CN114907050B - Mineral admixture and preparation method thereof - Google Patents
Mineral admixture and preparation method thereof Download PDFInfo
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- CN114907050B CN114907050B CN202210838411.2A CN202210838411A CN114907050B CN 114907050 B CN114907050 B CN 114907050B CN 202210838411 A CN202210838411 A CN 202210838411A CN 114907050 B CN114907050 B CN 114907050B
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a mineral admixture and a preparation method thereof, which greatly reduces the surface energy of materials by modifying the mixture of steel slag, zeolite powder and silica fume, by introducing the amino silicone oil, the mixture is favorably and uniformly dispersed in a cement system, the agglomeration is reduced, meanwhile, the amino silicone oil has hydrophobic effect, can reduce the surface energy of pores in concrete, reduces the absorption of moisture, further improves the fluidity, utilizes the benzenesulfonic acid to modify the carbon nano tube, improves the affinity between the carbon nano tube and the cement paste, obviously improves the crack resistance and the toughness of the cement, meanwhile, the modified carbon nano tube forms a space network structure in the cement paste, so that zeolite powder and silica fume can be effectively solidified, the problems of layered segregation, water seepage and the like caused by the floating of light materials such as the zeolite powder, the silica fume and the like are effectively solved, and the high strength performance of the concrete is ensured.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to a mineral admixture and a preparation method thereof.
Background
High performance concrete is widely used in the construction industry due to its excellent mechanical properties and durability. However, the preparation of high-performance concrete has higher requirements on the performance of various raw materials, and the mineral admixture widely applied to the high-performance concrete at present mainly comprises ground slag powder, silica micropowder and metakaolin, but has the defects of high price, unfavorable flowability of the concrete and the like, and has certain limitation in application. Therefore, there is a need to develop mineral admixtures that can improve both the mechanical properties and the flowability of concrete.
Patent document (CN 111072325A) discloses an easy-flowing composite mineral admixture, a preparation method thereof and mortar prepared by using the admixture, wherein the admixture comprises mineral powder, fly ash floating beads, quartz sand tailings and grinding aids; the preparation method comprises the steps of mixing mineral powder, quartz sand tailings and grinding aids, grinding, drying and cooling, and then adding fly ash floating beads and uniformly mixing to obtain the admixture; the mortar comprises water, cement, sand and an admixture, mineral powder, fly ash floating beads and quartz sand tailings are compounded, and grinding aids are combined, so that the prepared composite mineral admixture can effectively improve the fluidity of the mortar, but the 7d and 28d activity indexes of the composite mineral admixture are low and only 65%, and the composite mineral admixture cannot be applied to high-strength and high-performance concrete.
Patent document (CN 106495583A) discloses an early strength high performance composite steel slag powder admixture, which comprises mineral powder and raw steel slag powder, wherein the activity index of the prepared early strength high performance composite steel slag powder admixture is more than or equal to 80% in 7 days, more than or equal to 102% in 28 days, the fluidity ratio is more than or equal to 103%, and the performance of the admixture still needs to be further improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a mineral admixture and a preparation method thereof, and solves the technical problems of poor activity index and flowability of the existing mineral admixture.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a mineral admixture comprises the following steps:
(1) uniformly mixing the steel slag, the zeolite powder and the silica fume to obtain a mixture;
(2) placing the mixture in alkali liquor for dipping treatment, washing, drying and then carrying out heat treatment to obtain a pretreated mixture;
(3) dispersing the pretreated mixture in a methanol solvent, adding amino silicone oil and a silane coupling agent into the methanol solvent, heating, stirring, refluxing and reacting, and after the reaction is finished, washing and drying a reaction product to obtain a modified mixture;
(4) and grinding the modified mixture, the benzenesulfonic acid modified carbon nano tube and the grinding aid by using a ball mill to obtain the mineral admixture after the grinding is finished.
Preferably, in the step (1), the steel slag is silicate-containing and aluminoferrite-containing waste slag obtained in steel making, the mass percentage of CaO is more than or equal to 40wt%, and SiO is 2 The mass percentage content is more than or equal to 20wt percent, and the mass percentage content of MgO is less than or equal to 10wt percent.
Preferably, in the step (1), the mass ratio of the steel slag, the zeolite powder and the silica fume is 10-20:8-15: 6-10.
Preferably, in the step (2), the heat treatment temperature is 350-400 ℃, and the heat treatment time is 1-2 h.
Preferably, in the step (3), the mass ratio of the pretreatment mixture, the amino silicone oil and the silane coupling agent is 10-15:6-10: 3-6.
Preferably, in the step (3), the stirring reflux reaction temperature is 60-80 ℃, and the stirring reflux reaction time is 3-5 h.
Preferably, in the step (4), the preparation method of the benzenesulfonic acid modified carbon nanotube includes the following steps:
(01) adding the carbon nano tube into water, uniformly dispersing by ultrasonic, and drying for later use;
(02) and (2) adding the carbon nano tube obtained in the step (01) into 0.8-1.0mol/L benzenesulfonic acid solution, heating to 40-60 ℃, carrying out heat preservation treatment for 30-60min, then washing with water, and drying to obtain the benzenesulfonic acid modified carbon nano tube.
Preferably, in the step (4), the mass ratio of the modified mixture, the benzenesulfonic acid modified carbon nanotubes and the grinding aid is 100-200:5-10: 3-5.
Preferably, in the step (4), the grinding aid is composed of polyacrylamide, sodium polyacrylate and boric acid, wherein the mass ratio of the polyacrylamide to the sodium polyacrylate to the boric acid is 8-10:4-8: 3-6.
The invention also provides the mineral admixture prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
(1) the steel slag can delay the hydration of cement, so that the early activity of the cement is extremely low, and the fluidity is adversely affected, but the later activity is higher, the zeolite powder has a porous structure, plays a role in storing water in cement concrete, and improves the viscosity of the concrete.
(2) According to the invention, the carbon nano tube is modified by using the benzenesulfonic acid, so that the affinity between the carbon nano tube and the cement slurry is improved, the anti-cracking performance and the toughness of the cement are obviously improved, meanwhile, the modified carbon nano tube forms a space network structure in the cement slurry, the zeolite powder and the silica fume can be effectively solidified, the problems of layered segregation, water seepage and the like caused by the floating of light materials such as the zeolite powder and the silica fume are effectively avoided, and the high strength performance of the concrete is ensured; in addition, the initial fluidity of the cement paste is improved to a certain extent by introducing the sulfonic acid group, and the addition of the sulfonic acid group can promote the hydration of C3S, so that the 3d, 7d and 28d strength of the cement paste is improved.
(3) The steel slag, the zeolite powder and the silica fume provided by the invention have a superposition effect, fully play the advantages of various admixtures, can obviously improve the workability of concrete mixtures, have high early activity index, improve the early strength of concrete, and simultaneously ensure the stable development of the later strength of the concrete.
Detailed Description
The present invention will be described in more detail with reference to specific preferred embodiments, but the present invention is not limited to the following embodiments.
It should be noted that, unless otherwise specified, the chemical reagents involved in the present invention are commercially available.
The zeolite powder adopted by the invention is purchased from Taichang mineral products Limited company in Xinyang city, clinoptilolite, and the density is 1.8g/cm 3 ;
The silica fume is available from Henan JiuTai metallurgy materials Co., Ltd, and has a particle size of 0.1-0.3 μm;
polyacrylamide is purchased from Henan Edson environmental protection science and technology Limited and has a molecular weight of 1200 ten thousand;
sodium polyacrylate was purchased from Jiangsu Caosheng Biotech limited.
Example 1
A preparation method of a mineral admixture comprises the following steps:
(1) uniformly mixing 100g of steel slag, 80g of zeolite powder and 60g of silica fume to obtain a mixture;
(2) placing the mixture in 1mol/L NaOH solution for dipping treatment, washing and drying the mixture, and then carrying out heat treatment for 1h at 400 ℃ to obtain a pretreated mixture;
(3) dispersing 100g of the pretreated mixture in a methanol solvent, adding 60g of amino silicone oil and 30g of silane coupling agent KH560, heating, stirring and refluxing at 60 ℃ for reaction for 3h, and after the reaction is finished, washing and drying a reaction product to obtain a modified mixture;
(4) grinding 100g of the modified mixture, 5g of the benzenesulfonic acid modified carbon nanotube and 3g of the grinding aid by using a ball mill, and obtaining a mineral admixture after the grinding is finished;
the preparation method of the benzenesulfonic acid modified carbon nanotube comprises the following steps: adding 5g of carbon nano tube into water, uniformly dispersing by ultrasonic, drying, then adding into 1.0mol/L benzenesulfonic acid solution, heating to 50 ℃, carrying out heat preservation treatment for 30min, then washing with water, and drying to obtain benzenesulfonic acid modified carbon nano tube;
the grinding aid consists of polyacrylamide, sodium polyacrylate and boric acid, wherein the mass ratio of the polyacrylamide to the sodium polyacrylate to the boric acid is 10:4: 5.
Example 2
A preparation method of a mineral admixture comprises the following steps:
(1) uniformly mixing 150g of steel slag, 100g of zeolite powder and 100g of silica fume to obtain a mixture;
(2) placing the mixture in a 1mol/L NaOH solution for dipping treatment, washing and drying the mixture, and then carrying out heat treatment at 350 ℃ for 2 hours to obtain a pretreated mixture;
(3) dispersing 120g of the pretreated mixture in a methanol solvent, adding 80g of amino silicone oil and 40g of silane coupling agent KH560, heating, stirring and refluxing at 60 ℃ for 5h, and after the reaction is finished, washing and drying a reaction product to obtain a modified mixture;
(4) grinding 120g of the modified mixture, 8g of the benzenesulfonic acid modified carbon nanotube and 5g of the grinding aid by using a ball mill, and obtaining a mineral admixture after the grinding is finished;
the preparation method of the benzenesulfonic acid modified carbon nanotube comprises the following steps: adding 5g of carbon nano tube into water, uniformly dispersing by ultrasonic, drying, then adding into 0.8mol/L benzenesulfonic acid solution, heating to 40 ℃, carrying out heat preservation treatment for 60min, then washing with water, and drying to obtain benzenesulfonic acid modified carbon nano tube;
the grinding aid consists of polyacrylamide, sodium polyacrylate and boric acid, wherein the mass ratio of the polyacrylamide to the sodium polyacrylate to the boric acid is 8:5: 5.
Example 3
A method of preparing a mineral admixture comprising the steps of:
(1) uniformly mixing 160g of steel slag, 150g of zeolite powder and 90g of silica fume to obtain a mixture;
(2) placing the mixture in 1mol/L NaOH solution for dipping treatment, washing and drying the mixture, and then carrying out heat treatment for 1h at 400 ℃ to obtain a pretreated mixture;
(3) dispersing 150g of the pretreated mixture in a methanol solvent, then adding 100g of amino silicone oil and 60g of silane coupling agent KH560, heating, stirring and refluxing at 80 ℃ for reaction for 3 hours, and after the reaction is finished, washing and drying a reaction product to obtain a modified mixture;
(4) grinding 200g of the modified mixture, 10g of the benzenesulfonic acid modified carbon nanotube and 5g of the grinding aid by using a ball mill, and obtaining a mineral admixture after the grinding is finished;
the preparation method of the benzenesulfonic acid modified carbon nanotube comprises the following steps: adding 5g of carbon nano tube into water, uniformly dispersing by ultrasonic, drying, then adding into 0.8mol/L benzenesulfonic acid solution, heating to 60 ℃, carrying out heat preservation treatment for 30min, then washing with water, and drying to obtain benzenesulfonic acid modified carbon nano tube;
the grinding aid consists of polyacrylamide, sodium polyacrylate and boric acid, wherein the mass ratio of the polyacrylamide to the sodium polyacrylate to the boric acid is 10:4: 6.
Example 4
A preparation method of a mineral admixture comprises the following steps:
(1) uniformly mixing 200g of steel slag, 120g of zeolite powder and 100g of silica fume to obtain a mixture;
(2) placing the mixture in 1mol/L NaOH solution for dipping treatment, washing, drying, and then carrying out heat treatment for 2h at 350 ℃ to obtain a pretreated mixture;
(3) dispersing 120g of the pretreated mixture in a methanol solvent, adding 80g of amino silicone oil and 60g of silane coupling agent KH560, heating, stirring and refluxing at 70 ℃ for 4h, and after the reaction is finished, washing and drying a reaction product to obtain a modified mixture;
(4) grinding 180g of the modified mixture, 8g of the benzenesulfonic acid modified carbon nanotube and 5g of the grinding aid by using a ball mill, and obtaining a mineral admixture after the grinding is finished;
the preparation method of the benzenesulfonic acid modified carbon nanotube comprises the following steps: adding 5g of carbon nano tube into water, uniformly dispersing by ultrasonic, drying, then adding into 0.8mol/L benzenesulfonic acid solution, heating to 60 ℃, carrying out heat preservation treatment for 30min, then washing with water, and drying to obtain benzenesulfonic acid modified carbon nano tube;
the grinding aid consists of polyacrylamide, sodium polyacrylate and boric acid, wherein the mass ratio of the polyacrylamide to the sodium polyacrylate to the boric acid is 8:4: 6.
Comparative example 1
A preparation method of a mineral admixture comprises the following steps:
grinding 80g of steel slag, 75g of zeolite powder, 45g of silica fume, 10g of benzenesulfonic acid modified carbon nano tube and 5g of grinding aid by using a ball mill, and obtaining a mineral admixture after grinding;
the preparation method of the benzenesulfonic acid modified carbon nanotube comprises the following steps: adding 5g of carbon nano tube into water, uniformly dispersing by ultrasonic, drying, then adding into 0.8mol/L benzenesulfonic acid solution, heating to 60 ℃, carrying out heat preservation treatment for 30min, then washing with water, and drying to obtain benzenesulfonic acid modified carbon nano tube;
the grinding aid consists of polyacrylamide, sodium polyacrylate and boric acid, wherein the mass ratio of the polyacrylamide to the sodium polyacrylate to the boric acid is 10:4: 6.
Comparative example 2
A preparation method of a mineral admixture comprises the following steps:
(1) uniformly mixing 160g of steel slag, 150g of zeolite powder and 90g of silica fume to obtain a mixture;
(2) placing the mixture in 1mol/L NaOH solution for dipping treatment, washing and drying the mixture, and then carrying out heat treatment for 1h at 400 ℃ to obtain a pretreated mixture;
(3) dispersing 150g of the pretreated mixture in a methanol solvent, then adding 100g of amino silicone oil and 60g of silane coupling agent KH560, heating, stirring and refluxing at 80 ℃ for reaction for 3h, and after the reaction is finished, washing and drying a reaction product to obtain a modified mixture;
(4) grinding 200g of the modified mixture, 10g of the carbon nano tube and 5g of the grinding aid by using a ball mill to obtain a mineral admixture after the grinding is finished;
the grinding aid consists of polyacrylamide, sodium polyacrylate and boric acid, wherein the mass ratio of the polyacrylamide to the sodium polyacrylate to the boric acid is 10:4: 6.
After 30% by mass of cement was replaced with the mineral admixture prepared in examples 1 to 4 and comparative examples 1 to 2, the cement was ordinary Portland 42.5 cement, and the fluidity ratio was measured in accordance with GB/T17671 "Cement mortar Strength test" test Activity index, GB/T2419 "Cement mortar fluidity ratio measuring method", and the test results are shown in the following table:
3d Activity index/%) | 7d Activity index/%) | 28d Activity index/%) | Fluidity ratio/%) | |
Example 1 | 123 | 134 | 131 | 127 |
Example 2 | 125 | 135 | 133 | 125 |
Example 3 | 123 | 134 | 132 | 126 |
Example 4 | 124 | 135 | 130 | 126 |
Comparative example 1 | 109 | 118 | 117 | 102 |
Comparative example 2 | 112 | 124 | 121 | 109 |
Finally, it is to be noted that: the above examples do not limit the invention in any way. It will be apparent to those skilled in the art that various modifications and improvements can be made to the present invention. Accordingly, any modification or improvement made without departing from the spirit of the present invention is within the scope of the claimed invention.
Claims (10)
1. The preparation method of the mineral admixture is characterized by comprising the following steps:
(1) uniformly mixing the steel slag, the zeolite powder and the silica fume to obtain a mixture;
(2) placing the mixture in alkali liquor for dipping treatment, washing, drying and then carrying out heat treatment to obtain a pretreated mixture;
(3) dispersing the pretreated mixture in a methanol solvent, adding amino silicone oil and a silane coupling agent into the methanol solvent, heating, stirring, refluxing and reacting, and after the reaction is finished, washing and drying a reaction product to obtain a modified mixture;
(4) and grinding the modified mixture, the benzenesulfonic acid modified carbon nano tube and the grinding aid by using a ball mill to obtain the mineral admixture after the grinding is finished.
2. The method for preparing the mineral admixture according to claim 1, wherein in the step (1), the steel slag is silicate-containing and aluminoferrite-containing waste slag obtained in steel making, the mass percentage of CaO is more than or equal to 40wt%, and SiO is 2 The mass percentage content is more than or equal to 20wt percent, and the mass percentage content of MgO is less than or equal to 10wt percent.
3. The method for preparing the mineral admixture according to claim 1, wherein in the step (1), the mass ratio of the steel slag, the zeolite powder and the silica fume is 10-20:8-15: 6-10.
4. The method for preparing a mineral admixture as defined in claim 1 wherein, in the step (2), the heat treatment temperature is 350-400 ℃ and the heat treatment time is 1-2 h.
5. The method for preparing the mineral admixture according to claim 1, wherein in the step (3), the mass ratio of the pretreatment mixture, the amino silicone oil and the silane coupling agent is 10-15:6-10: 3-6.
6. The method for preparing a mineral admixture according to claim 1, wherein in the step (3), the reaction temperature of stirring reflux is 60-80 ℃ and the reaction time of stirring reflux is 3-5 h.
7. The method for preparing a mineral admixture according to claim 1, wherein in the step (4), the method for preparing the benzenesulfonic acid-modified carbon nanotubes comprises the steps of:
(01) adding the carbon nano tube into water, uniformly dispersing by ultrasonic, and drying for later use;
(02) and (2) adding the carbon nano tube obtained in the step (01) into 0.8-1.0mol/L benzenesulfonic acid solution, heating to 40-60 ℃, carrying out heat preservation treatment for 30-60min, then washing with water, and drying to obtain the benzenesulfonic acid modified carbon nano tube.
8. The method for preparing the mineral admixture as defined in claim 1 wherein in the step (4), the mass ratio of the modified mixture, the benzenesulfonic acid modified carbon nanotubes and the grinding aid is 100-200:5-10: 3-5.
9. The method for preparing the mineral admixture according to claim 1, wherein in the step (4), the grinding aid is composed of polyacrylamide, sodium polyacrylate and boric acid, wherein the mass ratio of the polyacrylamide to the sodium polyacrylate to the boric acid is 8-10:4-8: 3-6.
10. A mineral admixture obtainable by the process according to any one of claims 1 to 9.
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CN111908825A (en) * | 2020-07-24 | 2020-11-10 | 尧柏特种水泥技术研发有限公司 | Early strength type nano mineral admixture for concrete and preparation method thereof |
CN113754340A (en) * | 2021-08-16 | 2021-12-07 | 贵州工程应用技术学院 | Composite admixture for improving durability of common concrete through improved gradation |
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US20190315654A1 (en) * | 2016-08-15 | 2019-10-17 | Metna Co | Beneficiation of Inorganic Matrices with Wet, Non-Agglomerated, High-Concentration and Stable Graphite Nanoplatelets without Any Extra Measures to Disperse the Nanoplatelets |
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CN106977150A (en) * | 2017-05-05 | 2017-07-25 | 佛山慧创正元新材料科技有限公司 | A kind of preparation method using slag as the cement-base composite material of admixture |
CN110734255A (en) * | 2019-10-31 | 2020-01-31 | 中建材料技术研究成都有限公司 | Low-self-contraction high-toughness cement-based composite material and preparation method thereof |
CN111908825A (en) * | 2020-07-24 | 2020-11-10 | 尧柏特种水泥技术研发有限公司 | Early strength type nano mineral admixture for concrete and preparation method thereof |
CN113754340A (en) * | 2021-08-16 | 2021-12-07 | 贵州工程应用技术学院 | Composite admixture for improving durability of common concrete through improved gradation |
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