CN115636654A - Alkali-resistant heat-insulating cement mortar - Google Patents
Alkali-resistant heat-insulating cement mortar Download PDFInfo
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- CN115636654A CN115636654A CN202211359509.6A CN202211359509A CN115636654A CN 115636654 A CN115636654 A CN 115636654A CN 202211359509 A CN202211359509 A CN 202211359509A CN 115636654 A CN115636654 A CN 115636654A
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- 239000003513 alkali Substances 0.000 title claims abstract description 82
- 239000011083 cement mortar Substances 0.000 title claims abstract description 60
- 239000003365 glass fiber Substances 0.000 claims abstract description 130
- 239000004964 aerogel Substances 0.000 claims abstract description 80
- 238000000034 method Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 55
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- 238000002156 mixing Methods 0.000 claims description 44
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 37
- 239000003638 chemical reducing agent Substances 0.000 claims description 36
- 239000004568 cement Substances 0.000 claims description 33
- 239000000835 fiber Substances 0.000 claims description 30
- 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
- 239000000499 gel Substances 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 18
- 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
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 239000011398 Portland cement Substances 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 14
- 239000002131 composite material Substances 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 239000004115 Sodium Silicate Substances 0.000 claims description 9
- 238000001879 gelation Methods 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
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 230000032683 aging Effects 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
- 238000002791 soaking Methods 0.000 claims description 3
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 31
- 238000009413 insulation Methods 0.000 abstract description 19
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 3
- 239000004965 Silica aerogel Substances 0.000 description 23
- 239000004567 concrete Substances 0.000 description 16
- 229910008051 Si-OH Inorganic materials 0.000 description 13
- 229910006358 Si—OH Inorganic materials 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 10
- 230000014759 maintenance of location Effects 0.000 description 9
- 238000009833 condensation Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 230000002209 hydrophobic effect Effects 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 239000002585 base Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- 239000005051 trimethylchlorosilane Substances 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
- 230000007547 defect Effects 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 239000012774 insulation material Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000012546 transfer Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000007667 floating Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 239000007787 solid Substances 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
- 239000012670 alkaline solution Substances 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
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000003301 hydrolyzing effect Effects 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
- 238000011160 research Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002035 prolonged effect Effects 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
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009864 tensile test Methods 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
- 238000009941 weaving Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
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
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 prepared by the invention, the glass fiber is added in the gelling process, and the reaction conditions are controlled, so that the silicon dioxide 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. The prepared aerogel modified glass fiber is further added into cement mortar, so that the alkali resistance and heat insulation performance of the cement mortar are improved, and the alkali-resistant heat-insulating 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 and development of society, the demand of energy is increasing, and the energy crisis problem is receiving more and more attention. The energy consumption of the building industry accounts for about 40% of the total energy consumption, and the buildings in China are large in scale, so that the energy consumption of the buildings is reduced, and the energy use efficiency of the buildings is improved at present. The method for preserving heat and insulating heat of the building, reducing the energy loss of the building and improving the energy utilization efficiency of the building is one of the most effective methods for reducing the energy consumption of the building.
According to the preparation process of concrete, the formed concrete consists of solid cement base and closed air holes. The heat transfer mode in concrete includes four kinds, i.e. heat conduction in solid cement base, heat conduction of gas in closed pores, gas convection heat transfer in closed pores and radiation heat exchange between cement base surfaces in closed pores. When the pore size is smaller than 4mm, the convective heat transfer of the internal air is ignored. According to the Stefan-Boltzman radiation law, the radiation heat exchange between the cement-based surfaces in the closed pores is negligible. Therefore, the heat transfer in concrete is mainly the heat conduction between the solid cement matrix and the heat conduction of the air in the closed pores. From the above analysis, it can be known that the thermal insulation performance of concrete mainly depends on the volume ratio of the cement base to the air hole, and the factors such as the size of the internal hole, the shape of the hole, the communication condition of the holes and the like also have a certain influence. The aerogel is used as a novel thermal insulation material, and can well reduce the heat conduction between solid-phase cement bases and the heat conduction of air in the closed air holes.
The aerogel thermal insulation material has the characteristics of ultralow heat conductivity coefficient, ultrahigh porosity, 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 has a great deal of research as a thermal insulation material. However, pure aerogels are fragile due to their low mechanical strength and are expensive to produce. Therefore, it is one of the major issues of the current research to compound aerogel with other materials to improve its mechanical strength and reduce its cost. In recent years, aerogels have been used as aggregates for producing lightweight aerogel concrete with a density of 1000kg/m 3 The thermal conductivity is 0.26W/(m.K), and Serina et al, in Experimental information of aerogel-induced ultra-high performance concrete, have studied the influence of different aerogel addition amounts on the thermal conductivity of aerogel concrete, and the thermal conductivity is 0.55W/(m.K) when the content of aerogel is 50 vol%. Therefore, the density and the heat conductivity coefficient of the concrete can be effectively reduced by adding a certain amount of aerogel. However, the current aerogel concrete also has excessive density (C)>500kg/m 3 ) Too high a thermal conductivity coefficient (>0.10W/(m.K)), and the aerogel content in the aerogel concrete is high, and the manufacturing cost is high.
Glass fiber is an inorganic non-metallic material with excellent performance, and is formed by taking mineral materials such as quartz and the like as raw materials through means such as high-temperature melting, wire drawing, winding, weaving and the like. The filament diameter of the glass fiber can reach 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 a stable and complex cross-linking structure is formed. However, the glass fiber in the prior art often has the hidden troubles of corrosion, embrittlement, even cracking damage and the like in the cement matrix, so that the improvement treatment of the existing glass fiber preparation method 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 invention considers that if the advantages of aerogel and glass fiber can be combined and the defects can be mutually compensated, the heat insulation, alkali resistance and mechanical property of the concrete for construction can be well improved.
Disclosure of Invention
Aiming at the defects 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 materials comprise the following raw materials: 35-40 parts of cement, 5-10 parts of aerogel modified glass fiber, 0.2-1 part of water reducing agent and 0.2-1 part of sodium silicate in parts by mass.
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 reducing agent is at least one of a naphthalene-based high-efficiency water reducing agent, an aliphatic high-efficiency water reducing agent, an amino high-efficiency water reducing agent and a polycarboxylic acid high-performance water reducing agent; preferably, the water reducing agent is a polycarboxylic acid high-performance water reducing agent.
The preparation method of the aerogel modified glass fiber comprises the following steps:
s1, according to parts by mass, soaking 20-40 parts of glass fiber powder into 90-100 parts of 3-5wt% sodium hydroxide aqueous solution, stirring at a rotating speed of 200-300r/min for 20-30min, and filtering, washing and drying to obtain alkali-treated glass fiber;
s2, mixing 10-20 parts of tetraethyl orthosilicate and 80-90 parts of 75wt% ethanol aqueous solution by mass, adjusting the pH value to 3.0-4.0 by using 10-14wt% hydrochloric acid, and standing at 35-45 ℃ for 2-3 hours to obtain silica sol;
s3, mixing 2-4 parts by mass of dimethylformamide, 20-40 parts by mass of alkali-treated glass fiber powder prepared in the step S1 and 60-80 parts by mass of silica sol prepared in the step S2, dispersing for 10-20min at the rotating speed of 6000-8000r/min, adjusting the pH value to 8.0-9.0 by using triethylamine, stirring and reacting for 20-40min at the rotating speed of 60-80r/min, and then placing at 30-40 ℃ for gelation for 14-16h to obtain wet gel fiber;
s4, mixing the wet gel fiber and absolute ethyl alcohol according to a bath ratio of 1g: (5-10) mixing and aging for 12-24h, taking out the gel, drying at 80-100 ℃ for 12-24h, and cooling to room temperature to obtain aerogel fibers;
s5, crushing 20-40 parts of aerogel fiber to 100-500 microns by mass, then adding 90-100 parts of n-hexane, 10-20 parts of trimethylchlorosilane and 5-10 parts of absolute ethyl alcohol, uniformly mixing, reacting for 8-12 hours at 60-80 ℃ under the protection of nitrogen, cooling to room temperature, filtering, carrying out suction filtration on acetone, and drying for 12-24 hours at 80-100 ℃ to obtain the aerogel modified glass fiber.
The invention also provides a preparation method of the alkali-resistant heat-insulating cement mortar, which comprises the following steps: uniformly mixing 40.4-52 parts of dry materials and 50-60 parts of aggregates in parts by mass, adding 18-21 parts of water, and stirring at the rotating speed of 60-80r/min for 10-30min to obtain the alkali-resistant heat-insulating cement mortar.
The glass fiber is used as a commonly used additive in cement mortar, and can well improve the mechanical property and stability of the cement mortar, but the glass fiber has the hidden troubles of corrosion, embrittlement, even cracking damage and the like in a cement matrix. The silicon dioxide aerogel serving as an excellent heat insulation material is added into cement mortar, so that the heat insulation performance of the silica aerogel can be greatly improved, the building energy loss is reduced, and the building energy utilization efficiency is improved. However, the density is very low, and when the cement paste is directly added to cement mortar, floating phenomenon occurs, resulting in delamination or collapse. Therefore, the invention considers that if the glass fiber and the silica aerogel can be combined, the heat insulation, alkali resistance and mechanical property of the concrete for the building can be well improved.
The invention firstly adds the glass fiber directly into the cement mortar, and the heat conductivity coefficient is extremely high because the glass fiber does not have the heat insulation capability. The invention discloses a method for preparing alkali-resistant heat-insulating cement mortar, which comprises the steps of preparing a silica aerogel, adding glass fibers into the silica aerogel, and adding the obtained aerogel modified glass fibers into cement mortar to form the alkali-resistant heat-insulating cement mortar. Therefore, the embodiment of the invention is further improved, and in order to improve the adhesion rate of the silica aerogel on the surface of the glass fiber, the surface of the glass fiber is treated by the sodium hydroxide solution, and after the treatment by the sodium hydroxide solution, the surface of the glass fiber is slightly corroded to generate more defects and active sites, so that Si-OH bonds on the surface of the glass fiber are favorably formed, and an aerogel structure is formed by taking the glass fiber as a center, so that the adhesion amount of the silica aerogel on the surface of the glass fiber is improved, and the floating escape of the silica aerogel is reduced. However, the present inventors have found that, if the pH is adjusted to be alkaline using a conventional alkaline solution during the gelation process in step S3 (i.e., the pH is adjusted using a sodium hydroxide solution and an aqueous ammonia solution in step S3 in comparative example 2 and comparative example 3, respectively), a complete gel mass filled with glass fibers is obtained instead of glass fibers having a large amount of silica aerogel grown on the surface thereof. This shows that in the process of hydrolyzing the liquid gel with ethyl orthosilicate, the nucleation centers are not completely glass fibers, i.e. Si-OH does not completely build an aerogel structure network by taking the glass fibers as the centers, but a large amount of Si-OH can 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 use various alkali liquids to try to inhibit the self-condensation behavior of Si-OH, and finds that the triethylamine is used for replacing sodium hydroxide, the self-condensation behavior of Si-OH can be effectively inhibited, and finally the obtained gel block is extremely easy to crush into fibrous filaments after being dried, which shows that the formation of a gel structure by Si-OH condensation is carried out by taking glass fibers as the center, and the proportion of aerogel modified glass fibers is extremely high after the obtained product is crushed. However, since the self-condensation behavior of Si — OH is suppressed, the gel rate is slow, and thus the gel time needs to be prolonged. Therefore, after the aerogel modified glass fiber prepared by adjusting the pH value with triethylamine is added into cement mortar, the thermal 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 with sodium hydroxide and ammonia water.
The invention further carries out hydrophobic treatment on the prepared aerogel modified glass fiber, so that the aerogel modified glass fiber has dispersibility in cement mortar, improves the alkali resistance of the fiber and is beneficial to further improving the heat insulation performance of the prepared alkali-resistant heat-insulation cement mortar.
In addition, the silica aerogel also has excellent alkali resistance, so that the alkali resistance of the glass fiber can be improved by attaching the silica aerogel on the surface of the glass fiber, and the hidden danger that the glass fiber is corroded, embrittled and even cracked in a cement matrix is reduced.
The invention has the beneficial effects that:
1. according to the aerogel modified glass fiber prepared by the invention, the glass fiber is added in the gelling process, and the reaction conditions are controlled, so that the silicon dioxide 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. The prepared aerogel modified glass fiber is further added into cement mortar, so that the alkali resistance and heat insulation performance of the cement mortar are improved, and the alkali-resistant heat-insulating cement mortar is obtained.
Detailed Description
Composite portland cement p.c, strength grade: 42.5, cargo number: P.C42.5, shenzhen, huachangxin building materials, inc.
The fine aggregate is river sand with particle size of 2.2-3.0 mm.
Polycarboxylic acid high-performance water reducing agent, product number: h-136, dongguan, a good and many new materials Co., ltd.
Dimethylformamide: CAS number: 68-12-2.
Glass fiber powder, cargo number: MEF-13-1000, shenzhen, yataida science and technology Limited.
Example 1
The preparation method of the alkali-resistant heat-insulating cement mortar comprises the following steps: and uniformly mixing 49.4 parts of dry materials and 55 parts of aggregate in parts by mass, adding 20 parts of water, and stirring at the rotating speed of 80r/min for 30min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material comprises the following raw materials: 40 parts of cement, 8 parts of glass fiber powder, 0.6 part of water reducing agent 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 reducing agent is a polycarboxylic acid high-performance water reducing agent.
Example 2
The preparation method of the alkali-resistant heat-insulating cement mortar comprises the following steps: and (2) uniformly mixing 49.4 parts by mass of dry materials and 55 parts by mass of aggregate, adding 20 parts by mass of water, and stirring at the rotating speed of 80r/min for 30min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material comprises the following raw materials: by mass, 40 parts of cement, 8 parts of aerogel modified glass fiber, 0.6 part of water reducing agent 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 reducing agent is a polycarboxylic acid high-performance water reducing agent.
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 aqueous solution by mass, adjusting the pH value to 4.0 by using 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 in parts by mass, dispersing for 15min at the rotating speed of 8000r/min, adjusting the pH value to 8.0 by using triethylamine, stirring and reacting for 30min at the rotating speed of 70r/min, and then gelling for 15h at 35 ℃ to obtain wet gel fiber;
s3, mixing the wet gel fiber and absolute ethyl alcohol according to a bath ratio of 1g:10mL of the mixture is aged for 12 hours, then the gel is taken out, dried for 12 hours at 90 ℃, cooled to room temperature, and crushed 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 uniformly mixing 49.4 parts of dry materials and 55 parts of aggregate in parts by mass, adding 20 parts of water, and stirring at the rotating speed of 80r/min for 30min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material comprises the following raw materials: by mass, 40 parts of cement, 8 parts of aerogel modified glass fiber, 0.6 part of water reducing agent 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 reducing agent is a polycarboxylic acid high-performance water reducing agent.
The preparation method of the aerogel modified glass fiber comprises the following steps:
s1, according to parts by mass, immersing 30 parts of glass fiber powder into 100 parts of 4wt% sodium hydroxide aqueous solution, stirring for 30min at the rotating speed of 300r/min, and filtering, washing and drying to obtain alkali-treated glass fiber;
s2, mixing 15 parts of tetraethyl orthosilicate and 85 parts of 75wt% ethanol aqueous solution by mass, adjusting the pH value to 4.0 by using 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 fiber prepared in the step S1 and 70 parts of silica sol prepared in the step S2 in parts by mass, dispersing for 15min at the rotating speed of 8000r/min, adjusting the pH value to 8.0 by using triethylamine, stirring and reacting for 30min at the rotating speed of 70r/min, and then placing at 35 ℃ for gelation for 15h to obtain wet gel fiber;
s4, mixing the wet gel fiber and absolute ethyl alcohol according to a bath ratio of 1g:10mL of the aerogel-modified glass fiber was mixed and aged for 12 hours, and then the gel was taken out, dried at 90 ℃ for 12 hours, cooled to room temperature, and then pulverized to 200 μm 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 (2) uniformly mixing 49.4 parts by mass of dry materials and 55 parts by mass of aggregate, adding 20 parts by mass of water, and stirring at the rotating speed of 80r/min for 30min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material comprises the following raw materials: by mass, 40 parts of cement, 8 parts of aerogel modified glass fiber, 0.6 part of water reducing agent 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 reducing agent is a polycarboxylic acid high-performance water reducing agent.
The preparation method of the aerogel modified glass fiber comprises the following steps:
s1, according to parts by mass, immersing 30 parts of glass fiber powder into 100 parts of 4wt% sodium hydroxide aqueous solution, stirring for 30min at the rotating speed of 300r/min, and filtering, washing and drying to obtain alkali-treated glass fiber;
s2, mixing 15 parts of tetraethyl orthosilicate and 85 parts of 75wt% ethanol aqueous solution by mass, adjusting the pH value to 4.0 by using 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 fiber prepared in the step S1 and 70 parts of silica sol prepared in the step S2 in parts by mass, dispersing for 15min at the rotating speed of 8000r/min, adjusting the pH value to 8.0 by using triethylamine, stirring and reacting for 30min at the rotating speed of 70r/min, and then placing at 35 ℃ for gelation for 15h to obtain wet gel fiber;
s4, mixing the wet gel fiber and absolute ethyl alcohol according to a bath ratio of 1g: mixing 10mL of the mixed solution, aging for 12 hours, taking out the gel, drying at 90 ℃ for 12 hours, and cooling to room temperature to obtain aerogel fibers;
s5, according to parts by mass, crushing 30 parts of aerogel fiber to 200 microns, then adding 90 parts of n-hexane, 10 parts of trimethylchlorosilane and 5 parts of absolute ethyl alcohol, uniformly mixing, reacting for 10 hours at 70 ℃ under the protection of nitrogen, cooling to room temperature, filtering, carrying out suction filtration on acetone, and drying for 12 hours at 90 ℃ to obtain the aerogel modified glass fiber.
Comparative example 1
The preparation method of the alkali-resistant heat-insulating cement mortar comprises the following steps: and uniformly mixing 49.4 parts of dry materials and 55 parts of aggregate in parts by mass, adding 20 parts of water, and stirring at the rotating speed of 80r/min for 30min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material comprises the following raw materials: the composite material comprises, by mass, 40 parts of cement, 8 parts of aerogel modified glass fiber, 0.6 part of a water reducing agent 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 reducing agent is a polycarboxylic acid high-performance water reducing agent.
The preparation method of the aerogel modified glass fiber comprises the following steps:
s1, according to parts by mass, soaking 30 parts of glass fiber powder into 100 parts of 3wt% hydrofluoric acid aqueous solution, stirring for 30min at the rotating speed of 300r/min, and filtering, washing and drying to obtain acid-treated glass fiber;
s2, mixing 15 parts of tetraethyl orthosilicate and 85 parts of 75wt% ethanol aqueous solution by mass, adjusting the pH value to 4.0 by using 12wt% hydrochloric acid, and standing at 40 ℃ for 3 hours to obtain silica sol;
s3, mixing 3 parts by mass of dimethylformamide, 30 parts by mass of acid-treated glass fiber prepared in the step S1 and 70 parts by mass of silica sol prepared in the step S2, dispersing for 15min at the rotating speed of 8000r/min, adjusting the pH value to 8.0 by using triethylamine, stirring and reacting for 30min at the rotating speed of 70r/min, and then placing at 35 ℃ for gelation for 15h to obtain wet gel fiber;
s4, mixing the wet gel fiber and absolute ethyl alcohol according to a bath ratio of 1g: mixing 10mL of the mixed solution, aging for 12 hours, taking out the gel, drying at 90 ℃ for 12 hours, and cooling to room temperature to obtain aerogel fibers;
s5, according to parts by mass, crushing 30 parts of aerogel fiber to 200 microns, then adding 90 parts of n-hexane, 10 parts of trimethylchlorosilane and 5 parts of absolute ethyl alcohol, uniformly mixing, reacting for 10 hours at 70 ℃ under the protection of nitrogen, cooling to room temperature, filtering, carrying out suction filtration on acetone, and drying for 12 hours at 90 ℃ to obtain the aerogel modified glass fiber.
Comparative example 2
The preparation method of the alkali-resistant heat-insulating cement mortar comprises the following steps: and uniformly mixing 49.4 parts of dry materials and 55 parts of aggregate in parts by mass, adding 20 parts of water, and stirring at the rotating speed of 80r/min for 30min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material comprises the following raw materials: by mass, 40 parts of cement, 8 parts of aerogel modified glass fiber, 0.6 part of water reducing agent 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 reducing agent is a polycarboxylic acid high-performance water reducing agent.
The preparation method of the aerogel modified glass fiber comprises the following steps:
s1, according to parts by mass, immersing 30 parts of glass fiber powder into 100 parts of 4wt% sodium hydroxide aqueous solution, stirring for 30min at the rotating speed of 300r/min, and filtering, washing and drying to obtain alkali-treated glass fiber;
s2, mixing 15 parts of tetraethyl orthosilicate and 85 parts of 75wt% ethanol aqueous solution by mass, adjusting the pH value to 4.0 by using 12wt% hydrochloric acid, and standing at 40 ℃ for 3 hours to obtain silica sol;
s3, mixing 3 parts by mass of dimethylformamide, 30 parts by mass of alkali-treated glass fiber prepared in the step S1 and 70 parts by mass of silica sol prepared in the step S2, dispersing for 15min at a rotating speed of 8000r/min, adjusting the pH value to 8.0 by using 12wt% of sodium hydroxide, stirring for reaction for 30min at a rotating speed of 70r/min, and then placing at 35 ℃ for gelation for 15h to obtain wet gel fiber;
s4, mixing the wet gel fiber and absolute ethyl alcohol according to a bath ratio of 1g: mixing 10mL of the mixed solution, aging for 12 hours, taking out the gel, drying at 90 ℃ for 12 hours, and cooling to room temperature to obtain aerogel fibers;
s5, according to parts by mass, crushing 30 parts of aerogel fiber to 200 microns, then adding 90 parts of n-hexane, 10 parts of trimethylchlorosilane and 5 parts of absolute ethyl alcohol, uniformly mixing, reacting for 10 hours at 70 ℃ under the protection of nitrogen, cooling to room temperature, filtering, carrying out suction filtration on acetone, and drying for 12 hours at 90 ℃ to obtain the aerogel modified glass fiber.
Comparative example 3
The preparation method of the alkali-resistant heat-insulating cement mortar comprises the following steps: and (2) uniformly mixing 49.4 parts by mass of dry materials and 55 parts by mass of aggregate, adding 20 parts by mass of water, and stirring at the rotating speed of 80r/min for 30min to obtain the alkali-resistant heat-insulating cement mortar.
The dry material comprises the following raw materials: the composite material comprises, by mass, 40 parts of cement, 8 parts of aerogel modified glass fiber, 0.6 part of a water reducing agent 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 reducing agent is a polycarboxylic acid high-performance water reducing agent.
The preparation method of the aerogel modified glass fiber comprises the following steps:
s1, according to parts by mass, immersing 30 parts of glass fiber powder into 100 parts of 4wt% sodium hydroxide aqueous solution, stirring for 30min at the rotating speed of 300r/min, and filtering, washing and drying to obtain alkali-treated glass fiber;
s2, mixing 15 parts of tetraethyl orthosilicate and 85 parts of 75wt% ethanol aqueous solution by mass, adjusting the pH value to 4.0 by using 12wt% hydrochloric acid, and standing at 40 ℃ for 3 hours to obtain silica sol;
s3, mixing 3 parts by mass of dimethylformamide, 30 parts by mass of alkali-treated glass fiber prepared in the step S1 and 70 parts by mass of silica sol prepared in the step S2, dispersing for 15min at the rotating speed of 8000r/min, adjusting the pH value to 8.0 by using 12wt% ammonia water, stirring and reacting for 30min at the rotating speed of 70r/min, and then placing at 35 ℃ for gelation for 15h to obtain wet gel fiber;
s4, mixing the wet gel fiber and absolute ethyl alcohol according to a bath ratio of 1g: mixing 10mL of the aerogel and aging for 12h, taking out the gel, drying at 90 ℃ for 12h, and cooling to room temperature to obtain aerogel fibers;
s5, according to the mass parts, crushing 30 parts of aerogel fibers to 200 microns, then adding 90 parts of n-hexane, 10 parts of trimethylchlorosilane and 5 parts of absolute ethyl alcohol, uniformly mixing, reacting at 70 ℃ for 10 hours under the protection of nitrogen, cooling to room temperature, filtering, carrying out suction filtration on acetone, and drying at 90 ℃ for 12 hours to obtain the aerogel modified glass fiber.
Test example 1
And (3) heat insulation test: the heat conductivity of the alkali-resistant heat-insulating cement mortar prepared by the embodiments and the comparative examples of the invention is measured according to GB/T32064-2015 transient planar heat source test method for heat conductivity and thermal diffusivity of building materials, and the heat conductivity is used as an index for measuring heat insulating capability.
The alkali-resistant heat-insulating cement mortar prepared in each embodiment and the comparative example of the invention is used for obtaining a block-shaped sample with the length of 10cm, the width of 10cm and the thickness of 2cm by a conventional pouring mode (the temperature of a pouring environment is 23 ℃ and the relative humidity is 50%). The alkali-resistant heat-insulating cement mortar is adjusted in an environment with the temperature of 23 ℃ and the relative humidity of 50% after the pouring is finished, and the total time from the beginning of pouring to the completion of adjustment is 7 days.
The test environment temperature was 25 ℃ and the relative humidity was 55%. For each example, 5 different samples were taken and tested, and the results averaged. The test results are shown in table 1.
Table 1: heat insulation capability of alkali-resistant heat-insulation cement mortar
As can be seen from table 1, example 1, in which glass fiber is directly added to cement mortar, has the highest thermal conductivity in each of examples and comparative examples, because glass fiber does not have thermal insulation ability. In the embodiment 2, the glass fiber is added into the synthesis process of the silica aerogel, so that the silica aerogel with excellent heat insulation performance can be attached to the surface of the glass fiber, and 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. Therefore, the embodiment 3 further improves the scheme of the embodiment 2, and in order to improve the adhesion rate of the silica aerogel on the surface of the glass fiber, the invention firstly uses the sodium hydroxide solution to treat the surface of the glass fiber, and after the treatment of the sodium hydroxide solution, the surface of the glass fiber is slightly corroded to generate more defects and active sites, which is beneficial to forming bonds on the surface of Si-OH, and an aerogel structure is formed by taking the glass fiber as a center, so that the adhesion amount of the silica aerogel on the surface of the glass fiber is improved, and the floating escape of the silica aerogel is reduced. However, the present inventors have found that, when aerogel-modified glass fibers were prepared by the method of example 3, if the pH was adjusted to be alkaline by using a conventional alkaline solution during the gelation process in step S3 (i.e., the pH was adjusted by using a sodium hydroxide solution and an ammonia solution in step S3 in comparative example 2 and comparative example 3, respectively), the final product was a whole gel mass filled with glass fibers, rather than glass fibers having a large amount of silica aerogel grown on the surface thereof. This shows that in the process of hydrolyzing the liquid gel with ethyl orthosilicate, the nucleation centers are not completely glass fibers, i.e. Si-OH does not completely build an aerogel structure network by taking the glass fibers as the centers, but a large amount of Si-OH can 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 various alkali liquids to try to inhibit the self-condensation behavior of Si-OH, and finds that the triethylamine is used for replacing sodium hydroxide, the self-condensation behavior of Si-OH can be effectively inhibited, and finally the obtained gel block is easy to crush into fibrous filaments after being dried, which shows that the formation of a gel structure by Si-OH condensation is carried out by taking glass fibers as the center, so that the obtained product has extremely high proportion of aerogel modified glass fibers after being crushed. However, since the self-condensation behavior of Si-OH is suppressed, the gel rate is slow, and thus the gel time needs to be extended. Therefore, the alkali-resistant heat-insulating cement mortar prepared in example 3 has a significantly lower thermal conductivity than comparative examples 2 and 3. In example 4, the invention further performs hydrophobic treatment on the prepared aerogel modified glass fiber, 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 further improved. In comparative example 1, the glass fiber is treated by acid, which causes severe corrosion to the glass fiber, greatly affects the mechanical properties of the glass fiber, and reduces the surface area of the glass fiber, thereby reducing the attachment rate of the silica aerogel.
Test example 2
Alkali resistance test: the aerogel modified glass fibers prepared by the examples and comparative examples of the present invention were tested for their alkali-resistant strength retention according to GB/T38143-2019 alkali-resistant glass-filled fibers for cement concrete and mortar, and all aerogel modified glass fibers were retained for 35mm length for the test.
The sample is dried for 1h at 50 ℃. The tensile speed of the tensile testing machine was 1mm/min.
For each example, 20 different samples were taken and tested, and the results averaged. The test results are shown in table 2.
Table 2: alkali-resistant strength retention of glass-filled fibers
| Alkali-resistant Strength 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 resistance retention rate, because the silica aerogel on the surface of the aerogel modified glass fiber treated by the scheme in example 4 has the highest adhesion rate, and the alkali resistance of the aerogel modified glass fiber is further improved by the hydrophobic treatment, so that the alkali resistance retention rate of the aerogel modified glass fiber is the highest in the alkaline environment of the cement supernatant. The retention of alkali resistance strength of the aerogel-modified glass fibers prepared in example 3 was lower than that of example 4, because they were not subjected to hydrophobic treatment and were slightly lower in alkali resistance than the aerogel-modified glass fibers subjected to hydrophobic treatment. The alkali-resistant strength retention rate of the aerogel-modified glass fiber prepared in example 2 is further reduced, because the silica aerogel adhesion rate of the glass fiber adopted in example 2 is very low compared with that of example 3 because the glass fiber is not subjected to alkali treatment, and the alkali-resistant strength retention rate is lower. The glass fiber used in example 1 was not treated at all, and the alkali-resistant strength retention rate was the lowest because the glass fiber was very susceptible to alkali attack.
Claims (8)
1. The preparation method of the alkali-resistant heat-insulating cement mortar is characterized by comprising the following steps of: and uniformly mixing the dry materials and the aggregate, and then adding water for stirring to obtain the alkali-resistant heat-insulating cement mortar.
2. The method for preparing alkali-resistant heat-insulating cement mortar of claim 1, wherein the dry material comprises the following raw materials: cement, aerogel modified glass fiber, a water reducing agent and sodium silicate.
3. The method for preparing alkali-resistant heat-insulating cement mortar according to claim 2, wherein the cement is at least one of Portland cement P.I, portland cement P.II and composite Portland cement P.C.
4. The method for preparing alkali-resistant heat-insulating cement mortar as claimed in claim 2, wherein the aggregate is fine aggregate and has a water content of 2wt% or less.
5. The method for preparing alkali-resistant insulating cement mortar according to claim 2, wherein the water reducer is at least one of a naphthalene-based high-efficiency water reducer, an aliphatic high-efficiency water reducer, an amino high-efficiency water reducer and a polycarboxylic acid high-performance water reducer.
6. The method for preparing alkali-resistant heat-insulating cement mortar as claimed in claim 2, wherein the method for preparing aerogel modified glass fiber comprises the following steps:
s1, according to parts by mass, soaking 20-40 parts of glass fiber powder into 90-100 parts of sodium hydroxide aqueous solution, stirring at a rotating speed of 200-300r/min for 20-30min, and filtering, washing and drying to obtain alkali-treated glass fiber;
s2, mixing 10-20 parts of tetraethyl orthosilicate and 80-90 parts of 75wt% ethanol aqueous solution by mass, adjusting the pH value to 3.0-4.0 by using 10-14wt% hydrochloric acid, and standing at 35-45 ℃ for 2-3 hours to obtain silica sol;
s3, mixing 2-4 parts by mass of dimethylformamide, 20-40 parts by mass of alkali-treated glass fiber powder prepared in the step S1 and 60-80 parts by mass of silica sol prepared in the step S2, dispersing for 10-20min at the rotating speed of 6000-8000r/min, adjusting the pH value to 8.0-9.0 by using triethylamine, stirring and reacting for 20-40min at the rotating speed of 60-80r/min, and then placing at 30-40 ℃ for gelation for 14-16h to obtain wet gel fiber;
s4, mixing the wet gel fiber and absolute ethyl alcohol according to a bath ratio of 1g: (5-10) mL, mixing and aging for 12-24h, taking out the gel, drying at 80-100 ℃ for 12-24h, and cooling to room temperature to obtain the aerogel modified glass fiber.
7. The method for preparing alkali-resistant heat-insulating cement mortar as claimed in claim 2, wherein the concentration of the aqueous sodium hydroxide solution in step S1 is 3-5wt%.
8. An alkali-resistant heat-insulating cement mortar, characterized in that it is prepared by the method for preparing the alkali-resistant heat-insulating cement mortar of any one of claims 1 to 7.
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