CN114380525A - Slump-retaining type concrete antifreezing water reducing agent and preparation method thereof - Google Patents
Slump-retaining type concrete antifreezing water reducing agent and preparation method thereof Download PDFInfo
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- CN114380525A CN114380525A CN202111361853.4A CN202111361853A CN114380525A CN 114380525 A CN114380525 A CN 114380525A CN 202111361853 A CN202111361853 A CN 202111361853A CN 114380525 A CN114380525 A CN 114380525A
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- slump
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- reducing agent
- water reducing
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 106
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 79
- 239000004567 concrete Substances 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 42
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 14
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000001110 calcium chloride Substances 0.000 claims abstract description 13
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 13
- 235000010288 sodium nitrite Nutrition 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 9
- 239000007785 strong electrolyte Substances 0.000 claims abstract description 9
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 8
- 150000002148 esters Chemical class 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 21
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 18
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 18
- 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 14
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 12
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 12
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 12
- 238000007710 freezing Methods 0.000 claims description 12
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 9
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 9
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 9
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- MCVVUJPXSBQTRZ-ONEGZZNKSA-N methyl (e)-but-2-enoate Chemical compound COC(=O)\C=C\C MCVVUJPXSBQTRZ-ONEGZZNKSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229920000151 polyglycol Polymers 0.000 claims description 6
- 239000010695 polyglycol Substances 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 230000003472 neutralizing effect Effects 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- -1 Methyl crotonate Chemical compound 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 3
- XBTYSBUGTSUGJM-UHFFFAOYSA-N methyl prop-2-enoate;sodium Chemical compound [Na].COC(=O)C=C XBTYSBUGTSUGJM-UHFFFAOYSA-N 0.000 claims 1
- 235000011121 sodium hydroxide Nutrition 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 6
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 125000001424 substituent group Chemical group 0.000 description 8
- 230000008014 freezing Effects 0.000 description 6
- 238000010276 construction Methods 0.000 description 5
- 230000006378 damage Effects 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 229910001413 alkali metal ion Inorganic materials 0.000 description 3
- 230000003335 steric effect Effects 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 239000012986 chain transfer agent Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- MCVVUJPXSBQTRZ-UHFFFAOYSA-N methyl but-2-enoate Chemical compound COC(=O)C=CC MCVVUJPXSBQTRZ-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000008030 superplasticizer Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
-
- 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
- C04B2103/60—Agents for protection against chemical, physical or biological attack
- C04B2103/601—Agents for increasing frost resistance
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a slump retaining type concrete antifreezing water reducing agent and a preparation method thereof, and relates to the technical field of slump retaining and antifreezing. The slump-retaining type concrete antifreezing water reducing agent comprises water and the following components in parts by weight: 8-12 parts of slump-retaining water reducing agent, 8-16 parts of water-soluble organic compound, 2-5 parts of strong electrolyte inorganic salt, 0.02-0.08 part of air entraining agent and 1-5 parts of regulator. The preparation method of the slump-retaining type concrete antifreezing water reducing agent comprises the following steps: adding water into a 1000mL four-neck flask, sequentially adding sodium nitrite, calcium chloride, ethylene glycol, triethanolamine, a slump-retaining water reducer, an air entraining agent and a regulator, and uniformly stirring to obtain the slump-retaining concrete antifreezing water reducer. The slump-retaining type concrete antifreezing water reducing agent prepared by the method can improve the initial water reducing rate and slump-retaining performance of concrete, can also improve the early strength and antifreezing effect of the concrete, is economical and environment-friendly, and does not cause environmental pollution.
Description
Technical Field
The invention relates to the technical field of slump retaining and antifreezing, in particular to a slump retaining type concrete antifreezing water reducing agent and a preparation method thereof.
Background
The slump-retaining type concrete antifreezing water reducing agent is a substance capable of preventing moisture in concrete from freezing at low temperature, can harden the concrete at negative temperature, keeps the slump of the concrete stable under a long-time construction state, ensures the construction performance of the concrete, and achieves the expected performance under the specified maintenance condition. When the average outside temperature is lower than 0 ℃ or the continuous temperature is lower than 5 ℃ for 3 days, the project is judged to enter the winter construction. After the engineering is constructed in winter, the cast-in-place concrete has the problem of early freezing damage, the concrete with the planar structure suffers from early freezing damage, the phenomena of surface flour formation, edge missing and corner falling, loose structure and even steel bar exposure occur, and the engineering quality is seriously influenced.
In order to solve the problem of winter damage of the engineering, the engineering usually adopts heating methods, mainly comprises greenhouse heating, electric heating, steam heating and the like, but the processes of all the heating methods are complex, the cost is high, the method is not suitable for strip engineering such as railways and the like, and the most effective method for controlling early freezing damage is to add an antifreezing agent into concrete at present. In order to solve the construction problem of the concrete in the winter period of the engineering, a retarder is usually added during mixing. However, the currently used antifreezing agents and retarders have the problem of overhigh chloride ions and alkali metal ions, and meanwhile, substances polluting human bodies and the environment exist in the antifreezing agents, and the antifreezing effect is not obvious in the ultralow temperature environment.
Disclosure of Invention
In order to solve the problems, the invention provides a slump-retaining concrete antifreezing water reducing agent and a preparation method thereof.
The technical scheme of the invention is as follows:
the slump-retaining type concrete antifreezing water reducing agent comprises water and the following components in parts by weight: 8-12 parts of slump-retaining water reducing agent, 8-16 parts of water-soluble organic compound, 2-5 parts of strong electrolyte inorganic salt, 0.02-0.08 part of air entraining agent and 1-5 parts of regulator.
The slump-retaining water reducer is added, so that the initial water reducing rate and the slump-retaining performance of the concrete can be improved; the early strength and the antifreezing effect of the concrete can be improved by adding the water-soluble organic compound and the strong electrolyte inorganic salt; the air entraining agent is added, so that dense micro bubbles can be introduced into the concrete, the workability of the concrete is improved, the expansion pressure generated by the concrete freezing at low temperature is relieved, and the anti-freezing effect of the slump-retaining type concrete anti-freezing agent is obviously improved; the concrete regulator is added to reduce the viscosity of concrete, improve the workability and improve the pumping, construction and antifreezing performance of concrete.
Further, the water-soluble organic compound comprises ethylene glycol and triethanolamine, and the mass ratio of the ethylene glycol to the triethanolamine is 1: 1.
Further, strong electrolyte inorganic salts include sodium nitrite and calcium chloride or sodium chloride.
Further, the slump-retaining water reducer comprises: 2-methylprop-2-enylpolyglycol ether, Acrylic Acid (AA), sodium methallyl sulfonate (MAS-1), synthetic ester P, hydroxyethyl acrylate (MC) and ammonium persulfate.
The two esters in the slump-retaining water reducer have synergistic effect and are copolymerized with unsaturated acid to obtain a copolymer of a reaction active agent with double ester groups, so that the purposes of good dispersion, retardation and slump retaining are achieved; sodium methallyl sulfonate (MAS-1) is used as a chain transfer agent to control the molecular weight of a polymer on the one hand, and on the other hand, the sodium methallyl sulfonate is used as a chain transfer agent to generate high water reducing rate and improve cement fluidity when being dispersed efficiently.
Further, the raw materials for synthesizing the ester P are phthalic anhydride, methyl crotonate and a catalyst TiO2-Fe2O3Methyl crotonate, phthalic anhydride and catalyst TiO2-Fe2O3The molar ratio of (2.5-4.5) to (1) (0.03-0.04).
Further, the molar ratio of the 2-methylpropane-2-alkenyl polyglycol ether to the acrylic acid is (5.0-10.0): the molecular weight of the 1, 2-methylpropane-2-alkenyl polyglycol ether is 800-3000.
Further, the weight percentage of the sodium methallyl sulfonate in the slump-retaining water reducer is 0.5-0.9%, the weight percentage of the hydroxyethyl acrylate is 1.0-1.5%, the weight percentage of the synthetic ester P is 0.3-0.5%, the weight percentage of the ammonium persulfate is 1.1-1.5%, and the balance is water.
The invention also discloses a preparation method of the slump-retaining type concrete antifreezing water reducing agent, which comprises the following preparation steps:
s1, preparing synthetic ester P: phthalic anhydride, methyl crotonate and catalyst TiO2-Fe2O3Adding the mixture into a four-neck flask one by one, uniformly stirring, reacting at 105 ℃ for 2 hours, and cooling to room temperature after the reaction is finished to obtain synthetic ester P;
s2, preparing a material A and a material C: dissolving acrylic acid in water to prepare a material A, and dissolving ammonium persulfate in water to prepare a material C;
s3, preparing a slump-retaining water reducer: uniformly mixing MC and synthetic ester P in proportion, taking 2/3, transferring into a four-neck flask, starting stirring, transferring 2-methylpropane-2-alkenyl polyethylene glycol ether into the flask, then adding MAS-1, flushing and transferring the mixture of the rest ester into the four-neck flask together, heating to above 75 ℃, keeping the temperature for 10min, simultaneously dropwise adding material A and material C, carrying out heat preservation reaction for 90min after the dropwise addition is finished, and neutralizing with liquid alkali until the pH value is 5-7 to obtain the slump-retaining water reducer;
s4, preparing the slump-retaining type concrete antifreezing water reducing agent: and (4) adding water into a 1000mL four-neck flask, sequentially adding sodium nitrite, calcium chloride, ethylene glycol, triethanolamine, the slump-retaining water reducer prepared in the step S3, an air entraining agent and a regulator, and uniformly stirring to obtain the slump-retaining anti-freezing water reducer.
The invention adopts a water solution free radical polymerization mode to prepare the slump-retaining water reducer. The performance of the polycarboxylate superplasticizer is closely related to the molecular structure, the conjugated effect, the polar effect, the steric effect and the like of the substituent groups can influence the polymerization of monomers and the activity of free radicals, and the larger the conjugated effect of the substituent groups on the free radicals, the lower the activity of the substituent groups. In addition, the rate of reaction of free radicals with monomers is also related to steric effects: when the vinyl monomer contains a substituent, the volume exclusion of the substituent causes the reactivity between the radical and the monomer to decrease. If two substituents are on the same carbon atom, steric hindrance effect is not obvious, and monomer activity is enhanced due to superposition of electronic effects of the substituents; if the substituents are located on different carbon atoms, steric effects may again render them less active.
The invention has the beneficial effects that:
1. the slump-retaining type concrete antifreezing water reducing agent provided by the invention has the advantages of high water reducing rate (more than or equal to 25%), good antifreezing effect, strong slump-retaining performance, capability of keeping the slump of concrete from losing for 2 hours from the initial stage, good air entraining performance, environmental friendliness, no toxicity, no harm, no alkali, almost no chloride ions, sulfate ions, alkali metal ions and formaldehyde, and saving and environmental protection.
2. The slump-retaining type concrete antifreezing water reducing agent disclosed by the invention is simple in preparation process and environment-friendly, the preparation process is carried out according to the standard, and all indexes of the prepared slump-retaining type concrete antifreezing water reducing agent meet the requirements of first-class products of building material industry standard JC 475-.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments below:
the slump-retaining type antifreezing water reducing agent implemented by the invention is tested according to JC 475-3The sand rate is 38 percent, and the mixing amount of the slump-retaining type antifreezing water reducing agent is 1.5 to 2.5 percent.
The slump-retaining type concrete antifreezing water reducing agent comprises water and the following components in parts by weight: 8-12 parts of slump-retaining water reducing agent, 8-16 parts of water-soluble organic compound, 2-5 parts of strong electrolyte inorganic salt, 0.02-0.08 part of air entraining agent and 1-5 parts of regulator. The water-soluble organic compound comprises ethylene glycol and triethanolamine, and the mass ratio of the ethylene glycol to the triethanolamine is 1: 1. The strong electrolyte inorganic salt comprises sodium nitrite and calcium chloride or sodium chloride, preferably the calcium chloride and the sodium nitrite, wherein the mass ratio of the calcium chloride to the sodium nitrite is (0.1-1): 1, preferably 0.4: 1.
The slump-retaining water reducing agent comprises: 2-methylprop-2-enylpolyglycol ether, Acrylic Acid (AA), sodium methallyl sulfonate (MAS-1), synthetic ester P, hydroxyethyl acrylate (MC) and ammonium persulfate. The molecular weight of the 2-methylpropane-2-alkenyl polyglycol ether is 800-3000, preferably 2400; the molar ratio of the 2-methylpropane-2-alkenyl polyglycol ether to the acrylic acid is (5.0-10.0): 1, preferably 7.5: 1. The mass ratio of the sodium methallyl sulfonate in the slump-retaining water reducer is 0.5-0.9%, and the preferable ratio is as follows: 0.80 percent; the mass ratio of the hydroxyethyl acrylate is 1.0-1.5%, and the preferred ratio is: 1.30 percent; the mass ratio of the synthetic ester P is 0.3-0.5%, preferably: 0.40 percent; the mass ratio of ammonium persulfate is 1.1-1.5%, preferably: 1.30 percent; the rest is water.
The raw materials for synthesizing the ester P are phthalic anhydride, methyl crotonate and catalyst TiO2-Fe2O3Methyl butenoate, phthalic anhydride and catalyst TiO2-Fe2O3The molar ratio of (2.5-4.5) to (1) (0.03-0.04), preferably 3.5: 1: 0.036.
the materials are prepared according to the optimal preferential ratio to prepare the slump-retaining concrete antifreezing water reducer, and the operation steps are as follows: s1, preparing synthetic ester P: phthalic anhydride, methyl crotonate and catalyst TiO2-Fe2O3Adding the mixture into a four-neck flask one by one, uniformly stirring, reacting at 105 ℃ for 2 hours, and cooling to room temperature after the reaction is finished to obtain synthetic ester P;
s2, preparing a material A and a material C: dissolving acrylic acid in water to prepare a material A, and dissolving ammonium persulfate in water to prepare a material C;
s3, preparing a slump-retaining water reducer: uniformly mixing MC and synthetic ester P in proportion, taking 2/3, transferring into a four-neck flask, starting stirring, transferring 2-methylpropane-2-alkenyl polyethylene glycol ether into the flask, then adding MAS-1, flushing and transferring the mixture of the rest ester into the four-neck flask together, heating to above 75 ℃, keeping the temperature for 10min, simultaneously dropwise adding material A and material C, finishing dropping material A for 165min, finishing dropping material C for 180min, carrying out heat preservation reaction for 90min, neutralizing liquid alkali to pH 5-7 to obtain the slump-retaining water reducer, wherein the solid content of the slump-retaining water reducer is 45%;
s4, preparing the slump-retaining type concrete antifreezing water reducing agent: and (4) adding water into a 1000mL four-neck flask, sequentially adding sodium nitrite, calcium chloride, ethylene glycol, triethanolamine, the slump-retaining water reducer prepared in the step S3, an air entraining agent and a regulator, and uniformly stirring to obtain the slump-retaining anti-freezing water reducer.
Example 1
A slump-retaining concrete antifreezing water reducing agent is prepared by the following steps: slump loss resistant water reducing agent, water-soluble organic compound, strong electrolyte inorganic salt, air entraining agent and regulator. The slump-retaining type concrete antifreezing water reducing agent comprises the following components in percentage by mass: 8% of slump loss resistant water reducing agent, 4% of ethylene glycol, 4% of triethanolamine, 2% of sodium nitrite, 0.4% of calcium chloride, 0.2% of air entraining agent, 2% of regulator and 79.4% of water.
And then preparing the slump-retaining concrete antifreezing water reducing agent, wherein the operation steps are the same as the above. Adding water into a 1000mL four-neck flask, then sequentially adding sodium nitrite, calcium chloride, ethylene glycol, triethanolamine, a slump-retaining water reducer, an air entraining agent and a regulator, and uniformly stirring to obtain the slump-retaining anti-freezing water reducer.
After the prepared slump-retaining type concrete antifreezing water reducing agent is placed in a refrigerator at the temperature of-5 ℃ for freezing for 72 hours, the state is good, and the icing phenomenon does not occur.
The mixing amount of the slump-retaining type concrete antifreezing water reducing agent is 1.8%, and the detection results are shown in Table 1:
TABLE 1
Example 2
A slump retaining type concrete antifreezing water reducing agent comprises the following components in percentage by mass: 10% of slump-retaining water reducing agent, 6% of ethylene glycol, 6% of triethanolamine, 2% of sodium nitrite, 0.8% of calcium chloride, 0.4% of air entraining agent, 3% of regulator and 71.8% of water.
And then preparing the slump-retaining concrete antifreezing water reducing agent, wherein the operation steps are the same as the above. The prepared slump retaining type concrete antifreezing water reducing agent is frozen in a refrigerator at the temperature of-5 ℃ for 72 hours, the state is good, and the phenomenon of icing is avoided.
The mixing amount of the slump-retaining type concrete antifreezing water reducing agent is 2.1%, and the detection results are shown in Table 2:
TABLE 2
Example 3
A slump retaining type concrete antifreezing water reducing agent comprises the following components in percentage by mass: 12% of slump-retaining water reducing agent, 8% of ethylene glycol, 8% of triethanolamine, 2.0% of sodium nitrite, 1.2% of calcium chloride, 0.4% of air entraining agent, 4% of regulator and 64.4% of water.
And then preparing the slump-retaining concrete antifreezing water reducing agent, wherein the operation steps are the same as the above. The prepared slump retaining type concrete antifreezing water reducing agent is frozen in a refrigerator at the temperature of-5 ℃ for 72 hours, the state is good, and the phenomenon of icing is avoided.
The mixing amount of the slump-retaining type concrete antifreezing water reducing agent is 2.4%, and the detection results are shown in Table 3:
TABLE 3
As can be seen from tables 1, 2 and 3, the slump-retaining type concrete antifreezing water reducing agent researched by the invention has the advantages of high water reducing rate, good slump-retaining performance and good antifreezing effect, and the slump-retaining type concrete antifreezing water reducing agent hardly contains chloride ions, sulfate ions, alkali metal ions and formaldehyde, so that the slump-retaining type concrete antifreezing water reducing agent is very environment-friendly. All detection indexes meet the requirements of first-class products of building material industry standard JC 475-.
The foregoing is merely an example of the present invention and common general knowledge of known specific structures and features of the embodiments is not described herein in any greater detail. It should be noted that, for those skilled in the art, without departing from the structure of the present invention, several changes and modifications can be made, which should also be regarded as the protection scope of the present invention, and these will not affect the effect of the implementation of the present invention and the practicability of the patent. The scope of the claims of the present application shall be defined by the claims and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (8)
1. The slump-retaining type concrete antifreezing water reducing agent is characterized by comprising water and the following components in parts by weight: 8-12 parts of slump-retaining water reducing agent, 8-16 parts of water-soluble organic compound, 2-5 parts of strong electrolyte inorganic salt, 0.02-0.08 part of air entraining agent and 1-5 parts of regulator.
2. The slump-retaining type concrete antifreezing water reducing agent according to claim 1, wherein: the water-soluble organic compound comprises ethylene glycol and triethanolamine, and the mass ratio of the ethylene glycol to the triethanolamine is 1: 1.
3. The slump-retaining type concrete antifreezing water reducing agent according to claim 1, wherein: the strong electrolyte inorganic salt comprises sodium nitrite and calcium chloride or sodium chloride.
4. The slump-retaining concrete antifreezing water reducing agent according to claim 1, wherein the slump-retaining water reducing agent comprises: 2-methylprop-2-enylpolyglycol ether, Acrylic Acid (AA), sodium methallyl sulfonate (MAS-1), synthetic ester P, hydroxyethyl acrylate (MC) and ammonium persulfate.
5. The slump-retaining type concrete antifreezing water reducing agent according to claim 4, wherein: the raw materials for synthesizing the ester P are phthalic anhydride, methyl crotonate and a catalyst TiO2-Fe2O3Methyl crotonate, phthalic anhydride and catalyst TiO2-Fe2O3The molar ratio of (2.5-4.5) to (1) (0.03-0.04).
6. The slump-retaining type concrete antifreezing water reducing agent according to claim 4, wherein: the molar ratio of the 2-methylpropane-2-alkenyl polyglycol ether to the acrylic acid is (5.0-10.0): 1, the molecular weight of the 2-methylpropane-2-alkenyl polyglycol ether is 800-3000.
7. The slump-retaining type concrete antifreezing water reducing agent according to claim 4, wherein: in the slump loss resistant water reducing agent, the mass ratio of sodium methyl acrylate is 0.5-0.9%, the mass ratio of hydroxyethyl acrylate is 1.0-1.5%, the mass ratio of synthetic ester P is 0.3-0.5%, the mass ratio of ammonium persulfate is 1.1-1.5%, and the balance is water.
8. The preparation method of the slump-retaining concrete antifreezing water reducing agent according to any one of claims 1 to 7, characterized by comprising the following steps:
s1, preparing synthetic ester P: phthalic anhydride, methyl crotonate and catalyst TiO2-Fe2O3Adding the mixture into a four-neck flask one by one, uniformly stirring, reacting at 105 ℃ for 2 hours, and cooling to room temperature after the reaction is finished to obtain synthetic ester P;
s2, preparing a material A and a material C: dissolving acrylic acid in water to prepare a material A, and dissolving ammonium persulfate in water to prepare a material C;
s3, preparing a slump-retaining water reducer: uniformly mixing MC and synthetic ester P in proportion, taking 2/3, transferring into a four-neck flask, starting stirring, transferring 2-methylpropane-2-alkenyl polyethylene glycol ether into the flask, adding MAS-1, flushing and transferring the mixture of the residual ester into the four-neck flask together, heating to above 75 ℃, keeping the temperature for 10min, simultaneously dropwise adding material A and material C, carrying out heat preservation reaction for 90min after the dropwise adding is finished, and neutralizing with liquid caustic soda until the pH value is 5-7 to obtain the slump-retaining water reducer;
s4, preparing the slump-retaining type concrete antifreezing water reducing agent: and (4) adding water into a 1000mL four-neck flask, sequentially adding sodium nitrite, calcium chloride, ethylene glycol, triethanolamine, the slump-retaining water reducer prepared in the step S3, an air entraining agent and a regulator, and uniformly stirring to obtain the slump-retaining anti-freezing water reducer.
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