CN108774025A - A kind of silica-filled modified concrete material and preparation method thereof - Google Patents
A kind of silica-filled modified concrete material and preparation method thereof Download PDFInfo
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- CN108774025A CN108774025A CN201810633514.9A CN201810633514A CN108774025A CN 108774025 A CN108774025 A CN 108774025A CN 201810633514 A CN201810633514 A CN 201810633514A CN 108774025 A CN108774025 A CN 108774025A
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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
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
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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
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- Curing Cements, Concrete, And Artificial Stone (AREA)
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Abstract
The present invention relates to a kind of silica-filled modified concrete materials and preparation method thereof.The silica-filled modified concrete material is by cement, modified polyacrylamide, modified coal ash, sand and water composition, the modified polyacrylamide is by acrylamide, styrene, methyl methacrylate, SE-10 emulsifiers, water, Isooctyl acrylate monomer, hydroxy-ethyl acrylate, 2- acrylamide-2-methyl propane sulfonics sodium and the reaction of 184 photoinitiators are made, the modified coal ash is by flyash, porous alumina/porous silica, phenolic resin and ethanol synthesis are made, porous alumina/the porous silica is by alumina silicate, sodium ethoxide, ionic liquid, ethyl alcohol and tetraethyl orthosilicate reaction are made, the ionic liquid is by 1- butyl -3- methylimidazole villaumites, dodecyl benzene sulfonic acid, ethyl alcohol and ammonium hydroxide reaction are made.Silica-filled modified concrete material provided by the invention has excellent compression strength.
Description
Technical field
The present invention relates to concrete fields, and in particular to a kind of silica-filled modified concrete material and its preparation side
Method.
Background technology
With the quickening of modernization, the application field of concrete constantly expands, thus, different field is to agent on crack resistance of concrete
The requirement of Compressive Strength is constantly promoted.Since the compression strength of normal concrete can not be applied in some specific areas, coagulation
Soil is promoted in terms of compression strength.The invention using cement, modified polyacrylamide, modified coal ash, sand and
Water is prepared for silica-filled modified concrete material, and silica-filled modified concrete material prepared by this method has
Excellent compression strength.
Invention content
The purpose of the present invention is to provide a kind of silica-filled modified concrete material, the silica-filled modifications
Concrete material is prepared using cement, modified polyacrylamide, modified coal ash, sand and water, has excellent resistance to compression
Intensity.
Another object of the present invention is to provide the preparation methods of above-mentioned silica-filled modified concrete material.
To achieve the goals above, technical scheme is as follows：
A kind of silica-filled modified concrete material is 40 by quality parts ratio:0.6~5:23~35:3~12:18~
45 cement, modified polyacrylamide, modified coal ash, sand and water composition；Wherein, the modified polyacrylamide is by matter
It is 32 to measure portion rate:0.2~1:0.2~1:3~7:45~62:0.5~1:0.2~1:1~4:0.3~1 acrylamide, benzene
Ethylene, methyl methacrylate, SE-10 emulsifiers, water, Isooctyl acrylate monomer, hydroxy-ethyl acrylate, 2- acrylamide -2- first
Base propanesulfonate and the reaction of 184 photoinitiators are made；The modified coal ash is 36 by quality parts ratio:26~39:3~9:
41~55 flyash, porous alumina/porous silica, phenolic resin and ethanol synthesis is made；Described is porous
Alundum (Al2O3)/porous silica is by quality parts ratio 33:53~67:19~31:66~82:25~33 alumina silicate, second
Sodium alkoxide, ionic liquid, ethyl alcohol and tetraethyl orthosilicate reaction are made；The ionic liquid is 19 by quality parts ratio:32~41:
86~100:29~52 1- butyl -3- methylimidazole villaumites, dodecyl benzene sulfonic acid, ethyl alcohol and ammonium hydroxide reaction is made.
Preferably, the quality parts ratio of the cement, modified polyacrylamide, modified coal ash, sand and water is 40:
0.9:26:8:23。
The preparation method of above-mentioned silica-filled modified concrete material, includes the following steps：
(1), 1- butyl -3- methylimidazole villaumites, ethyl alcohol and ammonium hydroxide are added in reaction kettle, mixing speed is 90~103r/
Min reacts 12min under the conditions of 30 DEG C of maintenance system temperature, dodecyl benzene sulfonic acid is added to according to 0.08 mass parts/min
When reaction kettle, temperature of reaction kettle is risen to 133~146 DEG C, the reaction was continued under maintenance -0.06MPa reduced pressures 1~3h is obtained
Ionic liquid；The purpose of the ammonium hydroxide is in order to accelerate reaction system intermediate ion exchange rate；
(2), alumina silicate, sodium ethoxide, ionic liquid, ethyl alcohol and tetraethyl orthosilicate are added in hydrothermal reaction kettle, maintain hydro-thermal
Under the conditions of 173~198 DEG C of reaction temperature react 2~5h, product through 100 DEG C heat treatment 0.5h, 200 DEG C heat treatment 1h, 400 DEG C
It is heat-treated 1h, 600 DEG C of heat treatment 1h, 800 DEG C of heat treatment 1h, 1200 DEG C of heat treatment 2h, grinding, product is through 35 DEG C, 20% hydroxide
Sodium water solution ultrasonic immersing handles 10min, and product washs 2 times through 500mL water supersound washing 3 times, 500mL EtOH Sonicates, in 53
DEG C, -0.06MPa be dried in vacuo 16min, obtain porous alumina/porous silica；The sodium ethoxide and ionic liquid
The purpose of body is for dissolved material and improves material pore-creating rate；
(3), flyash, porous alumina/porous silica, phenolic resin and ethyl alcohol are added in ball mill, cylinder
Body rotating speed is 19~27r/min, reacts 30min under the conditions of 35 DEG C of maintenance system temperature, and product is through 200 DEG C of heat treatment 1h, 300
DEG C heat treatment 1h, 400 DEG C of heat treatment 1h, 500 DEG C of heat treatment 1h, 600 DEG C of heat treatment 2h are to get to modified coal ash；Described
The purpose of phenolic resin is in order to improve the mixing uniformity and compression strength of material；
(4), acrylamide, SE-10 emulsifiers, water, 2- acrylamide-2-methyl propane sulfonics sodium and 184 photoinitiators are added
Into reaction kettle, mixing speed is 88~100r/min, reacts 23min under the conditions of 32 DEG C of maintenance system temperature, by styrene,
Methyl methacrylate, Isooctyl acrylate monomer, hydroxy-ethyl acrylate mixture be added to reaction according to 0.03 mass parts/min
In kettle, the 35min that maintains under above-mentioned reaction condition that the reaction was continued, product is through 2000W 4~9s of lamp and high pressure mercury, and product is through 75
DEG C, -0.09MPa be dried in vacuo 35min, crush to get to modified polyacrylamide；The styrene, methyl methacrylate
The purpose of ester, Isooctyl acrylate monomer and hydroxy-ethyl acrylate is used to reduce the water of silica-filled modified concrete material
Amount；
(5), cement, modified polyacrylamide, modified coal ash, sand and water are added in high-speed mixer, it is mixed with high speed
Conjunction machine is in 25 DEG C of 5~15min of hybrid reaction of temperature to get to silica-filled modified concrete material.
The beneficial effects of the present invention are：
1, ammonium hydroxide exists in the form of ammonium ion in the reaction system, and thermally treated, ammonium ion and chloride binding are at chlorine in system
Change ammonium, while ethyl alcohol can quickly improve the rate of volatilization of ammonium chloride, intermediate and the dodecyl benzene sulfonic acid of generation are combined into
New ionic liquid；The ionic liquid of preparation can significantly improve dissolving and dispersion performance to different materials, can improve porous three
The dispersibility and high temperature porosity of Al 2 O/porous silica；
2, sodium ethoxide and ionic liquid have excellent dissolubility, can disperse to material dissolution, material is thermally treated, and ethyl alcohol is waved
Hair promotes the viscosity of ionic liquid constantly to become larger, and for ionic liquid while dispersed material, ionic liquid can also be because of its high temperature point
Solution and as the pore creating material of material；Porous alumina/porous silica of preparation is because its porous structure is as crosslinking knot
The compression strength of silica-filled modified concrete material can be significantly improved by closing site；
3, phenolic resin can carry the mechanical strength of material, after high-temperature roasting is handled, phenolic resin as inorganic material adhesive
The mechanical strength of modified coal ash can be significantly improved；The modified coal ash of preparation can significantly improve silica-filled modified coagulation
The compression strength of soil material；
4, the introducing of styrene, methyl methacrylate, Isooctyl acrylate monomer and hydroxyethyl acrylate monomers can significantly improve and change
The mechanical strength and water-saving performance of property polyacrylamide；The modified polyacrylamide of preparation can improve silica because water-saving and fill out
Fill the compression strength of modified concrete material；
5, under cement, modified polyacrylamide, modified coal ash, sand and water synergistic effect, silica-filled change is assigned
The property excellent compression strength of concrete material.
Specific implementation mode
The specific implementation mode of the present invention is described with reference to embodiment, to be better understood from the present invention.This
It is a little that examples are only for illustrating the present invention and not for limiting the scope of the present invention.Actual conditions are not specified in lower example embodiment
Experimental method, usually according to this field normal condition or the condition suggested according to manufacturer；Used raw material, reagent etc.,
Unless otherwise specified, it is the raw materials and reagents that can be obtained from commercial sources such as conventional markets.Those skilled in the art is at this
The variation and replacement of any unsubstantiality done on the basis of invention belong to scope of the present invention.
Embodiment 1
A kind of silica-filled modified concrete material, preparation method includes the following steps：
(1), it weighs 19 parts of 1- butyl -3- methylimidazole villaumites, 93 parts of ethyl alcohol and 36 parts of ammonium hydroxide to be added in reaction kettle, stirring speed
Degree is 97r/min, reacts 12min under the conditions of 30 DEG C of maintenance system temperature, by 37 parts of dodecyl benzene sulfonic acid according to 0.08 part/
When min is added to reaction kettle, temperature of reaction kettle is risen to 141 DEG C, the reaction was continued under maintenance -0.06MPa reduced pressures 2.5h,
Obtain ionic liquid；
(2), 33 parts of alumina silicate, 63 parts of sodium ethoxides, 23 parts of ionic liquids, 72 parts of ethyl alcohol and 26 parts of tetraethyl orthosilicates are weighed to be added to
It in hydrothermal reaction kettle, maintains to react 3.5h under the conditions of 185 DEG C of hydrothermal temperature, product is through 100 DEG C of heat treatment 0.5h, 200 DEG C
It is heat-treated 1h, 400 DEG C of heat treatment 1h, 600 DEG C of heat treatment 1h, 800 DEG C of heat treatment 1h, 1200 DEG C are heat-treated 2h, grinding, product warp
35 DEG C, 20% sodium hydrate aqueous solution ultrasonic immersing processing 10min, product are super through 500mL water supersound washing 3 times, 500mL ethyl alcohol
Sound washs 2 times, is dried in vacuo 16min in 53 DEG C, -0.06MPa, obtains porous alumina/porous silica；
(3), 36 parts of flyash, 34 parts of porous alumina/porous silicas, 5.5 parts of phenolic resin and 51 parts of second are weighed
Alcohol is added in ball mill, drum speed 23r/min, reacts 30min under the conditions of 35 DEG C of maintenance system temperature, product is through 200
DEG C heat treatment 1h, 300 DEG C of heat treatment 1h, 400 DEG C of heat treatment 1h, 500 DEG C of heat treatment 1h, 600 DEG C of heat treatment 2h are to get to modification
Flyash；
(4), 32 parts of acrylamides, 5.3 parts of SE-10 emulsifiers, 53 parts of water, 1.4 parts of 2- acrylamide-2-methyl propane sulfonics are weighed
Sodium and 0.5 part of 184 photoinitiator are added in reaction kettle, mixing speed 90r/min, under the conditions of 32 DEG C of maintenance system temperature
23min is reacted, by 0.2 part of styrene, 0.4 part of methyl methacrylate, 0.8 part of Isooctyl acrylate monomer and 0.2 part of acrylic acid hydroxyl
The mixture of ethyl ester is added to according to 0.03 part/min in reaction kettle, maintain under above-mentioned reaction condition that the reaction was continued 35min, product
Through 2000W lamp and high pressure mercury 5s, product is dried in vacuo 35min through 75 DEG C, -0.09MPa, crushes to get to modified polypropene
Amide；
(5), 40 parts of cement, 0.9 part of modified polyacrylamide, 26 parts of modified coal ash, 8 parts of sands and 23 parts of water are weighed to be added to
In high-speed mixer, with high-speed mixer in 25 DEG C of hybrid reaction 5min of temperature to get to silica-filled modified concrete
Material.
Embodiment 2
A kind of silica-filled modified concrete material, preparation method includes the following steps：
(1), it weighs 19 parts of 1- butyl -3- methylimidazole villaumites, 86 parts of ethyl alcohol and 29 parts of ammonium hydroxide to be added in reaction kettle, stirring speed
Degree is 90r/min, reacts 12min under the conditions of 30 DEG C of maintenance system temperature, by 32 parts of dodecyl benzene sulfonic acid according to 0.08 part/
When min is added to reaction kettle, temperature of reaction kettle is risen to 133 DEG C, the reaction was continued under maintenance -0.06MPa reduced pressures 3h is obtained
To ionic liquid；
(2), 33 parts of alumina silicate, 53 parts of sodium ethoxides, 19 parts of ionic liquids, 66 parts of ethyl alcohol and 25 parts of tetraethyl orthosilicates are weighed to be added to
In hydrothermal reaction kettle, maintain to react 5h under the conditions of 173 DEG C of hydrothermal temperature, product is through 100 DEG C of heat treatment 0.5h, 200 DEG C of warm
1h is handled, 400 DEG C of heat treatment 1h, 600 DEG C of heat treatment 1h, 800 DEG C of heat treatment 1h, 1200 DEG C of heat treatment 2h, grinding, product is through 35
DEG C, 20% sodium hydrate aqueous solution ultrasonic immersing handle 10min, product is through 500mL water supersound washing 3 times, 500mL EtOH Sonicates
Washing 2 times is dried in vacuo 16min in 53 DEG C, -0.06MPa, obtains porous alumina/porous silica；
(3), 36 parts of flyash, 26 parts of porous alumina/porous silicas, 3 parts of phenolic resin and 41 parts of ethyl alcohol are weighed
It is added in ball mill, drum speed 19r/min, 30min is reacted under the conditions of 35 DEG C of maintenance system temperature, product is through 200 DEG C
It is heat-treated 1h, 300 DEG C of heat treatments 1h, 400 DEG C of heat treatments 1h, 500 DEG C of heat treatments 1h, 600 DEG C of heat treatment 2h are to get to modified powder
Coal ash；
(4), weigh 32 parts of acrylamides, 3 parts of SE-10 emulsifiers, 45 parts of water, 1 part of 2- acrylamide-2-methyl propane sulfonics sodium and
0.3 part of 184 photoinitiator is added in reaction kettle, mixing speed 88r/min, is reacted under the conditions of 32 DEG C of maintenance system temperature
23min, by 0.2 part of styrene, 0.2 part of methyl methacrylate, 0.5 part of Isooctyl acrylate monomer and 0.2 part of hydroxy-ethyl acrylate
Mixture be added in reaction kettle according to 0.03 part/min, maintain under above-mentioned reaction condition that the reaction was continued 35min, product warp
2000W lamp and high pressure mercury 4s, product are dried in vacuo 35min through 75 DEG C, -0.09MPa, crush to get to modified polypropene acyl
Amine；
(5), 40 parts of cement, 0.6 part of modified polyacrylamide, 23 parts of modified coal ash, 3 parts of sands and 18 parts of water are weighed to be added to
In high-speed mixer, with high-speed mixer in 25 DEG C of hybrid reaction 5min of temperature to get to silica-filled modified concrete
Material.
Embodiment 3
A kind of silica-filled modified concrete material, preparation method includes the following steps：
(1), 19 parts of 1- butyl -3- methylimidazole villaumites, 100 parts of ethyl alcohol and 52 parts of ammonium hydroxide are weighed to be added in reaction kettle, are stirred
Speed is 103r/min, reacts 12min under the conditions of 30 DEG C of maintenance system temperature, by 41 parts of dodecyl benzene sulfonic acid according to 0.08
When part/min is added to reaction kettle, temperature of reaction kettle is risen to 146 DEG C, the reaction was continued under maintenance -0.06MPa reduced pressures 1h,
Obtain ionic liquid；
(2), 33 parts of alumina silicate, 67 parts of sodium ethoxides, 31 parts of ionic liquids, 82 parts of ethyl alcohol and 33 parts of tetraethyl orthosilicates are weighed to be added to
In hydrothermal reaction kettle, maintain to react 2h under the conditions of 198 DEG C of hydrothermal temperature, product is through 100 DEG C of heat treatment 0.5h, 200 DEG C of warm
1h is handled, 400 DEG C of heat treatment 1h, 600 DEG C of heat treatment 1h, 800 DEG C of heat treatment 1h, 1200 DEG C of heat treatment 2h, grinding, product is through 35
DEG C, 20% sodium hydrate aqueous solution ultrasonic immersing handle 10min, product is through 500mL water supersound washing 3 times, 500mL EtOH Sonicates
Washing 2 times is dried in vacuo 16min in 53 DEG C, -0.06MPa, obtains porous alumina/porous silica；
(3), 36 parts of flyash, 39 parts of porous alumina/porous silicas, 9 parts of phenolic resin and 55 parts of ethyl alcohol are weighed
It is added in ball mill, drum speed 27r/min, 30min is reacted under the conditions of 35 DEG C of maintenance system temperature, product is through 200 DEG C
It is heat-treated 1h, 300 DEG C of heat treatments 1h, 400 DEG C of heat treatments 1h, 500 DEG C of heat treatments 1h, 600 DEG C of heat treatment 2h are to get to modified powder
Coal ash；
(4), weigh 32 parts of acrylamides, 7 parts of SE-10 emulsifiers, 62 parts of water, 4 parts of 2- acrylamide-2-methyl propane sulfonics sodium and
1 part of 184 photoinitiator is added in reaction kettle, mixing speed 100r/min, is reacted under the conditions of 32 DEG C of maintenance system temperature
23min, by 1 part of styrene, the mixture of 1 part of methyl methacrylate, 1 part of Isooctyl acrylate monomer and 1 part of hydroxy-ethyl acrylate
It is added in reaction kettle according to 0.03 part/min, the 35min that maintains under above-mentioned reaction condition that the reaction was continued, product is through 2000W high pressures
Mercury lamp illumination 9s, product are dried in vacuo 35min through 75 DEG C, -0.09MPa, crush to get to modified polyacrylamide；
(5), 40 parts of cement, 5 parts of modified polyacrylamides, 35 parts of modified coal ash, 12 parts of sands and 45 parts of water are weighed to be added to
In high-speed mixer, with high-speed mixer in 25 DEG C of hybrid reaction 15min of temperature to get to silica-filled modified concrete
Material.
Embodiment 4
A kind of silica-filled modified concrete material, preparation method includes the following steps：
(1), it weighs 19 parts of 1- butyl -3- methylimidazole villaumites, 88 parts of ethyl alcohol and 32 parts of ammonium hydroxide to be added in reaction kettle, stirring speed
Degree is 93r/min, 12min is reacted under the conditions of 30 DEG C of maintenance system temperature, by 33.4 parts of dodecyl benzene sulfonic acid according to 0.08
When part/min is added to reaction kettle, temperature of reaction kettle is risen to 135 DEG C, the reaction was continued under maintenance -0.06MPa reduced pressures
1.3h obtains ionic liquid；
(2), 33 parts of alumina silicate, 55 parts of sodium ethoxides, 19.6 parts of ionic liquids, 67 parts of ethyl alcohol and 26 parts of tetraethyl orthosilicate additions are weighed
Into hydrothermal reaction kettle, maintaining to react 2.2h under the conditions of 175 DEG C of hydrothermal temperature, product is through 100 DEG C of heat treatment 0.5h, and 200
DEG C heat treatment 1h, 400 DEG C heat treatment 1h, 600 DEG C heat treatment 1h, 800 DEG C heat treatment 1h, 1200 DEG C heat treatment 2h, grinding, product
10min is handled through 35 DEG C, 20% sodium hydrate aqueous solution ultrasonic immersing, product is through 500mL water supersound washing 3 times, 500mL ethyl alcohol
Supersound washing 2 times is dried in vacuo 16min in 53 DEG C, -0.06MPa, obtains porous alumina/porous silica；
(3), 36 parts of flyash, 28 parts of porous alumina/porous silicas, 3.7 parts of phenolic resin and 42.3 parts are weighed
Ethyl alcohol is added in ball mill, drum speed 20r/min, and 30min, product warp are reacted under the conditions of 35 DEG C of maintenance system temperature
200 DEG C heat treatment 1h, 300 DEG C heat treatment 1h, 400 DEG C heat treatment 1h, 500 DEG C heat treatment 1h, 600 DEG C heat treatment 2h to get to
Modified coal ash；
(4), 32 parts of acrylamides, 3.4 parts of SE-10 emulsifiers, 46 parts of water, 1.4 parts of 2- acrylamide-2-methyl propane sulfonics are weighed
Sodium and 0.4 part of 184 photoinitiator are added in reaction kettle, mixing speed 89r/min, under the conditions of 32 DEG C of maintenance system temperature
23min is reacted, by 0.3 part of styrene, 0.4 part of methyl methacrylate, 0.7 part of Isooctyl acrylate monomer and 0.4 part of acrylic acid hydroxyl
The mixture of ethyl ester is added to according to 0.03 part/min in reaction kettle, maintain under above-mentioned reaction condition that the reaction was continued 35min, product
Through 2000W lamp and high pressure mercury 5s, product is dried in vacuo 35min through 75 DEG C, -0.09MPa, crushes to get to modified polypropene
Amide；
(5), 40 parts of cement, 0.9 part of modified polyacrylamide, 25 parts of modified coal ash, 5 parts of sands and 19 parts of water are weighed to be added to
In high-speed mixer, with high-speed mixer in 25 DEG C of hybrid reaction 7min of temperature to get to silica-filled modified concrete
Material.
Embodiment 5
A kind of silica-filled modified concrete material, preparation method includes the following steps：
(1), it weighs 19 parts of 1- butyl -3- methylimidazole villaumites, 89 parts of ethyl alcohol and 37 parts of ammonium hydroxide to be added in reaction kettle, stirring speed
Degree is 97r/min, reacts 12min under the conditions of 30 DEG C of maintenance system temperature, by 36 parts of dodecyl benzene sulfonic acid according to 0.08 part/
When min is added to reaction kettle, temperature of reaction kettle is risen to 138 DEG C, the reaction was continued under maintenance -0.06MPa reduced pressures 1.8h,
Obtain ionic liquid；
(2), 33 parts of alumina silicate, 57 parts of sodium ethoxides, 23 parts of ionic liquids, 73 parts of ethyl alcohol and 28 parts of tetraethyl orthosilicates are weighed to be added to
It in hydrothermal reaction kettle, maintains to react 2.9h under the conditions of 178 DEG C of hydrothermal temperature, product is through 100 DEG C of heat treatment 0.5h, 200 DEG C
It is heat-treated 1h, 400 DEG C of heat treatment 1h, 600 DEG C of heat treatment 1h, 800 DEG C of heat treatment 1h, 1200 DEG C are heat-treated 2h, grinding, product warp
35 DEG C, 20% sodium hydrate aqueous solution ultrasonic immersing processing 10min, product are super through 500mL water supersound washing 3 times, 500mL ethyl alcohol
Sound washs 2 times, is dried in vacuo 16min in 53 DEG C, -0.06MPa, obtains porous alumina/porous silica；
(3), 36 parts of flyash, 29 parts of porous alumina/porous silicas, 4.4 parts of phenolic resin and 46 parts of second are weighed
Alcohol is added in ball mill, drum speed 23r/min, reacts 30min under the conditions of 35 DEG C of maintenance system temperature, product is through 200
DEG C heat treatment 1h, 300 DEG C of heat treatment 1h, 400 DEG C of heat treatment 1h, 500 DEG C of heat treatment 1h, 600 DEG C of heat treatment 2h are to get to modification
Flyash；
(4), 32 parts of acrylamides, 4.5 parts of SE-10 emulsifiers, 51 parts of water, 2.2 parts of 2- acrylamide-2-methyl propane sulfonics are weighed
Sodium and 0.5 part of 184 photoinitiator are added in reaction kettle, mixing speed 93r/min, under the conditions of 32 DEG C of maintenance system temperature
23min is reacted, by 0.5 part of styrene, 0.3 part of methyl methacrylate, 0.8 part of Isooctyl acrylate monomer and 0.4 part of acrylic acid hydroxyl
The mixture of ethyl ester is added to according to 0.03 part/min in reaction kettle, maintain under above-mentioned reaction condition that the reaction was continued 35min, product
Through 2000W lamp and high pressure mercury 7s, product is dried in vacuo 35min through 75 DEG C, -0.09MPa, crushes to get to modified polypropene
Amide；
(5), 40 parts of cement, 1.9 parts of modified polyacrylamides, 28 parts of modified coal ash, 6 parts of sands and 28 parts of water are weighed to be added to
In high-speed mixer, with high-speed mixer in 25 DEG C of hybrid reaction 8min of temperature to get to silica-filled modified concrete
Material.
Embodiment 6
A kind of silica-filled modified concrete material, preparation method includes the following steps：
(1), it weighs 19 parts of 1- butyl -3- methylimidazole villaumites, 95 parts of ethyl alcohol and 34 parts of ammonium hydroxide to be added in reaction kettle, stirring speed
Degree is 98r/min, reacts 12min under the conditions of 30 DEG C of maintenance system temperature, by 36 parts of dodecyl benzene sulfonic acid according to 0.08 part/
When min is added to reaction kettle, temperature of reaction kettle is risen to 135 DEG C, the reaction was continued under maintenance -0.06MPa reduced pressures 2h is obtained
Ionic liquid；
(2), 33 parts of alumina silicate, 65 parts of sodium ethoxides, 20 parts of ionic liquids, 75 parts of ethyl alcohol and 30 parts of tetraethyl orthosilicates are weighed to be added to
In hydrothermal reaction kettle, maintain to react 4h under the conditions of 180 DEG C of hydrothermal temperature, product is through 100 DEG C of heat treatment 0.5h, 200 DEG C of warm
1h is handled, 400 DEG C of heat treatment 1h, 600 DEG C of heat treatment 1h, 800 DEG C of heat treatment 1h, 1200 DEG C of heat treatment 2h, grinding, product is through 35
DEG C, 20% sodium hydrate aqueous solution ultrasonic immersing handle 10min, product is through 500mL water supersound washing 3 times, 500mL EtOH Sonicates
Washing 2 times is dried in vacuo 16min in 53 DEG C, -0.06MPa, obtains porous alumina/porous silica；
(3), 36 parts of flyash, 35 parts of porous alumina/porous silicas, 6 parts of phenolic resin and 50 parts of ethyl alcohol are weighed
It is added in ball mill, drum speed 25r/min, 30min is reacted under the conditions of 35 DEG C of maintenance system temperature, product is through 200 DEG C
It is heat-treated 1h, 300 DEG C of heat treatments 1h, 400 DEG C of heat treatments 1h, 500 DEG C of heat treatments 1h, 600 DEG C of heat treatment 2h are to get to modified powder
Coal ash；
(4), weigh 32 parts of acrylamides, 6 parts of SE-10 emulsifiers, 60 parts of water, 2 parts of 2- acrylamide-2-methyl propane sulfonics sodium and
0.5 part of 184 photoinitiator is added in reaction kettle, mixing speed 95r/min, is reacted under the conditions of 32 DEG C of maintenance system temperature
23min, by 0.4 part of styrene, 0.7 part of methyl methacrylate, 0.8 part of Isooctyl acrylate monomer and 0.4 part of hydroxy-ethyl acrylate
Mixture be added in reaction kettle according to 0.03 part/min, maintain under above-mentioned reaction condition that the reaction was continued 35min, product warp
2000W lamp and high pressure mercury 7s, product are dried in vacuo 35min through 75 DEG C, -0.09MPa, crush to get to modified polypropene acyl
Amine；
(5), 40 parts of cement, 3 parts of modified polyacrylamides, 28 parts of modified coal ash, 10 parts of sands and 35 parts of water are weighed to be added to
In high-speed mixer, with high-speed mixer in 25 DEG C of hybrid reaction 10min of temperature to get to silica-filled modified concrete
Material.
Embodiment 7
A kind of silica-filled modified concrete material, preparation method includes the following steps：
(1), it weighs 19 parts of 1- butyl -3- methylimidazole villaumites, 98 parts of ethyl alcohol and 50 parts of ammonium hydroxide to be added in reaction kettle, stirring speed
Degree is 101r/min, reacts 12min under the conditions of 30 DEG C of maintenance system temperature, by 38 parts of dodecyl benzene sulfonic acid according to 0.08 part/
When min is added to reaction kettle, temperature of reaction kettle is risen to 141 DEG C, the reaction was continued under maintenance -0.06MPa reduced pressures 2.6h,
Obtain ionic liquid；
(2), 33 parts of alumina silicate, 65 parts of sodium ethoxides, 30 parts of ionic liquids, 81 parts of ethyl alcohol and 31 parts of tetraethyl orthosilicates are weighed to be added to
It in hydrothermal reaction kettle, maintains to react 4.3h under the conditions of 196 DEG C of hydrothermal temperature, product is through 100 DEG C of heat treatment 0.5h, 200 DEG C
It is heat-treated 1h, 400 DEG C of heat treatment 1h, 600 DEG C of heat treatment 1h, 800 DEG C of heat treatment 1h, 1200 DEG C are heat-treated 2h, grinding, product warp
35 DEG C, 20% sodium hydrate aqueous solution ultrasonic immersing processing 10min, product are super through 500mL water supersound washing 3 times, 500mL ethyl alcohol
Sound washs 2 times, is dried in vacuo 16min in 53 DEG C, -0.06MPa, obtains porous alumina/porous silica；
(3), 36 parts of flyash, 34 parts of porous alumina/porous silicas, 7.6 parts of phenolic resin and 52 parts of second are weighed
Alcohol is added in ball mill, drum speed 23r/min, reacts 30min under the conditions of 35 DEG C of maintenance system temperature, product is through 200
DEG C heat treatment 1h, 300 DEG C of heat treatment 1h, 400 DEG C of heat treatment 1h, 500 DEG C of heat treatment 1h, 600 DEG C of heat treatment 2h are to get to modification
Flyash；
(4), 32 parts of acrylamides, 5.1 parts of SE-10 emulsifiers, 60 parts of water, 3.3 parts of 2- acrylamide-2-methyl propane sulfonics are weighed
Sodium and 0.6 part of 184 photoinitiator are added in reaction kettle, mixing speed 90r/min, under the conditions of 32 DEG C of maintenance system temperature
23min is reacted, by 0.8 part of styrene, 0.9 part of methyl methacrylate, 0.6 part of Isooctyl acrylate monomer and 0.7 part of acrylic acid hydroxyl
The mixture of ethyl ester is added to according to 0.03 part/min in reaction kettle, maintain under above-mentioned reaction condition that the reaction was continued 35min, product
Through 2000W lamp and high pressure mercury 6s, product is dried in vacuo 35min through 75 DEG C, -0.09MPa, crushes to get to modified polypropene
Amide；
(5), 40 parts of cement, 3.8 parts of modified polyacrylamides, 33 parts of modified coal ash, 11 parts of sands and 41 parts of water are weighed to be added
Into high-speed mixer, with high-speed mixer in 25 DEG C of hybrid reaction 13min of temperature to get to silica-filled modified coagulation
Soil material.
Embodiment 8
A kind of silica-filled modified concrete material, preparation method includes the following steps：
(1), it weighs 19 parts of 1- butyl -3- methylimidazole villaumites, 94 parts of ethyl alcohol and 45 parts of ammonium hydroxide to be added in reaction kettle, stirring speed
Degree is 99r/min, reacts 12min under the conditions of 30 DEG C of maintenance system temperature, by 37 parts of dodecyl benzene sulfonic acid according to 0.08 part/
When min is added to reaction kettle, temperature of reaction kettle is risen to 143 DEG C, the reaction was continued under maintenance -0.06MPa reduced pressures 2.5h,
Obtain ionic liquid；
(2), 33 parts of alumina silicate, 63 parts of sodium ethoxides, 29 parts of ionic liquids, 77 parts of ethyl alcohol and 28 parts of tetraethyl orthosilicates are weighed to be added to
It in hydrothermal reaction kettle, maintains to react 3.5h under the conditions of 191 DEG C of hydrothermal temperature, product is through 100 DEG C of heat treatment 0.5h, 200 DEG C
It is heat-treated 1h, 400 DEG C of heat treatment 1h, 600 DEG C of heat treatment 1h, 800 DEG C of heat treatment 1h, 1200 DEG C are heat-treated 2h, grinding, product warp
35 DEG C, 20% sodium hydrate aqueous solution ultrasonic immersing processing 10min, product are super through 500mL water supersound washing 3 times, 500mL ethyl alcohol
Sound washs 2 times, is dried in vacuo 16min in 53 DEG C, -0.06MPa, obtains porous alumina/porous silica；
(3), 36 parts of flyash, 31 parts of porous alumina/porous silicas, 6.5 parts of phenolic resin and 49 parts of second are weighed
Alcohol is added in ball mill, drum speed 21r/min, reacts 30min under the conditions of 35 DEG C of maintenance system temperature, product is through 200
DEG C heat treatment 1h, 300 DEG C of heat treatment 1h, 400 DEG C of heat treatment 1h, 500 DEG C of heat treatment 1h, 600 DEG C of heat treatment 2h are to get to modification
Flyash；
(4), 32 parts of acrylamides, 5.5 parts of SE-10 emulsifiers, 56 parts of water, 2.3 parts of 2- acrylamide-2-methyl propane sulfonics are weighed
Sodium and 0.7 part of 184 photoinitiator are added in reaction kettle, mixing speed 95r/min, under the conditions of 32 DEG C of maintenance system temperature
23min is reacted, by 0.5 part of styrene, 0.8 part of methyl methacrylate, 0.7 part of Isooctyl acrylate monomer and 0.6 part of acrylic acid hydroxyl
The mixture of ethyl ester is added to according to 0.03 part/min in reaction kettle, maintain under above-mentioned reaction condition that the reaction was continued 35min, product
Through 2000W lamp and high pressure mercury 9s, product is dried in vacuo 35min through 75 DEG C, -0.09MPa, crushes to get to modified polypropene
Amide；
(5), 40 parts of cement, 2.5 parts of modified polyacrylamides, 27 parts of modified coal ash, 8 parts of sands and 33 parts of water are weighed to be added to
In high-speed mixer, with high-speed mixer in 25 DEG C of hybrid reaction 9min of temperature to get to silica-filled modified concrete
Material.
Reference examples 1
In this reference examples, ionic liquid is not added, other components and preparation method are same as Example 1.
Reference examples 2
In this reference examples, porous alumina/porous silica, other components and preparation method and embodiment 1 are not added
It is identical.
Reference examples 3
In this reference examples, modified coal ash is not added, other components and preparation method are same as Example 1.
Reference examples 4
In this reference examples, modified polyacrylamide is not added, other components and preparation method are same as Example 1.
Reference examples 5
The ion in common 1- butyl -3- methylimidazole villaumite ionic liquids alternate embodiment 1 is selected in this reference examples, in formula
Liquid, other components and preparation method are same as Example 1.
Reference examples 6
Porous alumina/porous silica in general silica alternate embodiment 1 is selected in this reference examples, in formula
Silicon, other components and preparation method are same as Example 1.
Reference examples 7
The modified coal ash in ordinary fly ash alternate embodiment 1, other components and preparation side are selected in this reference examples, in formula
Method is same as Example 1.
Reference examples 8
The modified polyacrylamide in plain polypropylene amide alternate embodiment 1, other components are selected in this reference examples, in formula
It is same as Example 1 with preparation method.
The compression strength of silica-filled modified concrete material made from Examples 1 to 8 and reference examples 1~8 is pressed
It is tested according to GB/T 50081-2002, test result sees below Tables 1 and 2.
The performance parameter of silica-filled modified concrete material made from 1 Examples 1 to 8 of table
The performance parameter of silica-filled modified concrete material made from 2 embodiment 1 of table and reference examples 1~8
By upper Tables 1 and 2 it is found that the coagulation for the silica-filled modified concrete material that various embodiments of the present invention are prepared
Native strength grade is more excellent, this shows the silica-filled modified concrete material tool being prepared with raw material provided by the invention
There is preferable strength grade of concrete；In contrast, the silica-filled modified coagulation that the raw material of each reference examples is prepared
The strength grade of concrete of soil material is poor.In addition, the silica-filled modified coagulation that various embodiments of the present invention are prepared
Soil material has preferable strength grade of concrete.
The above is the preferred embodiment of the invention, it is noted that for those skilled in the art
For, under the premise of not departing from the inventive principle, several improvements and modifications can also be made, these improvements and modifications are also considered as
The protection domain of the invention.
Claims (3)
1. a kind of silica-filled modified concrete material, which is characterized in that by quality parts ratio be 40:0.6~5:23~
35:3~12:18~45 cement, modified polyacrylamide, modified coal ash, sand and water composition；Wherein, the modification
Polyacrylamide is 32 by quality parts ratio:0.2~1:0.2~1:3~7:45~62:0.5~1:0.2~1:1~4:0.3~
1 acrylamide, styrene, methyl methacrylate, SE-10 emulsifiers, water, Isooctyl acrylate monomer, hydroxy-ethyl acrylate, 2-
Acrylamide-2-methyl propane sulfonic sodium and the reaction of 184 photoinitiators are made；The modified coal ash is by quality parts ratio
36:26~39:3~9:41~55 flyash, porous alumina/porous silica, phenolic resin and ethanol synthesis
It is made；Porous alumina/the porous silica is by quality parts ratio 33:53~67:19~31:66~82:25
~33 alumina silicate, sodium ethoxide, ionic liquid, ethyl alcohol and tetraethyl orthosilicate reaction is made；The ionic liquid is by mass parts
Number is than being 19:32~41:86~100:29~52 1- butyl -3- methylimidazole villaumites, dodecyl benzene sulfonic acid, ethyl alcohol and ammonia
Water reaction is made.
2. silica-filled modified concrete material according to claim 1, which is characterized in that the cement, modification
Polyacrylamide, modified coal ash, sand and water quality parts ratio be 40:0.9:26:8:23.
3. the preparation method of any silica-filled modified concrete material of claim 1~2, which is characterized in that packet
Include following steps：
(1), 1- butyl -3- methylimidazole villaumites, ethyl alcohol and ammonium hydroxide are added in reaction kettle, mixing speed is 90~103r/
Min reacts 12min under the conditions of 30 DEG C of maintenance system temperature, dodecyl benzene sulfonic acid is added to according to 0.08 mass parts/min
When reaction kettle, temperature of reaction kettle is risen to 133~146 DEG C, the reaction was continued under maintenance -0.06MPa reduced pressures 1~3h is obtained
Ionic liquid；
(2), alumina silicate, sodium ethoxide, ionic liquid, ethyl alcohol and tetraethyl orthosilicate are added in hydrothermal reaction kettle, maintain hydro-thermal
2~5h is reacted under the conditions of 173~198 DEG C of reaction temperature, for product through 100 DEG C of heat treatment 0.5h, 200 DEG C are heat-treated 1h, 400 DEG C of heat
1h is handled, 600 DEG C of heat treatment 1h, 800 DEG C of heat treatment 1h, 1200 DEG C of heat treatment 2h, grinding, product is through 35 DEG C, 20% hydroxide
Sodium water solution ultrasonic immersing handles 10min, and product washs 2 times through 500mL water supersound washing 3 times, 500mL EtOH Sonicates, in 53
DEG C, -0.06MPa be dried in vacuo 16min, obtain porous alumina/porous silica；
(3), flyash, porous alumina/porous silica, phenolic resin and ethyl alcohol are added in ball mill, cylinder
Body rotating speed is 19~27r/min, reacts 30min under the conditions of 35 DEG C of maintenance system temperature, and product is through 200 DEG C of heat treatment 1h, 300 DEG C
It is heat-treated 1h, 400 DEG C of heat treatment 1h, 500 DEG C of heat treatment 1h, 600 DEG C of heat treatment 2h are to get to modified coal ash；
(4), acrylamide, SE-10 emulsifiers, water, 2- acrylamide-2-methyl propane sulfonics sodium and 184 photoinitiators are added
Into reaction kettle, mixing speed is 88~100r/min, 23min is reacted under the conditions of 32 DEG C of maintenance system temperature, by styrene, first
Base methyl acrylate, Isooctyl acrylate monomer, hydroxy-ethyl acrylate mixture be added to reaction kettle according to 0.03 mass parts/min
In, the 35min that maintains under above-mentioned reaction condition that the reaction was continued, product through 2000W 4~9s of lamp and high pressure mercury, product through 75 DEG C ,-
0.09MPa is dried in vacuo 35min, crushes to get to modified polyacrylamide；
(5), cement, modified polyacrylamide, modified coal ash, sand and water are added in high-speed mixer, it is mixed with high speed
Conjunction machine is in 25 DEG C of 5~15min of hybrid reaction of temperature to get to silica-filled modified concrete material.
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