prepare an aqueous solution B;
and (3): uniformly mixing 1.2 parts of vitamin C and 70 parts of distilled water to prepare an aqueous solution C;
and (4): adding 0.4 part of hydrogen peroxide into the aqueous solution A in the flask, simultaneously dropwise adding the aqueous solution B and the aqueous solution C into the flask at the same speed within 2h, continuously stirring for 1h after dropwise adding is finished, and adjusting the pH to 5-6 by using an aqueous solution of sodium hydroxide to obtain a cross-linked water-retaining agent, which is marked as S2.
Example 3
A cross-linking polyether concrete water-retaining agent comprises the following raw materials in parts by weight: 56 parts of allyl polyoxyethylene ether, 20.5 parts of polyvinyl alcohol (the alcoholysis degree is 78%), 16 parts of acrylamide, 1.2 parts of 2-acrylamide-2-methylpropanesulfonic acid, 4.4 parts of unsaturated carboxylic acid monomer acrylic acid, 4.8 parts of unsaturated cationic monomer dimethyl diallyl ammonium chloride, 5 parts of cross-linking agent NN-methylene bisacrylamide, 0.4 part of oxidant hydrogen peroxide, 1.2 parts of reducing agent vitamin C and 890 parts of water.
A preparation method of a cross-linking polyether concrete water-retaining agent comprises the following steps:
step (1): weighing 56 parts of allyl polyoxyethylene ether (APEG-2400), 20.5 parts of polyvinyl alcohol (alcoholysis degree of 75), 16 parts of acrylamide, 1.2 parts of 2-acrylamide-2-methylpropanesulfonic acid and 5 parts of NN-methylene bisacrylamide, putting the mixture into a 1L round-bottom flask provided with a thermometer and a stirrer, adding 750 parts of distilled water, and stirring to prepare a uniform aqueous solution A;
step (2): uniformly mixing 3.6 parts of acrylic acid, 4.8 parts of dimethyl diallyl ammonium chloride and 70 parts of distilled water to prepare an aqueous solution B;
and (3): uniformly mixing 1.6 parts of vitamin C and 70 parts of distilled water to prepare an aqueous solution C;
and (4): adding 0.6 part of hydrogen peroxide into the aqueous solution A in the flask, simultaneously dropwise adding the aqueous solution B and the aqueous solution C into the flask at the same speed within 2h, continuously stirring for 1h after dropwise adding is finished, and adjusting the pH to 5-6 by using an aqueous solution of sodium hydroxide to obtain a cross-linked water-retaining agent, which is marked as S3.
Example 4
A cross-linking polyether concrete water-retaining agent comprises the following raw materials in parts by weight: 51 parts of allyl polyoxyethylene ether (APEG-2400), 20 parts of polyvinyl alcohol (the alcoholysis degree is 75%), 18 parts of unsaturated amide monomer acrylamide, 4.4 parts of unsaturated carboxylic acid monomer acrylic acid, 4.0 parts of unsaturated cationic monomer dimethyl diallyl ammonium chloride, 5.6 parts of cross-linking agent ethylene glycol dimethacrylate, 1.8 parts of oxidizing agent potassium persulfate, 1.4 parts of reducing agent sodium bisulfite and 890 parts of water.
A preparation method of a cross-linking polyether concrete water-retaining agent comprises the following steps:
step (1): weighing 51 parts of allyl polyoxyethylene ether (APEG-2400), 20.5 parts of polyvinyl alcohol (alcoholysis degree of 75), 16 parts of acrylamide, 1.2 parts of 2-acrylamide-2-methylpropanesulfonic acid and 5 parts of NN-methylene bisacrylamide, putting the mixture into a 1L round-bottom flask provided with a thermometer and a stirrer, adding 750 parts of distilled water, and stirring to prepare a uniform aqueous solution A;
step (2): uniformly mixing 4.4 parts of acrylic acid, 4.0 parts of dimethyl diallyl ammonium chloride and 70 parts of distilled water to prepare an aqueous solution B;
and (3): uniformly mixing 1.6 parts of sodium bisulfite and 70 parts of distilled water to prepare a water solution C;
and (4): adding 1.8 parts of potassium persulfate into the aqueous solution A in the flask, simultaneously dropwise adding the aqueous solution B and the aqueous solution C into the flask at a uniform speed within 2h, continuously stirring for 1h after dropwise adding is finished, and adjusting the pH to 5-6 by using an aqueous sodium hydroxide solution to obtain a cross-linking type water-retaining agent, which is marked as S4.
Experimental detection
The water-retaining agents prepared in example 1, example 2, example 3 and example 4 were added to concrete for concrete mixture workability tests, wherein the water-retaining agent was not incorporated in the comparative example.
The concrete mix formulation is shown in table 1:
table 1: concrete mixing ratio (kg/m)3)
| Strength grade | Cement | Fly ash | Sand | Crushing stone | Water (W) |
| C30 | 230 | 80 | 880 | 1050 | 160 |
Wherein the cement is PO42.5 cement, the fly ash is second-grade fly ash, the sand is machine-made sand with fineness modulus of 2.6, the particle size of the broken stone is 5mm-40mm, and 0.3% of water-retaining agent is added into 10% of polycarboxylic acid water reducing agent.
The working performance of the concrete mixture is tested according to a detection method in GB/T50080-2016 Standard test method for the Performance of common concrete mixtures, and the working performance of the concrete comprises the slump and the bleeding rate.
The concrete slump detection method specifically comprises the following steps:
1. measuring the initial slump value of the concrete mixture during the machine operation;
2. filling all concrete mixture samples into a plastic barrel, and sealing and standing the plastic barrel by using a barrel cover;
3. timing when stirring and water adding are started, after standing for 60min, pouring all concrete mixture samples in the barrel into a stirrer, stirring for 20s, and performing a slump test to obtain a slump value of 60 min;
4. timing when stirring and water adding are started, after standing for 120min, pouring all concrete mixture samples in the barrel into a stirrer, stirring for 20s, and performing a slump test to obtain a slump value of 120 min;
the concrete bleeding rate detection method specifically comprises the following steps:
1. immediately weighing the inner wall of the volumetric cylinder after the inner wall of the volumetric cylinder is wetted by wet cloth, and recording the mass of the volumetric cylinder;
2. filling the concrete mixture into a volumetric cylinder;
3. wiping the opening and the outer surface of the cylinder, weighing and recording the mass of the volumetric cylinder and the sample, covering the cylinder cover and starting timing;
4. sucking the surface bleeding of the sample for 1 time every 10min within 60min after the timing is started; after 60min, sucking the surface of the sample for 1 time every 30min until no bleeding occurs.
The bleeding rate was calculated according to the following formula: b ═ VW/[(W/mT)·m]
m＝m1-m2
Wherein, VWIs the total bleeding (mL), m is the concrete mixture sample mass (g), mTTotal mass (g) of the concrete mixture to be mixed for the test, W is water amount (mL) of the concrete mixture to be mixed for the test, and m1Is the volumetric cylinder mass (g), m2The volumetric cylinder and the total mass (g) of the sample were obtained.
The concrete mixture workability test results are shown in table 2:
table 2: working performance of concrete
As can be seen from table 2: the bleeding rate and the concrete slump of S1-S4 are smaller than those of the comparative example, and the bleeding rate and the concrete slump of S1-S4 are obviously different from those of the comparative example and have significant changes. Therefore, the water-retaining agent prepared by the invention can be added into concrete mixture to reduce the slump and bleeding rate of concrete and improve the water retention of concrete.
Therefore, the water-retaining agent prepared by the invention can reduce the slump and the bleeding rate of concrete, effectively improve the water retention of the concrete, and simultaneously has better improvement effect on the workability of the concrete.
While the present invention has been described in detail with reference to the illustrated embodiments, it should not be construed as limited to the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (10)
1. The cross-linking polyether concrete water-retaining agent is characterized by comprising the following raw materials in parts by weight:
50-80 parts of allyl polyoxyethylene ether, 20-40 parts of polyvinyl alcohol,
10 to 20 parts of unsaturated amide monomer, 1 to 10 parts of unsaturated carboxylic acid monomer,
3 to 6 parts of unsaturated cationic monomer, 3 to 10 parts of cross-linking agent,
0.1-3 parts of oxidant, 1-3 parts of reducer and 800-900 parts of water.
2. The crosslinking polyether concrete water-retaining agent as claimed in claim 1, wherein: the cross-linking polyether concrete water-retaining agent comprises the following raw materials in parts by weight:
52-76 parts of allyl polyoxyethylene ether, 23-35 parts of polyvinyl alcohol,
11 to 19 parts of unsaturated amide monomer, 3 to 9 parts of unsaturated carboxylic acid monomer,
3 to 6 parts of unsaturated cationic monomer, 4 to 10 parts of cross-linking agent,
0.3 to 3 portions of oxidant, 1 to 3 portions of reducer and 810 to 900 portions of water.
3. The crosslinking polyether concrete water-retaining agent as claimed in claim 1, wherein: the cross-linking polyether concrete water-retaining agent comprises the following raw materials in parts by weight:
55-73 parts of allyl polyoxyethylene ether, 26-32 parts of polyvinyl alcohol,
13 to 18 parts of unsaturated amide monomer, 5 to 8 parts of unsaturated carboxylic acid monomer,
3 to 5 parts of unsaturated cationic monomer, 4 to 8 parts of cross-linking agent,
1.5-2.6 parts of oxidant, 1-3 parts of reducer and 815-880 parts of water.
4. The crosslinking polyether concrete water-retaining agent as claimed in claim 1, wherein: the allyl polyoxyethylene ethers may have molecular weights of 1000, 1200, and 2400.
5. The crosslinking polyether concrete water-retaining agent as claimed in claim 1, wherein: the chemical formula of the polyvinyl alcohol is [ C ]2H4O]nWherein n is an integer and the alcoholysis degree is 75-90%.
6. The crosslinking polyether concrete water-retaining agent as claimed in claim 1, wherein: the unsaturated amide monomer is at least one of acrylamide, 2-acrylamide-2-methylpropanesulfonic acid and N-isopropylacrylamide; the unsaturated carboxylic acid monomer is at least one of acrylic acid, methacrylic acid and maleic anhydride.
7. The crosslinking polyether concrete water-retaining agent as claimed in claim 1, wherein: the unsaturated cationic monomer is at least one of acryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl trimethyl ammonium chloride, dimethyl diallyl ammonium chloride, (3-acrylamidopropyl) trimethyl ammonium chloride and dimethylaminoethyl methacrylate hydrochloride.
8. The crosslinking polyether concrete water-retaining agent as claimed in claim 1, wherein: the cross-linking agent is at least one of NN-methylene bisacrylamide, isocyanate and ethylene glycol dimethacrylate; the oxidant is at least one of ammonium persulfate, potassium persulfate and hydrogen peroxide; the reducing agent is at least one of vitamin C, sodium sulfite, sodium bisulfite, sodium hypophosphite and sodium thiosulfate.
9. A preparation method of a cross-linking polyether concrete water-retaining agent is characterized by comprising the following steps:
step (1): putting allyl polyoxyethylene ether, polyvinyl alcohol, unsaturated amide monomer and cross-linking agent into a round-bottom flask with a thermometer and a stirrer according to parts by weight, adding water, and stirring to prepare a uniform aqueous solution A;
step (2): adding water into an unsaturated carboxylic acid monomer and an unsaturated cationic monomer according to the weight parts, and uniformly mixing to prepare an aqueous solution B;
and (3): adding water into a reducing agent according to the parts by weight, and uniformly mixing to prepare an aqueous solution C;
and (4): and adding an oxidant into the aqueous solution A in the flask, simultaneously dropwise adding the aqueous solution B and the aqueous solution C into the flask, stirring after dropwise adding is finished, and adjusting the pH value by using a sodium hydroxide aqueous solution after stirring is finished to obtain the cross-linking water-retaining agent.
10. The preparation method of the cross-linking polyether concrete water-retaining agent as claimed in claim 10, wherein: the specification of the round-bottom flask in the step (1) is 1L; the dripping time in the step (4) is 1-3 h, the stirring time is 0.5-1.5 h, and the pH is adjusted to 5-6.
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