CN111454014A - Mortar and concrete shrinkage reducing agent containing organic silicon and preparation method thereof - Google Patents
Mortar and concrete shrinkage reducing agent containing organic silicon and preparation method thereof Download PDFInfo
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- CN111454014A CN111454014A CN202010254259.4A CN202010254259A CN111454014A CN 111454014 A CN111454014 A CN 111454014A CN 202010254259 A CN202010254259 A CN 202010254259A CN 111454014 A CN111454014 A CN 111454014A
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- reducing agent
- mortar
- mixture
- shrinkage reducing
- concrete shrinkage
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- 239000004567 concrete Substances 0.000 title claims abstract description 70
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 48
- 239000004570 mortar (masonry) Substances 0.000 title claims abstract description 33
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 26
- 239000010703 silicon Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000008367 deionised water Substances 0.000 claims abstract description 32
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 32
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000178 monomer Substances 0.000 claims abstract description 25
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 13
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 12
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims abstract description 11
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 10
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000003945 anionic surfactant Substances 0.000 claims abstract description 5
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 5
- 239000003999 initiator Substances 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims description 62
- 238000002156 mixing Methods 0.000 claims description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 16
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Chemical compound CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 14
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 12
- 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 12
- 239000002202 Polyethylene glycol Substances 0.000 claims description 12
- 229920001223 polyethylene glycol Polymers 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
- PMNLUUOXGOOLSP-UHFFFAOYSA-N 2-mercaptopropanoic acid Chemical compound CC(S)C(O)=O PMNLUUOXGOOLSP-UHFFFAOYSA-N 0.000 claims description 10
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 229920001296 polysiloxane Polymers 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 10
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 8
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 7
- 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
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 6
- 229930003268 Vitamin C Natural products 0.000 claims description 6
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 6
- SZHIIIPPJJXYRY-UHFFFAOYSA-M sodium;2-methylprop-2-ene-1-sulfonate Chemical compound [Na+].CC(=C)CS([O-])(=O)=O SZHIIIPPJJXYRY-UHFFFAOYSA-M 0.000 claims description 6
- 235000019154 vitamin C Nutrition 0.000 claims description 6
- 239000011718 vitamin C Substances 0.000 claims description 6
- RWXMAAYKJDQVTF-UHFFFAOYSA-N 2-(2-hydroxyethoxy)ethyl prop-2-enoate Chemical compound OCCOCCOC(=O)C=C RWXMAAYKJDQVTF-UHFFFAOYSA-N 0.000 claims description 5
- LDCRTTXIJACKKU-ARJAWSKDSA-N dimethyl maleate Chemical compound COC(=O)\C=C/C(=O)OC LDCRTTXIJACKKU-ARJAWSKDSA-N 0.000 claims description 5
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 5
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 5
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims description 5
- 229940006186 sodium polystyrene sulfonate Drugs 0.000 claims description 5
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 4
- GCSJLQSCSDMKTP-UHFFFAOYSA-N ethenyl(trimethyl)silane Chemical compound C[Si](C)(C)C=C GCSJLQSCSDMKTP-UHFFFAOYSA-N 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
- MWKJTNBSKNUMFN-UHFFFAOYSA-N trifluoromethyltrimethylsilane Chemical compound C[Si](C)(C)C(F)(F)F MWKJTNBSKNUMFN-UHFFFAOYSA-N 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000003814 drug Substances 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 235000001727 glucose Nutrition 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
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- SNVLJLYUUXKWOJ-UHFFFAOYSA-N methylidenecarbene Chemical compound C=[C] SNVLJLYUUXKWOJ-UHFFFAOYSA-N 0.000 claims description 2
- -1 sodium methyl propylene sulfonate Chemical compound 0.000 claims description 2
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 2
- 239000011083 cement mortar Substances 0.000 abstract description 12
- 238000001035 drying Methods 0.000 abstract description 12
- 239000004721 Polyphenylene oxide Substances 0.000 abstract description 5
- 229920000570 polyether Polymers 0.000 abstract description 5
- 125000003368 amide group Chemical group 0.000 abstract description 3
- 238000013461 design Methods 0.000 abstract description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract description 2
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical group NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 11
- 235000011121 sodium hydroxide Nutrition 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 238000004321 preservation Methods 0.000 description 6
- 239000004568 cement Substances 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 102100026788 ATP synthase subunit C lysine N-methyltransferase Human genes 0.000 description 2
- 101000833848 Homo sapiens ATP synthase subunit C lysine N-methyltransferase Proteins 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910001294 Reinforcing steel Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000004574 high-performance concrete Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 231100000989 no adverse effect Toxicity 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- ZHSKFONQCREGOG-UHFFFAOYSA-N triethyl(trifluoromethyl)silane Chemical compound CC[Si](CC)(CC)C(F)(F)F ZHSKFONQCREGOG-UHFFFAOYSA-N 0.000 description 1
- ORVBHOQTQDOUIW-UHFFFAOYSA-N trimethoxy(trifluoromethyl)silane Chemical compound CO[Si](OC)(OC)C(F)(F)F ORVBHOQTQDOUIW-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 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
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The invention discloses a mortar and concrete shrinkage reducing agent containing organosilicon and a preparation method thereof, wherein the mortar and concrete shrinkage reducing agent has a pH value of 5.5-6 and is prepared from the following raw materials: TPEG, unsaturated carboxylic acid and derivatives thereof, anionic surfactant, organosilicon monomer, ethylene glycol acrylate hydrophobic monomer, initiator, reducing agent, chain transfer agent, liquid alkali and deionized water. The TPEG, specific unsaturated carboxylic acid and derivatives thereof, specific organic silicon monomers and specific glycol acrylate hydrophobic monomers are used as basic raw materials, molecular structure design and regulation are carried out according to the functional requirements of shrinkage reduction and dispersion performance, unsaturated polyether and unsaturated carboxylic acid are copolymerized to form a main chain, amino, sulfonic acid groups, amide groups, siloxane structural monomers, glycol acrylate monomers and the like are introduced into the molecular structure of the polymer, and the drying shrinkage rate of cement mortar can be effectively reduced.
Description
Technical Field
The invention belongs to the technical field of concrete admixtures, and particularly relates to mortar and concrete shrinkage reducing agent containing organic silicon and a preparation method thereof.
Background
Cracks or crazes caused by the shrinkage of concrete affect the appearance of buildings, reduce the service life of concrete, and even cause serious problems in the safety of concrete structures. The problem of shrinkage cracking of concrete, especially high-performance concrete, has attracted great attention in the engineering industry, and although the shrinkage of concrete is reduced to a certain extent by polycarboxylic acid water reducing agent, the requirements of engineering are still difficult to meet.
At present, the early shrinkage cracking of concrete is mainly controlled or reduced by the following measures: (1) the shrinkage is reduced by comprehensively optimizing the matching ratio; (2) the shrinkage reducing agent, the fiber or the expanding agent are blended to improve the plastic shrinkage crack resistance of the concrete or compensate the plastic shrinkage of the concrete; (3) the plastic shrinkage is reduced by spraying a surface curing agent or early wet curing to reduce the evaporation rate of water on the surface of the concrete.
The concrete shrinkage reducing agent is mainly used for reducing the shrinkage of concrete by reducing the surface tension of water in concrete pores and reducing the shrinkage force in the water evaporation process so as to achieve the purpose of reducing concrete cracks. In China, no shaped concrete shrinkage-reducing agent product is sold, and foreign products are difficult to buy. As with other admixtures, each manufacturer is kept confidential with respect to the specific components of its shrinkage-reducing agent.
Therefore, the development of shrinkage reducing agent products capable of effectively reducing the shrinkage of concrete has important significance for improving the volume stability of concrete and improving the durability of concrete structures.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the mortar and concrete shrinkage reducing agent containing the organic silicon.
The invention also aims to provide a preparation method of the mortar and concrete shrinkage reducing agent containing the organic silicon.
The technical scheme of the invention is as follows:
a mortar and concrete shrinkage reducing agent containing organic silicon is characterized in that: the pH value is 5.5-6, and the medicine is prepared from the following raw materials in parts by weight:
the structural formula of the TPEG is CH2＝C(CH3)CH2CH2O(CH2CH2O)nH, wherein n is a positive integer;
the unsaturated carboxylic acid and its derivative comprises at least one of acrylic acid, acrylamide, methacrylic acid, maleic anhydride, methyl acrylate, and dimethyl maleate;
the organic silicon monomer comprises at least one of vinyltrimethylsilane, trifluoromethyltrimethylsilane, vinyltriethoxysilane and gamma-methacryloxypropyltrimethoxysilane;
the ethylene glycol acrylate hydrophobic monomer comprises at least one of polyethylene glycol dimethacrylate, polyethylene glycol acrylate, diethylene glycol monoacrylate and ethylene glycol dimethacrylate.
The TPEG, specific unsaturated carboxylic acid and derivatives thereof, specific organic silicon monomers and specific glycol acrylate hydrophobic monomers are used as basic raw materials, molecular structure design and regulation are carried out according to the functional requirements of shrinkage reduction and dispersion performance, unsaturated polyether and unsaturated carboxylic acid are copolymerized to form a main chain, amino, sulfonic acid groups, amide groups, siloxane structural monomers, glycol acrylate monomers and the like are introduced into the molecular structure of the polymer, and the drying shrinkage rate of cement mortar can be effectively reduced.
According to the invention, a certain amount of sulfonic acid groups are grafted to enhance the adsorption performance and charge adsorption capacity of the water reducing agent and the surface of concrete particles, so that the fluidity and the workability of concrete are improved. The amido is an amphoteric group, so that the sensitivity of the polyether to inorganic salt ions can be reduced, the polyether keeps an extended conformation, and the polyether can better play a dispersing role.
According to the invention, by introducing the amino functional group, the shrinkage reducing agent is more easily combined with water molecules to form a layer of water film, and the amino group has positive charges, and the shrinkage reducing molecules adsorbed on the surface of cement particles are more easily dispersed due to the repulsion of like charges.
The hydrophobic monomers such as ethylene glycol acrylate monomers and organic silicon monomers added in the invention can effectively reduce the surface tension of the solution, thereby reducing the drying shrinkage of the concrete. Furthermore, a water-retaining group with a siloxane structure is introduced, a micro-cross-linked structure can be formed, the viscosity of pore water in the concrete is increased, the adsorption effect of water in concrete colloid is enhanced, and the shrinkage of the concrete can be further reduced.
The shrinkage reducing agent and the water reducing agent are mixed together, so that the water reducing rate of mortar and concrete can be increased properly, and the synergistic effect is achieved.
The preparation method of the mortar and concrete shrinkage reducing agent containing the organic silicon comprises the following steps:
(1) TPEG, anionic surfactant and a proper amount of deionized water are uniformly mixed to obtain a first mixture; mixing unsaturated carboxylic acid and derivatives thereof, an organic silicon monomer, a glycol acrylate hydrophobic monomer and a proper amount of deionized water to obtain a second mixture; mixing a reducing agent, a chain transfer agent and a proper amount of deionized water to obtain a third mixture;
(2) placing the first mixture into a reaction kettle, heating to 37-43 ℃ while continuously stirring, adding an initiator once after the temperature is kept stable, dropwise adding the second mixture and the third mixture within 1-4h, and reacting at 37-43 ℃ for 1-2 h;
(3) and (3) adding liquid alkali into the material obtained in the step (2) to obtain the mortar containing the organic silicon and the concrete shrinkage reducing agent.
The preparation method of the invention adopts normal pressure production, has low equipment requirement and convenient operation, is beneficial to industrial production, does not contain chloride ions in the product, and has no corrosion hazard to reinforcing steel bars in concrete.
Drawings
FIG. 1 is a graph showing the change in concrete shrinkage at different loadings in a comparative test of the present invention.
Detailed Description
The technical solution of the present invention will be further illustrated and described below with reference to the accompanying drawings by means of specific embodiments.
In a preferred embodiment of the present invention, the unsaturated carboxylic acid and its derivative is at least one of acrylic acid, acrylamide, methacrylic acid, maleic anhydride, methyl acrylate, and dimethyl maleate.
In a preferred embodiment of the present invention, the silicone monomer is at least one of vinyltrimethylsilane, trifluoromethyltrimethylsilane, vinyltriethoxysilane, and gamma-methacryloxypropyltrimethoxysilane.
In a preferred embodiment of the present invention, the glycol acrylate hydrophobic monomer is at least one of polyethylene glycol dimethacrylate, polyethylene glycol acrylate, diethylene glycol monoacrylate and ethylene glycol dimethacrylate.
In a preferred embodiment of the present invention, the anionic surfactant comprises at least one of sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, sodium polystyrene sulfonate, and sodium methallyl sulfonate.
In a preferred embodiment of the present invention, the reducing agent includes at least one of sodium bisulfite, vitamin C, ferrous sulfate, and glucose.
In a preferred embodiment of the present invention, the initiator includes at least one of ammonium persulfate and potassium persulfate.
In a preferred embodiment of the present invention, the chain transfer agent comprises at least one of thioglycolic acid, 2-mercaptopropionic acid, 3-mercaptopropionic acid, and sodium methallylsulfonate.
In a preferred embodiment of the present invention, the solute in the liquid caustic soda comprises at least one of potassium hydroxide and sodium hydroxide.
Example 1
(1) 50g of TPEG (number average molecular weight of 2300-3) 10g of sodium dodecyl sulfate, deionized water and a proper amount of deionized water are uniformly mixed to obtain a first mixture; mixing 15g of acrylic acid, 10g of acrylamide, 1.2g of vinyltrimethoxysilane, 1.2g of ethylene glycol dimethacrylate and a proper amount of deionized water to obtain a second mixture; mixing 0.8g of vitamin C, 0.8g of thioglycolic acid and a proper amount of deionized water to obtain a third mixture;
(2) placing the first mixture into a reaction kettle, heating to 37-43 ℃ while continuously stirring, adding 1.2g of ammonium persulfate once after the temperature is kept stable, dropwise adding the second mixture and the third mixture within 1-4h, and reacting at 37-43 ℃ for 1-2h in a heat preservation way after dropwise adding;
(3) and (3) adding liquid caustic soda into the material obtained in the step (2), and adjusting the pH value to 5.5-6 to obtain the mortar containing the organic silicon and the concrete shrinkage reducing agent JS-1.
Example 2
(1) 50g of TPEG (number average molecular weight of 2300-3) 8g of sodium dodecyl benzene sulfonate and a proper amount of deionized water are uniformly mixed to obtain a first mixture; mixing 20g of methacrylic acid, 10g of acrylamide, 1.0g of vinyltriethoxysilane, 1.5g of polyethylene glycol acrylate and a proper amount of deionized water to obtain a second mixture; mixing 0.9g of vitamin C, 1.0g of 2-mercaptopropionic acid and a proper amount of deionized water to obtain a third mixture;
(2) placing the first mixture into a reaction kettle, heating to 37-43 ℃ while continuously stirring, adding 1.0g of potassium persulfate once after the temperature is kept stable, dropwise adding the second mixture and the third mixture within 1-4h, and keeping the temperature at 37-43 ℃ for 1-2h after dropwise adding;
(3) and (3) adding liquid caustic soda into the material obtained in the step (2), and adjusting the pH value to 5.5-6 to obtain the mortar containing the organic silicon and the concrete shrinkage reducing agent JS-2.
Example 3
(1) 50g of TPEG (number average molecular weight of 2300-3)、Uniformly mixing 8g of sodium methallyl sulfonate and a proper amount of deionized water to obtain a first mixture; mixing 16g of acrylic acid, 10g of acrylamide, 0.8g of gamma-methacryloxypropyltrimethoxysilane, 1.2g of polyethylene glycol dimethacrylate and a proper amount of deionized water to obtain a second mixture; mixing 0.6g of sodium bisulfite, 0.8g of 2-mercaptopropionic acid, and an appropriate amount of deionized water to obtain a third mixture;
(2) placing the first mixture into a reaction kettle, heating to 37-43 ℃ while continuously stirring, adding 1.6g of ammonium persulfate once after the temperature is kept stable, dropwise adding the second mixture and the third mixture within 1-4h, and reacting at 37-43 ℃ for 1-2h in a heat preservation way after dropwise adding;
(3) and (3) adding liquid caustic soda into the material obtained in the step (2), and adjusting the pH value to 5.5-6 to obtain the mortar containing the organic silicon and the concrete shrinkage reducing agent JS-3.
Example 4
(1) 50g of TPEG (number average molecular weight of 2300-3) Uniformly mixing 10g of sodium polystyrene sulfonate and a proper amount of deionized water to obtain a first mixture; mixing 20g of acrylic acid, 10g of acrylamide, 1.4g of trifluoromethyltriethylsilane, 1.6g of ethylene glycol dimethacrylate and a proper amount of deionized water to obtain a second mixture; mixing 1g of vitamin C, 0.8g of 3-mercaptopropionic acid and a proper amount of deionized water to obtain a third mixture;
(2) placing the first mixture into a reaction kettle, heating to 37-43 ℃ while continuously stirring, adding 1.2g of ammonium persulfate once after the temperature is kept stable, dropwise adding the second mixture and the third mixture within 1-4h, and reacting at 37-43 ℃ for 1-2h in a heat preservation way after dropwise adding;
(3) and (3) adding liquid caustic soda into the material obtained in the step (2), and adjusting the pH value to 5.5-6 to obtain the mortar containing the organic silicon and the concrete shrinkage reducing agent JS-4.
Example 5
(1) 50g of TPEG (number average molecular weight of 2300-3) Uniformly mixing 10g of sodium methallyl sulfonate and a proper amount of deionized water to obtain a first mixture; 18g of acrylic acid, 10g of acrylamide, 1.4g of vinyltrimethoxyMixing silane, 1.0g of polyethylene glycol dimethacrylate and a proper amount of deionized water to obtain a second mixture; mixing 0.8g of sodium bisulfite, 0.6g of thioglycolic acid and a suitable amount of deionized water to obtain a third mixture;
(2) placing the first mixture into a reaction kettle, heating to 37-43 ℃ while continuously stirring, adding 1.2g of ammonium persulfate once after the temperature is kept stable, dropwise adding the second mixture and the third mixture within 1-4h, and reacting at 37-43 ℃ for 1-2h in a heat preservation way after dropwise adding;
(3) and (3) adding liquid caustic soda into the material obtained in the step (2), and adjusting the pH value to 5.5-6 to obtain the mortar containing the organic silicon and the concrete shrinkage reducing agent JS-5.
Example 6
(1) 30g of TPEG (number average molecular weight of 2300-3) Uniformly mixing 10g of sodium polystyrene sulfonate and a proper amount of deionized water to obtain a first mixture; mixing 18g of methacrylic acid, 5g of maleic anhydride, 5g of acrylamide, 1.0g of trifluoromethyltrimethoxysilane, 0.8g of ethylene glycol dimethacrylate and a proper amount of deionized water to obtain a second mixture; mixing 0.8g of vitamin C, 0.6g of thioglycolic acid and a proper amount of deionized water to obtain a third mixture;
(2) placing the first mixture into a reaction kettle, heating to 37-43 ℃ while continuously stirring, adding 1.0g of potassium persulfate once after the temperature is kept stable, dropwise adding the second mixture and the third mixture within 1-4h, and keeping the temperature at 37-43 ℃ for 1-2h after dropwise adding;
(3) and (3) adding liquid caustic soda into the material obtained in the step (2), and adjusting the pH value to 5.5-6 to obtain the mortar containing the organic silicon and the concrete shrinkage reducing agent JS-6.
Example 7
(1) 30g of TPEG (number average molecular weight of 2300-3) Uniformly mixing 8g of sodium methallyl sulfonate and a proper amount of deionized water to obtain a first mixture; mixing 18g of acrylic acid, 5g of dimethyl maleate, 5g of acrylamide, 1.2g of vinyltrimethoxysilane, 1.0g of polyethylene glycol dimethacrylate and a suitable amount of deionized water to obtain a second mixture; 0.8g of sodium bisulfite,Mixing 0.6g of 2-mercaptopropionic acid and an appropriate amount of deionized water to obtain a third mixture;
(2) placing the first mixture into a reaction kettle, heating to 37-43 ℃ while continuously stirring, adding 1.2g of ammonium persulfate once after the temperature is kept stable, dropwise adding the second mixture and the third mixture within 1-4h, and reacting at 37-43 ℃ for 1-2h in a heat preservation way after dropwise adding;
(3) and (3) adding liquid caustic soda into the material obtained in the step (2), and adjusting the pH value to 5.5-6 to obtain the mortar containing the organic silicon and the concrete shrinkage reducing agent JS-7.
Example 8
(1) 50g of TPEG (number average molecular weight of 2300-3) 8g of sodium polystyrene sulfonate and a proper amount of deionized water are uniformly mixed to obtain a first mixture; mixing 15g of acrylic acid, 5g of methyl acrylate, 10g of acrylamide, 1.3g of gamma-methacryloxypropyltrimethoxysilane, 1.0g of diethylene glycol monoacrylate and a proper amount of deionized water to obtain a second mixture; mixing 0.8g of sodium bisulfite, 0.6g of 3-mercaptopropionic acid, and an appropriate amount of deionized water to obtain a third mixture;
(2) placing the first mixture into a reaction kettle, heating to 37-43 ℃ while continuously stirring, adding 1.2g of ammonium persulfate once after the temperature is kept stable, dropwise adding the second mixture and the third mixture within 1-4h, and reacting at 37-43 ℃ for 1-2h in a heat preservation way after dropwise adding;
(3) and (3) adding liquid caustic soda into the material obtained in the step (2), and adjusting the pH value to 5.5-6 to obtain the mortar containing the organic silicon and the concrete shrinkage reducing agent JS-8.
Comparative test
1. Drying shrinkage test of cement mortar
According to the regulation in JC/T603-2004, the mixing ratio of cement and sand is kept unchanged in a cement mortar drying shrinkage test, the mass ratio of cement mortar to standard sand is 1: 2, the cement used in the test is the reference cement, the sand is the standard sand, and the water consumption of the mortar is determined according to the fluidity of the prepared mortar to 130 mm-140 mm.A prepared mortar is put into a curing box or a fog chamber with the temperature of 20 +/-1 ℃ and the relative humidity of not less than 90 percent for curing for 24 +/-2 h and demoulding, then is put into water for curing for 2d, is taken out to measure the initial length L0, is put into a drying and curing chamber with the temperature of 20 +/-3 ℃ and the relative humidity of 50 +/-4 percent, measures the length L7 d from the molding day, measures the length L28 d from 28d, selects a certain shrinkage reducing agent product sold in the comparative example 1, adopts experimental water, and the experimental results are shown in a table 1:
table 1 cement mortar dry shrinkage test results for different embodiments
Note:
in table 1, the data before "/" indicates the drying shrinkage of cement mortar, and the data after "/" indicates the shrinkage ratio to comparative example 2.
As can be seen from the data in Table 1, the drying shrinkage of the cement mortar can be effectively reduced, the drying shrinkage of the cement mortar of 7d is reduced by about 10% compared with that of comparative example 2, the drying shrinkage of the cement mortar of 28d is reduced by about 20% compared with that of comparative example 2, and the cement mortar has no adverse effect on the strength of the cement mortar of 28 d.
2. Drying shrinkage test of concrete
The slump of the fresh concrete is kept at 200 +/-10 mm by adjusting the mixing amount of the water reducing agent, the mixing proportion of the concrete is shown in table 2, and the test result is shown in table 3.
TABLE 2 concrete mix proportions
TABLE 3 variation of concrete shrinkage for different embodiments
| Sample (I) | Mixing amount/% | 7d dry shrinkage/× 10-6 | 28d dry shrinkage/× 10-6 |
| Comparative example 1 | 0.2 | -98 | -178 |
| Comparative example 2 | 0.2 | -105 | -190 |
| JS-1 | 0.2 | -86 | -167 |
| JS-2 | 0.2 | -79 | -161 |
| JS-3 | 0.2 | -84 | -158 |
| JS-4 | 0.2 | -75 | -143 |
| JS-5 | 0.2 | -81 | -151 |
| JS-6 | 0.2 | -73 | -159 |
| JS-7 | 0.2 | -77 | -148 |
| JS-8 | 0.2 | -82 | -154 |
From the test results in table 3, it can be seen that the concrete performance test using the raw materials and the mixing ratio shown in table 2 according to the present invention can effectively reduce the drying shrinkage of concrete by up to 28.6% at age 7 days and by up to 24.7% at age 28 days, compared to comparative example 2.
Further, a better sample is selected, concrete performance tests of different doping amount shrinkage reducing agent products are carried out, the doping amount of the water reducing agent is adjusted to keep the slump of fresh concrete within 200 +/-10 mm, the concrete mixing ratio is shown in a table 5, the test result is shown in a table 6, and the visual chart is shown in a figure 1.
TABLE 5 concrete mix proportions
TABLE 6 variation of the invention in the dry shrinkage of the concrete with different blending amounts
| Sample (I) | Mixing amount/% | 1d dry shrinkage/× 10-6 | 3d Dry shrinkage/× 10-6 | 7d dry shrinkage/× 10-6 | 28d dry shrinkage/× 10-6 |
| Comparative example 2 | 0.2 | -68.3 | -205.7 | -377.3 | -672 |
| JS-4 | 0.2 | -41.7 | -140.7 | -259.3 | -463.7 |
| JS-4 | 0.15 | -49 | -167 | -301.3 | -510 |
| JS04 | 0.25 | -40.3 | -135.7 | -241.7 | -434.3 |
From the data in table 6 and fig. 1, it can be seen that the present invention can effectively reduce the dry shrinkage of concrete in the concrete performance test using the raw materials and the mixing ratio shown in table 5, and the shrinkage reducing ability is further improved as the mixing amount of the present invention is increased. Compared with comparative example 2, the addition amount of the additive is 0.25%, the addition amount can be reduced by 35.9% when the age is 7 days, and the addition amount can be reduced by 35.4% at the highest when the age is 28 days.
Experimental results show that the invention achieves the purpose of reduction.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (10)
1. A mortar and concrete shrinkage reducing agent containing organic silicon is characterized in that: the pH value is 5.5-6, and the medicine is prepared from the following raw materials in parts by weight:
the structural formula of the TPEG is CH2＝C(CH3)CH2CH2O(CH2CH2O)nH, wherein n is a positive integer;
the unsaturated carboxylic acid and its derivative comprises at least one of acrylic acid, acrylamide, methacrylic acid, maleic anhydride, methyl acrylate, and dimethyl maleate;
the organic silicon monomer comprises at least one of vinyltrimethylsilane, trifluoromethyltrimethylsilane, vinyltriethoxysilane and gamma-methacryloxypropyltrimethoxysilane;
the ethylene glycol acrylate hydrophobic monomer comprises at least one of polyethylene glycol dimethacrylate, polyethylene glycol acrylate, diethylene glycol monoacrylate and ethylene glycol dimethacrylate.
2. The silicone-containing mortar and concrete shrinkage reducing agent of claim 1, wherein: the unsaturated carboxylic acid and the derivative thereof are at least one of acrylic acid, acrylamide, methacrylic acid, maleic anhydride, methyl acrylate and dimethyl maleate.
3. The silicone-containing mortar and concrete shrinkage reducing agent of claim 1, wherein: the organic silicon monomer is at least one of vinyltrimethylsilane, trifluoromethyltrimethylsilane, vinyltriethoxysilane and gamma-methacryloxypropyltrimethoxysilane.
4. The silicone-containing mortar and concrete shrinkage reducing agent of claim 1, wherein: the ethylene glycol acrylate hydrophobic monomer is at least one of polyethylene glycol dimethacrylate, polyethylene glycol acrylate, diethylene glycol monoacrylate and ethylene glycol dimethacrylate.
5. The silicone-containing mortar and concrete shrinkage reducing agent of claim 1, wherein: the anionic surfactant comprises at least one of sodium dodecyl sulfonate, sodium dodecyl benzene sulfonate, sodium polystyrene sulfonate and sodium methyl propylene sulfonate.
6. The silicone-containing mortar and concrete shrinkage reducing agent of claim 1, wherein: the reducing agent includes at least one of sodium bisulfite, vitamin C, ferrous sulfate, and glucose.
7. The silicone-containing mortar and concrete shrinkage reducing agent of claim 1, wherein: the initiator comprises at least one of ammonium persulfate and potassium persulfate.
8. The silicone-containing mortar and concrete shrinkage reducing agent of claim 1, wherein: the chain transfer agent comprises at least one of thioglycolic acid, 2-mercaptopropionic acid, 3-mercaptopropionic acid and sodium methallylsulfonate.
9. The silicone-containing mortar and concrete shrinkage reducing agent of claim 1, wherein: the solute in the liquid alkali comprises at least one of potassium hydroxide and sodium hydroxide.
10. The method for preparing a silicone-containing mortar and concrete shrinkage reducing agent according to any one of claims 1 to 9, wherein: the method comprises the following steps:
(1) TPEG, anionic surfactant and a proper amount of deionized water are uniformly mixed to obtain a first mixture; mixing unsaturated carboxylic acid and derivatives thereof, an organic silicon monomer, a glycol acrylate hydrophobic monomer and a proper amount of deionized water to obtain a second mixture; mixing a reducing agent, a chain transfer agent and a proper amount of deionized water to obtain a third mixture;
(2) placing the first mixture into a reaction kettle, heating to 37-43 ℃ while continuously stirring, adding an initiator once after the temperature is kept stable, dropwise adding the second mixture and the third mixture within 1-4h, and reacting at 37-43 ℃ for 1-2 h;
(3) and (3) adding liquid alkali into the material obtained in the step (2) to obtain the mortar containing the organic silicon and the concrete shrinkage reducing agent.
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