CN111574082A - Preparation method of single-component geopolymer cement - Google Patents

Preparation method of single-component geopolymer cement Download PDF

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CN111574082A
CN111574082A CN202010411000.6A CN202010411000A CN111574082A CN 111574082 A CN111574082 A CN 111574082A CN 202010411000 A CN202010411000 A CN 202010411000A CN 111574082 A CN111574082 A CN 111574082A
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sio
cao
admixture
cement
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CN111574082B (en
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张会芝
刘纪峰
杨悦
陈孝国
连跃宗
付晓强
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Sanming University
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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
    • C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
    • C04B12/005—Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates
    • 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
    • C04B7/00—Hydraulic cements
    • C04B7/24—Cements from oil shales, residues or waste other than slag
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding

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  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The invention provides a preparation method of single-component geopolymer cement. The invention utilizes metal tailings, feldspar, papermaking white mud, cement kiln powder and the like as the main components of SiO2、Al2O3And industrial by-products of Ca-containing compounds, by adding a solid alkali activator. On one hand, the environmental pressure caused by the stockpiling of the metal tailings is reduced, and on the other hand, the resource utilization of the metal tailings and other solid wastes can be realized due to wide raw material sources and low price. The single-component geopolymer cement has the 28d cubic compressive strength of 35-45 MPa, and can be widely applied to production raw materials of building material products such as concrete preparation, rock and soil mass grouting reinforcement, rapid repair of highways or airport runways, concrete prefabricated part manufacturing, wall building block manufacturing, permeable pavement bricks, kerbs and the like.

Description

Preparation method of single-component geopolymer cement
Technical Field
The invention relates to the field of cement materials, and in particular relates to a preparation method of single-component geopolymer cement.
Background
Mineral resources are the material basis upon which society is based for survival and development. At present, more than 80% of industrial raw materials and more than 70% of agricultural production data in more than 95% of domestic disposable energy sources are from mineral resources. Because the effective comprehensive utilization rate of mineral resources is low, a large amount of useful resources enter the waste tailings. Industrial waste residues and metal tailings in China are almost everywhere, and the amount of some industrial waste residues is large, such as fly ash. If the tailings are not treated and comprehensively utilized, more and more land is occupied by the tailings, secondary environmental pollution is caused, resource waste is caused, and sustainable development of mineral resources is further influenced.
The single-component geopolymer cement with metal tailings is prepared by adding solid alkali activator into metal tailings or mixture thereof, is similar to common cement, can be directly used by adding water, and has good development prospect.
Disclosure of Invention
The invention aims to provide a method for preparing single-component geopolymer cement, which aims to solve the problems of tailing accumulation, resource waste, environmental pollution and the like caused by low comprehensive utilization rate of metal tailings.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a preparation method of single-component geopolymer cement, which comprises the following steps:
s1, obtaining raw materials, and respectively counting SiO in the raw materials2、Al2O3And the content of Ca-containing compounds is obtained to obtain an analysis result, wherein the Ca-containing compounds are CaO and/or CaCO3The raw material is selected from one or more of metal tailings, papermaking white mud, feldspar and cement kiln dust;
s2, blending the raw materials to obtain an admixture according to the analysis result;
s3, adding Na into the admixture2CO3Uniformly mixing, calcining, and immediately cooling the calcined molten material to obtain a calcined product;
and S4, grinding the calcined product to obtain the single-component geopolymer cement.
The preparation method of the single-component geopolymer cement has the beneficial effects that:
1. the invention utilizes the main components of metal tailings, feldspar, papermaking white mud, cement kiln dust and the like as SiO2、Al2O3And CaO (CaCO)3) The single-component geopolymer cement prepared from the industrial byproducts reduces the environmental pressure caused by the stockpiling of the metal tailings, and can realize the resource utilization of the solid wastes such as the metal tailings and the like, save energy and reduce the carbon emission due to wide raw material sources and low price.
2. The main component of the single-component geopolymer cement prepared by the invention is a glassy material which contains more than 95% of amorphous substances. The 28d cubic compressive strength of the single-component geopolymer cement is 35-45 MPa, and can reach the strength standard of No. 32.5 or No. 42.5 cement. The 3d and 7d cubic compressive strengths were 40% and 75% of the 28d cubic compressive strength, respectively. The single-component geopolymer cement has the advantages of convenience for engineering construction, good comprehensive performance, energy conservation, environmental protection and the like, and can be widely applied to the production raw materials of building material products such as concrete preparation, rock and soil mass grouting reinforcement, rapid repair of highways or airport runways, concrete prefabricated part manufacture, wall block manufacture, permeable pavement bricks, kerbs and the like.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The invention provides a preparation method of single-component geopolymer cement, which comprises the following steps:
s1, obtaining raw materials, and respectively counting SiO in the raw materials2、Al2O3And the content of Ca-containing compounds, and obtaining an analysis result, wherein the raw material is selected from metal tailings, feldspar, papermaking white mud, cement kiln dust and the like, and the main component of the raw material is SiO2、Al2O3And industrial by-products of Ca-containing compounds. The Ca-containing compound is CaO and/or CaCO3Wherein CaCO3CaO may be obtained by high temperature calcination. By comprehensively utilizing solid wastes such as metal tailings and the like, the environmental pressure caused by the stockpiling of the tailings can be reduced, and the resource utilization of the solid wastes such as the metal tailings and the like can be realized in a large scale and the energy is saved due to wide raw material sources and low price.
Further, according to the mass percentage, in the metal tailings, the SiO is contained in235 to 45 percent of Al2O35% -8% of the white mud, 25% -30% of CaO, and SiO in the white mud21 to 3 percent of Al2O30.2-0.8% of CaO, 45-55% of CaO, in the feldspar, the SiO265% -80% of Al2O313% -15%, CaO 1% -3%, and in the cement kiln dust, SiO26 to 8 percent of Al2O32 to 3 percent of CaO and 45 to 60 percent of CaO.
And S2, blending the raw materials according to the analysis result to obtain the admixture.
Further, in the admixture, the SiO is calculated by mass percentage230 to 45 percent of the Al2O36 to 15 percent of the CaO, and 30 to 40 percent of the CaO, wherein the SiO is2And said Al2O3The mass ratio of (A) to (B) is 4.5-6.5: 1.
further, the raw materials are the metal tailings, the papermaking white mud and the feldspar, the metal tailings, the papermaking white mud and the feldspar are blended according to the mass ratio of 5:3:2 to prepare the admixture, and in the admixture, the SiO is contained235 to 36 percent of the Al, 30 to 31 percent of the CaO, and the Al2O36 to 8 percent of SiO2And said Al2O3The mass ratio of (A) to (B) is 5.65: 1.
further, the raw materials are selectedThe metal tailings, the cement kiln dust and the feldspar are blended according to the mass ratio of 5:3:2 to prepare the admixture, and according to mass percent, in the admixture, the SiO is236 to 38 percent of the Al, 30 to 31 percent of the CaO, and the Al2O36 to 8 percent of SiO2And said Al2O3The mass ratio of (A) to (B) is 5.4: 1.
s3, adding Na into the admixture2CO3Uniformly mixing, then calcining, and immediately cooling the calcined molten material to obtain a calcined product.
Further, said Na2CO3The mass fraction in the admixture is 15 to 25 percent, and Na2CO3Used as solid alkali activator in the preparation process of single-component geopolymer cement. As the solid alkali-activator increases, the pH of the admixture increases, [ OH ]]-The concentration is increased and the activation reaction is accelerated, but when it reaches a peak, since the reaction is too rapid, the product is not easily diffused, adheres to the surface of the fine particles to form a protective film, but prevents the further reaction, and therefore, it is preferable that Na of the present invention is used2CO3The mass fraction of the admixture in the admixture is 15-25%, and the admixture is ensured to have a faster reaction speed under the reaction condition. The calcination temperature is 1250-1350 ℃, and the calcination time is 2.5-3.5 hours. Through Na2CO3The molten material obtained by excitation and calcination for 2.5-3.5 hours at the calcination temperature has a 28d cube compressive strength of 35-45 MPa after 28d curing and has good quality, so the activation mode is a better activation mode. The molten material is cooled by adopting rapid air flow, wherein the flow velocity of the air flow is 0.6-1.5 m/s. The method effectively utilizes air flow to enhance and accelerate cooling of the molten material to improve the quality of the single-component geopolymer cement and improve its wear resistance.
And S4, grinding the calcined product to obtain the single-component geopolymer cement.
Further, after grinding the cooled molten material, screening to obtain the single-component geopolymer cement with the grain size of less than 50 mu m, wherein the main component of the single-component geopolymer cement is a glassy material, and the mass fraction of amorphous substances in the glassy material is more than 95%.
And (3) adding water into the single-component geopolymer cement, and stirring for 5 minutes after adding the water. The water-solid ratio of the water to the single-component geopolymer cement is 0.29-0.31: 1. and then, filling the single-component geopolymer cement into a steel test mould with the specification of 150cm by 150cm for curing, wherein the relative humidity of curing is 99 +/-1, the curing temperature is 23 +/-2 ℃, and the curing time is 24 hours. After curing, the mold was removed and cured again under the same conditions for 28 days.
After curing for 28 days, the 28d cubic compressive strength of the single-component geopolymer cement is 35-45 MPa, the 28d cubic compressive strength of the single-component geopolymer cement reaches the No. 32.5 or No. 42.5 cement strength standard, and the 3d cubic compressive strength and the 7d cubic compressive strength of the single-component geopolymer cement are 40% and 75% of the 28d cubic compressive strength respectively.
The single-component geopolymer cement prepared by the invention is the same as common cement, and can be widely used as a raw material for producing building material products such as concrete preparation, rock and soil mass grouting reinforcement, rapid repair of highways or airport runways, concrete prefabricated member manufacturing, wall building block manufacturing or permeable pavement bricks, curbs and the like.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The preparation method of the single-component geopolymer cement provided by the embodiment comprises the following steps:
(1) preparing an admixture: the composition of the metal tailings, the papermaking white mud and the feldspar is shown in table 1. According to SiO in Table 12、Al2O3And CaO, wherein the metal tailings, the papermaking white mud and the feldspar are blended according to the mass percentage of 50 percent, 30 percent and 20 percent respectively to prepare the admixture. Wherein, in the admixture, SiO is calculated by mass percentage235.6% of CaO, 30.1% of Al2O36.3% of SiO2And Al2O3The mass ratio of (A) to (B) is 5.65: 1.
TABLE 1 analysis results (mass ratio%) of the components of the metal tailings, the papermaking white mud and the feldspar
Composition (I) SiO2 CaO MgO Fe2O3 Al2O3 SO3 Na2O K2O Loss on ignition
Metal tailings 41.0 28.6 4.0 8.4 6.7 3.1 0.2 0.2 7.8
Papermaking white mud 2.1 51.3 0.5 0.2 0.5 0.3 0.6 0.9 43.6
Feldspar 72.3 2.0 0.3 0.9 14.2 0.2 3.1 4.9 2.1
(2) Preparation of one-component geopolymer cement: adding Na into the admixture2CO3The Na is2CO3The mass fraction in the admixture is 25 percent. Admixture and Na2CO3After mixing uniformly, the mixture was calcined at a high temperature of 1350 ℃ for 2.5 hours, and the calcined molten material was immediately cooled by a rapid air flow having a flow rate of 1.5m/s and then ground. Grinding, sieving with 50 μm sieve, and retaining substances with particle size less than 50 μm, which is single-component geopolymer cement, mainly contains glassy material and amorphous substance more than 95%.
The one-component geopolymer cement obtained in this example had a 28d cubic compressive strength of 35MPa, and the 28d cubic compressive strength of the one-component geopolymer cement reached the cement strength standard No. 32.5, and the 3d cubic compressive strength and the 7d cubic compressive strength were 40% and 75% of the 28d cubic compressive strength, respectively. The concrete grouting reinforcement material has the advantages of convenience for engineering construction, good comprehensive performance, energy conservation, environmental protection and the like, and can be widely applied to production raw materials of building material products such as concrete preparation, rock-soil body grouting reinforcement, rapid repair of highways or airport runways, concrete prefabricated part manufacturing, wall block manufacturing and permeable pavement bricks, kerbs and the like.
Example 2
The embodiment provides a method for preparing single-component geopolymer cement, which is different from the embodiment 1 in that:
preparing the admixture in the step (1): the composition of the metal tailings, cement kiln dust and feldspar is shown in table 2. According to SiO in Table 22、Al2O3And CaO, and blending the metal tailings, the papermaking white mud and the feldspar according to the mass ratio of 5:3:2 to prepare the admixture. Wherein, in the admixture, SiO is calculated by mass percentage237.2 percent of CaO, 30.6 percent of CaO, and Al2O36.9% of SiO2And Al2O3The mass ratio of (A) to (B) is 5.4: 1.
TABLE 2 analysis results (mass%)
Figure BDA0002493237800000061
Figure BDA0002493237800000071
The one-component geopolymer cement obtained in this example had a 28d cubic compressive strength of 45MPa, and the 28d cubic compressive strength of the one-component geopolymer cement reached the 42.5 cement strength standard, with a 3d cubic compressive strength and a 7d cubic compressive strength of 40% and 75% of the 28d cubic compressive strength, respectively. The concrete grouting reinforcement material has the advantages of convenience for engineering construction, good comprehensive performance, energy conservation, environmental protection and the like, and can be widely applied to production raw materials of building material products such as concrete preparation, rock-soil body grouting reinforcement, rapid repair of highways or airport runways, concrete prefabricated part manufacturing, wall block manufacturing and permeable pavement bricks, kerbs and the like.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Claims (7)

1. A method for preparing single-component geopolymer cement, characterized by comprising the following steps:
s1, obtaining raw materials, and respectively counting SiO in the raw materials2、Al2O3And the content of Ca-containing compounds is obtained to obtain an analysis result, wherein the Ca-containing compounds are CaO and/or CaCO3The raw material is selected from one or more of metal tailings, papermaking white mud, feldspar and cement kiln dust;
s2, blending the raw materials to obtain an admixture according to the analysis result;
s3, adding Na into the admixture2CO3Uniformly mixing, calcining, and immediately cooling the calcined molten material to obtain a calcined product;
and S4, grinding the calcined product to obtain the single-component geopolymer cement.
2. The method for preparing single-component geopolymer cement according to claim 1, wherein in step S1, the SiO is in the metal tailings according to mass percentage235 to 45 percent of Al2O35% -8% of the white mud, 25% -30% of CaO, and SiO in the white mud21 to 3 percent of Al2O30.2-0.8% of CaO, 45-55% of CaO, in the feldspar, the SiO265% -80% of Al2O313% -15%, CaO 1% -3%, and in the cement kiln dust, SiO26 to 8 percent of Al2O32 to 3 percent of CaO and 45 to 60 percent of CaO.
3. The method for preparing single-component geopolymer cement according to claim 1, wherein in step S2, the SiO is contained in the admixture by mass percentage230 to 45 percent of the Al2O36 to 15 percent of the CaO, and 30 to 40 percent of the CaO, wherein the SiO is2And said Al2O3The mass ratio of (A) to (B) is 4.5-6.5: 1.
4. the method for preparing single-component geopolymer cement according to claim 1, wherein the raw materials are the metal tailings, the papermaking white mud and the feldspar, and in step S2, the metal tailings, the papermaking white mud and the feldspar are blended according to a mass ratio of 5:3:2 to prepare the admixture, wherein in the admixture, the SiO is in mass percentage235 to 36 percent of the Al, 30 to 31 percent of the CaO, and the Al2O36 to 8 percent of SiO2And said Al2O3The mass ratio of (A) to (B) is 5.65: 1.
5. the method for preparing single-component geopolymer cement as claimed in claim 1, wherein said raw materials are selected from said metal tailings, said cement kiln dust and said feldspar, and in step S2, said metal tailings, said cement kiln dust and said feldspar are blended in a mass ratio of 5:3:2 to prepare said admixture, wherein said SiO is included in said admixture by mass percentage236 to 38 percent of the Al, 30 to 31 percent of the CaO, and the Al2O36 to 8 percent of SiO2And said Al2O3The mass ratio of (A) to (B) is 5.4: 1.
6. the one-component geopolymer cement preparation method of claim 1The method is characterized in that in step S3, the Na is2CO3The mass fraction of the additive in the admixture is 15-25%, the calcining temperature is 1250-1350 ℃, the calcining time is 2.5-3.5 hours, and the molten material is cooled by adopting rapid air flow.
7. The method of claim 1, wherein the cooled molten material is ground and sieved to obtain the single-component geopolymer cement with a particle size of less than 50 μm, wherein the glassy material is mainly composed of amorphous substances with a mass fraction of more than 95%.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114960609A (en) * 2022-04-25 2022-08-30 三明学院 Composite foundation for reinforcing saturated soft soil by single-component geopolymer and construction method thereof
CN115611580A (en) * 2022-10-21 2023-01-17 广西大学 High-strength sound-insulation heat-insulation prefabricated inner partition plate based on papermaking white mud and preparation method thereof

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CN103508693A (en) * 2013-09-29 2014-01-15 四川利森建材集团有限公司 Cement modifier and production and application method thereof
CN102730996B (en) * 2012-07-11 2014-06-18 湖南科技大学 Preparation of single-component alkali-activated cement and application method thereof
CN104844023A (en) * 2015-04-29 2015-08-19 重庆大学 Method for manufacturing mine filling material by curing copper tailing using iron tailing
CN107129166A (en) * 2017-04-01 2017-09-05 三明学院 A kind of green composite cement and preparation method thereof
CN109437613A (en) * 2018-12-21 2019-03-08 福州大学 One pack system nickel slag ground polymers cement

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CN102730996B (en) * 2012-07-11 2014-06-18 湖南科技大学 Preparation of single-component alkali-activated cement and application method thereof
CN103508693A (en) * 2013-09-29 2014-01-15 四川利森建材集团有限公司 Cement modifier and production and application method thereof
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Publication number Priority date Publication date Assignee Title
CN114960609A (en) * 2022-04-25 2022-08-30 三明学院 Composite foundation for reinforcing saturated soft soil by single-component geopolymer and construction method thereof
CN115611580A (en) * 2022-10-21 2023-01-17 广西大学 High-strength sound-insulation heat-insulation prefabricated inner partition plate based on papermaking white mud and preparation method thereof

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