CN110128077B - Low-viscosity easy-pumping ultra-high-performance concrete and preparation method thereof - Google Patents
Low-viscosity easy-pumping ultra-high-performance concrete and preparation method thereof Download PDFInfo
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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
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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
- 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
- C04B2201/52—High compression strength concretes, i.e. with a compression strength higher than about 55 N/mm2, e.g. reactive powder concrete [RPC]
Abstract
The invention discloses low-viscosity easy-pumping ultra-high performance concrete and a preparation method thereof. The concrete comprises the following components in parts by mass: 300-500 parts of cement, 100-200 parts of silica fume, 300-600 parts of admixture, 400-800 parts of sand, 300-700 parts of broken stone, 80-240 parts of fiber, 5-30 parts of thixotropic reinforcing agent, 15-30 parts of water reducing agent, 0.1-0.3 part of defoaming agent and 140-180 parts of water. The low-viscosity easy-pumping ultra-high performance concrete has high fluidity and low viscosity, the pumping resistance is only 0.015-0.025 MPa/m, and the compressive strength reaches over 180MPa after standard curing for 28 days. In addition, the low-viscosity easy-pumping ultrahigh-performance concrete has the characteristic of low typical cement content, so that the shrinkage of the ultrahigh-performance concrete is remarkably reduced, the cement consumption is remarkably reduced, and the environmental pollution is reduced.
Description
Technical Field
The invention belongs to the technical field of building materials, relates to an ultra-high performance concrete, and particularly relates to a low-viscosity easy-pumping ultra-high performance concrete and a preparation method thereof.
Background
The Ultra-high performance concrete (UHPC) has excellent performances of Ultra-high strength, high toughness, high impermeability, high corrosion resistance, high antiknock and the like, can well meet the requirements of lightweight, high stratification, large span and high durability of civil engineering structures, and has important strategic significance and wide application prospect in important or special engineering such as large-span bridges, thin-wall structures, national defense engineering, deep water ocean platforms and the like. The ultra-high performance Concrete mainly represented by Reactive Powder Concrete (RPC) mainly improves the compactness by using large-mixing-amount ultrafine Powder and extremely low water consumption, thereby realizing the ultra-high performance of the Concrete. However, the viscosity of the ultra-high performance concrete is high, a series of construction problems such as concrete stirring, transportation, pumping and the like are caused, and the popularization and application of the ultra-high performance concrete are limited to a great extent. At present, the ultra-high performance concrete is mainly used for prefabricated parts, but an application example of large-scale structural engineering is not basically available, and pumping construction is not mentioned. With the large-scale popularization and application of the ultra-high performance concrete, the development of the low-viscosity easy-pumping ultra-high performance concrete becomes a necessary trend.
Patent CN201510987930 discloses an ultra-high strength concrete with ultra-high pumping performance and a preparation method thereof, which takes cement, sand, gravel, stone powder, water, fly ash, zeolite powder, mineral powder, a water reducing agent, silicon powder and an air entraining agent as main raw materials. The patent technology mainly improves the viscosity and the pumping performance of concrete through short side chain polycarboxylic acid high-performance water reducing agent and air entraining agent on the basis of high-strength concrete, and improves the concrete strength through reducing the water-cement ratio and improving the accumulation of particles, but the concrete strength is only about 120MPa, and no fiber is used, and the concrete is not ultrahigh-performance concrete. Patent CN 2014108531899 discloses a low-shrinkage low-viscosity ultra-high-strength concrete, which improves the viscosity of the concrete by double doping large-dosage micro-beads and ultra-fine mineral powder, but the strength of the concrete is only about 120MPa and the concrete has no fiber. Patent CN2017102107384 discloses decorative ultra-high performance concrete easy to pump, which is prepared from white cement, silica fume, metakaolin, quartz sand, color, water reducing agent, magnesium aluminum silicate, cellulose ether, fiber and the like. According to the technology, the viscosity of the concrete is increased through the higher collar, and the thixotropy of the ultra-high performance concrete is improved by adopting the magnesium aluminum silicate, so that the pumping performance of the ultra-high performance concrete is improved. However, the ultra-high performance concrete in the patent technology does not contain coarse aggregate (gravel) and does not consider the problem of difficult pouring due to high concrete viscosity.
Disclosure of Invention
Aiming at the problems that the conventional ultra-high performance concrete is high in viscosity, poor in pumping performance and difficult to construct on a large scale, the invention provides the low-viscosity easy-to-pump ultra-high performance concrete and the preparation method thereof. The ultra-high performance concrete has low viscosity and high fluidity, and has shear thinning characteristic in the pumping process, and the pumping resistance is greatly reduced; and the concrete has obvious thixotropic property, the wrapping property of the concrete is higher when the concrete is in a standing state, the fibers and the aggregates can be uniformly distributed, the risk of pump blockage is reduced, and the higher homogeneity of the ultrahigh-performance concrete in the pouring process is ensured. In addition, the invention adopts the mineral filler with large mixing amount to replace cement, has the characteristic of typical low cement content, not only obviously reduces the shrinkage of the ultra-high performance concrete, but also obviously reduces the cement consumption and reduces the environmental pollution.
The invention provides low-viscosity easy-pumping ultrahigh-performance concrete which comprises the following components in parts by mass:
the cement is Portland cement or ordinary Portland cement with the strength grade of 42.5 or above, and the average grain diameter is 10-20 mu m;
SiO in the silica fume2The content is more than 90 wt%, and the average grain diameter of the silica fume is 0.2-1 μm;
the admixture is a composition of micro silicon powder, micro beads and a filler; wherein the average particle size of the micro silicon powder is 1-5 μm; the average particle size of the microbeads is 2-10 microns; the filler is any one or more than one of fly ash, ground mineral powder and quartz powder which are mixed in any proportion, and the average particle size of the filler is 10-100 mu m;
the sand is continuous graded sand with the particle size of 0.075-4.75 mm;
the crushed stone is any one of limestone, granite, diabase and basalt, and the particle size of the crushed stone is 4.75-19 mm in continuous gradation;
the fiber is a metal fiber, the length of the fiber is 3-25 mm, and the diameter of the fiber is 0.1-0.3 mm;
the thixotropic reinforcing agent is selected from one or two of inorganic thixotropic reinforcing agent and organic thixotropic reinforcing agent which are mixed in any proportion;
the water reducing agent is a viscosity-reducing high-performance water reducing agent;
the defoaming agent is any one of polyether modified organic silicon defoaming agent or polyether defoaming agent or the mixture of the two in any proportion;
the inorganic thixotropic reinforcing agent is modified nano clay, and the preparation method comprises the following steps:
pouring nano clay into a beaker, adding acid with the mass concentration of 5-30% according to the mass ratio of the nano clay to the acid of 1: 3-1: 20, heating to 40-60 ℃, keeping the temperature for 5-20 min, continuously stirring, standing, cooling for 2-4 h, performing suction filtration, and drying in a drying oven at 105 ℃ until the mass is constant;
wherein the acid is selected from any one or two of hydrochloric acid, sulfuric acid and phosphoric acid which are mixed in any proportion;
mixing the nano clay obtained after drying in the step one with water according to the mass ratio of 1: 3-1: 10, and performing ultrasonic vibration for l-2 hours to obtain nano clay slurry;
mixing the nano clay slurry obtained in the step two with a silane coupling agent according to the mass ratio of 100: 1-200: 1, stirring for 10-20 min at the rotating speed of 2000-10000 rpm by using a high-speed stirrer, and then performing ultrasonic oscillation for 0.5-1 h;
mixing the slurry obtained in the step (III) with an anionic surfactant in a mass ratio of 5: 1-20: 1, stirring in a constant-temperature water bath at 40-80 ℃ for 1-2 hours, and then performing ultrasonic oscillation for 0.5-1 hour to obtain the modified nano clay;
in the step (iv), the anionic surfactant is selected from one or more of sodium stearate, sodium dodecyl benzene sulfonate, polyacrylic acid, polyacrylamide, alkyl phosphorus carboxylate and alkyl alcohol ether carboxylate, and is mixed in any proportion;
the organic thixotropic reinforcing agent is any one or two of complex polyurethane water-soluble polymer, guar gum, xanthan gum, propylene glycol alginate, polyacrylamide, starch ether and polyvinyl alcohol which are mixed in any proportion;
the viscosity-reducing high-performance water reducer is a polymer with the following general formula (1):
wherein z represents a functional group R0The number of the connected repetitive structures X is an integer in the range of 1-4; r0Represents H or a linear or branched saturated hydrocarbon function containing 1 to 12 carbon atoms, R0For H, z must be 1; x is any one of functional groups corresponding to the following general formula (2):
wherein, X1、X1'、X1"independently of one another represents a carbonyl group or-CH2-or-CH2CH2-；X2Represents any one of the following functional groups: (1) saturated alkyl radicals having 1 to 12 carbon atoms or- (CH)2CH2O)mCH2CH2-, where m represents the number of ethoxy repeating units, which range from an integer of 1 to 11, (2) -CH (NH2) -, C is L chirality; r2、R2'、R2"independently represents H or CH3；R4' represents-CH2CH2-、 -CH2CH2SCH2CH2-、-CH2CH2SCH2CH2OCH2CH2-、-CO-CH2CH2SCH2CH2-、 -CO-CH2CH2CH2CH2OCH2CH2-any of; r5Represents H or a saturated alkyl group having 1 to 12 carbon atoms; m2 +Represents H+Alkali metal ions or ammonium ions; r9Represents a saturated alkyl group having 1 to 12 carbon atoms;
the general formula (2) is not limited by-X1"the order of the attachment of the ethoxy and isopropoxy segments in the attached side chain structure, the ethoxy and isopropoxy segments may be in a block distribution or a random distribution. Likewise, the general formula (2) does not limit the sequence of the linkage of the individual substituted ethoxy units of the polymer backbone, these substitutionsThe ethoxy units of (a) may be distributed in blocks or randomly. c. d represents the average molar addition number of ethoxy and isopropoxy chain segments in the polymer and satisfies 11 ≦ (c + d) 114, d/c<1/2；
x1、x2And y represents the average molar addition number of each chain unit in the polymer superplasticizer respectively, and satisfies the following relationship: (1) (x)1+x2The value range of the product of + y) and z is 8-150; (2) y/(x)1+x2+ y) is in the range of 0.15-0.5; (3) (x)1+x2)/(x1+x2+ y) is in the range of 0.5-0.85; (4) x is the number of2/x1The value range of (A) is 0-0.5;
the molecular weight distribution index PDI of the viscosity-reducing high-performance water reducing agent is not more than 1.4, and the weight average molecular weight range is 5000-100000.
Preferably, the low-viscosity easy-pumping ultrahigh-performance concrete disclosed by the invention comprises the following components in parts by mass:
the viscosity-reducing high-performance water reducer can be prepared by the following steps:
(1) removing water and oxygen in a reactor, preparing a polymer intermediate by bulk polymerization or solution polymerization and anion ring-opening polymerization of a monomer a under the condition of a strong base initiator, wherein the main chain of the polymer intermediate is a polyethylene glycol chain, and a large number of double bonds are grafted on the main chain;
(2) in the presence of a catalyst, connecting an adsorption functional group and a long polyether side chain with steric hindrance by Michael addition reaction of sulfydryl and a double bond to prepare the polymer, namely the viscosity-reducing high-performance water reducer; wherein the adsorption functional group is from a functional micromolecule monomer b, and the long polyether side chain is from a macromonomer E simultaneously having sulfydryl and a polyether chain structure;
in the step (1), the monomer a is a monomer containing double bonds and epoxy functional groups and meets any one of the structures shown in the following general formula (3):
wherein R is2Represents H or CH3Y represents a carbonyl group, -CH2-or-CH2CH2-；
The strong base initiator in the step (1) is sodium alkoxide or potassium alkoxide, and the alcohol refers to organic alcohol formed by straight chain or branched chain saturated hydrocarbon functional groups containing 1-12 carbon atoms and 1-4 terminal hydroxyl groups;
if solution polymerization is adopted in the step (1), the solvent in the solution is any one of tetrahydrofuran, dioxane, dimethyl sulfoxide, N-dimethylacetamide, N-methylmorpholine, N-ethylmorpholine and N-methylpyrrolidone; the mass of the solvent is 0 to 300% of the mass of the monomer a, including 0% and 300%.
The polymerization temperature in the step (1) is 50-150 ℃, the reaction time is 2-24h, and professionals in related fields can adjust the reaction temperature and the reaction time within the range according to the reaction rate;
the molar ratio of the strong base initiator to the monomer a in the step (1) is 1: 8-150.
The catalyst in step (2) is also known to those skilled in the relevant art, and specifically, reference may be made to chem.mater.2014,26, 724-744. The catalyst is preferably sodium hydroxide or potassium hydroxide or sodium alkoxide or potassium alkoxide corresponding to organic alcohol containing saturated alkyl with 1-12 carbon atoms or any one of structures corresponding to general formula (4-1) and general formula (4-2):
in the general formula (4-1), R10、R11、R12Each independently represents H or a saturated alkyl group having 1 to 6 carbon atoms, and in the general formula (4-2), R13、R14、R15Each independently represents H or a saturated alkyl group having 1 to 6 carbon atoms or a phenyl group or a cyclohexyl group or a cyclopentyl group or 1 to 3 carbon atomsSaturated alkyl substituted phenyl or saturated alkyl substituted cyclohexyl of 1-3 carbon atoms or saturated alkyl substituted cyclopentyl of 1-3 carbon atoms.
In the step (2), the functional small molecular monomer B is a monomer simultaneously having a sulfydryl group and a carboxyl group or a sulfonic group, the monomer B is a composition, the composition is a mixture of a component A and a component B, and the molar weight of the component B accounts for 0-50% of the total molar weight of the component A and the component B;
wherein the component A is one or two of (a) or (b): (a) any one or any combination of more than one of the following structures according to the following general formula (5):
R8represents a saturated alkyl group having 1 to 12 carbon atoms or- (CH)2CH2O)mCH2CH2-, where m represents the number of ethoxy repeating units and ranges from 1 to 11.
Or (b) a hydrochloride or sulfate salt of cysteine;
the component B is any one or any combination of more than one of the structures shown in the following general formula (6):
wherein M is2 +Represents H+Alkali metal ion or ammonium ion, R9Represents a saturated alkyl group having 1 to 12 carbon atoms.
In the step (2), the macromonomer E is one or more than one arbitrary mixture of the following structures represented by the general formula (7):
R5represents H or a saturated alkyl radical having 1 to 12 carbon atoms, R4Indicating that the terminal contains a thiol groupThe organic functional group of the group is the following functional group-CH2CH2SH、-CH2CH2SCH2CH2SH、 -CH2CH2SCH2CH2OCH2CH2SH、-CO-CH2CH2SCH2CH2SH or-CO-CH2CH2CH2CH2OCH2CH2Any one of SH, c and d respectively represent the average molar addition number of ethoxy and isopropoxy chain links in a polyether H structure, and the sum of (c + d) and d/c is more than or equal to 11 and less than or equal to 114<1/2. The general formula (5) does not limit the order of connection of the ethoxy and isopropoxy segments, and the ethoxy and isopropoxy segments may be distributed in blocks or randomly. The macromonomers are commercially available or can be prepared simply by literature and industrial methods, the relevant preparation methods being referred to in the examples section. Meanwhile, it is necessary to control the molecular weight distribution index PDI of the macromonomer to be not higher than 1.3, and if the molecular weight distributions of both are broad, the result is that although a superplasticizer sample can be prepared as well, the molecular weight distribution of the sample may be broad.
The temperature of the addition reaction in the step (2) is 0-100 ℃, and the reaction time is 3-24 h.
In the step (2), the molar weight of the macromonomer E accounts for 15-50% of the molar weight of the monomer a; the molar weight of the catalyst accounts for 0.2-5% of the molar weight of the monomer a; the molar amount of the functional small molecular monomer b is respectively calculated by the molar amount of the sulfydryl contained in the functional small molecular monomer b, the total molar amount of the functional small molecular monomer b accounts for 50-85% of the molar amount of the monomer a, and the total molar amount of the large monomer E and the functional small molecular monomer b is not less than the molar amount of the monomer a.
Preferably, the admixture comprises the following components in percentage by mass: microbeads: filler 80:70: 300; the filler component and the mass ratio of each component are that the fly ash: grinding slag: the ratio of quartz powder is 80:120: 100.
Preferably, the fiber of the invention is a mixture of straight fine high-strength steel fiber with the length of 13mm and the diameter of 0.2mm and end hook type high-strength steel fiber with the length of 25mm and the diameter of 0.25mm according to the mass ratio of 2: 1.
The preparation method of the low-viscosity easy-pumping ultra-high performance concrete comprises the following steps: firstly, mixing cement, silica fume, an admixture, sand and broken stones for 0.5-2 min, then adding water, a defoaming agent, a thixotropic reinforcing agent and a water reducing agent which are mixed in advance, stirring for 2-4 min, then adding fibers, and stirring for 2-4 min to obtain the low-viscosity easy-pumping ultrahigh-performance concrete.
The invention has the beneficial effects that:
(1) the cement is replaced by the mineral filler with large doping amount, and the optimal combination of powder particles with different particle sizes improves the grain composition of the cementing material, improves the stacking compactness, improves the compactness of the concrete and further realizes the improvement of the concrete strength; in addition, the cement has the characteristic of low typical cement content, the cement consumption is obviously reduced, and the environmental pollution is reduced.
(2) Through 1-5 mu m of silica fume and 2-10 mu m of micro-beads, the interaction force between particles is reduced based on the morphology action and the surface charge action of powder particles, the thickness of a water film layer on the surfaces of the particles is increased, the adsorption efficiency of an additive is improved, the viscosity of the ultra-high performance concrete is effectively reduced, and further the pumping resistance is reduced.
(3) The viscosity reduction type high-performance water reducing agent with hydrophilic main chain and narrow molecular weight distribution is adopted, so that uniform and rapid dispersion of large-volume ultrafine powder in ultra-high-performance concrete with extremely low water-gel ratio is realized, the agglomeration problem of the ultrafine powder in slurry caused by ultra-strong interparticle acting force is reduced, the wet accumulation compactness of particles in slurry is increased, more free water is released, the fluidity of the ultra-high-performance concrete is improved, the viscosity is reduced, and the pumping resistance is reduced.
(4) By using organic thixotropic reinforcing agents such as modified nano clay or complex polyurethane water-soluble polymer, guar gum, xanthan gum, propylene glycol alginate, polyacrylamide, starch ether, polyvinyl alcohol and the like, the shear thinning characteristic is realized under the shearing action of concrete, the viscosity is obviously reduced, the fluidity is obviously improved, and the friction resistance in a lubricating layer is greatly reduced in the pumping process, namely the pumping resistance is obviously reduced; after the shear is removed, the viscosity of the concrete is recovered, the workability of the concrete is better, the problem of settlement of aggregates and fibers caused by overlarge fluidity is solved, the risk of pump blockage caused by uneven distribution of the aggregates and the fibers is reduced, the uniformity of hardened UHPC is improved, and the strength of the ultrahigh-performance concrete is further improved.
(5) The problem of gas content increase caused by large-volume fiber and water reducing agent is solved by introducing the defoaming agent, and simultaneously, the gas content of the ultra-high-performance concrete caused by gas introduction in the pumping process is also prevented from being greatly increased, so that the ultra-high compactness of the concrete is ensured, and the ultra-high performance of the concrete is realized.
By the technical measures, the pumping resistance of the prepared low-viscosity easy-pumping ultra-high performance concrete is 0.015-0.025 MPa/m, and the compressive strength of the concrete after standard curing for 28 days is more than 180 MPa.
Detailed Description
To more fully explain the practice of the present invention, the following examples of low viscosity easy to pump ultra high performance concrete preparations are provided. These examples are merely illustrative and do not limit the scope of the invention.
All the following units are parts by mass, and all the used compounds are commercial products or synthetic products according to literature reports;
the sources of strong base initiator, monomer a, solvent, catalyst, polyether macromonomer, functional monomer b (except b3) are all commercially available (carbofuran reagent, TCI reagent, Sigma-Aldrich, and Huntsman);
b3 is a synthetic product according to the literature report (J.Phys.chem.C 2009,113, 12950-12953).
Table 1 compound names used in the examples
Some of the compounds listed in Table 1 have the following structures:
the cement in the examples is Portland cement P.II 52.5;
the "silica fume" in the examples is an Angen 95 grade silica fume, SiO295 percent of the total weight and 0.2 mu m of average grain diameter;
in the example, "silica fume" in the "admixture" has an average particle size of 1.8 μm, "microbeads" have an average particle size of 6 μm, "fillers" have an average particle size of 50 μm;
the sand in the embodiment is continuous river sand with the particle size of 0.075-4.75 mm;
in the embodiment, the crushed stone is basalt crushed stone with 4.75-19 mm of grain size in continuous gradation;
in the embodiment, the fiber is straight steel fiber with the length of 13mm and the diameter of 0.2mm, and end hook type fiber with the length of 25mm and the diameter of 0.25mm, which are mixed according to a certain proportion;
in the embodiment, the inorganic thixotropic reinforcing agent is modified nano clay, and the preparation method comprises the following steps:
(1) pouring the nano clay into a beaker, adding hydrochloric acid with the concentration of 8% according to the solid-to-liquid ratio of 1:10, heating to 60 ℃, keeping the temperature for 10min while continuously stirring, standing, cooling for 2h, and then performing suction filtration; drying in a drying oven at 105 deg.C to constant mass; (2) mixing the nano clay obtained in the step (1) with water according to a ratio of 1:5, and oscillating lh by ultrasonic; (3) mixing the slurry obtained in the step (2) with a silane coupling agent in a ratio of 100:1, and stirring for 10min at a rotating speed of 8000rpm by using a high-speed stirrer; then ultrasonic oscillation is adopted for 1 h; (4) mixing the slurry obtained in the step (3) with sodium dodecyl benzene sulfonate in a ratio of 8:1, stirring for 2 hours in a constant-temperature water bath at 60 ℃, and then carrying out ultrasonic oscillation for 0.5 hour;
the viscosity-reducing high-performance water reducing agent in the embodiment is PCE1, PCE2, PCE3 or PCE 4;
the molecular weight distribution index of PCE1 is 1.38, the weight-average molecular weight is 31.1kDa, and the preparation process is as follows:
(1) removing water and oxygen from a reactor, adding 142.15 parts of solvent 1 into the reactor under the protection of an inert (nitrogen) atmosphere, adding 1.922 parts of strong base initiator 1 into the reactor, adjusting the temperature of the reactor to 100 ℃, gradually and uniformly adding 142.15 parts of monomer a1 into the reactor within 8 hours, and stirring the mixture to react for 12 hours to obtain an intermediate polymer;
(2) adding 500 parts of polyether macromonomer 1 into another reactor, adjusting the temperature of the reactor to 50 ℃, adding 0.27 part of catalyst 1, 57.37 parts of functional monomer b1, 11.72 parts of functional monomer b2 and the intermediate polymer obtained in the step (1), stirring for reacting for 6 hours, removing volatilizable micromolecules in vacuum, and recovering the reactor to normal pressure and room temperature to obtain a viscosity-reducing PCE type high-performance water reducer sample 1;
PCE2 has a molecular weight distribution index of 1.26, a weight average molecular weight of 6.4kDa, and is prepared as follows:
(1) removing water and oxygen from a reactor, adding 128.13 parts of solvent 2 into the reactor under the protection of an inert (nitrogen) atmosphere, then adding 9.415 parts of strong base initiator 2 into the reactor, adjusting the temperature of the reactor to 120 ℃, gradually and uniformly adding 128.13 parts of monomer a2 into the reactor within 1 hour, and stirring the mixture to react for 2 hours to obtain an intermediate polymer;
(2) adding 583.6 parts of polyether macromonomer 2 into another reactor, adjusting the temperature of the reactor to 20 ℃, adding 2.623 parts of catalyst 2, 161 parts of functional monomer b3, 26.73 parts of functional monomer b4 and the intermediate polymer obtained in the step (1), stirring for reacting for 6 hours, removing volatilizable micromolecules in vacuum, and recovering the reactor to normal pressure and room temperature to obtain a viscosity-reducing high-performance water reducer sample PCE 2;
the molecular weight distribution index of PCE3 is 1.29, the weight average molecular weight is 21.0kDa, and the preparation process is as follows:
(1) removing water and oxygen from a reactor, adding 426.45 parts of solvent 3 into the reactor under the protection of an inert (nitrogen) atmosphere, adding 4.991 parts of strong base initiator 3 into the reactor, adjusting the temperature of the reactor to 150 ℃, gradually and uniformly adding 142.15 parts of monomer a1 into the reactor within 3 hours, and stirring the mixture to react for 8 hours to obtain an intermediate polymer;
(2) adding 284.6 parts of polyether macromonomer 3 into another reactor, adjusting the temperature of the reactor to 0 ℃, adding 0.32 part of catalyst 3, 21.33 parts of functional monomer b2, 131.02 parts of functional monomer b5 and the intermediate polymer obtained in the step (1), stirring for reaction for 12 hours, removing volatilizable micromolecules in vacuum, and recovering the reactor to normal pressure and room temperature to obtain a viscosity-reducing high-performance water reducer sample PCE 3;
PCE4 has a molecular weight distribution index of 1.21, a weight average molecular weight of 59.0kDa, and is prepared as follows:
(1) removing water and oxygen from a reactor, adding 1.348 parts of strong base initiator 3 into the reactor under the protection of inert (nitrogen) atmosphere, adjusting the temperature of the reactor to 125 ℃, gradually and uniformly adding 128.13 parts of monomer a2 into the reactor within 3 hours, and stirring for reacting for 4 hours to obtain an intermediate polymer;
(2) adding 772.2 parts of polyether macromonomer 4 into another reactor, adjusting the temperature of the reactor to 50 ℃, adding 2.002 parts of catalyst 4, 7.11 parts of functional monomer b2, 214.66 parts of functional monomer b3 and the intermediate polymer obtained in the step (1), stirring for reacting for 4 hours, removing volatilizable micromolecules in vacuum, and recovering the reactor to normal pressure and room temperature to obtain a viscosity-reducing type high-performance water reducer sample PCE 4;
in the examples "antifoam" is a polyether modified silicone antifoam.
Table 1 contents of components of low viscosity easy pumping ultra high performance concrete in each example
In the embodiment 1, the admixture component is micro silicon powder, micro beads and filler which are mixed according to the mass ratio of 80:70: 300; the filler component and the mass ratio of each component are that the fly ash: grinding mineral powder: quartz powder 80:120: 100; the thixotropic reinforcing agent is an inorganic thixotropic reinforcing agent and an organic thixotropic reinforcing agent which are mixed according to the mass ratio of 10:5, and the organic thixotropic reinforcing agent is propylene glycol alginate; the water reducing agent is PCE 1; the fiber is a mixture of straight steel fiber and end hook type fiber according to the mass ratio of 2: 1.
In the embodiment 2, the admixture component is the mixture of micro silicon powder, micro beads and filler according to the mass ratio of 80:70: 300; the filler component and the mass ratio of each component are that the fly ash: grinding mineral powder: quartz powder 80:120: 100; the thixotropic reinforcing agent is an inorganic thixotropic reinforcing agent and an organic thixotropic reinforcing agent which are mixed according to the mass ratio of 10:5, and the organic thixotropic reinforcing agent is starch ether; the water reducing agent is PCE 2; the fiber is a mixture of straight steel fiber and end hook type fiber according to the mass ratio of 2: 1.
In the embodiment 3, the admixture component is micro silicon powder, micro beads and filler which are mixed according to the mass ratio of 100:100: 250; the filler component and the mass ratio of each component are that the fly ash: grinding mineral powder: quartz powder 70:80: 100; the thixotropic reinforcing agent is an inorganic thixotropic reinforcing agent; the water reducing agent is PCE 3; the fiber is end hook type steel fiber.
In the embodiment 4, the admixture component is micro silicon powder, micro beads and filler which are mixed according to the mass ratio of 120:80: 250; the filler component and the mass ratio of each component are that the fly ash: grinding mineral powder: quartz powder 100:80: 70; the thixotropic reinforcing agent is an inorganic thixotropic reinforcing agent and an organic thixotropic reinforcing agent which are mixed according to the mass ratio of 10:5, and the organic thixotropic reinforcing agent is polyvinyl alcohol; the water reducing agent is PCE 4; the fiber is a mixture of straight steel fiber and end hook type fiber according to the mass ratio of 1: 1.
In the embodiment 5, the admixture component is micro silicon powder, micro beads and filler which are mixed according to the mass ratio of 120:80: 200; the filler component and the mass ratio of each component are that the fly ash: grinding mineral powder: quartz powder 80:70: 50; the thixotropic reinforcing agent is an inorganic thixotropic reinforcing agent; the water reducing agent is PCE 1; the fiber is a mixture of straight steel fiber and end hook type steel fiber according to the mass ratio of 3: 1.
In the embodiment 6, the admixture component is micro silicon powder, micro beads and filler which are mixed according to the mass ratio of 40:60: 200; the filler component and the mass ratio of each component are that the fly ash: grinding mineral powder: quartz powder 50:50: 100; the thixotropic reinforcing agent is an inorganic thixotropic reinforcing agent and an organic thixotropic reinforcing agent which are mixed according to the mass ratio of 5:10, and the organic thixotropic reinforcing agent is guar gum; the water reducing agent is PCE 4; the fiber is a mixture of straight steel fiber and end hook type steel fiber according to the mass ratio of 1: 1.
In the embodiment 7, the admixture component is micro silicon powder, micro beads and filler which are mixed according to the mass ratio of 50:100: 200; the filler component and the mass ratio of each component are that the fly ash: grinding mineral powder: quartz powder 80:70: 50; the thixotropic reinforcing agent is a complex polyurethane water-soluble polymer; the water reducing agent is PCE 2; the fiber is end hook type steel fiber.
In the embodiment 8, the admixture component is micro silicon powder, micro beads and filler which are mixed according to the mass ratio of 70:80: 350; the filler component and the mass ratio of each component are that the fly ash: grinding mineral powder: the ratio of quartz powder to quartz powder is 100:150: 100; the thixotropic reinforcing agent is an inorganic thixotropic reinforcing agent; the water reducing agent is PCE 3; the fiber is a mixture of straight steel fiber and end hook type steel fiber according to the mass ratio of 1: 2.
In the embodiment 9, the admixture component is micro silicon powder, micro beads and filler which are mixed according to the mass ratio of 120:130: 350; the filler component and the mass ratio of each component are that the fly ash: grinding mineral powder: the ratio of quartz powder to quartz powder is 100:100: 150; the thixotropic reinforcing agent is inorganic thixotropic reinforcing agent and organic thixotropic reinforcing agent which are mixed according to the mass ratio of 10:5, and the organic thixotropic reinforcing agent is xanthan gum; the water reducing agent is PCE 1; the fiber is a mixture of straight steel fiber and end hook type steel fiber according to the mass ratio of 2: 1.
Comparative example
TABLE 2 contents of the constituents of the low viscosity pumpable ultra-high performance concrete in each proportion
Comparative example 1: the water reducing agent is a common high-performance water reducing agent, and other components are the same as those in the example 1.
Comparative example 2: the admixture lacks microsilica ash and microbeads, and other components are the same as in example 1.
Comparative example 3: the thixotropic enhancer was absent and the other components were the same as in example 1.
Comparative example 4: the blending ratio of the conventional ultrahigh-performance concrete is that the admixture is ground quartz powder, the water reducing agent is a common high-performance water reducing agent, and other component materials are the same as those in the example 1.
The low-viscosity easy-pumping ultra-high performance concrete in the above examples 1 to 9 and the ultra-high performance concrete in the comparative examples 1 to 4 were prepared by mixing cement, silica fume, admixture, quartz powder, river sand and crushed stone for 1min, adding water, defoamer, thixotropic enhancer and water reducer which had been mixed in advance, stirring for 3min, adding fiber, and stirring for 3 min.
Application examples
Comparative tests of slump expansion, viscosity, pumping resistance and compressive strength were carried out using the ultra-high performance concretes of examples 1 to 9 and comparative examples 1 to 4.
The expansion degree of the ultra-high performance concrete is tested according to a method specified in GB50080-2016 standard of common concrete mixture performance test methods; viscosity through T50The time is reflected, the test is carried out according to a method specified in CECS203-2006 technical Specification for application of self-compacting concrete, and the longer the time is, the larger the viscosity of the concrete is; the pumping resistance is obtained through a tribometer test result and is characterized by pumping pressure loss per unit distance; the compressive strength was tested according to GBT 31387-.
The test results are as follows:
properties of the Low viscosity Pumping ultra high Performance concretes in the examples of Table 3
TABLE 4 Performance of the ultra high Performance concrete of the comparative examples
The test results show that the ultra-high performance concrete prepared by the admixture, the thixotropic reinforcing agent and the viscosity-reducing high-performance water reducing agent through adjusting the fiber dosage, the sand, the stone and the water consumption and the defoaming agent has higher fluidity, lower viscosity, lower pumping resistance and higher compressive strength, and the compressive strength of the concrete can reach over 180MPa after standard curing for 28 days. In addition, the invention adopts the mineral filler with large mixing amount to replace cement, has the characteristic of typical low cement content, obviously reduces the cement consumption and reduces the environmental pollution.
In comparative example 1, a common high-performance water reducing agent was used, and the other components were the same as in example 1, and the performance data shows that: by adopting the common high-performance water reducing agent, the fluidity, the viscosity, the pumping resistance and the compressive strength of the concrete are obviously inferior to those of the concrete in the example 1. The viscosity reduction type high-performance water reducing agent with hydrophilic main chain and narrow molecular weight distribution realizes uniform and rapid dispersion of ultrafine powder, thereby improving the fluidity of the ultra-high performance concrete, reducing the viscosity and reducing the pumping resistance.
In comparative example 2, lacking microsilica, microbeads and other components as in example 1, the performance data shows: after the micro silica fume and the micro beads, the viscosity and the pumping resistance of the concrete are obviously inferior to those of the concrete in the example 1. The shape effect and the surface charge effect of the micro silicon powder and the micro bead powder particles reduce the interaction force among the particles, increase the thickness of a water film layer on the surfaces of the particles, improve the adsorption efficiency of the additive, effectively reduce the viscosity of the ultra-high performance concrete and further reduce the pumping resistance.
In comparative example 3, lacking the thixotropic enhancer, and the other components are the same as in example 1, the performance data shows: in the absence of the thixotropic enhancing agent, the concrete viscosity and pumping resistance were significantly higher than those of example 1. The thixotropic reinforcing agent is doped, so that the shear thinning characteristic of the concrete under the shearing action can be realized, the viscosity is obviously reduced, and the friction resistance in a lubricating layer in the pumping process is greatly reduced, namely the pumping resistance is obviously reduced.
Comparative example 4 is the conventional ultra-high performance concrete mix proportion, the admixture is ground quartz powder, the water reducing agent is a common high performance water reducing agent, other component materials are the same as example 1, and the performance data shows that: the low-viscosity easy-pumping ultrahigh-performance concrete has the advantages that the fluidity is obviously superior to that of the common ultrahigh performance, and the viscosity and the pumping resistance are both greatly reduced. In addition, the compressive strength of the low-viscosity easy-pumping concrete is superior to that of the conventional ultrahigh-performance concrete.
Claims (8)
1. The low-viscosity easy-pumping ultrahigh-performance concrete is characterized by comprising the following components in parts by mass:
the cement is Portland cement or ordinary Portland cement with the strength grade of 42.5 or above, and the average grain diameter is 10-20 mu m;
SiO in the silica fume2The content is more than 90 wt%, and the average grain diameter of the silica fume is 0.2-1 μm;
the admixture is a composition of micro silicon powder, micro beads and a filler; wherein the average particle size of the micro silicon powder is 1-5 μm; the average particle size of the microbeads is 2-10 microns; the filler is any one or more than one of fly ash, ground mineral powder and quartz powder which are mixed in any proportion, and the average particle size of the filler is 10-100 mu m;
the sand is continuous graded sand with the particle size of 0.075-4.75 mm;
the crushed stone is any one of limestone, granite, diabase and basalt, and the particle size of the crushed stone is 4.75-19 mm in continuous gradation;
the fiber is a metal fiber, the length of the fiber is 3-25 mm, and the diameter of the fiber is 0.1-0.3 mm;
the thixotropic reinforcing agent is selected from one or two of inorganic thixotropic reinforcing agent and organic thixotropic reinforcing agent which are mixed in any proportion;
the water reducing agent is a viscosity-reducing high-performance water reducing agent;
the defoaming agent is any one of polyether modified organic silicon defoaming agent or polyether defoaming agent or the mixture of the two in any proportion;
the inorganic thixotropic reinforcing agent is modified nano clay, and the preparation method comprises the following steps:
pouring nano clay into a beaker, adding acid with the mass concentration of 5-30% according to the mass ratio of the nano clay to the acid of 1: 3-1: 20, heating to 40-60 ℃, keeping the temperature for 5-20 min, continuously stirring, standing, cooling for 2-4 h, performing suction filtration, and drying in a drying oven at 105 ℃ until the mass is constant;
wherein the acid is selected from any one or two of hydrochloric acid, sulfuric acid and phosphoric acid which are mixed in any proportion;
mixing the nano clay obtained after drying in the step one with water according to the mass ratio of 1: 3-1: 10, and performing ultrasonic vibration for l-2 hours to obtain nano clay slurry;
mixing the nano clay slurry obtained in the step two with a silane coupling agent according to the mass ratio of 100: 1-200: 1, stirring for 10-20 min at the rotating speed of 2000-10000 rpm by using a high-speed stirrer, and then performing ultrasonic oscillation for 0.5-1 h;
mixing the slurry obtained in the step (III) with an anionic surfactant in a mass ratio of 5: 1-20: 1, stirring in a constant-temperature water bath at 40-80 ℃ for 1-2 hours, and then performing ultrasonic oscillation for 0.5-1 hour to obtain the modified nano clay; wherein the anionic surfactant is selected from one or more of sodium stearate, sodium dodecyl benzene sulfonate, polyacrylic acid, polyacrylamide, alkyl phosphorus carboxylate and alkyl alcohol ether carboxylate;
the organic thixotropic reinforcing agent is any one or two of complex polyurethane water-soluble polymer, guar gum, xanthan gum, propylene glycol alginate, polyacrylamide, starch ether and polyvinyl alcohol which are mixed in any proportion;
the viscosity-reducing high-performance water reducer is a polymer with the following general formula (1):
wherein z represents a functional group R0The number of the connected repetitive structures X is an integer in the range of 1-4; r0Represents H or a linear or branched saturated hydrocarbon function containing 1 to 12 carbon atoms, R0For H, z must be 1; x is any one of functional groups corresponding to the following general formula (2):
wherein, X1、X1'、X1"independently of one another represents a carbonyl group or-CH2-or-CH2CH2-；X2Represents the following functional groupsAny one of: (1) saturated alkyl radicals having 1 to 12 carbon atoms or- (CH)2CH2O)mCH2CH2-, where m represents the number of ethoxy repeating units, which range from an integer of 1 to 11, (2) -CH (NH2) -, C is L chirality; r2、R2'、R2"independently represents H or CH3；R4' represents-CH2CH2-、-CH2CH2SCH2CH2-、-CH2CH2SCH2CH2OCH2CH2-、-CO-CH2CH2SCH2CH2-、-CO-CH2CH2CH2CH2OCH2CH2-any of; r5Represents H or a saturated alkyl group having 1 to 12 carbon atoms; m2 +Represents H+Alkali metal ions or ammonium ions; r9Represents a saturated alkyl group having 1 to 12 carbon atoms; c. d represents the average molar addition number of ethoxy and isopropoxy chain segments in the polymer and satisfies 11 ≦ (c + d) 114, d/c<1/2；x1、x2And y represents the average molar addition number of each chain unit in the polymer superplasticizer respectively, and satisfies the following relationship: (1) (x)1+x2The value range of the product of + y) and z is 8-150; (2) y/(x)1+x2+ y) is in the range of 0.15-0.5; (3) (x)1+x2)/(x1+x2+ y) is in the range of 0.5-0.85; (4) x is the number of2/x1The value range of (A) is 0-0.5;
the molecular weight distribution index PDI of the viscosity-reducing high-performance water reducing agent is not more than 1.4, and the weight average molecular weight range is 5000-100000.
2. The low-viscosity easy-pumping ultrahigh-performance concrete as claimed in claim 1, which is prepared from the following components in parts by mass:
3. the low-viscosity easy-pumping ultrahigh-performance concrete as claimed in claim 1 or 2, wherein the viscosity-reducing high-performance water reducer is prepared by the following steps:
(1) removing water and oxygen in a reactor, preparing a polymer intermediate by bulk polymerization or solution polymerization and anion ring-opening polymerization of a monomer a under the condition of a strong base initiator, wherein the main chain of the polymer intermediate is a polyethylene glycol chain, and a large number of double bonds are grafted on the main chain;
the molar ratio of the strong base initiator to the monomer a is 1: 8-150;
the monomer a is a monomer containing double bonds and epoxy functional groups and meets any one of the structures shown in the following general formula (3):
wherein R is2Represents H or CH3Y represents a carbonyl group, -CH2-or-CH2CH2-；
The strong base initiator is sodium alkoxide or potassium alkoxide, and the 'alcohol' refers to 'an organic alcohol consisting of a straight-chain or branched-chain saturated hydrocarbon functional group containing 1-12 carbon atoms and 1-4 terminal hydroxyl groups';
the polymerization temperature is 50-150 ℃, and the reaction time is 2-24 h;
(2) in the presence of a catalyst, connecting an adsorption functional group and a long polyether side chain with steric hindrance by Michael addition reaction of sulfydryl and a double bond to prepare the polymer, namely the viscosity-reducing high-performance water reducer; wherein the adsorption functional group is from a functional micromolecule monomer b, and the long polyether side chain is from a macromonomer E simultaneously having sulfydryl and a polyether chain structure;
in the step (2), the functional small molecular monomer B is a monomer simultaneously having a sulfydryl group and a carboxyl group or a sulfonic group, the monomer B is a composition, the composition is a mixture of a component A and a component B, and the molar weight of the component B accounts for 0-50% of the total molar weight of the component A and the component B;
wherein the component A is one or two of (a) or (b): (a) any one or any combination of more than one of the following structures according to the following general formula (5):
R8represents a saturated alkyl group having 1 to 12 carbon atoms or- (CH)2CH2O)mCH2CH2-wherein m represents the number of ethoxy repeating units and ranges from an integer of 1 to 11;
or (b) a hydrochloride or sulfate salt of cysteine;
the component B is any one or any combination of more than one of the structures shown in the following general formula (6):
wherein M is2 +Represents H+Alkali metal ion or ammonium ion, R9Represents a saturated alkyl group having 1 to 12 carbon atoms;
in the step (2), the macromonomer E is one or more than one arbitrary mixture of the following structures represented by the general formula (7):
R5represents H or a saturated alkyl radical having 1 to 12 carbon atoms, R4Represents an organic functional group having a mercapto group at the terminal, and is the following functional group-CH2CH2SH、-CH2CH2SCH2CH2SH、-CH2CH2SCH2CH2OCH2CH2SH、-CO-CH2CH2SCH2CH2SH or-CO-CH2CH2CH2CH2OCH2CH2Any one of SH, c and d respectively represent the average molar addition number of ethoxy and isopropoxy chain links in a polyether H structure, and the sum of (c + d) and d/c is more than or equal to 11 and less than or equal to 114<1/2, respectively; and the molecular weight distribution index PDI of the macromonomer E is not higher than 1.3;
the temperature of the addition reaction in the step (2) is 20-100 ℃, and the reaction time is 3-24 h;
in the step (2), the molar weight of the macromonomer E accounts for 15-50% of the molar weight of the monomer a; the molar weight of the catalyst accounts for 0.2-5% of the molar weight of the monomer a; the molar amount of the functional small molecular monomer b is respectively calculated by the molar amount of the sulfydryl contained in the functional small molecular monomer b, the total molar amount of the functional small molecular monomer b accounts for 50-85% of the molar amount of the monomer a, and the total molar amount of the large monomer E and the functional small molecular monomer b is not less than the molar amount of the monomer a.
4. The concrete with low viscosity, easy pumping and ultra-high performance as claimed in claim 3, wherein if solution polymerization is adopted in the step (1) of preparing the viscosity-reducing type high-performance water reducing agent, the solvent in the solution is any one of tetrahydrofuran, dioxane, dimethyl sulfoxide, N-dimethylacetamide, N-methylmorpholine, N-ethylmorpholine and N-methylpyrrolidone; the mass of the solvent is 0 to 300% of the mass of the monomer a, including 0% and 300%.
5. The concrete with low viscosity, easy pumping and ultra-high performance as claimed in claim 3, wherein the catalyst in the step (2) of preparing the viscosity-reducing type high-performance water reducer is sodium hydroxide or potassium hydroxide or sodium alkoxide or potassium alkoxide corresponding to organic alcohol containing saturated alkyl with 1-12 carbon atoms or any one of structures shown in general formula (4-1) and general formula (4-2):
in the general formula (4-1), R10、R11、R12Each independently represents H or a saturated alkyl group having 1 to 6 carbon atoms, and in the general formula (4-2), R13、R14、R15Each independently represents H or a saturated alkyl group having 1 to 6 carbon atoms or a phenyl group or a cyclohexyl group or a cyclopentyl group or a phenyl group substituted by a saturated alkyl group having 1 to 3 carbon atoms or a cyclohexyl group substituted by a saturated alkyl group having 1 to 3 carbon atoms or a cyclopentyl group substituted by a saturated alkyl group having 1 to 3 carbon atoms.
6. The concrete of claim 1 or 2, wherein the admixture comprises the following components in percentage by mass: microbeads: filler 80:70: 300; the filler component and the mass ratio of each component are that the fly ash: grinding mineral powder: the ratio of quartz powder is 80:120: 100.
7. The low viscosity easy pumping ultra high performance concrete according to claim 1 or 2, wherein the fiber is a mixture of straight fine high strength steel fiber with a length of 13mm and a diameter of 0.2mm and end hook type high strength steel fiber with a length of 25mm and a diameter of 0.25mm in a mass ratio of 2: 1.
8. The method for preparing a low-viscosity easy-pumping ultra-high performance concrete as claimed in any one of claims 1 to 7, comprising the steps of: firstly, mixing cement, silica fume, an admixture, sand and broken stones for 0.5-2 min, then adding water, a defoaming agent, a thixotropic reinforcing agent and a water reducing agent which are mixed in advance, stirring for 2-4 min, then adding fibers, and stirring for 2-4 min to obtain the low-viscosity easy-pumping ultrahigh-performance concrete.
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