CN115636654B - Alkali-resistant heat-insulating cement mortar - Google Patents
Alkali-resistant heat-insulating cement mortar Download PDFInfo
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- CN115636654B CN115636654B CN202211359509.6A CN202211359509A CN115636654B CN 115636654 B CN115636654 B CN 115636654B CN 202211359509 A CN202211359509 A CN 202211359509A CN 115636654 B CN115636654 B CN 115636654B
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- 239000003513 alkali Substances 0.000 title claims abstract description 79
- 239000011083 cement mortar Substances 0.000 title claims abstract description 59
- 239000003365 glass fiber Substances 0.000 claims abstract description 131
- 239000004964 aerogel Substances 0.000 claims abstract description 80
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- 238000002156 mixing Methods 0.000 claims description 45
- 239000004568 cement Substances 0.000 claims description 32
- 239000003638 chemical reducing agent Substances 0.000 claims description 32
- 239000000835 fiber Substances 0.000 claims description 32
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 28
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 23
- 238000001035 drying Methods 0.000 claims description 21
- 239000000499 gel Substances 0.000 claims description 21
- 238000002360 preparation method Methods 0.000 claims description 21
- 230000001105 regulatory effect Effects 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 16
- 239000011240 wet gel Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000011398 Portland cement Substances 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 10
- 239000004115 Sodium Silicate Substances 0.000 claims description 9
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 9
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 9
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 6
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 4
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 2
- 239000008030 superplasticizer Substances 0.000 claims 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 41
- 239000004965 Silica aerogel Substances 0.000 abstract description 37
- 238000009413 insulation Methods 0.000 abstract description 25
- 239000004567 concrete Substances 0.000 description 16
- 229910008051 Si-OH Inorganic materials 0.000 description 14
- 229910006358 Si—OH Inorganic materials 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 230000014759 maintenance of location Effects 0.000 description 9
- 238000009833 condensation Methods 0.000 description 8
- 239000002585 base Substances 0.000 description 6
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- 238000005260 corrosion Methods 0.000 description 6
- 230000002209 hydrophobic effect Effects 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 239000012774 insulation material Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000007667 floating Methods 0.000 description 3
- 238000001879 gelation Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 229910002808 Si–O–Si Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000004566 building material Substances 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
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- 239000000017 hydrogel Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- 238000004458 analytical method Methods 0.000 description 1
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- 230000033228 biological regulation Effects 0.000 description 1
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
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- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- MTCFGRXMJLQNBG-UHFFFAOYSA-N serine Chemical compound OCC(N)C(O)=O MTCFGRXMJLQNBG-UHFFFAOYSA-N 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 239000011374 ultra-high-performance concrete Substances 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Silicon Compounds (AREA)
Abstract
The invention relates to the technical field of cement mortar, in particular to alkali-resistant heat-insulating cement mortar. According to the aerogel modified glass fiber, the glass fiber is added in the gel process, and the reaction conditions are controlled, so that the silica aerogel grows by taking the glass fiber as a core, and the aerogel modified glass fiber with excellent alkali resistance, heat insulation and mechanical properties is obtained. According to the invention, the prepared aerogel modified glass fiber is further added into the cement mortar, so that the alkali resistance and heat insulation performance of the aerogel modified glass fiber are improved, and the alkali-resistant heat insulation cement mortar is obtained.
Description
Technical Field
The invention relates to the technical field of cement mortar, in particular to alkali-resistant heat-insulating cement mortar.
Background
In recent decades, with the continuous progress of society, the demand of energy is continuously increased, and the energy crisis problem is also receiving more and more attention. The energy consumption of the building industry is about 40% of the total energy consumption, and the large-scale buildings of the population of China are huge, so that the energy consumption of the building is reduced, and the energy use efficiency of the building is improved. The heat preservation and heat insulation of the building can reduce the energy loss of the building and improve the energy utilization efficiency of the building, and is one of the most effective methods for reducing the energy consumption of the building.
According to the preparation process of the concrete, the formed concrete consists of a solid-phase cement base and closed pores. The heat transfer modes in the concrete comprise four modes, namely heat conduction in the solid-phase cement base, heat conduction of gas in the closed air hole, convective heat transfer of gas in the closed air hole and radiation heat exchange between the surfaces of the cement base in the closed air hole. The convective heat transfer of the internal air is negligible at pore sizes less than 4 mm. From Stefan-Boltzman radiation law, it is known that the radiative heat transfer between cement-based surfaces in closed pores is negligible. Therefore, the heat transfer mode in concrete is mainly heat conduction between solid-phase cement bases and heat conduction of air in closed pores. The analysis shows that the heat insulation performance of the concrete mainly depends on the volume ratio of the cement base to the air holes, and the internal hole size, the hole shape, the mutual communication condition of the holes and other factors have a certain influence. The aerogel is used as a novel heat insulation material, and can well reduce heat conduction between solid-phase cement bases and heat conduction of air in closed pores.
The aerogel thermal insulation material has the characteristics of ultralow thermal conductivity, ultrahigh void ratio, specific surface area, super-strong hydrophobic property, strong sound absorption, shock absorption and the like, and can be well applied to the field of thermal insulation, so that the aerogel is used as the thermal insulation material for a large amount of researches. However, pure aerogels are fragile due to their low mechanical strength and relatively high cost of preparation. Therefore, compounding aerogel with other materials to improve its mechanical strength and reduce its cost of use is one of the key points of current research. In recent years, aerogel has been used as aggregate to prepare lightweight aerogel concrete with a density of 1000kg/m 3 The influence of different aerogel addition amounts on the thermal conductivity of aerogel concrete was studied by Serina et al under Experimental investigations of aerogel-incorporated ultra-high performance concrete, wherein the thermal conductivity was 0.55W/(m.K) at 50vol% of the aerogel content. It can be seen that the density and thermal conductivity of concrete can be effectively reduced by adding a certain amount of aerogel. However, the existing aerogel concrete also has overlarge density>500kg/m 3 ) High heat conductivity>0.10W/(m.K)), and the aerogel content in the aerogel concrete is large, and the manufacturing cost is high.
Glass fiber is an inorganic nonmetallic material with excellent performance, takes mineral materials such as quartz and the like as raw materials, and is molded by means of high-temperature melting, wire drawing, winding, weaving and the like. The filament diameter of the glass fiber can reach the micron level. The glass fiber has the advantages of good insulativity, strong heat resistance, good corrosion resistance, high mechanical strength and the like, can be used as an auxiliary reinforcing material in a raw material system of cement concrete, and improves the stability of the concrete after forming a stable and complex crosslinked structure. However, the glass fiber in the prior art often has hidden troubles such as corrosion, embrittlement, cracking and damage and the like in the cement matrix, so that the improvement treatment of the existing glass fiber preparation means is extremely needed, and the alkali corrosion resistance of the cement matrix is improved, so that the concrete is prevented from being subjected to physical and chemical corrosion.
Therefore, the present invention considers that if the advantages of aerogel and glass fiber can be combined and the disadvantages thereof can be mutually compensated, the heat insulation, alkali resistance and mechanical properties of the concrete for construction can be well improved.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides alkali-resistant heat-insulating cement mortar which comprises the following raw materials in parts by mass: 40.4-52 parts of dry materials, 50-60 parts of aggregate and 18-21 parts of water.
The dry material comprises the following raw materials: according to the mass parts, 35-40 parts of cement, 5-10 parts of aerogel modified glass fiber, 0.2-1 part of water reducer and 0.2-1 part of sodium silicate.
The cement is at least one of Portland cement P.I, portland cement P.II and composite Portland cement P.C.
The aggregate is fine aggregate, and the water content is less than or equal to 2wt%.
The water reducer is at least one of naphthalene-based high-efficiency water reducer, aliphatic high-efficiency water reducer, amino high-efficiency water reducer and polycarboxylic acid high-performance water reducer; preferably, the water reducer is a polycarboxylic acid high-performance water reducer.
The preparation method of the aerogel modified glass fiber comprises the following steps:
s1, immersing 20-40 parts of glass fiber powder into 90-100 parts of 3-5wt% sodium hydroxide aqueous solution according to parts by mass, stirring for 20-30min at a rotating speed of 200-300r/min, filtering, washing and drying to obtain alkali-treated glass fibers;
s2, mixing 10-20 parts of tetraethyl orthosilicate and 80-90 parts of 75wt% ethanol water solution according to parts by weight, then regulating the pH value to 3.0-4.0 by using 10-14wt% hydrochloric acid, and standing for 2-3 hours at 35-45 ℃ to obtain silica sol;
s3, mixing 2-4 parts of dimethylformamide, 20-40 parts of alkali-treated glass fiber powder prepared in the step S1 and 60-80 parts of silica sol prepared in the step S2 according to parts by mass, dispersing for 10-20min at a rotating speed of 6000-8000r/min, regulating the pH value to 8.0-9.0 by using triethylamine, stirring and reacting for 20-40min at a rotating speed of 60-80r/min, and then gelatinizing for 14-16h at a temperature of 30-40 ℃ to obtain wet gel fibers;
s4, mixing wet gel fibers and absolute ethyl alcohol according to a bath ratio of 1g: (5-10) mixing and aging for 12-24h, then taking out the gel, drying for 12-24h at 80-100 ℃, and cooling to room temperature to obtain aerogel fibers;
and S5, crushing 20-40 parts of aerogel fibers to 100-500 mu m according to parts by mass, adding 90-100 parts of n-hexane, 10-20 parts of trimethylchlorosilane and 5-10 parts of absolute ethyl alcohol, uniformly mixing, carrying out nitrogen protection reaction for 8-12h at 60-80 ℃, cooling to room temperature, filtering, carrying out suction filtration on acetone, and drying at 80-100 ℃ for 12-24h to obtain the aerogel modified glass fibers.
The invention also provides a preparation method of the alkali-resistant heat-insulating cement mortar, which comprises the following steps: and uniformly mixing 40.4-52 parts of dry materials and 50-60 parts of aggregates by mass, adding 18-21 parts of water, and stirring at a rotating speed of 60-80r/min for 10-30min to obtain the alkali-resistant heat-insulating cement mortar.
Glass fiber is used as a common additive in cement mortar, and can well improve the mechanical property and stability of the cement mortar, but the glass fiber has hidden troubles such as corrosion, embrittlement, cracking and even damage in a cement matrix. The silica aerogel is used as an excellent heat insulation material, and can be added into cement mortar to greatly improve the heat insulation performance, reduce the building energy loss and improve the building energy utilization efficiency. However, the density is extremely low, and when the mortar is directly added into cement mortar, the phenomenon of floating up occurs, and layering or collapse is caused. Therefore, the invention considers that if the glass fiber and the silicon dioxide aerogel can be combined, the heat insulation, alkali resistance and mechanical property of the concrete for building can be well improved.
The invention firstly adds glass fiber directly into cement mortar, which has extremely high heat conductivity coefficient, because glass fiber does not have heat insulating capability. The silica aerogel has excellent heat insulation performance, so that the silica aerogel with excellent heat insulation performance can be adhered to the surface of the glass fiber in the synthesis process of the silica aerogel, the obtained aerogel modified glass fiber is added into the cement mortar, so that the heat conductivity coefficient of the cement mortar is obviously reduced, however, the alkali-resistant heat insulation cement mortar prepared by the method has the silica aerogel which floats up and is easy to fall off after solidification, and the invention considers that most of the silica aerogel exists independently due to the fact that the silica aerogel adhered to the glass fiber is less, and the silica aerogel floats up very easily due to low density, so that the silica aerogel escapes from the cement mortar, not only is wasted, but also the heat insulation performance of the alkali-resistant heat insulation cement mortar is affected. Therefore, in order to improve the adhesion rate of the silica aerogel on the surface of the glass fiber, the invention firstly adopts sodium hydroxide solution to treat the surface of the glass fiber, and after the sodium hydroxide solution is treated, the surface of the glass fiber is slightly corroded to generate more defects and active sites, which are favorable for bonding Si-OH on the surface of the glass fiber and forming an aerogel structure by taking the glass fiber as the center, thereby improving the adhesion amount of the silica aerogel on the surface of the glass fiber and further reducing the floating escape of the silica aerogel. However, the present inventors found that if the pH was adjusted to be alkaline using a conventional alkali solution during gelation in step S3 (i.e., the pH was adjusted using a sodium hydroxide solution and an aqueous ammonia solution in step S3 in comparative example 2 and comparative example 3, respectively), the final gel block filled with glass fibers was still obtained instead of glass fibers having a large amount of silica aerogel grown on the surface. This shows that during the process of hydrolysis of the hydrogel by tetraethyl orthosilicate, the nucleation centers are not completely glass fibers, i.e. the Si-OH is not completely building up the aerogel structure network with glass fibers as the center, but also a large amount of Si-OH will self-condense to form Si-O-Si. The gel mass obtained in this case still produces a large amount of a mixture of silica aerogel and aerogel-modified glass fibers after pulverization, and the silica aerogel occupies a small proportion. Therefore, the invention tries to inhibit the self-condensation behavior of Si-OH by various lye and finds that the self-condensation behavior of Si-OH can be effectively inhibited by using triethylamine instead of sodium hydroxide, and finally the obtained gel block is extremely easy to crush into fibrous filaments after drying, which indicates that the condensation of Si-OH to form a gel structure is carried out by taking glass fibers as the center, and the obtained product has extremely high proportion of aerogel modified glass fibers after crushing. However, since the self-condensation behavior of Si-OH is suppressed, the gel rate thereof is slow, and thus it is necessary to lengthen the gel time thereof. Therefore, after the aerogel modified glass fiber prepared by adjusting the pH value by using triethylamine is added into cement mortar, the heat conductivity coefficient of the aerogel modified glass fiber is obviously lower than that of the aerogel modified glass fiber prepared by adjusting the pH value by using sodium hydroxide and ammonia water.
The prepared aerogel modified glass fiber is subjected to hydrophobic treatment, so that the dispersibility of the aerogel modified glass fiber in cement mortar is realized, the alkali resistance of the fiber is improved, and the heat insulation performance of the prepared alkali-resistant heat insulation cement mortar is improved.
In addition, the silica aerogel has excellent alkali resistance, so that the alkali resistance of the glass fiber can be improved, and the hidden trouble that the glass fiber can be corroded, embrittled and even cracked and damaged in a cement matrix can be reduced by attaching the silica aerogel on the surface of the glass fiber.
The invention has the beneficial effects that:
1. according to the aerogel modified glass fiber, the glass fiber is added in the gel process, and the reaction conditions are controlled, so that the silica aerogel grows by taking the glass fiber as a core, and the aerogel modified glass fiber with excellent alkali resistance, heat insulation and mechanical properties is obtained.
2. According to the invention, the prepared aerogel modified glass fiber is further added into the cement mortar, so that the alkali resistance and heat insulation performance of the aerogel modified glass fiber are improved, and the alkali-resistant heat insulation cement mortar is obtained.
Detailed Description
Composite portland cement P.C, strength grade: 42.5, cargo number: p.c42.5, shenzhen Hua Changxin building materials limited.
The fine aggregate is river sand with the grain diameter of 2.2-3.0 mm.
Polycarboxylic acid high-performance water reducer, product number: h-136, dongguan, inc. of new materials.
Dimethylformamide: CAS number: 68-12-2.
Glass fiber powder, product number: MEF-13-1000, shenzhen, sub-Tadak technologies Co.
Example 1
The preparation method of the alkali-resistant heat-insulating cement mortar comprises the following steps: and (3) uniformly mixing 49.4 parts of dry materials and 55 parts of aggregates according to parts by mass, adding 20 parts of water, and stirring for 30min at a rotating speed of 80r/min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material consists of the following raw materials: according to the mass parts, 40 parts of cement, 8 parts of glass fiber powder, 0.6 part of water reducer and 0.8 part of sodium silicate.
The cement is composite Portland cement P.C.
The aggregate is fine aggregate, and the water content is less than or equal to 2wt%.
The water reducer is a polycarboxylic acid high-performance water reducer.
Example 2
The preparation method of the alkali-resistant heat-insulating cement mortar comprises the following steps: and (3) uniformly mixing 49.4 parts of dry materials and 55 parts of aggregates according to parts by mass, adding 20 parts of water, and stirring for 30min at a rotating speed of 80r/min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material consists of the following raw materials: according to the mass parts, 40 parts of cement, 8 parts of aerogel modified glass fiber, 0.6 part of water reducer and 0.8 part of sodium silicate.
The cement is composite Portland cement P.C.
The aggregate is fine aggregate, and the water content is less than or equal to 2wt%.
The water reducer is a polycarboxylic acid high-performance water reducer.
The preparation method of the aerogel modified glass fiber comprises the following steps:
s1, mixing 15 parts of tetraethyl orthosilicate and 85 parts of 75wt% ethanol water solution according to parts by weight, then regulating the pH value to 4.0 by 12wt% hydrochloric acid, and standing at 40 ℃ for 3 hours to obtain silica sol;
s2, mixing 3 parts of dimethylformamide, 30 parts of glass fiber powder and 70 parts of silica sol prepared in the step S1 according to parts by mass, dispersing for 15min at 8000r/min, regulating the pH value to 8.0 by using triethylamine, stirring and reacting for 30min at 70r/min, and then gelatinizing for 15h at 35 ℃ to obtain wet gel fibers;
s3, mixing wet gel fibers and absolute ethyl alcohol according to a bath ratio of 1g:10mL was mixed and aged for 12 hours, then the gel was taken out, dried at 90℃for 12 hours, cooled to room temperature, and then pulverized to 200. Mu.m, to obtain the aerogel-modified glass fiber.
Example 3
The preparation method of the alkali-resistant heat-insulating cement mortar comprises the following steps: and (3) uniformly mixing 49.4 parts of dry materials and 55 parts of aggregates according to parts by mass, adding 20 parts of water, and stirring for 30min at a rotating speed of 80r/min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material consists of the following raw materials: according to the mass parts, 40 parts of cement, 8 parts of aerogel modified glass fiber, 0.6 part of water reducer and 0.8 part of sodium silicate.
The cement is composite Portland cement P.C.
The aggregate is fine aggregate, and the water content is less than or equal to 2wt%.
The water reducer is a polycarboxylic acid high-performance water reducer.
The preparation method of the aerogel modified glass fiber comprises the following steps:
s1, immersing 30 parts of glass fiber powder into 100 parts of 4wt% sodium hydroxide aqueous solution, stirring for 30min at a rotating speed of 300r/min, filtering, washing and drying to obtain alkali-treated glass fibers;
s2, mixing 15 parts of tetraethyl orthosilicate and 85 parts of 75wt% ethanol water solution according to parts by weight, then regulating the pH value to 4.0 by 12wt% hydrochloric acid, and standing at 40 ℃ for 3 hours to obtain silica sol;
s3, mixing 3 parts of dimethylformamide, 30 parts of alkali-treated glass fibers prepared in the step S1 and 70 parts of silica sol prepared in the step S2 according to parts by mass, dispersing at 8000r/min for 15min, regulating the pH value to 8.0 by using triethylamine, stirring at 70r/min for 30min for reaction, and then gelatinizing at 35 ℃ for 15h to obtain wet gel fibers;
s4, mixing wet gel fibers and absolute ethyl alcohol according to a bath ratio of 1g:10mL was mixed and aged for 12 hours, then the gel was taken out, dried at 90℃for 12 hours, cooled to room temperature, and then pulverized to 200. Mu.m, to obtain the aerogel-modified glass fiber.
Example 4
The preparation method of the alkali-resistant heat-insulating cement mortar comprises the following steps: and (3) uniformly mixing 49.4 parts of dry materials and 55 parts of aggregates according to parts by mass, adding 20 parts of water, and stirring for 30min at a rotating speed of 80r/min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material consists of the following raw materials: according to the mass parts, 40 parts of cement, 8 parts of aerogel modified glass fiber, 0.6 part of water reducer and 0.8 part of sodium silicate.
The cement is composite Portland cement P.C.
The aggregate is fine aggregate, and the water content is less than or equal to 2wt%.
The water reducer is a polycarboxylic acid high-performance water reducer.
The preparation method of the aerogel modified glass fiber comprises the following steps:
s1, immersing 30 parts of glass fiber powder into 100 parts of 4wt% sodium hydroxide aqueous solution, stirring for 30min at a rotating speed of 300r/min, filtering, washing and drying to obtain alkali-treated glass fibers;
s2, mixing 15 parts of tetraethyl orthosilicate and 85 parts of 75wt% ethanol water solution according to parts by weight, then regulating the pH value to 4.0 by 12wt% hydrochloric acid, and standing at 40 ℃ for 3 hours to obtain silica sol;
s3, mixing 3 parts of dimethylformamide, 30 parts of alkali-treated glass fibers prepared in the step S1 and 70 parts of silica sol prepared in the step S2 according to parts by mass, dispersing at 8000r/min for 15min, regulating the pH value to 8.0 by using triethylamine, stirring at 70r/min for 30min for reaction, and then gelatinizing at 35 ℃ for 15h to obtain wet gel fibers;
s4, mixing wet gel fibers and absolute ethyl alcohol according to a bath ratio of 1g: mixing 10mL, aging for 12h, taking out gel, drying at 90 ℃ for 12h, and cooling to room temperature to obtain aerogel fibers;
and S5, crushing 30 parts of aerogel fibers to 200 mu m according to parts by mass, adding 90 parts of n-hexane, 10 parts of trimethylchlorosilane and 5 parts of absolute ethyl alcohol, uniformly mixing, reacting for 10 hours under the protection of nitrogen at 70 ℃, cooling to room temperature, filtering, carrying out suction filtration on acetone, and drying at 90 ℃ for 12 hours to obtain the aerogel modified glass fibers.
Comparative example 1
The preparation method of the alkali-resistant heat-insulating cement mortar comprises the following steps: and (3) uniformly mixing 49.4 parts of dry materials and 55 parts of aggregates according to parts by mass, adding 20 parts of water, and stirring for 30min at a rotating speed of 80r/min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material consists of the following raw materials: according to the mass parts, 40 parts of cement, 8 parts of aerogel modified glass fiber, 0.6 part of water reducer and 0.8 part of sodium silicate.
The cement is composite Portland cement P.C.
The aggregate is fine aggregate, and the water content is less than or equal to 2wt%.
The water reducer is a polycarboxylic acid high-performance water reducer.
The preparation method of the aerogel modified glass fiber comprises the following steps:
s1, immersing 30 parts of glass fiber powder into 100 parts of 3wt% hydrofluoric acid aqueous solution, stirring for 30min at a rotating speed of 300r/min, filtering, washing and drying to obtain acid-treated glass fibers;
s2, mixing 15 parts of tetraethyl orthosilicate and 85 parts of 75wt% ethanol water solution according to parts by weight, then regulating the pH value to 4.0 by 12wt% hydrochloric acid, and standing at 40 ℃ for 3 hours to obtain silica sol;
s3, mixing 3 parts of dimethylformamide, 30 parts of the acid-treated glass fiber prepared in the step S1 and 70 parts of the silica sol prepared in the step S2 according to parts by mass, dispersing at 8000r/min for 15min, regulating the pH value to 8.0 by using triethylamine, stirring at 70r/min for 30min for reaction, and then gelatinizing at 35 ℃ for 15h to obtain wet gel fiber;
s4, mixing wet gel fibers and absolute ethyl alcohol according to a bath ratio of 1g: mixing 10mL, aging for 12h, taking out gel, drying at 90 ℃ for 12h, and cooling to room temperature to obtain aerogel fibers;
and S5, crushing 30 parts of aerogel fibers to 200 mu m according to parts by mass, adding 90 parts of n-hexane, 10 parts of trimethylchlorosilane and 5 parts of absolute ethyl alcohol, uniformly mixing, reacting for 10 hours under the protection of nitrogen at 70 ℃, cooling to room temperature, filtering, carrying out suction filtration on acetone, and drying at 90 ℃ for 12 hours to obtain the aerogel modified glass fibers.
Comparative example 2
The preparation method of the alkali-resistant heat-insulating cement mortar comprises the following steps: and (3) uniformly mixing 49.4 parts of dry materials and 55 parts of aggregates according to parts by mass, adding 20 parts of water, and stirring for 30min at a rotating speed of 80r/min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material consists of the following raw materials: according to the mass parts, 40 parts of cement, 8 parts of aerogel modified glass fiber, 0.6 part of water reducer and 0.8 part of sodium silicate.
The cement is composite Portland cement P.C.
The aggregate is fine aggregate, and the water content is less than or equal to 2wt%.
The water reducer is a polycarboxylic acid high-performance water reducer.
The preparation method of the aerogel modified glass fiber comprises the following steps:
s1, immersing 30 parts of glass fiber powder into 100 parts of 4wt% sodium hydroxide aqueous solution, stirring for 30min at a rotating speed of 300r/min, filtering, washing and drying to obtain alkali-treated glass fibers;
s2, mixing 15 parts of tetraethyl orthosilicate and 85 parts of 75wt% ethanol water solution according to parts by weight, then regulating the pH value to 4.0 by 12wt% hydrochloric acid, and standing at 40 ℃ for 3 hours to obtain silica sol;
s3, mixing 3 parts of dimethylformamide, 30 parts of alkali-treated glass fibers prepared in the step S1 and 70 parts of silica sol prepared in the step S2 according to parts by mass, dispersing at 8000r/min for 15min, regulating pH value to 8.0 by using 12wt% of sodium hydroxide, stirring at 70r/min for 30min, and carrying out reaction, and then, carrying out gelation at 35 ℃ for 15h to obtain wet gel fibers;
s4, mixing wet gel fibers and absolute ethyl alcohol according to a bath ratio of 1g: mixing 10mL, aging for 12h, taking out gel, drying at 90 ℃ for 12h, and cooling to room temperature to obtain aerogel fibers;
and S5, crushing 30 parts of aerogel fibers to 200 mu m according to parts by mass, adding 90 parts of n-hexane, 10 parts of trimethylchlorosilane and 5 parts of absolute ethyl alcohol, uniformly mixing, reacting for 10 hours under the protection of nitrogen at 70 ℃, cooling to room temperature, filtering, carrying out suction filtration on acetone, and drying at 90 ℃ for 12 hours to obtain the aerogel modified glass fibers.
Comparative example 3
The preparation method of the alkali-resistant heat-insulating cement mortar comprises the following steps: and (3) uniformly mixing 49.4 parts of dry materials and 55 parts of aggregates according to parts by mass, adding 20 parts of water, and stirring for 30min at a rotating speed of 80r/min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material consists of the following raw materials: according to the mass parts, 40 parts of cement, 8 parts of aerogel modified glass fiber, 0.6 part of water reducer and 0.8 part of sodium silicate.
The cement is composite Portland cement P.C.
The aggregate is fine aggregate, and the water content is less than or equal to 2wt%.
The water reducer is a polycarboxylic acid high-performance water reducer.
The preparation method of the aerogel modified glass fiber comprises the following steps:
s1, immersing 30 parts of glass fiber powder into 100 parts of 4wt% sodium hydroxide aqueous solution, stirring for 30min at a rotating speed of 300r/min, filtering, washing and drying to obtain alkali-treated glass fibers;
s2, mixing 15 parts of tetraethyl orthosilicate and 85 parts of 75wt% ethanol water solution according to parts by weight, then regulating the pH value to 4.0 by 12wt% hydrochloric acid, and standing at 40 ℃ for 3 hours to obtain silica sol;
s3, mixing 3 parts of dimethylformamide, 30 parts of alkali-treated glass fibers prepared in the step S1 and 70 parts of silica sol prepared in the step S2 according to parts by mass, dispersing at 8000r/min for 15min, regulating pH value to 8.0 by using 12wt% ammonia water, stirring at 70r/min for 30min for reaction, and then gelatinizing at 35 ℃ for 15h to obtain wet gel fibers;
s4, mixing wet gel fibers and absolute ethyl alcohol according to a bath ratio of 1g: mixing 10mL, aging for 12h, taking out gel, drying at 90 ℃ for 12h, and cooling to room temperature to obtain aerogel fibers;
and S5, crushing 30 parts of aerogel fibers to 200 mu m according to parts by mass, adding 90 parts of n-hexane, 10 parts of trimethylchlorosilane and 5 parts of absolute ethyl alcohol, uniformly mixing, reacting for 10 hours under the protection of nitrogen at 70 ℃, cooling to room temperature, filtering, carrying out suction filtration on acetone, and drying at 90 ℃ for 12 hours to obtain the aerogel modified glass fibers.
Test example 1
And (3) heat insulation test: the heat conductivity of the alkali-resistant heat-insulating cement mortar prepared by the examples and the comparative examples of the invention is measured according to GB/T32064-2015 "transient plane heat source test method for heat conductivity and thermal diffusion coefficient of building materials", and the heat conductivity is used as an index for measuring heat insulating capacity.
The alkali-resistant and heat-insulating cement mortar prepared in each example and comparative example of the present invention was poured in a conventional manner (the temperature of the pouring environment was 23 ℃ C., the relative humidity was 50%) to obtain a block-shaped specimen having a length of 10cm, a width of 10cm and a thickness of 2 cm. The alkali-resistant heat-insulating cement mortar is regulated in an environment with the temperature of 23 ℃ and the relative humidity of 50% after pouring is finished, and the total time is 7 days from the beginning of pouring to the completion of regulation.
The test environment temperature was 25℃and the relative humidity was 55%. For each example, 5 different samples were taken for testing and the test results averaged. The test results are shown in Table 1.
Table 1: heat insulating ability of alkali-proof heat insulating cement mortar
As can be seen from table 1, example 1 directly added glass fiber to cement mortar, its thermal conductivity was greatest among examples and comparative examples, since glass fiber does not have heat insulating ability. In the embodiment 2, glass fiber is added into the synthesis process of silica aerogel, so that silica aerogel with excellent heat insulation performance can be attached to the surface of glass fiber, and the obtained aerogel modified glass fiber is added into cement mortar, so that the heat conductivity coefficient of the cement mortar is obviously reduced, however, the alkali-resistant heat-insulation cement mortar prepared in the embodiment 2 is found to have silica aerogel which floats up more or less and is easy to fall off after solidification, and the invention considers that the silica aerogel attached to the glass fiber is less, most of silica aerogel exists independently, and the silica aerogel is easy to float up due to low density of the silica aerogel, so that the silica aerogel escapes from the cement mortar, waste is caused, and the heat insulation performance of the silica aerogel is influenced. Therefore, in order to improve the adhesion rate of the silica aerogel on the surface of the glass fiber, the method of the invention adopts the sodium hydroxide solution to treat the surface of the glass fiber, and after the sodium hydroxide solution is treated, the surface of the glass fiber is slightly corroded to generate more defects and active sites, which is favorable for bonding Si-OH on the surface of the glass fiber and forming an aerogel structure by taking the glass fiber as the center, thereby improving the adhesion amount of the silica aerogel on the surface of the glass fiber and further reducing the floating escape of the silica aerogel. However, the present inventors have found that, in the gelation process in step S3, if the pH is adjusted to be alkaline using a conventional alkali solution (i.e., the pH is adjusted by using a sodium hydroxide solution and an aqueous ammonia solution in step S3 in comparative examples 2 and 3, respectively), the aerogel modified glass fiber is prepared in the same manner as in example 3, and the resultant gel mass filled with glass fiber is not one but a glass fiber having a large amount of silica aerogel grown on the surface. This shows that during the process of hydrolysis of the hydrogel by tetraethyl orthosilicate, the nucleation centers are not completely glass fibers, i.e. the Si-OH is not completely building up the aerogel structure network with glass fibers as the center, but also a large amount of Si-OH will self-condense to form Si-O-Si. The gel mass obtained in this case still produces a large amount of a mixture of silica aerogel and aerogel-modified glass fibers after pulverization, and the silica aerogel occupies a small proportion. Therefore, the invention tries to inhibit the self-condensation behavior of Si-OH by various lye and finds that the self-condensation behavior of Si-OH can be effectively inhibited by using triethylamine instead of sodium hydroxide, and finally the obtained gel block is extremely easy to crush into fibrous filaments after drying, which indicates that the condensation of Si-OH to form a gel structure is carried out by taking glass fibers as the center, and the obtained product has extremely high proportion of aerogel modified glass fibers after crushing. However, since the self-condensation behavior of Si-OH is suppressed, the gel rate thereof is slow, and thus it is necessary to lengthen the gel time thereof. Thus, the thermal conductivity of the alkali-resistant and heat-insulating cement mortar prepared in example 3 is significantly lower than that of comparative examples 2 and 3. In the embodiment 4, the prepared aerogel modified glass fiber is subjected to hydrophobic treatment, so that the dispersibility of the aerogel modified glass fiber in cement mortar is improved, the alkali resistance of the fiber is improved, and the heat insulation performance of the prepared alkali-resistant heat insulation cement mortar is improved. In comparative example 1, the glass fiber is subjected to acid treatment, so that the corrosion to the glass fiber is serious, the mechanical property of the glass fiber is greatly influenced, the surface area of the glass fiber is reduced, and the attachment rate of the silica aerogel is reduced.
Test example 2
Alkali resistance test: the alkali-resistant strength retention of the aerogel modified glass fibers prepared by the examples and comparative examples of the present invention was tested according to GB/T38143-2019 alkali-resistant glass filled fibers for Cement concrete and mortar, and all aerogel modified glass fibers were retained for a length of 35mm for testing.
The sample was dried at 50℃for 1h. The tensile speed of the tensile tester was 1mm/min.
For each example, 20 different samples were taken for testing and the test results averaged. The test results are shown in Table 2.
Table 2: alkali-resistant strength retention of glass-filled fibers
| Alkali-resistant Strong retention (%) | |
| Example 1 | 81.2 |
| Example 2 | 86.1 |
| Example 3 | 95.7 |
| Example 4 | 97.9 |
As can be seen from table 2, the aerogel modified glass fiber prepared in example 4 has the highest alkali-resistant strong retention rate, because the silica aerogel on the surface of the aerogel modified glass fiber treated by the solution of example 4 has the highest adhesion rate, and the alkali resistance is further improved by hydrophobic treatment, so that the alkali-resistant strong retention rate is the largest in the alkaline environment of cement supernatant. The alkali strength retention of the aerogel modified glass fiber produced in example 3 was lower than that of example 4, since it was not subjected to a hydrophobic treatment, and the alkali resistance was slightly lower than that of the hydrophobically treated aerogel modified glass fiber. The alkali strength retention of the aerogel-modified glass fiber produced in example 2 was further reduced because the glass fiber used in example 2 was not alkali treated and the silica aerogel adhesion was extremely low compared to example 3, so that the alkali strength retention was lower. The glass fiber used in example 1 was not subjected to any treatment, and since the glass fiber was extremely susceptible to alkali attack, its alkali strength retention was the lowest.
Claims (5)
1. The preparation method of the alkali-resistant heat-insulating cement mortar is characterized by comprising the following steps of: uniformly mixing the dry material and 50-60 parts by mass of aggregate, and then adding 18-21 parts by mass of water to stir to obtain alkali-resistant heat-insulating cement mortar;
the dry material comprises the following raw materials in parts by mass: 35-40 parts of cement, 5-10 parts of aerogel modified glass fiber, 0.2-1 part of water reducer and 0.2-1 part of sodium silicate;
the preparation method of the aerogel modified glass fiber comprises the following steps:
s1, immersing 20-40 parts of glass fiber powder into 90-100 parts of 3-5wt% sodium hydroxide aqueous solution according to parts by mass, stirring for 20-30min at a rotating speed of 200-300r/min, filtering, washing and drying to obtain alkali-treated glass fibers;
s2, mixing 10-20 parts of tetraethyl orthosilicate and 80-90 parts of 75wt% ethanol water solution according to parts by weight, then regulating the pH value to 3.0-4.0 by using 10-14wt% hydrochloric acid, and standing for 2-3 hours at 35-45 ℃ to obtain silica sol;
s3, mixing 2-4 parts of dimethylformamide, 20-40 parts of alkali-treated glass fiber powder prepared in the step S1 and 60-80 parts of silica sol prepared in the step S2 according to parts by mass, dispersing for 10-20min at a rotating speed of 6000-8000r/min, regulating the pH value to 8.0-9.0 by using triethylamine, stirring and reacting for 20-40min at a rotating speed of 60-80r/min, and then gelatinizing for 14-16h at a temperature of 30-40 ℃ to obtain wet gel fibers;
s4, mixing wet gel fibers and absolute ethyl alcohol according to a bath ratio of 1g: (5-10) mixing and aging for 12-24h, then taking out the gel, drying for 12-24h at 80-100 ℃, and cooling to room temperature to obtain aerogel fibers;
and S5, crushing 20-40 parts of aerogel fibers to 100-500 mu m according to parts by mass, adding 90-100 parts of n-hexane, 10-20 parts of trimethylchlorosilane and 5-10 parts of absolute ethyl alcohol, uniformly mixing, carrying out nitrogen protection reaction for 8-12h at 60-80 ℃, cooling to room temperature, filtering, carrying out suction filtration on acetone, and drying at 80-100 ℃ for 12-24h to obtain the aerogel modified glass fibers.
2. The method for preparing alkali-resistant and heat-insulating cement mortar according to claim 1, wherein the cement is at least one of Portland cement P.I, portland cement P.II and composite Portland cement P.C.
3. The method for preparing alkali-resistant and heat-insulating cement mortar according to claim 1, wherein the aggregate is fine aggregate and the water content is less than or equal to 2wt%.
4. The method for preparing alkali-resistant and heat-insulating cement mortar according to claim 1, wherein the water reducer is at least one of naphthalene-based superplasticizer, aliphatic superplasticizer, amino superplasticizer and polycarboxylic acid superplasticizer.
5. An alkali-resistant and heat-insulating cement mortar, which is characterized by being prepared by the preparation method of the alkali-resistant and heat-insulating cement mortar according to any one of claims 1-4.
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