CN112358241A - High-strength fly ash-based porous geopolymer heat-insulating material filled with potassium titanate whiskers and preparation method and application thereof - Google Patents
High-strength fly ash-based porous geopolymer heat-insulating material filled with potassium titanate whiskers and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/006—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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00017—Aspects relating to the protection of the environment
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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
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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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
- 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
Abstract
The invention relates to a high-strength fly ash-based porous geopolymer heat-insulating material filled with potassium titanate whiskers, and a preparation method and application thereof. The material is prepared by taking fly ash, metakaolin, potassium titanate whisker, an alkali activator, a foaming agent, a foam stabilizer and the like as raw materials, mixing powder and solid to obtain slurry, and then performing injection molding, foaming and curing. The potassium titanate whisker is creatively introduced into the porous geopolymer, so that the prepared composite material has both mechanical property and thermal insulation property, and the compressive strength and the thermal conductivity coefficient respectively reach 6.32MPa and 0.042W/m.K. The invention is beneficial to recycling the inorganic solid waste fly ash, has simple whole preparation process, does not need high-temperature sintering and high-temperature maintenance, has lower cost, does not discharge harmful substances in the production process, has good environmental protection advantage, is expected to be popularized and applied as a wall thermal insulation material in a large area, and further improves the energy-saving and environmental protection level of buildings in China.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to a high-strength fly ash-based porous geopolymer heat-insulating material filled with potassium titanate whiskers, and a preparation method and application thereof.
Background
With the increasing world energy consumption and the increasing environmental problems, building energy conservation and environmental protection become the key points of government attention of all countries. Research shows that the building energy consumption accounts for about 30% of the total social energy consumption, and effective realization of building energy conservation is an important way for solving energy crisis and environmental problems. Therefore, the development and popularization of an energy-saving and environment-friendly building material system are imperative.
At present, the wall thermal insulation materials used at home and abroad mainly comprise two main types of traditional inorganic thermal insulation materials and organic synthetic thermal insulation materials. However, the traditional inorganic heat-insulating material has some defects in the aspects of energy consumption, performance stability, process complexity, price and the like; although organic synthetic thermal insulation materials such as polyurethane foam materials, polystyrene boards and the like have certain advantages in the aspect of thermal insulation compared with traditional inorganic materials, the greatest defect is that fire safety hazards exist, and great threat is formed on life, property and social economy. Therefore, developing a novel building thermal insulation material which is safe, environment-friendly, green, energy-saving, simple in process, economical and feasible is a technical problem faced by researchers.
Geopolymers (Geopolymers) were a new type of green gelling material, and their research began in the 70's of the 20 th century. Geopolymers are alumino-silicate geopolymers formed by geochemical combination or artificial imitation of geopolymerization, whose basic structure is a three-dimensional network gel of the polymerization of aluminoxy tetrahedra and siloxy tetrahedra, with both amorphous and semi-crystalline characteristics. The porous geopolymer has great application potential in the aspects of heat insulation materials, noise reduction materials, filtering and adsorbing materials and the like.
Chinese patent CN107344863A discloses a geopolymer porous heat-insulating material based on fly ash and a preparation method thereof, wherein H is adopted in the scheme2O2As blowing agents, but the land produced therefromThe hole distribution of the polymer thermal insulation material is uneven and the strength is low. Chinese patent CN109704663A discloses a method for efficiently preparing a porous geopolymer by using vegetable oil, wherein H accounts for 0.2-15% of the mass fraction of slurry2O2As a foaming agent, one or a mixture of more of vegetable oil such as rapeseed oil, soybean oil, coconut oil, linseed oil, peanut oil, olive oil, sesame oil and corn oil is added into the geopolymer slurry as a foam stabilizer, and the porous geopolymer obtained through curing has a high thermal conductivity coefficient (0.093W/m.k) although the pore distribution is uniform and the pore defects are few. Chinese patent CN106830990A discloses a porous geopolymer/aerogel composite heat-insulating material and a preparation method thereof, wherein SiO is mixed with a solvent to prepare the composite heat-insulating material2The aerogel is embedded into the matrix pores of the porous geopolymer, so that the porous geopolymer/aerogel composite heat-insulating material is prepared. Although the material has good mechanical strength and high temperature resistance, the preparation process is more complex and the cost is higher.
In conclusion, the performance (especially the heat preservation performance) of the existing geopolymer composite material is still to be improved, and the preparation method has many problems.
Disclosure of Invention
The invention aims to overcome the problems in the prior art, and creatively introduces the potassium titanate whisker into the preparation process of the geopolymer, so as to successfully prepare the high-efficiency heat-insulation geopolymer material with high compressive strength, low density and low heat conductivity coefficient on the basis of recycling the solid waste fly ash. The preparation method of the material comprises the following steps: uniformly mixing the fly ash, the metakaolin and the potassium titanate whisker, adding the alkali activator and the foaming agent, uniformly mixing to obtain slurry, and finally injecting, foaming and maintaining the slurry.
Further, the mass ratio of the fly ash, the metakaolin and the potassium titanate whisker is 5.0-7.0:3.0-5.0: 0.1-2.0.
Furthermore, the maximum particle sizes of the fly ash and the metakaolin are not more than 200 meshes.
Further, the potassium titanate whisker is at least one selected from the group consisting of a potassium tetratitanate whisker and a potassium hexatitanate whisker, and preferably a potassium hexatitanate whisker.
Furthermore, the potassium titanate whisker has the diameter of 0.2-0.5 micron and the length of 8-100 micron. The fly ash, the metakaolin and the potassium titanate whisker with reasonable particle size matching not only meet the grading requirement during mixing, but also have better compactness of the prepared geopolymer.
Further, the alkali activator is prepared by mixing and standing sodium hydroxide or potassium hydroxide and at least one of sodium silicate solution and potassium silicate solution, and the modulus of the alkali activator is between 1.2 and 1.8.
Furthermore, the mass ratio of the total mass of the fly ash, the metakaolin and the potassium titanate whisker to the alkali activator is 1.0: 0.5-0.9.
Further, the foaming agent is selected from H2O2At least one of trimethyl hexadecyl ammonium bromide, lauryl sodium sulfate, aluminum powder, sodium tetraborate and urea, preferably H2O2。
Furthermore, the mass fraction of the foaming agent in the slurry is 1.0-15.0%.
Further, a foam stabilizer is added into the slurry, and the foam stabilizer is selected from at least one of sodium dodecyl benzene sulfonate, stearic acid, olive oil, hydroxyethyl cellulose and sodium polyacrylate.
Furthermore, the mass fraction of the foam stabilizer in the slurry is 0.5% -10.0%.
Further, the stirring speed during the mixing preparation of the slurry was 200-800rpm, and the stirring time was not more than 30 minutes.
Furthermore, the stirring is carried out in two times, the stirring is not more than 20min after the alkali activator is added, and the stirring is continued for not more than 10min after the foaming agent and the foam stabilizer are added.
Further, the curing conditions are as follows: curing in a constant temperature and humidity box with the temperature of 25-40 ℃ and the humidity of 95% for 24-72h, demolding, and curing for 4-7 days under the same conditions.
The invention also aims to provide a high-strength fly ash-based porous geopolymer heat-insulating material filled with potassium titanate whiskers, which is prepared by the method, has the compressive strength of 6.32MPa and the heat conductivity coefficient of 0.042W/m.K.
The third purpose of the invention is to apply the high-strength fly ash-based porous geopolymer heat-insulating material filled with the potassium titanate whiskers as a wall heat-insulating material.
The fly ash is a byproduct in the production process of coal-fired thermal power plants or similar coal-fired equipment, and is one of main solid wastes in China. The yield of the fly ash is increased year by year, and if the fly ash is not treated well, the fly ash can have great influence on human health and natural environment. The method takes the fly ash as the main raw material, has larger demand for the fly ash after popularization and application, is beneficial to changing waste into valuable and recycling, and has great significance in the aspects of environmental protection and solid waste disposal.
The potassium titanate whisker has excellent mechanical property and physical property, stable chemical property, excellent heat resistance and corrosion resistance, extremely low thermal conductivity (0.00534W/m.k), high infrared reflectivity and the like, and has important application value in heat insulation materials. Before the application, potassium titanate whiskers are usually mixed with silica aerogel, yttria gel, nano silicon nitride and the like to prepare a coating used as a high-temperature-resistant coating of a fireproof building material (such as Chinese patent CN107954745A), and no report related to a geopolymer heat-insulating material based on potassium titanate whiskers is found at present.
Compared with the prior art, the invention has the following unexpected beneficial effects: (1) the invention creatively introduces the reinforcing filler potassium titanate whisker with extremely low heat conductivity coefficient into the porous geopolymer heat-insulating material, and gives consideration to the mechanical property and the heat-insulating property of the material; (2) compared with polystyrene series organic heat-insulating materials, the porous geopolymer heat-insulating material provided by the invention has higher mechanical strength, and the compressive strength of the porous geopolymer heat-insulating material can reach 6.32 MPa; (3) the porous geopolymer thermal insulation material provided by the invention has a very low thermal conductivity coefficient (0.042W/m.K) and a very outstanding thermal insulation effect; (4) the invention takes the inorganic solid waste fly ash as the main matrix raw material, the target product has good fireproof performance and simple preparation process, and high-temperature sintering and high-temperature maintenance are not needed, so the production and use cost is lower, in addition, no harmful substance is discharged in the production process, and the invention has good environmental protection advantage.
Drawings
FIG. 1 is a process flow diagram of the method of the present invention.
FIG. 2 is an SEM photograph of the product obtained in example 1.
FIG. 3 is an SEM photograph of the product obtained in example 2.
FIG. 4 is an SEM photograph of the product obtained in example 3.
FIG. 5 is an SEM photograph of the product obtained in example 4.
Detailed Description
In order to make those skilled in the art fully understand the technical solutions and advantages of the present invention, the following description is further provided with reference to the specific embodiments and the accompanying drawings.
Example 1
The first step is as follows: and (3) respectively sieving the fly ash and the metakaolin through a 200-mesh sieve to obtain corresponding solid powder raw materials. Weighing fly ash, metakaolin and potassium hexatitanate whiskers (the diameter is 0.2 micrometer and the length is 20 micrometers) according to the mass ratio of 5.0:3.0:0.1, respectively, adding the fly ash, the metakaolin and the potassium hexatitanate whiskers into a mechanical stirrer, and stirring for 15min to obtain a mixture;
the second step is that: adjusting the modulus of the sodium silicate solution of the water glass to 1.2 by using sodium hydroxide solid powder to obtain an alkali activator, and standing for 24 hours for later use;
the third step: adding the alkali activator solution prepared in the second step and the mixture prepared in the first step into a mechanical stirrer according to the mass ratio of 0.5:1.0, and stirring and mixing for 5min at the rotating speed of 800rpm to obtain geopolymer slurry; then adding foam stabilizer sodium dodecyl benzene sulfonate and foaming agent H2O2Continuously stirring the solution for 2min to obtain geopolymer mixed foaming slurry; wherein the mass fractions of the foam stabilizer and the foaming agent in the foaming slurry are 0.5 percent and 1.0 percent respectively;
the fourth step: and (3) injecting the geopolymer foamed slurry prepared in the third step into a 40mm multiplied by 160mm mould, putting the mould into a constant temperature and humidity box with the temperature of 25 ℃ and the humidity of 95% for curing for 72 hours, and continuing curing for 4 days under the conditions after demoulding to obtain the porous geopolymer heat-insulating material product.
The preparation process of the porous geopolymer thermal insulation material product is shown in figure 1, and the micro-pore structure of the final product is shown in figure 2. Figure 2 shows that the geopolymer pores are uniformly distributed with few cracks. The test results of mechanical properties and heat conductivity show that the compressive strength of the porous geopolymer heat-insulating material is 6.02MPa, and the heat conductivity coefficient is 0.045W/m.K.
Example 2
The first step is as follows: and (3) respectively sieving the fly ash and the metakaolin through a 200-mesh sieve to obtain corresponding solid powder raw materials. Weighing fly ash, metakaolin and potassium tetratitanate whiskers (the diameter is 0.3 micron and the length is 30 microns) according to the mass ratio of 6.0:4.0:0.5, respectively, adding the fly ash, the metakaolin and the potassium tetratitanate whiskers into a mechanical stirrer, and stirring for 15min to obtain a mixture;
the second step is that: adjusting the modulus of the potassium silicate solution to 1.4 by using potassium hydroxide solid powder to obtain an alkali activator, and standing for 24 hours for later use;
the third step: adding the alkali activator solution prepared in the second step and the mixture prepared in the first step into a mechanical stirrer according to the mass ratio of 0.7:1.0, and stirring and mixing for 10min at the rotating speed of 600rpm to obtain geopolymer slurry; then adding a composite foam stabilizer of sodium dodecyl benzene sulfonate/hydroxyethyl cellulose (the mass ratio is 1:1) and a foaming agent H2O2Continuously stirring the solution for 5min to obtain geopolymer mixed foaming slurry; wherein the mass fractions of the foam stabilizer and the foaming agent in the foaming slurry are respectively 2.0% and 5.0%;
the fourth step: and (3) injecting the geopolymer foamed slurry prepared in the third step into a mould with the thickness of 40mm multiplied by 160mm, putting the mould into a constant-temperature constant-humidity box with the temperature of 30 ℃ and the humidity of 95% for curing for 48 hours, and continuing curing for 5 days under the conditions after demoulding to obtain the porous geopolymer heat-insulating material product.
The micro-pore structure of the porous geopolymer insulation product is shown in figure 3. Also, figure 3 shows that the geopolymer pores are uniformly distributed with few cracks. The test results of mechanical properties and heat conductivity show that the compressive strength of the porous geopolymer heat-insulating material product is 6.11MPa, and the heat conductivity coefficient is 0.044W/m.K.
Example 3
The first step is as follows: and (3) respectively sieving the fly ash and the metakaolin through a 200-mesh sieve to obtain corresponding solid powder raw materials. Weighing fly ash, metakaolin and potassium hexatitanate whiskers (the diameter is 0.4 micron and the length is 40 microns) according to the mass ratio of 6.5:4.5:1.0, respectively, adding the fly ash, the metakaolin and the potassium hexatitanate whiskers into a mechanical stirrer, and stirring for 15min to obtain a mixture;
the second step is that: adjusting the modulus of the sodium silicate solution of the water glass to 1.6 by using sodium hydroxide solid powder to obtain an alkali activator, and standing for 24 hours for later use;
the third step: adding the alkali activator solution prepared in the second step and the mixture raw material prepared in the first step into a mechanical stirrer according to the mass ratio of 0.8:1.0, and stirring and mixing for 15min at the rotating speed of 400rpm to obtain geopolymer slurry; then adding the foam stabilizer olive oil and the foaming agent H2O2Continuously stirring the solution for 8min to obtain geopolymer mixed foaming slurry; wherein the mass fractions of the foam stabilizer and the foaming agent in the foaming slurry are 5.0 percent and 10.0 percent respectively;
the fourth step: and (3) injecting the geopolymer foamed slurry prepared in the third step into a mould with the thickness of 40mm multiplied by 160mm, putting the mould into a constant-temperature constant-humidity box with the temperature of 30 ℃ and the humidity of 95% for curing for 48 hours, and continuing curing for 5 days under the conditions after demoulding to obtain the porous geopolymer heat-insulating material product.
The micro-pore structure of the porous geopolymer insulation product is shown in figure 4. Figure 4 shows that the geopolymer pores are uniformly distributed and have no crack phenomenon. The test results of mechanical properties and heat conductivity show that the compressive strength of the porous geopolymer heat-insulating material product is 6.32MPa, and the heat conductivity coefficient is 0.042W/m.K.
Example 4
The first step is as follows: and (3) respectively sieving the fly ash and the metakaolin through a 200-mesh sieve to obtain corresponding solid powder raw materials. Weighing fly ash, metakaolin and potassium tetratitanate whiskers (the diameter is 0.5 micron and the length is 60 microns) according to the mass ratio of 7.0:5.0:1.5, respectively, adding into a mechanical stirrer, and stirring for 15min to obtain a mixture;
the second step is that: adjusting the modulus of the potassium silicate solution to 1.8 by using potassium hydroxide solid powder to obtain an alkali activator, and standing for 24 hours for later use;
the third step: adding the alkali activator solution prepared in the second step and the mixture raw material prepared in the first step into a mechanical stirrer according to the mass ratio of 0.9:1.0, and stirring and mixing for 20min at the rotating speed of 200rpm to obtain geopolymer slurry; then adding foam stabilizer sodium polyacrylate and foaming agent H2O2Continuously stirring the solution for 10min to obtain geopolymer mixed foaming slurry; wherein the mass fractions of the foam stabilizer and the foaming agent in the foaming slurry are respectively 8.0% and 15.0%;
the fourth step: and (3) injecting the geopolymer foamed slurry prepared in the third step into a mould with the size of 40mm multiplied by 160mm, putting the mould into a constant-temperature constant-humidity box with the temperature of 40 ℃ and the humidity of 95%, maintaining for 24 hours, demolding, and continuing to maintain for 4 days under the conditions to obtain the porous geopolymer heat-insulating material product.
The micro-pore structure of the porous geopolymer insulation product is shown in figure 5. Figure 5 shows that the geopolymer pores are uniformly distributed and that cracking is less likely to occur. The test results of mechanical properties and heat conductivity show that the compressive strength of the porous geopolymer heat-insulating material product is 6.30MPa, and the heat conductivity coefficient is 0.042W/m.K.
Claims (10)
1. A preparation method of a high-strength fly ash-based porous geopolymer heat-insulating material filled with potassium titanate whiskers is characterized by comprising the following steps: the method comprises the following steps: uniformly mixing the fly ash, the metakaolin and the potassium titanate whisker, adding the alkali activator and the foaming agent, uniformly mixing to obtain slurry, and finally injecting, foaming and maintaining the slurry.
2. The method of claim 1, wherein: the mass ratio of the fly ash to the metakaolin to the potassium titanate whisker is 5.0-7.0:3.0-5.0:0.1-2.0, and the maximum particle size of the fly ash to the metakaolin is not more than 200 meshes; the potassium titanate whisker is selected from at least one of potassium tetratitanate whisker and potassium hexatitanate whisker, the diameter of the potassium titanate whisker is 0.2-0.5 micrometer, and the length of the potassium titanate whisker is 8-100 micrometers.
3. The method of claim 1, wherein: the alkali activator is prepared by mixing and standing sodium hydroxide or potassium hydroxide and at least one of sodium silicate solution and potassium silicate solution, and the modulus of the alkali activator is between 1.2 and 1.8.
4. The method of claim 1, wherein: the mass ratio of the total mass of the fly ash, the metakaolin and the potassium titanate whisker to the alkali activator is 1.0: 0.5-0.9.
5. The method of claim 1, wherein: the blowing agent is selected from H2O2At least one of trimethyl hexadecyl ammonium bromide, lauryl sodium sulfate, aluminum powder, sodium tetraborate and urea, wherein the mass fraction of the foaming agent in the slurry is 1.0-15.0%.
6. The method of claim 1, wherein: the slurry is also added with a foam stabilizer, the foam stabilizer is selected from at least one of sodium dodecyl benzene sulfonate, stearic acid, olive oil, hydroxyethyl cellulose and sodium polyacrylate, and the mass fraction of the foam stabilizer in the slurry is 0.5-10.0%.
7. The method of claim 1, wherein: the stirring speed in the process of mixing and preparing the slurry is 200-800rpm, and the stirring time is not more than 30 minutes; the curing conditions are as follows: curing in a constant temperature and humidity box with 25-40 deg.C and 95% humidity for 24-72h, demolding, and curing under the same conditions for 4-7 days.
8. The method of claim 1, wherein: stirring is carried out twice, stirring is carried out for no more than 20min after the alkali activator is added, and stirring is continued for no more than 10min after the foaming agent and the foam stabilizer are added.
9. A high strength fly ash based porous geopolymer thermal insulation material filled with potassium titanate whiskers, characterized in that the thermal insulation material is prepared according to any one of the methods of claims 1-8.
10. Use of a high strength fly ash based porous geopolymer thermal insulation material filled with potassium titanate whiskers as claimed in claim 9 as a wall insulation material.
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| CN116375493A (en) * | 2023-03-21 | 2023-07-04 | 长沙理工大学 | Method for preparing foaming geopolymer from waste incineration fly ash |
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