CN114262179A - Mullite fiber reinforced geopolymer composite material and preparation method and application thereof - Google Patents

Mullite fiber reinforced geopolymer composite material and preparation method and application thereof Download PDF

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CN114262179A
CN114262179A CN202111555476.8A CN202111555476A CN114262179A CN 114262179 A CN114262179 A CN 114262179A CN 202111555476 A CN202111555476 A CN 202111555476A CN 114262179 A CN114262179 A CN 114262179A
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mullite fiber
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CN114262179B (en
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乐恢榕
韦庆昕
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Tsinghua University
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Abstract

The invention relates to the technical field of fiber-reinforced geopolymer composite materials, in particular to a mullite fiber-reinforced phosphoric acid-excited geopolymer composite material and a preparation method and application thereof. The acid-excited geopolymer composite material provided by the invention contains a mullite fiber reinforced phase structure. According to the invention, the mullite fiber is selected to be uniformly doped into the geopolymer material, so that the formed reinforcing phase can obviously improve the mechanical property of the acid-excited geopolymer material and reduce the high-temperature shrinkage rate of the acid-excited geopolymer material. Research shows that the compressive strength of the geopolymer added with 10% of mullite fiber can reach 26.1MPa (mean value) in 7 days, and the bending strength of the geopolymer reaches 10.4MPa in 7 days; geopolymer samples with 20% fiber added have a line shrinkage as low as 3.13% after 1 hour of 1350 degrees treatment. Meanwhile, the invention has the advantages of less raw material components, lower cost and simple process, and is expected to be applied to the fields of structural materials, building materials, refractory materials, solid waste and solid nuclear materials, antibacterial filter materials and the like.

Description

Mullite fiber reinforced geopolymer composite material and preparation method and application thereof
Technical Field
The invention relates to the technical field of fiber-reinforced geopolymer composite materials, in particular to a mullite fiber-reinforced phosphoric acid-excited geopolymer composite material and a preparation method and application thereof.
Background
Geopolymer materials are generally classified into base-activated geopolymer materials and acid-activated geopolymer materials.
Compared with the acid-excited geopolymer material, the alkali-excited geopolymer material has higher curing speed and can greatly shorten the construction time, so that the alkali-excited geopolymer material is mainly used in the current industry. However, the alkali activator introduces alkali metal elements to form a glass phase at a high temperature, so that the alkali-activated geopolymer material has poor temperature resistance, and the use environment temperature is not more than 800 ℃, so that the alkali-activated geopolymer material cannot be applied to an application scene with high temperature requirement.
Compared with the alkali-activated geopolymer material, the acid-activated geopolymer material has better high-temperature resistance. CN101560071A discloses a phosphoric acid-activated geopolymer material, which can resist high temperature of 1300 ℃ and can be used for the preparation of ceramic filter elements. However, the composite material is of a porous structure, the compressive strength of the composite material is between 2 and 15MPa, and the strength of the composite material is low, so that more application scenes of the composite material are limited.
Disclosure of Invention
In order to solve the above technical problems, the present invention provides a fiber-reinforced geopolymer composite material. The composite material belongs to an acid-excited geopolymer material, has high-temperature resistance and excellent mechanical properties; compared with the existing phosphate-based geopolymer material, the phosphate-based geopolymer material has higher temperature resistance and higher bending strength, thereby overcoming the problems of high brittleness and easy generation of cracks of the existing phosphate-excited geopolymer material and expanding the application scene of the phosphate-excited geopolymer material. In addition, the geopolymer composite material provided by the invention has the advantages of fewer components, lower cost and simpler preparation process.
In a first aspect, the present invention provides an acid-activated geopolymer composite having a mullite fiber reinforcement phase structure.
The research of the invention finds that the mechanical properties of the composite material, including compressive strength and bending strength, can be remarkably improved by introducing the fiber reinforced phase into the existing acid-excited geopolymer material; however, the existing fiber types are very large, such as natural fibers, such as hemp, cotton, coconut fibers, animal hair, basalt fibers, or synthetic fibers, such as nylon fibers, steel fibers, alumina fibers, glass fibers, etc.; in the research and exploration of the invention, the natural plant fibers have limited reinforcing effect on the matrix, and part of the natural fibers have negative influence on the solidification of the geopolymer and have lower strength; although the glass fiber, the steel fiber and the basalt fiber play a good reinforcing role, the enduring temperature cannot exceed 1500 ℃; while pure alumina fiber and silicon carbide fiber with melting points over 2000 ℃ have excellent heat resistance, but the cost is too high, the use on a large scale is not facilitated, the melting points of the pure alumina fiber and the silicon carbide fiber are far greater than that of geopolymer, and the high-temperature performance is redundant. After a large number of screens, the invention finally determines that the mullite fiber is taken as the reinforcing phase fiber, the melting point of the mullite fiber is about 1850 ℃, the strength can be still maintained at 1600 ℃, the cost is relatively low, and the mullite fiber becomes a more optimal choice.
The solidification process of the geopolymer is similar to the polymerization process of a high molecular material, and finally, a three-dimensional grid porous structure similar to zeolite is formed, and the main component of the geopolymer is similar to mullite fiber and Al2O3And SiO2. Because the components are similar, the fiber has good affinity with the surface of the matrix, the binding force is enhanced, and the mechanical property is improved. In the high-temperature treatment process, because the shrinkage rate of the fibers is lower than that of the matrix, the shrinkage of the matrix is hindered, and the overall shrinkage rate is reduced.
Further, the mullite fiber is preferably the mullite fiber with the diameter of 3-5 μm, the length of less than 2mm and the weight percentage of alumina of 70-80%. Researches show that compared with mullite fibers of other specifications, the mullite fibers meeting the specification conditions have better dispersibility and affinity in a phosphate group geopolymer material system, and are further favorable for improving the mechanical property and the temperature resistance of the composite material.
Further, the acid-activated geopolymer composite material is prepared from geopolymer slurry containing mullite fibers and metakaolin. The invention discovers that the short-cut fibers are difficult to disperse in the geopolymer and have more defects in the preparation process of the slurry, and the mechanical property of the prepared composite material is reduced to some extent. To this end, the present invention proposes to overcome this problem by controlling the proportional relationship between the two. Research shows that the mass ratio of the mullite fiber to the metakaolin is controlled to be (5-20): 100, the obtained composite material has higher fiber dispersibility, so that the mechanical property of the composite material is improved; tests have shown that a geopolymer with a fibre addition of 10% has a higher strength, whereas a geopolymer with a fibre addition of 20% has a higher and lower heat shrinkage.
The metakaolin is powder obtained by calcining kaolin crude ore powder in air at the temperature of 600-900 ℃ for 2 hours. Preferably, the kaolin has a mesh number of more than 200 meshes and a specific surface area of 300-500m2The kaolin crude ore powder is/Kg. Further preferably, the calcination temperature is 850 ℃. The research of the invention finds that the kaolin with the mesh number and the specific surface area range has better fluidity, and the metakaolin obtained after calcination has higher reaction activity and can further improve the strength of the composite material.
Further, the geopolymer slurry also contains an acid activator; the acid activator can be phosphoric acid, hydrochloric acid, sulfuric acid, etc. Phosphoric acid is preferred in the present invention in view of the operability under laboratory conditions.
Further research of the invention finds that the mechanical property and temperature resistance of the acid-excited geopolymer composite material are also related to the dosage of the phosphoric acid excitant; h3PO4When the relative proportion is too low, the polymerization cannot be sufficiently carried out, but H3PO4Too high a proportion will reduce the strength of the composite; to this end, the invention proposes to control Al in the system2O3And H3PO4In a molar ratio of 1: (1-1.3), the function of regulating and controlling the chain structure strength of the geopolymer can be achieved by regulating the proportional relation between Al and P, and the purpose of regulating and controlling the strength and the high temperature resistance of the geopolymer is further achieved.
As one of the specific embodiments of the present invention, the acid-activated geopolymer composite material is prepared from raw materials containing the following mass proportions;
the feedstock comprises a solid phase and a liquid phase;
preferably, the mass ratio of the solid phase to the liquid phase is 1: 1;
in the solid phase, by mass, 5-20 parts of mullite fiber and 100 parts of kaolin are added;
45-54 parts of 85% phosphoric acid and 55-46 parts of water by mass in the liquid phase.
The research of the invention shows that the acid-excited geopolymer composite material prepared by the raw materials according to the specific proportion has the average compressive strength of 19.8-26.1MPa after being cured for 7 days, has the average bending strength of 7.86-10.4MPa after being cured for 7 days, and has the linear shrinkage rate of 3.13-5.34 percent after being baked for 1 hour at 1350 ℃. In specific implementation, different compressive strengths, bending strengths and linear shrinkage rates can be obtained by adjusting the dosage relationship of the mullite fiber, the kaolin and the acid excitant, so that different application requirements are met.
In a second aspect, the present invention also provides a method for preparing the above acid-activated geopolymer composite material, comprising: pouring geopolymer slurry containing mullite fiber, metakaolin and an acid excitant into a mould for curing; and (6) demolding.
Research shows that the acid-excited geopolymer composite material with high mechanical property and temperature resistance can be obtained by maintaining and demolding the slurry containing the components.
Further, the geopolymer slurry is obtained by mixing a liquid phase and a solid phase; the solid phase can be obtained by the following method: the slurry containing mullite fiber and kaolin is filtered, dried, ball-milled and calcined in high-temperature air to form the mullite fiber/kaolin composite material.
Preferably, in the slurry stirring process, the slurry should be stirred in the same direction as much as possible, so that the clustered mullite fibers are dispersed and the directions are as consistent as possible, which is more beneficial to improving the mechanical property and the high temperature resistance of the composite material.
Preferably, in the preparation of the slurry, mullite fiber is added into water, and after the mullite fiber is stirred uniformly, kaolin is added; the dispersion degree of the mullite fiber in the system is improved by controlling the adding sequence of the raw materials.
Preferably, the ball milling conditions adopted by the invention are low-speed ball milling and high-speed ball milling; the specific implementation conditions are as follows: firstly, ball-milling at the rotating speed of 140-; for example, the ball milling is carried out at a rotation speed of 150r/min for 10 minutes and then at a rotation speed of 300r/min for 10 minutes. In the past, the ball milling treatment is usually carried out at high speed from the beginning, so that filter cakes which are not broken up are easily pressed onto the outer wall of a ball milling pot. The invention adopts low-speed ball milling to break the filter cake, and then high-speed ball milling to ensure that the powder is more fully mixed with water; meanwhile, the ball milling time is controlled not to be too long, so that the strength reduction of the composite material caused by too high mesh number is avoided.
Preferably, the calcination temperature is 600-900 ℃, preferably 850 ℃ and the time is 1.5-2 h. The mullite fiber reinforced phosphoric acid excited geopolymer composite material can be prepared at a lower calcining temperature, and compared with the conventional similar product sintered at a high temperature, the mullite fiber reinforced phosphoric acid excited geopolymer composite material greatly reduces the production energy consumption.
Preferably, the curing conditions are: standing at room temperature for 24h, and maintaining at 50-90 deg.C for 8-24 h.
Further, after the mold release, the material was left to stand at room temperature and humidity of 80% or more for 7 to 28 days.
As one embodiment of the present invention, the method for preparing the acid-activated geopolymer composite material comprises the following steps:
(1) liquid phase raw material preparation
Uniformly mixing phosphoric acid and water in the liquid phase formula according to a proportion for later use;
(2) preparation of solid phase starting materials
Step 1: mixing mullite fibers into water, and stirring along the same direction to disperse the clustered mullite fibers and make the directions of the clustered mullite fibers consistent as much as possible to obtain slurry 1;
step 2: gradually adding kaolin into the slurry 1 which is kept to be stirred, and continuously stirring to obtain a slurry 2;
and step 3: filtering the slurry 2, and drying the obtained filter cake;
and 4, step 4: carrying out low-speed ball milling on the obtained filter cake, and then carrying out high-speed ball milling to obtain mixture powder of kaolin and mullite fiber which are uniformly mixed;
and 5: roasting the obtained mixture powder to obtain mixed powder containing mullite fiber and metakaolin;
(3) uniformly mixing the obtained liquid phase and solid phase components to obtain geopolymer slurry;
(4) pouring the geopolymer slurry into a mould, sealing, and vibrating on a vibrating table/a shaking table for 1 hour to remove bubbles; standing at room temperature for 24h, and maintaining at 50-90 deg.C for 8-24 h; taking out, demoulding, and standing for 7-28 days at room temperature and at a humidity of more than 80% to obtain the fiber reinforced geopolymer material.
In a third aspect, the invention also provides application of the acid-excited geopolymer composite material in the fields of structural materials, building materials, refractory materials, solid-waste solid-core materials, antibacterial filter materials and the like.
Compared with the prior art, the invention has the following advantages:
1. the phosphate mullite fiber reinforced geopolymer composite material provided by the invention has higher temperature resistance and mechanical property; the mechanical property of the phosphate-based geopolymer material reaches or is superior to that of a concrete material, the mean value of compressive strength of the phosphate-based geopolymer material after curing for 7 days is 19.8-26.1MPa, the mean value of bending strength of the phosphate-based geopolymer material after curing for 7.86-10.4MPa, and the linear shrinkage rate of the phosphate-based geopolymer material after baking for 1h at 1350 ℃ is as low as 3.13-5.34%, so that the defects of high brittleness and easiness in cracking of the conventional phosphate-based geopolymer material are overcome, and the application scene of the phosphate-based geopolymer material is further expanded.
2. Compared with the existing similar products, the phosphoric acid excited mullite fiber reinforced geopolymer composite material provided by the invention has fewer components, lower cost, simpler preparation process, lower preparation temperature and less energy consumption, thereby being more beneficial to industrial production and construction use.
3. The phosphate mullite fiber reinforced geopolymer composite material provided by the invention is expected to be applied to the fields of structural materials, refractory materials, solid-waste solid-core materials, antibacterial filtering materials and the like
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Each of the components in the following examples is commercially available.
In the following examples, the test data were obtained by a mechanical property tester and a high temperature sintering furnace, and each set of data was averaged with three samples.
Example 1
The embodiment provides a preparation method of a phosphate mullite fiber reinforced geopolymer composite material, which comprises the following steps:
(1) preparing a liquid-phase raw material:
uniformly mixing 50 parts of industrial phosphoric acid with the mass fraction of 85% and 50 parts of water for later use;
(2) preparation of solid phase raw materials:
step 1: mixing 5 parts of mullite fiber into 200 parts of water, and stirring for 30min along the same direction to disperse the clustered mullite fiber and make the directions of the mullite fiber consistent as much as possible to obtain slurry 1;
the diameter of the mullite fiber is 4 mu m, the length of the mullite fiber is 1.5mm, and the content of alumina is 75 percent;
step 2: gradually adding 100 parts of kaolin into the slurry 1 which is kept to be stirred, and continuously stirring for 30min to obtain uniform slurry 2;
and step 3: filtering the slurry 2 to obtain a filter cake, and drying the filter cake;
and 4, step 4: ball-milling the obtained filter cake for 10min at the rotating speed of 150r/min, and then ball-milling for 10min at the rotating speed of 300r/min to obtain mixture powder of kaolin and mullite fiber which are uniformly mixed;
and 5: roasting the obtained mixture powder at 850 ℃ for 2h to obtain mixed powder containing mullite fiber and metakaolin for later use;
(3) mixing the liquid phase and the solid phase components obtained in the steps (1) and (2), and putting the mixture into a stirrer to stir for 30min to obtain uniform geopolymer slurry;
(4) pouring the slurry obtained in the step (3) into a mould, sealing, and vibrating on a vibrating table/a shaking table for 1h to remove bubbles; standing at room temperature for 24h, and curing in a constant temperature box at 60 ℃ for 24 h; and taking out, demolding, and standing for 7 days at room temperature and at the humidity of more than 80% to obtain the mullite fiber reinforced geopolymer composite material.
Tests prove that the average value of the compressive strength of the mullite fiber reinforced geopolymer composite material after being cured for 7 days is 19.8MPa, the average value of the bending strength of the mullite fiber reinforced geopolymer composite material after being cured for 7 days is 7.86MPa, and the linear shrinkage rate of the mullite fiber reinforced geopolymer composite material after being baked for 1 hour at 1350 ℃ is 5.34 percent.
Example 2
The embodiment provides a preparation method of a phosphate mullite fiber reinforced geopolymer composite material, which comprises the following steps:
(1) liquid phase raw material preparation
Uniformly mixing 50 parts of industrial phosphoric acid with the mass fraction of 85% and 50 parts of water for later use;
(2) preparation of solid phase starting materials
Step 1: mixing 20 parts of mullite fiber into 200 parts of water, and stirring for 30min along the same direction to disperse the clustered mullite fiber and make the directions of the mullite fiber consistent as much as possible to obtain slurry 1;
the diameter of the mullite fiber is 4 mu m, the length of the mullite fiber is 1.5mm, and the content of alumina is 75 percent;
step 2: gradually adding 100 parts of kaolin into the slurry 1 which is kept to be stirred, and continuously stirring for 30min to obtain uniform slurry 2;
and step 3: filtering the slurry 2 to obtain a filter cake; drying the filter cake;
and 4, step 4: ball-milling the obtained filter cake for 10min at the rotating speed of 150r/min, and then ball-milling for 10min at the rotating speed of 300r/min to obtain mixture powder of kaolin and mullite fiber which are uniformly mixed;
and 5: roasting the obtained mixture powder at 850 ℃ for 2h to obtain mixed powder containing mullite fiber and metakaolin for later use;
(3) mixing the liquid phase and the solid phase components obtained in the steps (1) and (2), and putting the mixture into a stirrer to stir for 30min to obtain uniform geopolymer slurry;
(4) pouring the slurry obtained in the step (3) into a mould, sealing, and vibrating on a vibrating table/a shaking table for 1 hour to remove bubbles; standing at room temperature for 24h, and curing in a constant temperature box at 60 ℃ for 24 h; and taking out, demolding, and standing for 7 days at room temperature and at the humidity of more than 80% to obtain the mullite fiber reinforced geopolymer composite material.
Tests prove that the average value of the compressive strength of the mullite fiber reinforced geopolymer composite material after being cured for 7 days is 23.0MPa, the average value of the bending strength of the mullite fiber reinforced geopolymer composite material after being cured for 7 days is 9.76MPa, and the linear shrinkage rate of the mullite fiber reinforced geopolymer composite material after being baked for 1 hour at 1350 ℃ is 3.13 percent.
Example 3
The present example provides a preparation method of a phosphate-based mullite fiber reinforced geopolymer composite, which is different from example 1 in that the amount of the mullite fiber is 10 parts.
The results show that: the average compressive strength of the obtained mullite fiber reinforced geopolymer composite material after being cured for 7 days is 26.1MPa, the average bending strength of the mullite fiber reinforced geopolymer composite material after being cured for 7 days is 10.36MPa, and the linear shrinkage rate of the mullite fiber reinforced geopolymer composite material after being baked for 1 hour at 1350 ℃ is 5.01 percent.
From the performance test results of the composite materials obtained in the above examples 1 to 3, it can be seen that the geopolymer with 10% mullite fiber added has the best mechanical properties, while the mechanical properties with 20% mullite fiber added are reduced, but the geopolymer has a lower high-temperature shrinkage rate.
Comparative example 1
This comparative example provides a phosphate-based mullite fiber reinforced geopolymer composite that differs from example 1 only in that: the fiber reinforced phase is basalt fiber, the addition amount is 10 percent, and the melting point is 1250 ℃.
The results show that the acid-excited geopolymer composite material has an average compressive strength of 25.7MPa after curing for 7 days and a bending strength of 8.33MPa after curing for 7 days, and the basalt fibers are melted after being roasted for 1h at 1350 ℃ and lose the reinforcing effect, so that more cavities in the geopolymer sample are left, and the performance is reduced.
Therefore, compared with the mullite fiber, the basalt fiber can play a certain role in enhancing at normal temperature, but has insufficient high-temperature performance compared with the mullite fiber.
Comparative example 2
This comparative example provides a phosphoric acid-activated geopolymer composite differing from example 1 only in that: the usage amount of the mullite fiber is 0 part.
The results show that the acid-excited geopolymer composite material has an average compressive strength of 18.3MPa after curing for 7 days, an average bending strength of 7.79MPa after curing for 7 days, and a linear shrinkage rate of 5.63% after baking for 1 hour at 1350 ℃.
Therefore, the mechanical property of the acid-excited geopolymer composite material without the mullite fiber is reduced, and the high-temperature shrinkage rate is increased.
Comparative example 3
This comparative example provides a phosphate-based mullite fiber reinforced geopolymer composite that differs from example 2 only in that: in the preparation process, 20 parts of mullite fiber is directly added into the solid phase powder, and then ball milling is carried out.
The results show that the acid-excited geopolymer composite material has an average compressive strength of 20.5MPa after being cured for 7 days and an average bending strength of 6.01MPa after being cured for 7 days.
It can be seen that, in the case of directly adding the fibers without taking appropriate dispersion measures, the mechanical properties of the obtained composite material may even be reduced, and the reason for this is that the agglomerated mullite fibers are more likely to cause the reduction of fluidity during the casting process of the geopolymer sample, and cannot be completely filled, thereby increasing more defects in the sample. Therefore, the reasonable dispersion of the fibers plays an important role in improving the performance of the composite material.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (10)

1. An acid-activated geopolymer composite characterized by containing a mullite fiber-reinforced phase structure.
2. The acid-activated geopolymer composite of claim 1 wherein the mullite fibers are mullite fibers having a diameter of 3-5 μ ι η and a length of < 2mm and a weight percent of alumina of 70-80%.
3. The acid-activated geopolymer composite of claim 2, wherein said acid-activated geopolymer composite is prepared from a geopolymer slurry containing mullite fibers, metakaolin;
the mass ratio of the mullite fiber to the metakaolin is (5-20): 100.
4. the acid-activated geopolymer composite of claim 3, wherein the metakaolin is a powder obtained by calcining raw kaolin ore powder in air at 600-900 ℃ for 2 hours;
the kaolin has the mesh number of more than 200 meshes and the specific surface area of 300-500m2The kaolin crude ore powder is/Kg.
5. The acid-activated geopolymer composite of claim 3 or 4, wherein the geopolymer slurry further comprises an acid activator;
the acid excitant is one or more of phosphoric acid, hydrochloric acid or sulfuric acid;
preferably, the acid activator is phosphoric acid, Al2O3And H3PO4In a molar ratio of 1: (1-1.3).
6. The acid-activated geopolymer composite of claim 5, wherein said acid-activated geopolymer composite is made from raw materials comprising, by mass; the feedstock comprises a solid phase and a liquid phase; the mass ratio of the solid phase to the liquid phase is 1: 1;
in the solid phase, by mass, 5-20 parts of mullite fiber and 100 parts of kaolin are added;
45-54 parts of 85% phosphoric acid and 55-46 parts of water by mass in the liquid phase.
7. The acid-activated geopolymer composite of claim 6, wherein the acid-activated geopolymer composite has an average compressive strength of 19.8-26.1MPa for 7 days of curing, an average flexural strength of 7.86-10.4MPa for 7 days, and a linear shrinkage of 3.13-5.34% after baking at 1350 ℃ for 1 hour.
8. A method of preparing an acid-activated geopolymer composite as claimed in any one of claims 1 to 7, comprising: pouring geopolymer slurry containing mullite fiber, metakaolin and an acid excitant into a mould for curing; and (6) demolding.
9. The method of claim 8, wherein the geopolymer slurry is obtained by mixing a liquid phase with a solid phase;
the solid phase can be obtained by the following method: carrying out suction filtration, drying and ball milling on slurry containing mullite fiber and kaolin, and then calcining in high-temperature air to obtain the mullite fiber/kaolin-containing slurry;
during the stirring process of the slurry, the slurry is stirred in the same direction as much as possible;
in the preparation of the slurry, mullite fiber is added into water, and after the mullite fiber is stirred uniformly, kaolin is added;
the ball milling is carried out at low speed firstly and then at high speed;
the calcination temperature is 600-900 ℃ and the time is 1.5-2 h.
10. Use of the acid-activated geopolymer composite material according to any one of claims 1 to 7 in the field of structural materials, building materials, fire-resistant materials, solid-waste solid-core materials, antibacterial filter materials.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115180887A (en) * 2022-07-22 2022-10-14 清华大学 Method for fixing heavy metal by using phosphate group geopolymer
US11932578B1 (en) * 2022-11-08 2024-03-19 Wuhan University Of Technology Granite stone powder phosphoric acid-based geopolymer and preparation method thereof

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