CN118894695B - Modified mineral admixture concrete and preparation method thereof - Google Patents
Modified mineral admixture concrete and preparation method thereof Download PDFInfo
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- CN118894695B CN118894695B CN202411390010.0A CN202411390010A CN118894695B CN 118894695 B CN118894695 B CN 118894695B CN 202411390010 A CN202411390010 A CN 202411390010A CN 118894695 B CN118894695 B CN 118894695B
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- 239000004567 concrete Substances 0.000 title claims abstract description 58
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 43
- 239000011707 mineral Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 51
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000002156 mixing Methods 0.000 claims abstract description 34
- 239000010881 fly ash Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000004576 sand Substances 0.000 claims abstract description 19
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 18
- 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 abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 18
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000003469 silicate cement Substances 0.000 claims abstract description 10
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 44
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 42
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 20
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 14
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- PCLIMKBDDGJMGD-UHFFFAOYSA-N N-bromosuccinimide Chemical compound BrN1C(=O)CCC1=O PCLIMKBDDGJMGD-UHFFFAOYSA-N 0.000 claims description 10
- -1 isopentenyl Chemical group 0.000 claims description 9
- DTNODBHGOLWROS-UHFFFAOYSA-N 3-amino-4-methylbenzenesulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1N DTNODBHGOLWROS-UHFFFAOYSA-N 0.000 claims description 8
- BFKXHILYGIQGCB-UHFFFAOYSA-N 52083-08-6 Chemical compound O=C1OC(=O)C2=CC=CC3=C2C1=CC=C3O BFKXHILYGIQGCB-UHFFFAOYSA-N 0.000 claims description 8
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 8
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 8
- 239000011398 Portland cement Substances 0.000 claims description 8
- HFBMWMNUJJDEQZ-UHFFFAOYSA-N acryloyl chloride Chemical compound ClC(=O)C=C HFBMWMNUJJDEQZ-UHFFFAOYSA-N 0.000 claims description 8
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 8
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- 239000010413 mother solution Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 239000005457 ice water Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000007792 addition Methods 0.000 claims description 2
- 229920000151 polyglycol Polymers 0.000 claims description 2
- 239000010695 polyglycol Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 6
- 238000000034 method Methods 0.000 claims 4
- 239000004568 cement Substances 0.000 abstract description 8
- 239000012452 mother liquor Substances 0.000 abstract description 8
- 230000014759 maintenance of location Effects 0.000 abstract description 6
- 238000010276 construction Methods 0.000 abstract description 5
- 239000004566 building material Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 27
- 238000002390 rotary evaporation Methods 0.000 description 15
- SXOZXLUKVXWUGL-UHFFFAOYSA-M sodium;formaldehyde;hydrogen sulfate Chemical compound [Na+].O=C.OS([O-])(=O)=O SXOZXLUKVXWUGL-UHFFFAOYSA-M 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000012044 organic layer Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 238000003760 magnetic stirring Methods 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical class [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000010883 coal ash Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004574 high-performance concrete Substances 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical group [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 238000007112 amidation reaction Methods 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 230000002140 halogenating effect Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- DGVVJWXRCWCCOD-UHFFFAOYSA-N naphthalene;hydrate Chemical compound O.C1=CC=CC2=CC=CC=C21 DGVVJWXRCWCCOD-UHFFFAOYSA-N 0.000 description 1
- 238000010534 nucleophilic substitution reaction Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/40—Compounds containing silicon, titanium or zirconium or other organo-metallic compounds; Organo-clays; Organo-inorganic complexes
- C04B24/42—Organo-silicon compounds
-
- 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
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/2015—Sulfate resistance
-
- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
本发明涉及一种改性矿物掺合料混凝土及其制备方法，属于建筑材料技术领域；本发明以粉煤灰掺合料、硅酸盐水泥、砂子、丙烯酸、次亚磷酸钠、甲醛次硫酸氢钠、过硫酸铵、改性减水剂为原料，制备了一种改性矿物掺合料混凝土；本发明还公布了该改性矿物掺合料混凝土的制备方法，包括先制备一种减水剂母液，再将粉煤灰掺合料与水泥和砂子混合得到混合料，最后将减水剂母液加入混合料中得到改性矿物掺合料混凝土。本发明的改性矿物掺合料混凝土制备方法简单，原料易得，固化后的强度高，固化28天后抗压强度最高可达51.6MPa，初始流动性好，保坍性优异，可以在建筑领域广泛应用。The present invention relates to a modified mineral admixture concrete and a preparation method thereof, and belongs to the technical field of building materials; the present invention uses fly ash admixture, silicate cement, sand, acrylic acid, sodium hypophosphite, sodium formaldehyde sulfoxylate, ammonium persulfate, and modified water reducer as raw materials to prepare a modified mineral admixture concrete; the present invention also discloses a preparation method of the modified mineral admixture concrete, including first preparing a water reducer mother liquor, then mixing the fly ash admixture with cement and sand to obtain a mixture, and finally adding the water reducer mother liquor to the mixture to obtain the modified mineral admixture concrete. The preparation method of the modified mineral admixture concrete of the present invention is simple, the raw materials are easy to obtain, the strength after curing is high, the compressive strength after curing for 28 days can reach up to 51.6MPa, the initial fluidity is good, the collapse retention is excellent, and it can be widely used in the construction field.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to modified mineral admixture concrete and a preparation method thereof.
Background
Concrete is an indispensable building material in modern buildings, and with the continuous development of modern building technology, the requirements for concrete materials are increasing. In order to meet the demands of buildings in terms of mechanical properties, durability, building quality and the like, high-performance concrete is becoming an important development direction in the building field. The mineral admixture concrete is an important form of high-performance concrete, and the active ingredients in the admixture react with calcium hydroxide in cement hydration products to generate hydration products with gelling property, so that the durability of the concrete is enhanced, and the mineral admixture concrete has wide application prospect.
However, this technology still has some disadvantages, although the appropriate amount of mineral admixture can improve the durability of concrete, when the admixture is excessively large, the strength of concrete will be reduced, in addition, the initial fluidity and slump retention of the concrete doped with mineral admixture will be reduced, which greatly increases the construction difficulty, the construction time may lead to problems of segregation, bleeding and the like of concrete, influences the construction quality and progress, and how to improve the strength and slump retention of the mineral admixture concrete becomes the primary problem of the prior art.
Disclosure of Invention
The invention aims to provide modified mineral admixture concrete and a preparation method thereof, which are used for solving the problems in the background art.
The aim of the invention can be achieved by the following technical scheme:
15-23 parts of fly ash admixture, 3-4 parts of Portland cement, 74-85 parts of sand, 0.08-0.1 part of acrylic acid, 0.001-0.002 part of sodium hypophosphite, 0.001-0.0015 part of sodium formaldehyde sulfoxylate, 0.002-0.006 part of ammonium persulfate and 0.05-0.08 part of modified water reducer;
A preparation method of modified mineral admixture concrete comprises the following steps:
15-23 parts of fly ash admixture, 3-4 parts of Portland cement, 74-85 parts of sand, 0.08-0.1 part of acrylic acid, 0.001-0.002 parts of sodium hypophosphite, 0.001-0.0015 part of formaldehyde sodium bisulfate, 0.002-0.006 part of ammonium persulfate and 0.05-0.08 part of modified water reducer are weighed according to parts by weight, and the modified water reducer, sodium hypophosphite and ammonium persulfate are dissolved by water and uniformly stirred to obtain solution A;
Secondly, dissolving acrylic acid and formaldehyde sodium bisulfate with water, and uniformly stirring to obtain a solution B;
Thirdly, stirring and mixing the solution A and the solution B to obtain a water reducer mother solution;
grinding the fly ash admixture, uniformly mixing the fly ash admixture with silicate cement, sand and water, and stirring to obtain a mixture;
fifthly, adding the water reducer mother liquor obtained in the third step into the mixture obtained in the fourth step, and uniformly stirring to obtain modified mineral admixture concrete;
further, in the third step, the temperature condition for stirring and mixing the solution A and the solution B is 10-40 ℃.
Further, the particle size specification of the pulverized coal ash admixture in the fourth step is 0.1-0.5mm.
Further, the modified water reducing agent is prepared by the following steps:
Step 1, mixing 4-hydroxy-1, 8-naphthalic anhydride, acryloyl chloride, triethylamine and tetrahydrofuran in a three-neck flask, starting magnetic stirring, reacting for 5 hours under the ice water bath condition, washing with saturated sodium carbonate solution after the reaction is finished, separating an organic layer by a separating funnel, and performing rotary evaporation to obtain an intermediate 1;
step 2, mixing the intermediate 1, a platinum complex and tetrahydrofuran in a three-neck flask, installing a condenser tube and a thermometer, starting magnetic stirring, dropwise adding trimethoxysilane into the three-neck flask by using a high-pressure dropwise adding pump at the temperature of 110 ℃, continuing to react for 2-3h at the temperature of 140 ℃ after the dropwise adding is finished, and performing rotary evaporation to obtain an intermediate 2 after the reaction is finished;
step 3, mixing 2-aminotoluene-4-sulfonic acid, N-bromosuccinimide, benzoyl peroxide and chloroform in a three-neck flask, mounting a condenser tube and a thermometer, starting magnetic stirring, reacting for 12 hours at the temperature of 80 ℃, and performing rotary evaporation after the reaction is finished to obtain an intermediate 3;
Step 4, mixing the intermediate 2, the intermediate 3, tetrabutylammonium bromide and tetrahydrofuran in a three-neck flask, installing a condenser tube and a thermometer, starting magnetic stirring, reacting for 10-12h at the temperature of 110-120 ℃, adding diethyl ether into the three-neck flask after the reaction is finished, vacuum filtering, and recrystallizing the obtained solid to obtain an intermediate 4;
Step 5, mixing an intermediate 4, isopentenyl polyethylene glycol ether, sodium hydroxide and dimethyl sulfoxide in a three-neck flask, mounting a condenser tube and a thermometer, starting magnetic stirring, reacting for 10 hours at the temperature of 120 ℃ under the protection of nitrogen, adding hydrochloric acid into the three-neck flask after the reaction is finished to adjust the pH value to be less than 2, separating an organic layer by using a separating funnel, and performing rotary evaporation to obtain the modified water reducer;
Further, the amount ratio of 4-hydroxy-1, 8-naphthalene dicarboxylic anhydride, acryloyl chloride, triethylamine, and tetrahydrofuran used in step 1 is 0.1mol:0.1-0.12mol:0.08-0.1mol:80-100mL.
Further, the intermediate 1, platinum complex, tetrahydrofuran, trimethoxysilane are used in the step 2 in an amount ratio of 0.08mol to 1mL to 60-80mL to 0.08-0.1mol.
Further, the 2-aminotoluene-4-sulfonic acid, N-bromosuccinimide, benzoyl peroxide and chloroform were used in the amount ratio of 0.1mol:0.1mol:3-4g:60-80mL in step 3.
Further, the amount ratio of intermediate 2, intermediate 3, tetrabutylammonium bromide, tetrahydrofuran used in step 4 was 0.05mol:0.05mol:5-8g:100-120mL.
Further, the intermediate 4, isopentenyl polyethylene glycol ether, sodium hydroxide, dimethyl sulfoxide are used in step 5 in a ratio of 3g to 27g to 6-9g to 150-200mL.
The invention has the beneficial effects that:
(1) The invention takes fly ash admixture, silicate cement, sand, acrylic acid, sodium hypophosphite, formaldehyde sodium bisulfate, ammonium persulfate and modified water reducer as raw materials to prepare modified mineral admixture concrete, the invention prepares solution A by firstly mixing the modified water reducer, sodium hypophosphite and ammonium persulfate, prepares solution B by mixing the acrylic acid and formaldehyde sodium bisulfate, and then the solution A and the solution B are mixed and reacted to prepare a water reducing agent mother liquor, then the water reducing agent mother liquor is mixed into a mixture prepared by stirring and mixing pulverized coal ash admixture, silicate cement and sand, the preparation method of the modified mineral admixture concrete is simple, green and environment-friendly, and the prepared concrete has good slump retention and high curing strength and is beneficial to popularization.
(2) The invention takes 4-hydroxy-1, 8-naphthalic anhydride as raw material, and takes esterification reaction with acryloyl chloride under the condition of triethylamine as acid-binding agent to obtain intermediate 1 with double bond, then makes the double bond of intermediate 1 take addition reaction with trimethoxy silane under the catalysis of platinum complex to obtain intermediate 2 with end group containing organic silicon structure, takes 2-amino toluene-4-sulfonic acid as raw material, takes N-bromosuccinimide as halogenating agent, takes halogenation reaction under the condition of benzoyl peroxide as initiator to obtain intermediate 3, and then makes intermediate 3 and intermediate 2 take amidation reaction under the catalysis of tetrabutylammonium bromide to obtain intermediate 4, and finally makes bromine atom of intermediate 4 take nucleophilic substitution reaction with hydroxyl of isopentenyl polyglycol ether to obtain modified water reducing agent; the modified water reducer has larger steric hindrance and a rigid structure, can effectively prevent the adsorption of cement paste when in action and improve the initial fluidity of concrete paste, and the side chain of benzene ring in the water reducer also contains sulfonic acid groups which can be hydrolyzed to form anchoring groups, so that electrostatic repulsion force is generated on the surface of cement particles, the flocculation structure of the cement paste is destroyed, the dispersibility of the cement paste in the concrete is improved, in addition, the water reducer has the structures of naphthalene water reducer and carboxylate water reducer, can jointly play a role, has higher water reducing effect, achieves higher fluidity and pumpability, can reduce air holes and defects in the concrete, and enhances the stability and working performance of the concrete, and besides, the water reducer also has an organosilicon structure, improves the fluidity of the cement paste, the toughness of the cement paste can be improved, so that the cured concrete not only has higher strength, but also has certain sulfate resistance.
(3) The preparation method of the modified mineral admixture concrete is simple, raw materials are easy to obtain, the prepared concrete is environment-friendly, the slump loss resistance is good, the curing strength is high, and the modified mineral admixture concrete has a certain sulfate resistance and can be widely applied to the field of buildings.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A modified water reducer is prepared by the following steps:
Step 1, mixing 0.1mol of 4-hydroxy-1, 8-naphthalene dicarboxylic anhydride, 0.1mol of acryloyl chloride, 0.08mol of triethylamine and 80mL of tetrahydrofuran in a container, uniformly stirring, reacting for 5 hours under the ice water bath condition, washing with saturated sodium carbonate solution after the reaction is finished, separating an organic layer, and performing rotary evaporation to obtain an intermediate 1;
Step 2, mixing 0.08mol of intermediate 1, 1mL of platinum complex and 60mL of tetrahydrofuran in a container, uniformly stirring, dropwise adding 0.08mol of trimethoxysilane into the container at the temperature of 110 ℃, continuously reacting for 2 hours at the temperature of 140 ℃ after the dropwise adding is finished, and performing rotary evaporation to obtain an intermediate 2 after the reaction is finished;
step 3, mixing 0.1mol of 2-aminotoluene-4-sulfonic acid, 0.1 molN-bromosuccinimide, 3g of benzoyl peroxide and 60mL of chloroform in a container, uniformly stirring, reacting for 12 hours at the temperature of 80 ℃, and performing rotary evaporation after the reaction is finished to obtain an intermediate 3;
step 4, mixing 0.05mol of intermediate 2, 0.05mol of intermediate 3, 5g of tetrabutylammonium bromide and 100mL of tetrahydrofuran in a container, uniformly stirring, reacting for 10 hours at the temperature of 110 ℃, adding diethyl ether into the container after the reaction is finished, vacuum filtering, and recrystallizing the obtained solid to obtain an intermediate 4;
And 5, mixing 3g of intermediate 4, 27g of isopentenyl polyethylene glycol ether, 6g of sodium hydroxide and 150mL of dimethyl sulfoxide in a container, uniformly stirring, reacting for 10 hours at the temperature of 120 ℃ under the protection of nitrogen, adding hydrochloric acid into the container to adjust the pH to be less than 2 after the reaction is finished, and separating an organic layer, and performing rotary evaporation to obtain the modified water reducer.
Example 2
A modified water reducer is prepared by the following steps:
Step1, mixing 0.1mol of 4-hydroxy-1, 8-naphthalene dicarboxylic anhydride, 0.11mol of acryloyl chloride, 0.09mol of triethylamine and 90mL of tetrahydrofuran in a container, uniformly stirring, reacting for 5 hours under the ice water bath condition, washing with saturated sodium carbonate solution after the reaction is finished, separating an organic layer, and performing rotary evaporation to obtain an intermediate 1;
Step 2, mixing 0.08mol of intermediate 1, 1mL of platinum complex and 70mL of tetrahydrofuran in a container, uniformly stirring, dropwise adding 0.09mol of trimethoxysilane into the container at the temperature of 110 ℃, continuously reacting for 2.5h at the temperature of 140 ℃ after the dropwise adding is finished, and performing rotary steaming to obtain an intermediate 2;
Step 3, mixing 0.1mol of 2-aminotoluene-4-sulfonic acid, 0.1 molN-bromosuccinimide, 3.5g of benzoyl peroxide and 70mL of chloroform in a container, uniformly stirring, reacting for 12 hours at the temperature of 80 ℃, and performing rotary evaporation after the reaction is finished to obtain an intermediate 3;
step 4, mixing 0.05mol of intermediate 2, 0.05mol of intermediate 3, 7g of tetrabutylammonium bromide and 110mL of tetrahydrofuran in a container, uniformly stirring, reacting for 11 hours at the temperature of 115 ℃, adding diethyl ether into the container after the reaction is finished, vacuum filtering, and recrystallizing the obtained solid to obtain an intermediate 4;
and 5, mixing 3g of intermediate 4, 27g of isopentenyl polyethylene glycol ether, 7g of sodium hydroxide and 175mL of dimethyl sulfoxide in a container, uniformly stirring, reacting for 10 hours at the temperature of 120 ℃ under the protection of nitrogen, adding hydrochloric acid into the container to adjust the pH to be less than 2 after the reaction is finished, and separating an organic layer, and performing rotary evaporation to obtain the modified water reducer.
Example 3
A modified water reducer is prepared by the following steps:
Step1, mixing 0.1mol of 4-hydroxy-1, 8-naphthalene dicarboxylic anhydride, 0.12mol of acryloyl chloride, 0.1mol of triethylamine and 100mL of tetrahydrofuran in a container, uniformly stirring, reacting for 5 hours under the ice water bath condition, washing with saturated sodium carbonate solution after the reaction is finished, separating an organic layer, and performing rotary evaporation to obtain an intermediate 1;
step 2, mixing 0.08mol of intermediate 1, 1mL of platinum complex and 80mL of tetrahydrofuran in a container, uniformly stirring, dropwise adding 0.1mol of trimethoxysilane into the container at the temperature of 110 ℃, continuously reacting for 3 hours at the temperature of 140 ℃ after the dropwise adding is finished, and performing rotary evaporation to obtain an intermediate 2 after the reaction is finished;
Step 3, mixing 0.1mol of 2-aminotoluene-4-sulfonic acid, 0.1 molN-bromosuccinimide, 4g of benzoyl peroxide and 80mL of chloroform in a container, uniformly stirring, reacting for 12 hours at the temperature of 80 ℃, and performing rotary evaporation after the reaction is finished to obtain an intermediate 3;
Step 4, mixing 0.05mol of intermediate 2, 0.05mol of intermediate 3, 8g of tetrabutylammonium bromide and 120mL of tetrahydrofuran in a container, uniformly stirring, reacting for 12 hours at the temperature of 120 ℃, adding diethyl ether into the container after the reaction is finished, vacuum filtering, and recrystallizing the obtained solid to obtain an intermediate 4;
And 5, mixing 3g of intermediate 4, 27g of isopentenyl polyethylene glycol ether, 9g of sodium hydroxide and 200mL of dimethyl sulfoxide in a container, uniformly stirring, reacting for 10 hours at the temperature of 120 ℃ under the protection of nitrogen, adding hydrochloric acid into the container to adjust the pH to be less than 2 after the reaction is finished, and separating an organic layer, and performing rotary evaporation to obtain the modified water reducer.
Example 4
15 Parts of fly ash admixture, 3 parts of Portland cement, 74 parts of sand, 0.08 part of acrylic acid, 0.001 part of sodium hypophosphite, 0.001 part of sodium formaldehyde sulfoxylate, 0.002 part of ammonium persulfate and 0.05 part of the modified water reducer obtained in the example 1;
A preparation method of modified mineral admixture concrete comprises the following steps:
15 parts of fly ash admixture, 3 parts of silicate cement, 74 parts of sand, 0.08 part of acrylic acid, 0.001 part of sodium hypophosphite, 0.001 part of formaldehyde sodium bisulfate, 0.002 part of ammonium persulfate and 0.05 part of modified water reducer obtained in the example 1 are weighed according to the parts by weight, and the modified water reducer, the sodium hypophosphite and the ammonium persulfate are dissolved in water and stirred uniformly to obtain solution A;
Secondly, dissolving acrylic acid and formaldehyde sodium bisulfate with water, and uniformly stirring to obtain a solution B;
Thirdly, stirring and mixing the solution A and the solution B at the temperature of 10 ℃ to obtain a water reducer mother solution;
grinding the fly ash admixture into particles with the particle size of 0.1-0.5mm, uniformly mixing the particles with Portland cement, sand and water, and stirring to obtain a mixture;
And fifthly, adding the water reducing agent mother liquor obtained in the third step into the mixture obtained in the fourth step, and uniformly stirring to obtain the modified mineral admixture concrete.
Example 5
15 Parts of fly ash admixture, 3 parts of silicate cement, 74 parts of sand, 0.1 part of acrylic acid, 0.002 part of sodium hypophosphite, 0.0015 part of sodium formaldehyde sulfoxylate, 0.006 part of ammonium persulfate and 0.08 part of modified water reducer obtained in example 2;
A preparation method of modified mineral admixture concrete comprises the following steps:
15 parts of fly ash admixture, 3 parts of silicate cement, 74 parts of sand, 0.1 part of acrylic acid, 0.002 part of sodium hypophosphite, 0.0015 part of formaldehyde sodium bisulfate, 0.006 part of ammonium persulfate and 0.08 part of modified water reducer obtained in the example 2 are weighed according to parts by weight, and the modified water reducer, the sodium hypophosphite and the ammonium persulfate are dissolved in water and stirred uniformly to obtain solution A;
Secondly, dissolving acrylic acid and formaldehyde sodium bisulfate with water, and uniformly stirring to obtain a solution B;
thirdly, stirring and mixing the solution A and the solution B at the temperature of 25 ℃ to obtain a water reducer mother solution;
grinding the fly ash admixture into particles with the particle size of 0.1-0.5mm, uniformly mixing the particles with Portland cement, sand and water, and stirring to obtain a mixture;
And fifthly, adding the water reducing agent mother liquor obtained in the third step into the mixture obtained in the fourth step, and uniformly stirring to obtain the modified mineral admixture concrete.
Example 6
The modified mineral admixture concrete comprises the following raw materials, by mass, 23 parts of fly ash admixture, 4 parts of Portland cement, 85 parts of sand, 0.08 part of acrylic acid, 0.001 part of sodium hypophosphite, 0.001 part of sodium formaldehyde sulfoxylate, 0.002 part of ammonium persulfate and 0.05 part of the modified water reducer obtained in the embodiment 3;
A preparation method of modified mineral admixture concrete comprises the following steps:
The first step, weighing 23 parts of fly ash admixture, 4 parts of silicate cement, 85 parts of sand, 0.08 part of acrylic acid, 0.001 part of sodium hypophosphite, 0.001 part of formaldehyde sodium bisulfate, 0.002 part of ammonium persulfate and 0.05 part of modified water reducer obtained in the example 3, dissolving the modified water reducer, the sodium hypophosphite and the ammonium persulfate in water, and uniformly stirring to obtain solution A;
Secondly, dissolving acrylic acid and formaldehyde sodium bisulfate with water, and uniformly stirring to obtain a solution B;
Thirdly, stirring and mixing the solution A and the solution B at the temperature of 40 ℃ to obtain a water reducer mother solution;
grinding the fly ash admixture into particles with the particle size of 0.1-0.5mm, uniformly mixing the particles with Portland cement, sand and water, and stirring to obtain a mixture;
And fifthly, adding the water reducing agent mother liquor obtained in the third step into the mixture obtained in the fourth step, and uniformly stirring to obtain the modified mineral admixture concrete.
Comparative example 1
The "modified water reducing agent obtained in example 3" used in example 6 was changed to the same mass part of isopentenyl polyethylene glycol ether, and the remaining conditions were unchanged.
Comparative example 2
The comparative example is fly ash lightweight aggregate concrete sold by Zhengzhou Nissan building materials Co., ltd.
The concrete slump properties and loss comparative tests were conducted with reference to national standard GB8076-2008 concrete admixture, the concrete of examples 4-6 and comparative examples 1-2 were respectively subjected to slump, compressive strength was tested, and the test results are shown in Table 1:
TABLE 1
As can be seen from Table 1, the mineral admixture concrete of the present invention is superior to the commercial fly ash lightweight aggregate concrete in both initial fluidity, slump retention and compressive strength, whereas the mineral admixture concrete of comparative example 1 is inferior in comparison with the mineral admixture of examples 4 to 6 in comparison with the mineral admixture, because the modified water reducer of the present invention is not used, and in combination, the preparation method of the mineral admixture modified concrete of the present invention is simple, the raw materials are easily available, the initial fluidity and slump retention are good, and the compressive strength is excellent, and can be widely used in the construction field.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (9)
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| CN101602834A (en) * | 2009-06-08 | 2009-12-16 | 江苏博特新材料有限公司 | A kind of preparation method of polycarboxylic acid concrete dispersers |
| CA3159587A1 (en) * | 2019-11-05 | 2021-05-14 | Carbon Upcycling Technologies Inc. | Compositions comprising a mechanochemically carboxylated mineral filler and a cement and/or asphalt binder |
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| DE102006007004A1 (en) * | 2006-02-15 | 2007-08-16 | Construction Research & Technology Gmbh | Water-soluble sulfo-containing copolymers, process for their preparation and their use |
| CN109535341A (en) * | 2018-11-16 | 2019-03-29 | 中交二航武汉港湾新材料有限公司 | Hydrophobically modified viscosity reduction type polycarboxylate water-reducer and preparation method thereof |
| CN112831048B (en) * | 2021-01-29 | 2022-06-17 | 桐庐宏基源混凝土有限公司 | Slow-release polycarboxylate superplasticizer |
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| CA3159587A1 (en) * | 2019-11-05 | 2021-05-14 | Carbon Upcycling Technologies Inc. | Compositions comprising a mechanochemically carboxylated mineral filler and a cement and/or asphalt binder |
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