CN110218035B - Preparation method of plastic deformation geopolymer material - Google Patents
Preparation method of plastic deformation geopolymer material Download PDFInfo
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- CN110218035B CN110218035B CN201910553396.5A CN201910553396A CN110218035B CN 110218035 B CN110218035 B CN 110218035B CN 201910553396 A CN201910553396 A CN 201910553396A CN 110218035 B CN110218035 B CN 110218035B
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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
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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
- C04B28/006—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 mineral polymers, e.g. geopolymers of the Davidovits type
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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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- 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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- Environmental & Geological Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Consolidation Of Soil By Introduction Of Solidifying Substances Into Soil (AREA)
- Soil Conditioners And Soil-Stabilizing Materials (AREA)
Abstract
The invention discloses a preparation method of a plastically deformable geopolymer material, which is prepared by mixing, casting and molding metakaolin, industrial water glass, sodium silicate nonahydrate and sodium hydroxide according to a certain mass fraction ratio and curing at normal temperature. The preparation process is simple, and the prepared geopolymer material has the characteristics of no toxicity, low cost, early strength, quick hardening, acid and alkali resistance, environmental friendliness and stable performance, can meet the requirement of the geopolymer material in the low-temperature phase-change heat storage field, and is expected to be applied in the phase-change heat storage field.
Description
Technical Field
The invention belongs to the technical field of material engineering, and relates to a preparation method of a plastic deformation geopolymer material.
Background
The Geopolymer (Geopolymer) is prepared by reacting a mixture containing amorphous SiO under strong alkaline or strong acid conditions 2 And Al 2 O 3 The aluminosilicate mineral is mixed with alkali solution, alkaline salt solution or phosphoric acid and phosphate solution, and amorphous three-dimensional network gel formed by silicon-oxygen tetrahedron, aluminum-oxygen tetrahedron or phosphorus-oxygen tetrahedron is generated through polycondensation reaction. The application of geopolymer materials dates back to ancient times, namely, kaolin, dolomite or limestone and salt lake component Na 2 CO 3 And plant ash component K 2 CO 3 And the mixture of silica is added with water and mixed to generate strong alkali NaOH and KOH which react with other components to generate mineral polymerization adhesive to prepare the artificial stone. The material has small volume density (1.3-1.9 g-cm) -3 ) Light weight and high strength; corrosion resistance, hydrothermal resistance, small volume shrinkage, high-temperature thermal stability and durability are good; meanwhile, the method has the advantages of environmental protection and the like. Making it increasingly one of the materials that has been studied internationally in recent years. However, the problems of low bending strength and tensile strength, poor impact strength, high brittleness, easy cracking and the like limit the development and application of the composite material.
Phase change materials are substances that change form with temperature and provide latent heat. Solid-liquid phase change materials are widely used at present, and the process of changing a phase change material from a solid state to a liquid state or from a liquid state to a solid state is called a phase change process, and then the phase change material absorbs or releases a large amount of latent heat. The research at home and abroad shows that the geological polymer has good plasticity when being prepared into a paste shape. Research researchers research the impact deformation characteristics of geopolymer concrete, and the research shows that geopolymer materials such as slag, fly ash and the like are adopted to replace cement to serve as a cementing material, and sodium silicate and sodium hydroxide are used as exciting agents to prepare the geopolymer material which has good deformation performance and can store heat through phase change.
The invention patent (patent number 201711455186. X) discloses a preparation method of a polyvinyl chloride phase change heat storage plate, wherein the heat storage capacity of the phase change heat storage material prepared by the method is improved, but polyvinyl chloride is decomposed under high temperature and open fire to generate toxic gas, so that risks exist in some fields. The patent No. CN201810889301.2 is a preparation method of an organic/inorganic composite energy storage phase change material, the preparation method has certain phase change and heat storage performances, but the material prepared by the method has corrosivity and high cost, which limits the development and application of the material.
Disclosure of Invention
The invention aims to provide a preparation method of a plastic deformation geopolymer material aiming at the defects of corrosivity, pyrolysis, high cost, non-plastic deformation and the like of the existing phase-change heat storage material.
The scheme of the invention is realized by the following steps:
a method for preparing a plastic deformation geopolymer material is mainly prepared by mixing metakaolin, industrial water glass, sodium silicate nonahydrate and sodium hydroxide according to a certain mass ratio, casting and molding, and curing at normal temperature.
As a further illustration of the present invention, the method of preparing the plastically deformable geopolymeric material specifically comprises the steps of:
(a) preparation of a water glass solution: weighing industrial water glass and sodium hydroxide according to the mass ratio of (3.3-3.5): 1, and carrying out ultrasonic stirring and dissolving on the industrial water glass and the sodium hydroxide to prepare a water glass solution with a fixed modulus of 1.0;
(b) preparation of liquid phase L: weighing the water glass solution and the sodium silicate nonahydrate according to the mass ratio of (2.5-4.7): 1, carrying out ultrasonic stirring and mixing on the water glass solution and the sodium silicate nonahydrate for 60min by using a stirrer, and standing for a period of time to obtain a liquid phase L;
(c) the method comprises the following steps of taking metakaolin as a solid phase S, placing the solid phase S and a liquid phase L in a high-speed dispersion machine, and mixing and stirring for 15min under the condition of the rotating speed of 2000r/min to obtain the plastic deformation geopolymer slurry, wherein the mass ratio of the liquid phase L to the solid phase S is about: l is S = 2.95-325.52;
(d) and pouring the plastic deformation geopolymer slurry into a mold, standing for 30min at normal temperature, demolding, and curing to obtain the plastic deformation geopolymer material.
As a further illustration of the invention, the metakaolin is powder obtained by calcining kaolin for 2 hours at 800 ℃, and the metakaolin obtained by calcining comprises the following components in percentage by mass: SiO 2 2 ：52.89%，Al 2 O 3 ：43.50%，K 2 O：1.8%，Fe 2 O 3 : 1.38%, MgO: 0.43 percent; the sodium silicate nonahydrate is a solid particle and is a laboratory analysis pure reagent containing 96% of mass fraction, and the sodium hydroxide is a laboratory analysis pure reagent containing 96% of mass fraction.
As a further explanation of the invention, the specification of the die is 20X 20 mm.
As a further illustration of the invention, the modulus of the industrial water glass is 3.31.
The technical principle of the invention is as follows:
the metakaolin provided by the invention provides a silicon-aluminum source, and the silicon-oxygen bond and the aluminum-oxygen bond of the metakaolin are subjected to fracture-recombination reaction under the action of a water glass solution and then polymerized to generate the geopolymer. Industrial Water in the Material of the inventionThe main component of the glass is sodium silicate, and the molecular formula of the glass is Na 2 SiO 3 . The molecular formula of the sodium silicate nonahydrate is Na 2 SiO 3 ·9H 2 The sodium silicate nonahydrate is a charged carrier, has small molecular weight, is adsorbed on the surface of a substance particle through the actions of charge adsorption, hydrogen bonds, van der waals force and the like, ensures that the surface of the particle generates chemical adsorption characteristics and has the action of serving as an adhesive and a dispersing agent; the prepared geopolymer has the advantages that the components are compatible, the stability of the geopolymer is improved, the melting point of the sodium silicate nonahydrate is about 40-48 ℃, the melting point of the industrial water glass is about 1089 ℃, and the sodium silicate nonahydrate can release crystallization water to become liquid or paste at a lower temperature (such as 30-40 ℃), so that the state of the geopolymer is promoted to change along with the change of the temperature. The geopolymer material can be coagulated and hardened in a short time at normal temperature and has certain compressive strength; after the molding material is left to stand in an environment higher than room temperature (about 60 ℃) for a while, the material becomes soft and a small amount of water is separated out. Such plastically deformable geopolymeric materials can assume different states depending on the temperature variation: the material is a solid substance with a fixed form at room temperature and a substance with a solid-liquid phase coexisting as a mud state at a high temperature, and the two states of the substance can be transformed multiple times according to the transformation of the external environment temperature, thereby having plastic deformation.
The invention has the following good effects:
1. the invention adopts normal temperature casting molding and normal temperature maintenance, and has simple process, no toxicity and no pollution.
2. The alkali-activated active material, the metakaolin, the industrial water glass and other raw materials have wide sources or are industrial waste residues, the cost is low, and the problem of waste utilization can be solved.
3. When the external temperature changes, the shape of the plastic deformation geopolymer material prepared by the invention changes, and the plastic deformation geopolymer material has a certain application prospect in the field of phase change heat storage.
Detailed Description
The process for the preparation of a plastically deformable geopolymeric material according to the invention is described below with reference to the examples, which are not intended to limit the content of the invention further.
(1) The metakaolin in the invention is powder obtained by calcining kaolin for 2 hours at 800 ℃, and the mass percentage content of each chemical component of the metakaolin obtained by calcining is shown in the following table.
(2) In the invention, the sodium silicate nonahydrate is solid particles and is a laboratory analytical reagent containing 96% of mass fraction, and the sodium hydroxide is a laboratory analytical reagent containing 96% of mass fraction.
Example 1:
(a) preparation of a water glass solution: weighing 28.85g of 96% sodium hydroxide by mass per 100g of industrial water glass with the modulus of 3.31, and ultrasonically stirring and dissolving the weighed industrial water glass and the sodium hydroxide to prepare a water glass solution with the fixed modulus of 1.0;
(b) preparation of liquid phase L: weighing 27.40g of sodium silicate nonahydrate per 133.58g of water glass solution, carrying out ultrasonic stirring and mixing on the weighed water glass solution and the sodium silicate nonahydrate by using a stirrer for 60min, and standing for 4 hours to obtain a liquid phase L;
(c) using metakaolin as a solid phase S, weighing 160.98g of liquid phase L and 32.48g of metakaolin solid phase S, placing the solid phase S and the liquid phase L in a high-speed dispersion machine, and mixing and stirring for 15min under the condition of the rotating speed of 2000r/min to obtain the plastic deformation geopolymer slurry;
(d) and pouring the plastic deformation geopolymer slurry into a 20 multiplied by 20mm mould, standing for 30min at normal temperature, demoulding, and curing to obtain the plastic deformation geopolymer material.
The compression strength of the plastic deformation geopolymer material after normal temperature curing is measured to reach 19.75Mpa, and the DSC test result shows that the phase transition temperature of the prepared plastic deformation geopolymer material is 60 ℃.
Example 2:
(a) preparation of a water glass solution: weighing 28.85g of 96% sodium hydroxide by mass per 100g of industrial water glass with the modulus of 3.31, and ultrasonically stirring and dissolving the weighed industrial water glass and the sodium hydroxide to prepare a water glass solution with the fixed modulus of 1.0;
(b) preparation of liquid phase L: weighing 37.40g of sodium silicate nonahydrate according to 128.85g of water glass solution, carrying out ultrasonic stirring and mixing on the weighed water glass solution and the sodium silicate nonahydrate by using a stirrer for 60min, and standing for 4 hours to obtain a liquid phase L;
(c) weighing 166.25g of liquid phase L and 32.48g of metakaolin solid phase S by taking metakaolin as the solid phase S, placing the solid phase S and the liquid phase L in a high-speed dispersion machine, and mixing and stirring for 15min under the condition that the rotating speed is 2000r/min to obtain the plastic deformation geopolymer slurry;
(d) and pouring the plastic deformation geopolymer slurry into a 20 multiplied by 20mm mould, standing for 30min at normal temperature, demoulding, and curing to obtain the plastic deformation geopolymer material.
The compression strength of the plastic deformation geopolymer material after normal temperature curing is measured to reach 22.74Mpa, and the DSC test result shows that the phase transition temperature of the prepared plastic deformation geopolymer material is 66 ℃.
Example 3:
(a) preparation of a water glass solution: weighing 28.85g of 96% sodium hydroxide by mass per 100g of industrial water glass with the modulus of 3.31, and ultrasonically stirring and dissolving the weighed industrial water glass and the sodium hydroxide to prepare a water glass solution with the fixed modulus of 1.0;
(b) preparation of liquid phase L: weighing 27.40g of sodium silicate nonahydrate according to 128.85g of water glass solution, carrying out ultrasonic stirring and mixing on the weighed water glass solution and the sodium silicate nonahydrate by using a stirrer for 60min, and standing for 4 hours to obtain a liquid phase L;
(c) taking metakaolin as a solid phase S, weighing 156.25g of liquid phase L and 34.48g of metakaolin solid phase S, placing the solid phase S and the liquid phase L in a high-speed dispersion machine, and mixing and stirring for 15min under the condition of the rotating speed of 2000r/min to obtain the plastic deformation geopolymer slurry;
(d) and pouring the plastic deformation geopolymer slurry into a 20 multiplied by 20mm mould, standing for 30min at normal temperature, demoulding, and curing to obtain the plastic deformation geopolymer material.
The compression strength of the plastic deformation geopolymer material after normal temperature curing is measured to reach 60.74Mpa, and DSC test results show that the phase transition temperature of the prepared plastic deformation geopolymer material is 63 ℃.
Example 4:
(a) preparation of a water glass solution: weighing 28.85g of 96% sodium hydroxide by mass per 100g of industrial water glass with the modulus of 3.31, and ultrasonically stirring and dissolving the weighed industrial water glass and the sodium hydroxide to prepare a water glass solution with the fixed modulus of 1.0;
(b) preparation of liquid phase L: weighing 27.40g of sodium silicate nonahydrate according to 128.85g of water glass solution, carrying out ultrasonic stirring and mixing on the weighed water glass solution and the sodium silicate nonahydrate by using a stirrer for 60min, and standing for 4 hours to obtain a liquid phase L;
(c) weighing 156.25g of liquid phase L and 0.48g of metakaolin solid phase S by taking metakaolin as the solid phase S, placing the solid phase S and the liquid phase L in a high-speed dispersion machine, and mixing and stirring for 15min under the condition that the rotating speed is 2000r/min to obtain the plastic deformation geopolymer slurry;
(d) and pouring the plastic deformation geopolymer slurry into a mold with the size of 20 multiplied by 20mm, placing for 30min at normal temperature, demolding, and then curing to obtain the plastic deformation geopolymer material.
The compression strength of the plastic deformation geopolymer material after normal temperature curing is measured to reach 0.627Mpa, and DSC test results show that the phase transition temperature of the prepared plastic deformation geopolymer material is 55 ℃.
Example 5:
(a) preparation of a water glass solution: weighing 28.85g of 96% sodium hydroxide by mass per 100g of industrial water glass with the modulus of 3.31, and ultrasonically stirring and dissolving the weighed industrial water glass and the sodium hydroxide to prepare a water glass solution with the fixed modulus of 1.0;
(b) preparation of liquid phase L: weighing 27.40g of sodium silicate nonahydrate according to 68.58g of water glass solution, carrying out ultrasonic stirring and mixing on the weighed water glass solution and the sodium silicate nonahydrate by using a stirrer for 60min, and standing for 4 hours to obtain a liquid phase L;
(c) using metakaolin as a solid phase S, weighing 95.98g of liquid phase L and 32.48g of metakaolin solid phase S, placing the solid phase S and the liquid phase L in a high-speed dispersion machine, and mixing and stirring for 15min under the condition of the rotating speed of 2000r/min to obtain the plastic deformation geopolymer slurry;
(d) and pouring the plastic deformation geopolymer slurry into a 20 multiplied by 20mm mould, standing for 30min at normal temperature, demoulding, and curing to obtain the plastic deformation geopolymer material.
The compression strength of the plastic deformation geopolymer material after normal temperature curing is measured to 50.146Mpa, and the DSC test result shows that the phase transition temperature of the prepared plastic deformation geopolymer material is 70 ℃.
The above-described embodiments of the present invention are intended to be illustrative only and not limiting, and the scope of the invention is indicated in the claims, along with the full range of ingredients, ratios of ingredients, and process parameters of manufacture, and the above description is not intended to be exhaustive of the invention, and thus, any changes that come within the meaning and range of equivalency of the claims are intended to be embraced therein.
Claims (1)
1. A method of preparing a plastically deformable geopolymer material, comprising the steps of:
(a) preparation of a water glass solution: weighing 28.85g of 96% sodium hydroxide by mass per 100g of industrial water glass with the modulus of 3.31, and ultrasonically stirring and dissolving the weighed industrial water glass and the sodium hydroxide to prepare a water glass solution with the fixed modulus of 1.0;
(b) preparation of liquid phase L: weighing 27.40g of sodium silicate nonahydrate per 128.85g of water glass solution, carrying out ultrasonic stirring and mixing on the weighed water glass solution and the sodium silicate nonahydrate by using a stirrer for 60min, and standing for 4 hours to obtain a liquid phase L;
(c) taking metakaolin as a solid phase S, weighing 156.25g of liquid phase L and 34.48g of metakaolin solid phase S, placing the solid phase S and the liquid phase L in a high-speed dispersion machine, and mixing and stirring for 15min under the condition of the rotating speed of 2000r/min to obtain the plastic deformation geopolymer slurry;
(d) pouring the plastic deformation geopolymer slurry into a 20 multiplied by 20mm mould, placing for 30min at normal temperature, demoulding, and then curing to obtain the plastic deformation geopolymer material;
or, the preparation method of the plastically deformable geopolymer material comprises the following steps:
(a) preparation of a water glass solution: weighing 28.85g of 96% sodium hydroxide by mass per 100g of industrial water glass with the modulus of 3.31, and ultrasonically stirring and dissolving the weighed industrial water glass and the sodium hydroxide to prepare a water glass solution with the fixed modulus of 1.0;
(b) preparation of liquid phase L: weighing 27.40g of sodium silicate nonahydrate per 68.58g of water glass solution, carrying out ultrasonic stirring and mixing on the weighed water glass solution and the sodium silicate nonahydrate by using a stirrer for 60min, and standing for 4 hours to obtain a liquid phase L;
(c) using metakaolin as a solid phase S, weighing 95.98g of liquid phase L and 32.48g of metakaolin solid phase S, placing the solid phase S and the liquid phase L in a high-speed dispersion machine, and mixing and stirring for 15min under the condition of the rotating speed of 2000r/min to obtain the plastic deformation geopolymer slurry;
(d) pouring the plastic deformation geopolymer slurry into a 20 multiplied by 20mm mould, placing for 30min at normal temperature, demoulding, and then curing to obtain the plastic deformation geopolymer material;
wherein the metakaolin is powder obtained by calcining kaolin for 2 hours at 800 ℃, and the metakaolin obtained by calcining comprises the following components in percentage by mass: SiO 2 2 ：52.89％，Al 2 O 3 ：43.50％，K 2 O：1.8％，Fe 2 O 3 : 1.38%, MgO: 0.43 percent; the sodium silicate nonahydrate is a solid particle and is a laboratory analysis pure reagent containing 96% of mass fraction, and the sodium hydroxide is a laboratory analysis pure reagent containing 96% of mass fraction.
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