CN114772992B - Light heat-insulating geopolymer containing modified aerogel and preparation method thereof - Google Patents
Light heat-insulating geopolymer containing modified aerogel and preparation method thereof Download PDFInfo
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- 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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- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/08—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
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- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
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- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
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- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00008—Obtaining or using nanotechnology related materials
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- 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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- 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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- 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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- 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
Abstract
The invention discloses a light heat-insulating geological polymer containing modified aerogel and a preparation method thereof, wherein the light heat-insulating geological polymer containing the modified aerogel comprises, by weight, 9.5-9.8 parts of granular blast furnace slag, 0.92-1.0 part of silica fume, 2.93-3.30 parts of water, 2.2-2.73 parts of water glass, 0.25-0.38 part of NaOH, 0.3-0.45 part of carbon nanotube aerogel and 0.05-0.07 part of silane coupling agent. According to the light heat-insulating geological polymer containing the modified aerogel, the carbon nano tube is used for reinforcing the aerogel, so that the compression strength of the aerogel is improved, meanwhile, the carbon nano tube aerogel is modified into an open-close and open-close state by using the surfactant, the carbon nano tube aerogel is favorably and uniformly dispersed in the geological polymer, the interface performance between the geological polymer and the carbon nano tube aerogel is improved, the bonding performance is improved, so that the carbon nano tube aerogel is tightly combined with a geological polymer base, and the light heat-insulating geological polymer containing the modified aerogel is a preferred material for producing the light heat-insulating geological polymer.
Description
Technical Field
The invention relates to the technical field of preparation of light heat-insulating geopolymers, in particular to a light heat-insulating geopolymer containing modified aerogel and a preparation method thereof.
Background
A large amount of energy is consumed in the development process of the building industry, excessive greenhouse gas emission is a problem which needs to be solved urgently in modern development, and reduction of building energy consumption is an effective measure for realizing carbon emission reduction, so that recently, attention is paid to production of light-heat-preservation geopolymers, on one hand, solid waste utilization can be realized by using the geopolymers as cementing materials, and important contribution to environmental protection is provided, and researches show that production of one ton of geopolymers is more than production of one ton of cement greenhouse gas CO 2 The emission is reduced by 60-80%. On the other hand, the light heat-insulating geopolymer has a lower heat conductivity coefficient, reduces heat exchange with the external environment, and greatly reduces energy consumption. It can be seen that the light heat-insulating geopolymer has the advantages of carbon emission reduction and building energy consumption reductionHas positive significance, is a green, environment-friendly and sustainable-development building material, has wide application and can be used as a building heat-insulation outer wall.
The aerogel can be used as a preferred material for preparing heat-insulating concrete due to the extremely low thermal conductivity and the extremely low density, and many researchers try to mix the aerogel into the concrete to improve the heat-insulating performance, and researches show that the porosity (the porosity is as high as more than 90 percent) of the aerogel is beneficial to reducing the thermal conductivity and improving the heat-insulating performance, but due to the brittleness and poor mechanical property, the prepared concrete has the phenomenon of lower compressive strength, and due to the hydrophobicity of the aerogel, the aerogel is easy to float on the surface of the concrete in the concrete preparation and stirring process and has poor workability, and the aerogel is observed to be separated from the concrete material by a distance of several microns through an electron microscope after being formed.
Under the existing patent names: a porous geopolymer/aerogel composite heat-insulating material and a preparation method thereof are disclosed, wherein the application number is 201710025180.2, the fly ash raw material is activated by sodium silicate alkali, silica aerogel is used as a filler and embedded into the geopolymer (fly ash), and meanwhile, physical foaming is adopted to prepare the light porous heat-insulating concrete. The concrete is prepared by adopting a foaming process, the preparation process is relatively complex, the aerogel which is fragile and low in strength is directly doped into the geopolymer, so that the geopolymer is high in brittleness and low in strength, the fly ash is used as a cementing material through alkali activation, the strength is relatively low, and the aerogel with surface hydrophobicity is relatively dispersed in the geopolymer.
In the prior patent, the application number is 202010202926.4, fly ash and metakaolin are used as raw materials, alkali activation is carried out on the fly ash and the metakaolin through water glass and NaOH, EPS particles obtained by processing broken foam polystyrene plates are doped into a geopolymer, and light heat-insulating concrete is prepared through a foaming process. The EPS particles are used as lightweight aggregate, the heat preservation and the strength are poor, and the foaming process is adopted, so that the process is complex.
The prior patent names aerogel coating and preparation method thereof, and aerogel coating and preparation method thereofAccording to the method, the fly ash and the slag powder are used as raw materials in application number 202110034734.1, and are activated by sodium silicate, and the aerogel is doped into the geopolymer, so that the light heat-insulating concrete is prepared. The aerogel is directly added into the geopolymer, has high brittleness and low strength, and adopts CO 2 And the collapse of pores inside the material in the drying process is reduced by a supercritical drying mode, and the mechanical property is poor.
Disclosure of Invention
The invention aims to provide a light heat-insulating geopolymer containing modified aerogel and a preparation method thereof, wherein the aerogel is enhanced by a carbon nano tube, the compressive strength of the aerogel is improved, meanwhile, the carbon nano tube aerogel is modified into an open-air and open-air state by using a surfactant, so that the carbon nano tube aerogel is favorably and uniformly dispersed in the geopolymer, the interface performance between the geopolymer and the geopolymer is improved, the bonding performance is improved, and the carbon nano tube aerogel is tightly combined with a geopolymer base, so that the light heat-insulating geopolymer is a preferred material for producing the light heat-insulating geopolymer.
In order to achieve the purpose, the invention provides a light heat-insulating geopolymer containing modified aerogel, which comprises 9.5-9.8 parts of granular blast furnace slag, 0.92-1.0 part of silica fume, 2.93-3.30 parts of water, 2.2-2.73 parts of water glass, 0.25-0.38 part of NaOH, 0.3-0.45 part of carbon nanotube aerogel and 0.05-0.07 part of silane coupling agent in parts by weight.
Preferably, the density of the granular blast furnace slag is 2800- 3 Specific surface area 400-450m 2 Perkg of granulated blast furnace slag containing CaO, SiO 2 、MgO、A1 2 O 3 、Fe 2 O 3 The mass contents are 37.42%, 34.23%, 9.64%, 16.62% and 0.46% respectively.
Preferably, the silica fume contains 98 percent of amorphous silica by mass fraction, the average particle diameter is 0.3-60 mu m, and the density is 560-720kg/m 3 Specific surface area of 19-26m 2 /g。
Preferably, the carbon nano tube aerogel has the particle size of 0.1-6mm, the pore diameter of 15-60nm and the bulk density of 60-180kg/m in a natural bulk state 3 The specific surface area is 500-800m 2 G, conducting at normal temperatureThe thermal coefficient is 0.01-0.021W/mK.
Preferably, the density of the water glass is 1526-1559kg/m 3 SiO of 2 29.99% by mass of Na 2 The mass content of O is 13.75 percent, the mass content of Fe is 0.02 percent, the mass content of water-insoluble substances is 0.2 percent, and the modulus is 2.25.
Preferably, the silane coupling agent is KH-560.
Preferably, the mass content of the silane coupling agent is more than 98 percent, and the density is 1065-1072kg/m at the temperature of 25 DEG C 3 Boiling point 286-293 ℃ and flash point 109-113 ℃.
A preparation method of a light heat-insulating geopolymer containing modified aerogel comprises the following steps:
s1, preparing the carbon nano tube aerogel by adopting a sol-gel normal pressure drying preparation process;
s2, weighing the granular blast furnace slag, the carbon nano tube aerogel, the silica fume, the NaOH, the water glass, the water and the silane coupling agent according to the weight ratio for later use;
s3, dividing water into two parts according to the ratio of 8.5:1.5, wherein one part is used for preparing an alkali activator, and the other part is mixed with a silane coupling agent to be used for modifying the carbon nanotube aerogel;
s4, mixing the NaOH flaky solid with 17/20 water, and stirring for 2-3min by using a glass rod until the NaOH is completely dissolved to prepare an alkali solution A;
s5, mixing the alkali solution A with the weighed water glass solution, adjusting the modulus of the water glass to 1.3, stirring with a glass rod for 2-3min to uniformly disperse the water glass solution to obtain an alkali activator solution B, and standing for 24h for use;
s6, adding the carbon nanotube aerogel into the residual 3/20 of water, stirring for 3-5min, then adding 0% -1% of silane coupling agent, and fully stirring for 1h to obtain a modified carbon nanotube aerogel solution C;
s7, adding the granular blast furnace slag and the silica fume into a stirring pot, and stirring the dry materials for 3-5min until the dry materials are uniformly mixed;
s8, slowly adding the alkali activator solution B into a stirring pot, and stirring for 1-2min until slurry with certain fluidity is formed;
s9, adding the modified carbon nanotube aerogel solution C into a stirring pot, and fully stirring for 2-3min to prepare a heat-preservation geopolymer;
s10, pouring the heat-preservation geopolymer into a mold with the thickness of 50mm multiplied by 50mm, sealing the film and curing for 24 hours indoors;
s11, placing the sample into a standard curing room, and curing for 3-28 days under the conditions of 20-25 ℃ and 90-95% of humidity in the curing room;
s12, after the sample is cured, testing the compressive strength, and after the sample is dried, testing the density and the heat conductivity coefficient of the sample, wherein the drying condition is 60-110 ℃ and 24-48 h.
Preferably, the specific process of preparing the carbon nanotube aerogel by using the sol-gel normal pressure drying preparation process in step S1 is as follows:
firstly, ultrasonically dispersing a carbon nano tube with the mass content of 0.6% in water for 1.5h to obtain a solution A, adding hexyl orthosilicate, ethanol and deionized water into a beaker according to the molar ratio of 1:12:9, stirring for 30min by magnetic force to mix the mixture fully and uniformly, dropwise adding 0.5mol/L dilute hydrochloric acid into the beaker to adjust the pH value of the solution to be 2-3, stirring for 1h by magnetic force to hydrolyze the solution fully, then adding 0.5mol/L dilute ammonia water to control the pH value to be 8-9 to obtain a solution B, uniformly mixing the solution A and the solution B, sealing the mixture, gelatinizing the mixture at room temperature until the mixture does not flow at 40 ℃ in the beaker, forming alcogel, aging the alcogel for 48h, repeatedly soaking the gel in ethanol to remove all water, adding n-hexane to soak for 30min, and drying at normal pressure to prepare the carbon nano tube aerogel.
The granular blast furnace slag has the density of 2800-. The activity of geopolymers is related to the fineness, vitreous content and chemical composition of geopolymers, and the slag has high vitreous content and contains a large amount of CaO, so that the activity of the slag is improved, and the development of early strength is promoted. The granular blast furnace slag is industrial waste, the utilization rate of solid waste can be effectively improved by preparing the heat-insulating concrete by utilizing the slag, and the emission of CO2 is reduced to a great extent at the same time, and researches show that the emission of carbon dioxide is reduced by 70-80% when one ton of slag-based geopolymer is produced compared with one ton of cement, so that the granular blast furnace slag is a low-carbon, green and sustainable-development energy-saving material.
The silica fume is amorphous silica with the mass fraction of about 98 percent, and has higher volcanic ash activity. An average particle diameter of 0.3 to 60 μm, more preferably 0.3 to 30 μm, most preferably 0.3 to 18 μm, a density of 560- 3 Specific surface area of 19-26m 2 (ii) in terms of/g. According to the invention, the silica fume with the thickness of 0.3-18 μm is selected, and the micro-filling effect of the silica fume can improve the compactness of concrete, so that the internal structure of the concrete is more compact, and the strength of the concrete is improved; alleviating or even avoiding alkali-aggregate reactions.
The process for preparing the carbon nanotube modified aerogel has the following advantages: compared with freeze drying and supercritical drying methods, the method adopting normal pressure drying does not need specific equipment and extreme conditions, has relatively simple process and low cost, and is beneficial to large-scale production; secondly, in order to avoid the damage of the pore structure and the collapse of the network skeleton structure of the aerogel caused by the capillary force during normal pressure drying, the aerogel is repeatedly soaked by ethanol until all water is removed, and the surface tension is adjusted by an organic solvent (ethanol) so as to avoid the damage of the pore structure of the aerogel caused by the capillary force in the drying process. The carbon nano tube has excellent mechanical property due to the existence of stronger carbon atom covalent bond, is introduced into the aerogel and forms interface bonding force with aerogel nano particles, thereby improving the network framework strength of the aerogel and solving the defects of high brittleness, low strength and the like of the aerogel.
NaOH, white, translucent, uniform granular or flaky solid, readily soluble in water, 98% pure, pH 12.7, melting point 318.4 ℃, boiling point 1390 ℃, density 2.93g/cm 3.
Water glass, colorless transparent viscous liquid with the density of 1526- 3 SiO of 2 29.99% by mass of Na 2 The mass content of O is 13.75 percent, the mass content of Fe is 0.02 percent, the mass content of water-insoluble substances is 0.2 percent, and the modulus is 2.25. The water glass has good excitation effect on granular blast furnace slag, and the active silicon in the sodium silicate participates in the formation of reaction products to promote the generation of more C-, (The N) -A-S-H gel has the interface bonding effect, so that the mechanical property of the heat-insulating concrete is improved.
The hydrophilic surfactant is a silane coupling agent KH-560; the silane coupling agent (mass content > 98 percent) is colorless or yellowish transparent liquid, and the density is 1065-1072kg/m at the temperature of 25 DEG C 3 Boiling point 286-; action of surfactant: the hydrophobic aerogel can be modified into an inner lyophobic state and an outer lyophobic state, the surface of the aerogel is easily and uniformly distributed in the geopolymer after being hydrophilic, the phenomena of floating on the surface of concrete and flying in the stirring process due to the surface hydrophobic characteristic are avoided, the interface performance between the modified aerogel and the geopolymer is improved, and the bonding performance is improved to ensure that the modified aerogel is tightly combined with the geopolymer matrix; secondly, the internal hydrophobicity protects the aerogel porous structure from being damaged in an alkaline environment, the extremely low heat conductivity coefficient is kept, and the heat insulation performance of concrete is improved;
ethyl silicate as colorless transparent liquid at normal temperature and with density of 0.96-1.03g/cm 3 Melting point-77 deg.C, boiling point 166-.
Anhydrous ethanol, 99.6% ethanol solution with density of 0.81g/cm 3 Melting point-113 deg.C, boiling point 78 deg.C. Flash point 12 ℃.
Water, tap water.
This patent adopts two kinds of techniques to modify the aerogel: the first technique is to graft carbon nanotubes to aerogel, the carbon nanotubes have excellent mechanical properties and form a better interface combination effect with aerogel nanoparticles, the network framework structure of the aerogel is improved, and the defects of high brittleness, low compressive strength and the like of the aerogel are overcome; the diameter of the carbon nano tube is 15-25nm and is smaller than the pore diameter among aerogel particles, so that the carbon nano tube is added in a small amount to be wrapped in the aerogel and uniformly dispersed, the pore diameter of the aerogel is reduced, the heat conduction of air in pores is reduced, and the heat conductivity coefficient is reduced to a certain extent; compared with pure aerogel, the thermal stability is higher, and the preparation of the heat-insulation concrete is facilitated. The second technique is to modify the surface of the carbon nano tube aerogel by using a silane coupling agent (KH-560); the hydrophobic aerogel can be modified into an inner lyophobic state and an outer lyophobic state, the surface of the aerogel is easily and uniformly distributed in the geopolymer after being hydrophilic, the phenomena of floating on the surface of concrete and flying in the preparation process due to the surface hydrophobic property are avoided, the interface performance between the modified aerogel and the geopolymer is improved, and the bonding performance is improved to ensure that the modified aerogel is tightly combined with the geopolymer matrix; the internal hydrophobicity protects the aerogel porous structure from being damaged in an alkaline environment, keeps the extremely low heat conductivity coefficient of the aerogel porous structure, and improves the heat insulation performance of concrete. The optimal content of the modified carbon nanotube aerogel doped with the geopolymer is adjusted according to the material proportion, the concentration of the alkali activator is optimized, the optimal doping amount of the silane coupling agent (KH-560) is determined, the aerogel is seriously damaged in an alkaline environment when being doped too much, the surface hydrophilic effect of the aerogel is not obvious when being doped too little, and then the lightweight-heat-preservation-higher-strength concrete is prepared.
Therefore, according to the light heat-insulating geopolymer containing the modified aerogel and the preparation method thereof, the carbon nano tube is used for reinforcing the aerogel, so that the compressive strength of the aerogel is improved, meanwhile, the carbon nano tube aerogel is modified into an open-air and open-air state by using the surfactant, so that the carbon nano tube aerogel is favorably and uniformly dispersed in the geopolymer, the interface performance between the geopolymer and the geopolymer is improved, the bonding performance is improved, and the carbon nano tube aerogel is tightly combined with the geopolymer base, so that the light heat-insulating geopolymer containing the modified aerogel and the preparation method thereof are preferred materials for producing the light heat-insulating geopolymer.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a photomicrograph of an aerogel prior to modification;
FIG. 2 is a photomicrograph of granulated blast furnace slag;
fig. 3 is a top view of the compression resistant sample of comparative example 2.
Detailed Description
The invention provides a light heat-insulating geopolymer containing modified aerogel, which comprises 9.5-9.8 parts of granular blast furnace slag, 0.92-1.0 part of silica fume, 2.93-3.30 parts of water, 2.2-2.73 parts of water glass, 0.25-0.38 part of NaOH, 0.3-0.45 part of carbon nanotube aerogel and 0.05-0.07 part of silane coupling agent in parts by weight.
The density of the granular blast furnace slag is 2800- 3 Specific surface area 400-450m 2 Per Kg, granulated blast furnace slag containing CaO, SiO 2 、MgO、A1 2 O 3 、Fe 2 O 3 The mass contents are 37.42%, 34.23%, 9.64%, 16.62% and 0.46% respectively.
The silica fume contains 98 percent of amorphous silica by mass fraction, the average particle diameter is 0.3-60 mu m, the density is 560- 3 Specific surface area of 19-26m 2 /g。
The carbon nanotube aerogel has particle diameter of 0.1-6mm, pore diameter of 15-60nm, and natural bulk density of 60-180kg/m 3 The specific surface area is 500-800m 2 The thermal conductivity coefficient is 0.01-0.021W/mK at normal temperature.
The density of the water glass is 1526-1559kg/m 3 SiO of 2 29.99% by mass of Na 2 The mass content of O is 13.75 percent, the mass content of Fe is 0.02 percent, the mass content of water-insoluble substances is 0.2 percent, and the modulus is 2.25.
The silane coupling agent is KH-560, the mass content of the silane coupling agent is more than 98 percent, and the density is 1065-silane 1072kg/m at the temperature of 25 DEG C 3 Boiling point 286-293 ℃ and flash point 109-113 ℃.
A preparation method of a light heat-insulating geopolymer containing modified aerogel comprises the following steps:
s1, preparing the carbon nano tube aerogel by adopting a sol-gel normal pressure drying preparation process, which comprises the following specific steps:
firstly, ultrasonically dispersing a carbon nano tube with the mass content of 0.6% in water for 1.5h to obtain a solution A, adding hexyl orthosilicate, ethanol and deionized water into a beaker according to the molar ratio of 1:12:9, stirring for 30min by magnetic force to mix the mixture fully and uniformly, adding 0.5mol/L dilute hydrochloric acid into the beaker to adjust the pH value of the solution to be 2-3, stirring for 1h by magnetic force to hydrolyze the solution fully, then adding 0.5mol/L dilute ammonia water to control the pH value to be 8-9 to obtain a solution B, mixing the solution A and the solution B uniformly, sealing the mixture, gelatinizing the mixture at room temperature until the mixture keeps 40 ℃ in the beaker and does not flow, forming alcogel, aging the gel for 48h, repeatedly soaking the gel in ethanol to remove all water, adding n-hexane to soak for 30min, and drying under normal pressure to prepare the carbon nano tube aerogel;
s2, weighing granular blast furnace slag, carbon nano tube aerogel, silica fume, NaOH, water glass, water and a silane coupling agent according to the weight ratio for later use;
s3, dividing water into two parts according to the ratio of 8.5:1.5, wherein one part is used for preparing an alkali activator, and the other part is mixed with a silane coupling agent to be used for modifying the carbon nanotube aerogel;
s4, mixing the NaOH flaky solid with 17/20 water, and stirring for 2-3min by using a glass rod until the NaOH is completely dissolved to prepare an alkali solution A;
s5, mixing the alkali solution A with the weighed water glass solution, adjusting the modulus of the water glass to 1.3, stirring with a glass rod for 2-3min to uniformly disperse the water glass solution to obtain an alkali activator solution B, and standing for 24h for use;
s6, adding the carbon nanotube aerogel into the residual 3/20 of water, stirring for 3-5min, then adding 0% -1% of silane coupling agent, and fully stirring for 1h to obtain a modified carbon nanotube aerogel solution C;
s7, adding the granular blast furnace slag and the silica fume into a stirring pot, and stirring the dry materials for 3-5min until the dry materials are uniformly mixed;
s8, slowly adding the alkali activator solution B into a stirring pot, and stirring for 1-2min until slurry with certain fluidity is formed;
s9, adding the modified carbon nanotube aerogel solution C into a stirring pot, and fully stirring for 2-3min to prepare a heat-preservation geopolymer;
s10, pouring the heat-preservation geopolymer into a mould with the thickness of 50mm, 50mm and 50mm, sealing the film and curing in a room for 24 hours;
s11, placing the sample into a standard curing room, and curing for 3-28 days under the conditions of 20-25 ℃ and 90-95% of humidity in the curing room;
s12, after the sample is cured, testing the compressive strength, and after the sample is dried, testing the density and the heat conductivity coefficient of the sample, wherein the drying condition is 60-110 ℃ and 24-48 h.
The technical solution of the present invention is further illustrated by the accompanying drawings and examples.
Example 1
The light heat-insulating geopolymer containing the modified aerogel comprises the following components in parts by weight:
9.63 parts of granular blast furnace slag, 0.96 part of silica fume with the particle size of 0.3 to 18 mu m, 2.97 parts of water, 2.68 parts of water glass, 0.35 part of NaOH, 98 percent of NaOH purity and 0.42 part of 0.1 to 0.6mm carbon nano tube aerogel (the density is 60 to 180 kg/m) 3 0.012W/m.K thermal conductivity), 0.07 part of silane coupling agent (KH-560).
The material preparation process comprises the following steps:
(1) the carbon nano tube aerogel is prepared by adopting a sol-gel normal pressure drying preparation process, and the method comprises the following steps: firstly, ultrasonically dispersing a carbon nano tube with the mass content of 0.6% in water for 1.5h to obtain a solution A, adding hexyl orthosilicate, ethanol and deionized water into a beaker according to the molar ratio of 1:12:9, stirring for 30min by magnetic force to mix the mixture evenly, dropwise adding 0.5mol/L dilute hydrochloric acid into the beaker to adjust the pH value of the solution to be 2-3, stirring for 1h by magnetic force to hydrolyze the solution fully, then adding 0.5mol/L dilute ammonia water to control the pH value to be 8-9 to obtain a solution B, mixing the solution A and the solution B evenly, sealing the mixture, gelatinizing the mixture at room temperature until the mixture does not flow at 40 ℃ in the beaker, forming alcogel, aging the alcogel for 48h, repeatedly soaking the gel in ethanol to remove all water, adding n-hexane to soak for 30min, and drying at normal pressure to prepare the carbon nano tube aerogel.
(2) Weighing granular blast furnace slag, carbon nano tube aerogel, silica fume, NaOH, water glass, water and silane coupling agent (KH-560) according to the weight ratio.
(3) Dividing water into two parts according to the ratio of 8.5:1.5, wherein one part is used for preparing an alkali activator, and the other part is mixed with a silane coupling agent (KH-560) to be used for modifying the carbon nano tube aerogel.
(4) Mixing the NaOH flaky solid with 17/20 water, and stirring for 2-3min with a glass rod until the NaOH is completely dissolved to obtain an alkali solution A.
(5) Mixing NaOH solution with weighed water glass solution, and adding water glassAdjusting modulus to 1.3, stirring with glass rod for 2-3min to disperse uniformly to obtain alkali activator solution B (Na in alkali activator) 2 O content 6%), and was used after standing for 24 hours.
(6) Adding the carbon nano tube aerogel into the residual 3/20 water, stirring for 3-5min, then adding 0.7% of silane coupling agent (KH 560), and fully stirring for 1h to obtain a modified carbon nano tube aerogel solution C.
(7) Adding the granular blast furnace slag and the silica fume into a stirring pot, and stirring the dry materials for 3-5min until the dry materials are uniformly mixed.
(8) And slowly adding the alkali-activated solution B into a stirring pot, and stirring for 1-2min until slurry with certain fluidity is formed.
(9) And adding the modified carbon nano tube aerogel solution C into a stirring pot, and fully stirring for 2-3min to prepare the heat-preservation geopolymer.
(10) Pouring the heat-preservation geopolymer into a mold with the thickness of 50mm multiplied by 50mm to seal the film chamber for curing for 24 hours to prevent water from evaporating.
(11) And putting the sample into a standard curing room, and curing for 3-28 days under the conditions of 20-25 ℃ and the humidity of 90-95%.
(12) And after the sample is cured, testing the compressive strength, and after the sample is dried, testing the density and the heat conductivity coefficient of the sample, wherein the drying condition is 110 ℃ for 24 hours.
Example 2
The light heat-insulating geopolymer containing the modified aerogel comprises the following components in parts by weight:
9.63 parts of granular blast furnace slag, 0.96 part of silica fume with the particle size of 0.3 to 18 mu m, 2.97 parts of water, 2.68 parts of water glass, 0.35 part of NaOH, 98 percent of NaOH purity and 0.32 part of 0.1 to 0.6mm carbon nano tube aerogel (the density is 60 to 180 kg/m) 3 0.012W/m.K) of thermal conductivity, and 0.07 part of silane coupling agent (KH-560).
The material preparation procedure was the same as in example 1
Example 3
The light heat-insulating geopolymer containing the modified aerogel comprises the following components in parts by weight:
9.63 parts of granular blast furnace slag, 0.96 part of silica fume with the particle size of 0.3 to 18 mu m, 3.26 parts of water, 2.23 parts of water glass, 0.29 part of NaOH, 98 percent of NaOH purity and 0.42 part of 0.1 to 0.6mm carbon nano tube aerogel (the density is 60 to 180 kg/m) 3 0.012W/m.K thermal conductivity), 0.07 part of silane coupling agent (KH-560).
The material preparation process comprises (5) mixing NaOH solution with weighed water glass solution, adjusting water glass modulus to 1.3, stirring with glass rod for 2-3min to disperse uniformly to obtain alkali activator solution B (Na in alkali activator) 2 O content 5%), was used after standing for 24 hours, and the procedure was the same as in example 1.
Example 4
The light heat-insulating geopolymer containing the modified aerogel comprises the following components in parts by weight:
9.63 parts of granular blast furnace slag, 0.96 part of silica fume with the particle size of 0.3 to 18 mu m, 2.97 parts of water, 2.68 parts of water glass, 0.35 part of NaOH, 98 percent of NaOH purity and 0.42 part of 0.1 to 0.6mm carbon nano tube aerogel (the density is 60 to 180 kg/m) 3 0.012W/m.K thermal conductivity), 0.05 portion of silane coupling agent (KH-560).
The material preparation procedure was the same as in example 1
Comparative example 1
The light heat-preservation geopolymer of the comparative example 1 comprises the following components in parts by weight:
9.63 parts of granular blast furnace slag, 0.96 part of silica fume with the particle size of 0.3 to 18 mu m, 3.22 parts of water, 2.68 parts of water glass, 0.35 part of NaOH, 98 percent of NaOH purity and 0.95 part of 0.1 to 0.6mm carbon nano tube aerogel (the density is 60 to 180 kg/m) 3 0.012W/m.K thermal conductivity), 0.07 part of silane coupling agent (KH-560).
The material preparation procedure was the same as in example 1
Comparative example 2
The light heat-insulating geopolymer of the comparative example 2 comprises the following components in parts by weight:
9.63 parts of granular blast furnace slag, 0.96 part of silica fume with the particle size of 0.3-18 mu m, 2.97 parts of water, 2.68 parts of water glass, 0.35 part of NaOH, 98 percent of NaOH purity and 0.42 part of 0.1-0.6mm carbon nano tube aerogel (the density is 60-180kg/m3, the thermal conductivity is 0.012W/m.K) without adding a silane coupling agent (KH-560).
The material preparation procedure was the same as in example 1
Comparative example 3
The comparative example 3 light heat-insulating geopolymer comprises the following components in parts by weight:
9.63 parts of granular blast furnace slag, 0.96 part of silica fume with the particle size of 0.3 to 18 mu m, 2.97 parts of water, 2.68 parts of water glass, 0.35 part of NaOH, 98 percent of NaOH purity and 0.42 part of 0.1 to 0.6mm aerogel (the density is 60 to 180kg/m 3 0.012W/m.K) of thermal conductivity, 0.07 part of silane coupling agent (KH-560) is added, and no aerogel doped with carbon nano tubes is added.
The material preparation procedure was the same as in example 1
The results of the performance tests of the light-weight heat-insulating geopolymers of examples 1-4 of the invention and comparative examples 1-3 are shown in table 1.
Table 1 test results of light weight insulating geopolymers of examples 1-3 and comparative examples 1-3
Therefore, according to the light heat-insulating geopolymer containing the modified aerogel and the preparation method thereof, the carbon nano tube is used for reinforcing the aerogel, so that the compressive strength of the aerogel is improved, meanwhile, the carbon nano tube aerogel is modified into an open-air and open-air state by using the surfactant, so that the carbon nano tube aerogel is favorably and uniformly dispersed in the geopolymer, the interface performance between the geopolymer and the geopolymer is improved, the bonding performance is improved, and the carbon nano tube aerogel is tightly combined with the geopolymer base, so that the light heat-insulating geopolymer containing the modified aerogel and the preparation method thereof are preferred materials for producing the light heat-insulating geopolymer.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (7)
1. A light heat-insulating geopolymer containing modified aerogel is characterized in that: according to weight portion, the material comprises 9.5 to 9.8 portions of granular blast furnace slag, 0.92 to 1.0 portion of silica fume, 2.93 to 3.30 portions of water, 2.2 to 2.73 portions of water glass, 0.25 to 0.38 portion of NaOH, 0.3 to 0.45 portion of carbon nanotube aerogel and 0.05 to 0.07 portion of silane coupling agent; the preparation method of the light heat-insulating geopolymer containing the modified aerogel comprises the following steps:
s1, preparing the carbon nano tube aerogel by adopting a sol-gel normal pressure drying preparation process;
s2, weighing the granular blast furnace slag, the carbon nano tube aerogel, the silica fume, the NaOH, the water glass, the water and the silane coupling agent according to the weight ratio for later use;
s3, dividing water into two parts according to the ratio of 8.5:1.5, wherein one part is used for preparing an alkali activator, and the other part is mixed with a silane coupling agent for modifying the carbon nanotube aerogel;
s4, mixing the NaOH flaky solid with 17/20 water, and stirring for 2-3min by using a glass rod until the NaOH is completely dissolved to prepare an alkali solution A;
s5, mixing the alkali solution A with the weighed water glass solution, adjusting the modulus of the water glass to 1.3, stirring with a glass rod for 2-3min to uniformly disperse the water glass to obtain an alkali activator solution B, and standing for 24h for use;
s6, adding the carbon nanotube aerogel into the residual 3/20 of water, stirring for 3-5min, then adding 0% -1% of silane coupling agent, and fully stirring for 1h to obtain a modified carbon nanotube aerogel solution C;
s7, adding the granular blast furnace slag and the silica fume into a stirring pot, and stirring the dry materials for 3-5min until the dry materials are uniformly mixed;
s8, slowly adding the alkali activator solution B into a stirring pot, and stirring for 1-2min until slurry with certain fluidity is formed;
s9, adding the modified carbon nanotube aerogel solution C into a stirring pot, and fully stirring for 2-3min to prepare a heat-preservation geopolymer;
s10, pouring the heat-preservation geopolymer into a mold with the thickness of 50mm multiplied by 50mm, sealing the film and curing for 24 hours indoors;
s11, placing the sample into a standard curing room, and curing for 3-28 days under the conditions of 20-25 ℃ and 90-95% of humidity in the curing room;
s12, testing the compressive strength after the sample maintenance is finished, and testing the density and the heat conductivity coefficient of the sample after the sample is dried, wherein the drying condition is 60-110 ℃ and 24-48 h;
the specific process of preparing the carbon nanotube aerogel by adopting the sol-gel normal pressure drying preparation process in the step S1 is as follows:
firstly, ultrasonically dispersing a carbon nano tube with the mass content of 0.6% in water for 1.5h to obtain a solution A, adding hexyl orthosilicate, ethanol and deionized water into a beaker according to the molar ratio of 1:12:9, stirring the mixture for 30min by magnetic force to mix the mixture evenly, adding 0.5mol/L dilute hydrochloric acid into the beaker to adjust the pH value of the solution to be 2-3, stirring the mixture for 1h by magnetic force to hydrolyze the mixture fully, then adding 0.5mol/L dilute ammonia water to control the pH value to be 8-9 to obtain a solution B, mixing the solution A and the solution B evenly, sealing the mixture, placing the mixture at room temperature to be gelatinized until the mixture keeps not flowing at 40 ℃ in the beaker to form alcohol gel, aging the gel for 48h, repeatedly soaking the gel in ethanol to remove all water, adding n-hexane to soak for 30min, and drying the mixture at normal pressure to prepare the carbon nano tube aerogel.
2. A lightweight insulating geopolymer containing modified aerogel as claimed in claim 1, characterized by: the density of the granular blast furnace slag is 2800-3100kg/m 3 Specific surface area 400-450m 2 /kg, granulated blast furnace slag containing CaO, SiO 2 、MgO、A1 2 O 3 、Fe 2 O 3 The mass contents are 37.42%, 34.23%, 9.64%, 16.62% and 0.46% respectively.
3. A lightweight insulating geopolymer containing modified aerogel as claimed in claim 1, characterized by: the silica fume contains 98 percent of amorphous silica by mass fraction, the average grain diameter is 0.3-60 mu m, and the density560-720kg/m 3 Specific surface area of 19-26m 2 /g。
4. The light-weight thermal insulation geopolymer containing modified aerogel as claimed in claim 1, characterized in that: the carbon nano tube aerogel has the particle size of 0.1-6mm, the pore diameter of 15-60nm and the stacking density of 60-180kg/m in a natural stacking state 3 The specific surface area is 500-800m 2 The thermal conductivity coefficient is 0.01-0.021W/mK at normal temperature.
5. The light-weight thermal insulation geopolymer containing modified aerogel as claimed in claim 1, characterized in that: the density of the water glass is 1526-1559kg/m 3 SiO of 2 29.99% by mass of Na 2 The mass content of O is 13.75 percent, the mass content of Fe is 0.02 percent, the mass content of water-insoluble substances is 0.2 percent, and the modulus is 2.25.
6. A lightweight insulating geopolymer containing modified aerogel as claimed in claim 1, characterized by: the silane coupling agent is KH-560.
7. A lightweight insulating geopolymer containing modified aerogel as claimed in claim 1, characterized by: the mass content of the silane coupling agent is more than 98 percent, and the density is 1065-1072kg/m at the temperature of 25 DEG C 3 Boiling point 286-293 ℃ and flash point 109-113 ℃.
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