CN110981499A - Composite ceramic fiber for building concrete and preparation method thereof - Google Patents

Composite ceramic fiber for building concrete and preparation method thereof Download PDF

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CN110981499A
CN110981499A CN201911335181.2A CN201911335181A CN110981499A CN 110981499 A CN110981499 A CN 110981499A CN 201911335181 A CN201911335181 A CN 201911335181A CN 110981499 A CN110981499 A CN 110981499A
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sol
mixed solution
hours
stirring
composite ceramic
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彭雄义
王慧鹏
张延�
陈卓
董雄伟
刘仰硕
吕少仿
梁永红
蔡映杰
王强
杨锋
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Wuhan Textile University
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Abstract

The invention relates to a composite ceramic fiber used in building concrete and a preparation method thereof. The invention uses SiO2Sol, Al2O3And uniformly mixing the sol and the SiC sol to prepare mixed sol, spinning the mixed sol to prepare gel fiber, and roasting the gel fiber at high temperature to prepare the composite ceramic fiber. The invention compares the compressive strength of the finished products of cement mortar doped with composite ceramic fiber and PP fiber in 3 days, 7 days and 28 days, and in 28 daysIn the process, the compressive strength of the finished product of the cement mortar doped with the composite ceramic fiber is obviously higher than that of the finished product of the cement mortar doped with the PP fiber.

Description

Composite ceramic fiber for building concrete and preparation method thereof
Technical Field
The invention belongs to the technical field of preparation of composite ceramic fibers, and particularly relates to a composite ceramic fiber used in building concrete and a preparation method thereof.
Background
At present, with the continuous development of concrete technology, various new types of concrete are continuously developed. The short fibers are added into the plain concrete, so that the brittleness problem of the plain concrete can be effectively improved, and the mechanical properties of the plain concrete such as compression resistance, tensile resistance, fracture resistance and the like are obviously enhanced. Particularly, in concrete in contact with water, corrosion of water may cause damage to reinforcing bars, thereby seriously affecting the durability of concrete, and thus, adding a small amount of short fibers to concrete in contact with water may effectively increase the lifespan of concrete. With regard to the mechanism of action of the short fibers in concrete, the following can be analyzed: the concrete short fibers can be quickly and uniformly dispersed in the concrete to form an irregular supporting system, so that the directional stress of the concrete is effectively dispersed, the number and the size of primary microcracks are reduced, the generation and the expansion of the primary cracks are inhibited, the anti-cracking and anti-permeability capacity of the concrete is obviously enhanced, the toughness of the concrete is enhanced, and the service life of the concrete is obviously prolonged.
The short fibers that can be used in concrete are mainly: polypropylene (PP) fibers, and the like, PP fibers have found wide use in many concrete applications. However, PP fiber has limited its wide application in concrete due to its high price. Currently, the research on concrete fibers is also receiving a lot of attention, such as: chinese invention patent application No. 201510991237.5 discloses a composite concrete fiber material and a manufacturing method thereof, wherein the fiber material of the patent mainly comprises the following raw materials: polyethylene glycol terephthalate, polypropylene, ethylene-vinyl acetate copolymer, paraffin, color master batch and the like, and has the defects that the raw materials are relatively complex in source, part of the raw materials are relatively expensive, and the compatibility between the raw materials and concrete needs to be further studied; the publication No. CN201024367Y discloses a fiber for asphalt concrete, the cross section of the fiber is irregular diamond-shaped, the disadvantage is that the application target is asphalt concrete, and the application range has certain limitation. Along with the large-scale construction of concrete buildings, the demand of concrete fibers is increasing, so that the invention of the concrete fiber with low price and wide application field becomes a problem to be solved urgently.
Disclosure of Invention
The invention aims to provide a composite ceramic fiber for building concrete, which can be used for building concrete and can obviously improve the compressive strength of a cement mortar finished product so as to solve the defects in the prior art.
The invention aims to provide a composite ceramic fiber used in building concrete, which can be obtained by the following preparation method: mixing SiO2Sol, Al2O3Uniformly mixing the sol and the SiC sol to prepare mixed sol, spinning the mixed sol to prepare gel fibers, and roasting the gel fibers at high temperature to prepare the composite ceramic fibers, namely the composite ceramic fibers used in the building concrete.
Another object of the present invention is to provide the above method for preparing composite ceramic fiber for use in building concrete, the method comprising the steps of:
(1)SiO2preparing sol: mixing absolute ethyl alcohol, deionized water and 10% hydrochloric acid aqueous solution to prepare a mixed solution a; dissolving ethyl orthosilicate in absolute ethyl alcohol to prepare a mixed solution b; slowly dripping the mixed solution a into the mixed solution b for 1-3 hours; after the dropwise addition is finished, stirring for 1-3 hours; after stirring, standing and aging for 3-6 hours; the temperature of the whole process control system is as follows: 70-85 ℃; and preparing the sol.
Preferably, the volume ratio of the absolute ethyl alcohol (mL), the deionized water (mL) and the 10% hydrochloric acid aqueous solution (mL) in the mixed solution a is as follows: 30-40: 10-20; the volume ratio of the ethyl orthosilicate (mL) to the absolute ethyl alcohol (mL) in the mixed solution b is as follows: 1: 2-4.
(2)Al2O3Preparing sol: mixing absolute ethyl alcohol, deionized water and 10% hydrochloric acid aqueous solution to prepare a mixed solution a; dissolving aluminum isopropoxide and aluminum nitrate in deionized water to prepare a mixed solution b; slowly dripping the mixed solution a into the mixed solution b for 1-3 hours; after the dropwise addition is finished, stirring for 60-72 hours, wherein the stirring reaction temperature is 85-90 ℃; after stirring, standing and aging for 10-20 hours at the temperature of 30-40 ℃; and preparing the sol.
Preferably, the volume ratio of the absolute ethyl alcohol (mL), the deionized water (mL) and the 10% hydrochloric acid aqueous solution (mL) in the mixed solution a is as follows: 30-40: 10-20; the mass-volume ratio of aluminum isopropoxide (g), aluminum nitrate (g) and deionized water (mL) in the mixed solution b is as follows: 1: 2-4: 20-40.
(3) Preparation of SiC sol: mixing ethyl orthosilicate, deionized water and 3% ammonia water solution, and stirring for 1-3 hours at 40-60 ℃ to prepare a mixed solution a; dissolving sucrose in deionized water to prepare a mixed solution b; slowly dripping the mixed solution b into the mixed solution a for 1-3 hours; after the dropwise addition is finished, stirring for 5-8 hours, wherein the stirring reaction temperature is 85-90 ℃; after stirring, standing for 10-20 hours at the temperature of 30-40 ℃; and preparing the sol.
Preferably, the volume ratio of the tetraethoxysilane (mL), the deionized water (mL) and the 10% ammonia water solution (mL) in the mixed solution a is as follows: 30-40: 10-20; the mass-to-volume ratio of the sucrose (g) to the deionized water (mL) in the mixed solution b is as follows: 1: 2-4.
(4) Preparing the composite ceramic fiber: SiO prepared in the step (1)2Sol, Al prepared in step (2)2O3Stirring and mixing the sol and the SiC sol prepared in the step (3) to prepare mixed sol, wherein the stirring time is 3-5 hours, so as to prepare initial mixed sol; standing and aging the mixture for 4-8 hours at the temperature of 20-40 ℃, continuously measuring the viscosity of the mixed sol, namely immersing the mixed sol into the sol by using a glass rod and slowly lifting the glass rod, observing the formation state of the long and thin silk threads, and preparing the mixed sol to be spun when the sol meets the viscosity of spinning and the viscosity of the sol reaches 30-90 Pa.s; spinning the mixed sol on spinning equipment to form silk threads, drying the silk threads for 5-8 hours at the temperature of 80-90 ℃ to form gel fibers, and roasting the gel fibers for 3-5 hours at the temperature of 800-900 ℃ to form SiO2-Al2O3-SiC composite ceramic fibers, i.e. composite ceramic fibers used in building concrete; SiO 22-Al2O3The diameter of the-SiC composite ceramic fiber is: 5 to 25 μm.
Preferably, the SiO prepared in step (1)2Sol, Al prepared in step (2)2O3The volume ratio of the sol to the SiC sol prepared in the step (3) is as follows: 40-60: 10-20.
The invention has the following remarkable characteristics:
(1) the invention uses SiO2Sol, Al2O3Uniformly mixing the sol and the SiC sol to prepare SiO2-Al2O3-SiC composite ceramic fibers; the composite ceramic fiber has the excellent performances of three single fibers.
(2) Compares the compressive strength of the finished products of cement mortar doped with composite ceramic fiber and PP fiber in 3 days, 7 days and 28 days, and is doped with SiO2-Al2O3The strength of the cement mortar finished product of the-SiC composite ceramic fiber is slightly higher than that of the cement mortar finished product doped with the PP fiber at 3 days and 7 days; however, as the curing time increases, at 28 days, the admixture is addedSiO2-Al2O3The compression strength of the cement mortar finished product of the-SiC composite ceramic fiber is obviously higher than that of the cement mortar finished product doped with the PP fiber.
(3) The preparation method is simple, has wide raw material sources, and has good application and popularization prospects.
Drawings
FIG. 1 is a schematic view of a spinning apparatus according to examples 1 to 3 (1. a spinning solution container; 2. a metering pump; 3. a gas inlet; 4. a spinning disk; 5. a spinning bar; 6. an oiling device; 7. a godet roll; 8. a take-up device);
FIG. 2 SiO preparation of example 12-Al2O3Electron micrographs of-SiC composite ceramic fiber a.
Detailed Description
The examples described below illustrate the invention in detail.
Example 1
In this embodiment, a composite ceramic fiber for use in building concrete is prepared by the following method, including the steps of:
(1)SiO2preparing sol: mixing 70mL of absolute ethyl alcohol, 70mL of deionized water and 30mL of 10% hydrochloric acid aqueous solution to prepare a mixed solution a; dissolving 70mL of ethyl orthosilicate in 210mL of absolute ethanol to prepare a mixed solution b; slowly dripping the mixed solution a into the mixed solution b for 2 hours; after the dropwise addition is finished, stirring for 2 hours; after stirring, standing and aging for 4 hours; the temperature of the whole process control system is as follows: 80 ℃; and preparing the sol.
(2)Al2O3Preparing sol: mixing 70mL of absolute ethyl alcohol, 70mL of deionized water and 30mL of 10% hydrochloric acid aqueous solution to prepare a mixed solution a; dissolving 10g of aluminum isopropoxide and 30g of aluminum nitrate in 300mL of deionized water to prepare a mixed solution b; slowly dripping the mixed solution a into the mixed solution b for 2 hours; after the dropwise addition is finished, stirring for 65 hours, wherein the stirring reaction temperature is 86 +/-1 ℃; after stirring, standing and aging for 15 hours at the standing and aging temperature of 35 ℃; and preparing the sol.
(3) Preparation of SiC sol: mixing 70mL of ethyl orthosilicate, 70mL of deionized water and 30mL of 3% ammonia water solution, and stirring at 50 ℃ for 2 hours to prepare a mixed solution a; dissolving 50g of sucrose in 150mL of deionized water to prepare a mixed solution b; slowly dripping the mixed solution b into the mixed solution a for 2 hours; after the dropwise addition is finished, stirring for 6 hours, wherein the stirring reaction temperature is 88 +/-1 ℃; after stirring, standing for 15 hours at the standing temperature of 35 ℃; and preparing the sol.
(4) Preparing ceramic fibers: 100mL of SiO prepared in step (1)2Sol, 100mL of Al prepared in step (2)2O3Stirring and mixing the sol and 30mL of the SiC sol prepared in the step (3) to prepare mixed sol, wherein the stirring time is 4 hours, so as to prepare initial mixed sol; aging at 30 deg.C for 6 hr to obtain mixed sol with viscosity of 66.8 Pa.s; spinning the mixed sol into silk threads on spinning equipment, wherein the spinning equipment is shown as figure 1; drying the silk thread at 85 deg.C for 6 hr to obtain gel fiber, and calcining the gel fiber at 850 deg.C for 4 hr to obtain SiO2-Al2O3-SiC composite ceramic fibers a; SiO 22-Al2O3The electron micrograph of the-SiC composite ceramic fiber a is shown in FIG. 2, SiO2-Al2O3The diameter of the-SiC composite ceramic fiber a is: 21.3 μm.
Example 2
In this embodiment, a composite ceramic fiber for use in building concrete is prepared by the following method, including the steps of:
(1)SiO2preparing sol: mixing 60mL of absolute ethyl alcohol, 60mL of deionized water and 20mL of 10% hydrochloric acid aqueous solution to prepare a mixed solution a; dissolving 70mL of ethyl orthosilicate in 140mL of absolute ethyl alcohol to prepare a mixed solution b; slowly dripping the mixed solution a into the mixed solution b for 2 hours; after the dropwise addition is finished, stirring for 2 hours; after stirring, standing and aging for 4 hours; the temperature of the whole process control system is as follows: 82 +/-1 ℃; and preparing the sol.
(2)Al2O3Preparing sol: mixing 60mL of absolute ethyl alcohol, 60mL of deionized water and 20mL of 10% hydrochloric acid aqueous solution to prepare a mixed solution a; will be provided withDissolving 10g of aluminum isopropoxide and 20g of aluminum nitrate in 200mL of deionized water to prepare a mixed solution b; slowly dripping the mixed solution a into the mixed solution b for 2 hours; after the dropwise addition is finished, stirring for 60 hours, wherein the stirring reaction temperature is 86 +/-1 ℃; after stirring, standing and aging for 15 hours at the standing and aging temperature of 35 ℃; and preparing the sol.
(3) Preparation of SiC sol: mixing 60mL of ethyl orthosilicate, 60mL of deionized water and 20mL of 3% ammonia water solution, and stirring at 50 ℃ for 2 hours to prepare a mixed solution a; dissolving 50g of sucrose in 100mL of deionized water to prepare a mixed solution b; slowly dripping the mixed solution b into the mixed solution a for 2 hours; after the dropwise addition is finished, stirring for 6 hours, wherein the stirring reaction temperature is 86 +/-1 ℃; after stirring, standing for 15 hours at the standing temperature of 35 ℃; and preparing the sol.
(4) Preparing ceramic fibers: 80mL of SiO prepared in step (1)2Sol, 80mL of Al prepared in step (2)2O3Stirring and mixing the sol and 20mL of the SiC sol prepared in the step (3) to prepare mixed sol, wherein the stirring time is 4 hours, so as to prepare initial mixed sol; aging at 20 deg.C for 4 hr to obtain mixed sol with viscosity of 45.8 Pa.s; spinning the mixed sol into silk threads on spinning equipment, wherein the spinning equipment is shown as figure 1; drying the silk thread at 85 deg.C for 6 hr to obtain gel fiber, and calcining the gel fiber at 800 deg.C for 4 hr to obtain SiO2-Al2O3-SiC composite ceramic fibers b; SiO 22-Al2O3The diameter of the-SiC composite ceramic fiber b is: 18.6 μm.
Example 3
In this embodiment, a composite ceramic fiber for use in building concrete is prepared by the following method, including the steps of:
(1)SiO2preparing sol: mixing 80mL of absolute ethyl alcohol, 80mL of deionized water and 40mL of 10% hydrochloric acid aqueous solution to prepare a mixed solution a; dissolving 70mL of ethyl orthosilicate in 280mL of absolute ethanol to prepare a mixed solution b; slowly dripping the mixed solution a into the mixed solution b for 3 hours; after the dropwise addition, the mixture was stirred for 3 hoursWhen the current is over; after stirring, standing and aging for 4 hours; the temperature of the whole process control system is as follows: 80 ℃; and preparing the sol.
(2)Al2O3Preparing sol: mixing 80mL of absolute ethyl alcohol, 80mL of deionized water and 40mL of 10% hydrochloric acid aqueous solution to prepare a mixed solution a; dissolving 10g of aluminum isopropoxide and 40g of aluminum nitrate in 400mL of deionized water to prepare a mixed solution b; slowly dripping the mixed solution a into the mixed solution b for 3 hours; after the dropwise addition is finished, stirring for 72 hours, wherein the stirring reaction temperature is 88 +/-1 ℃; after stirring, standing and aging for 15 hours at the standing and aging temperature of 35 ℃; and preparing the sol.
(3) Preparation of SiC sol: mixing 80mL of ethyl orthosilicate, 80mL of deionized water and 40mL of 3% ammonia water solution, and stirring at 50 ℃ for 2 hours to prepare a mixed solution a; dissolving 50 parts of sucrose in 200mL of deionized water to prepare a mixed solution b; slowly dripping the mixed solution b into the mixed solution a for 3 hours; after the dropwise addition is finished, stirring for 6 hours, wherein the stirring reaction temperature is 88 +/-1 ℃; after stirring, standing for 15 hours at the standing temperature of 35 ℃; and preparing the sol.
(4) Preparing ceramic fibers: 120mL of SiO prepared in step (1)2Sol, 120mL of Al prepared in step (2)2O3Stirring and mixing the sol and 40mL of the SiC sol prepared in the step (3) to prepare mixed sol, wherein the stirring time is 5 hours, so as to prepare initial mixed sol; aging at 40 deg.C for 8 hr to obtain mixed sol with viscosity of 81.5 Pa.s; spinning the mixed sol into silk threads on spinning equipment, wherein the spinning equipment is shown as figure 1; drying the silk thread at 90 deg.C for 8 hr to obtain gel fiber, and calcining the gel fiber at 900 deg.C for 4 hr to obtain SiO2-Al2O3-SiC composite ceramic fibers c; SiO 22-Al2O3The diameter of the-SiC composite ceramic fiber c is: 20.5 μm.
Application performance evaluation example:
SiO prepared in the above embodiments 1 to 3 of the present invention2-Al2O3-SiC composite ceramic fibers a, b, c and PP fibers purchased from market for waterAnd (5) testing the influence of the strength of the finished mud mortar product.
Preparing cement mortar: 400g of cement and 1200g of sand are weighed respectively and mixed with 1g of SiO2-Al2O3Adding a water reducing agent with specified mixing amount and a certain amount of water into the SiC composite ceramic fibers a, B and c and PP fibers, controlling the mortar consistency to be standard consistency, stirring the mixture by a mortar stirrer, filling the mixture into a cube test mold with the side length of 40 multiplied by 160mm, carrying out vibration molding, curing the mixture in a standard curing box for 24 hours, then demolding, and continuously curing the demolded test piece in the curing box (HBY-40B type cement constant temperature and humidity standard curing box, produced by Dongfu test instrument Co., Ltd. of Wu county, Suzhou) to a specified age (3 days, 7 days and 28 days). Samples incorporating each fiber were sampled 20 times and the test results were averaged.
Testing the compressive strength of cement mortar: the cement mortar cured to the specified age is respectively tested for compressive strength by a compression tester (NYL-300A type digital compression tester, produced by a tin-free double-Newton building material instrument and equipment factory). The test results are shown in table 1:
TABLE 1SiO2-Al2O3Effect of-SiC composite ceramic fibers a, b, c and PP fibers on compressive Strength (MPa) of Cement mortar
Doped fibers 3 days 7 days 28 days
Blank space 28.4 33.7 51.6
SiO2-Al2O3-SiC composite ceramic fiber a 51.1 59.7 82.6
SiO2-Al2O3-SiC composite ceramic fiber b 50.2 58.5 83.7
SiO2-Al2O3-SiC composite ceramic fiber c 52.3 59.8 83.1
PP fiber 47.6 55.8 75.7
As can be seen from Table 1, SiO was added2-Al2O3The strength of the cement mortar finished products of the-SiC composite ceramic fibers a, b and c is slightly higher than that of the cement mortar finished products doped with the PP fibers at 3 days and 7 days; however, with the increase of the curing time, at 28 days, SiO is doped2-Al2O3The compression strength of the cement mortar finished products of the-SiC composite ceramic fibers a, b and c is obviously higher than that of the cement mortar finished products doped with the PP fibers. This shows that the composite ceramic fiber prepared by the method of the invention is a good fiber for enhancing the strength of the finished cement-based material.

Claims (6)

1. A preparation method of composite ceramic fiber used in building concrete is characterized by comprising the following steps:
mixing SiO2Sol, Al2O3Stirring and mixing the sol and the SiC sol to prepare mixed sol, wherein the stirring time is 3-5 hours, and preparing initial mixed sol; aging the mixture for 4 to 8 hours at the temperature of between 20 and 40 ℃ until the viscosity of the mixture reaches 30 to 90 Pa.s, and preparing mixed sol to be spun; spinning the mixed sol on spinning equipment to form silk threads, drying the silk threads for 5-8 hours at the temperature of 80-90 ℃ to form gel fibers, and roasting the gel fibers for 3-5 hours at the temperature of 800-900 ℃ to form SiO2-Al2O3The SiC composite ceramic fiber is the composite ceramic fiber used in building concrete.
2. The method of claim 1, wherein the SiO is formed by a process comprising mixing the SiO with a binder to form a composite ceramic fiber2The preparation method of the sol comprises the following steps: mixing absolute ethyl alcohol, deionized water and 10% hydrochloric acid aqueous solution to prepare a mixed solution a; dissolving ethyl orthosilicate in absolute ethyl alcohol to prepare a mixed solution b; slowly dripping the mixed solution a into the mixed solution b for 1-3 hours; after the dropwise addition is finished, stirring for 1-3 hours; after stirring, standing and aging for 3-6 hours; the temperature of the whole process control system is as follows: 70-85 ℃; to obtain SiO2Sol; the volume ratio of the absolute ethyl alcohol, the deionized water and the 10% hydrochloric acid aqueous solution in the mixed solution a is as follows: (30-40) mL, (10-20) mL; the volume ratio of the ethyl orthosilicate to the absolute ethyl alcohol in the mixed solution b is as follows: 1mL to (2-4) mL.
3. The method of claim 1, wherein the Al is selected from the group consisting of Al, and ti2O3The preparation method of the sol comprises the following steps: mixing absolute ethyl alcohol, deionized water and 10% hydrochloric acid aqueous solution to prepare a mixed solution a; dissolving aluminum isopropoxide and aluminum nitrate in deionized water to prepare a mixed solution b; slowly dripping the mixed solution a into the mixed solution b for 1-3 hours; stirring for 60-72 hours after the dropwise addition is finished, and stirring for reaction at a temperatureThe temperature is 85-90 ℃; after stirring, standing and aging for 10-20 hours at the temperature of 30-40 ℃; to obtain Al2O3Sol; the volume ratio of the absolute ethyl alcohol, the deionized water and the 10% hydrochloric acid aqueous solution in the mixed solution a is as follows: (30-40) mL, (10-20) mL; the mass-volume ratio of the aluminum isopropoxide to the aluminum nitrate to the deionized water in the mixed solution b is as follows: 1g, (2-4) g, (20-40) mL.
4. The method for preparing the composite ceramic fiber for building concrete according to claim 1, wherein the SiC sol is prepared by the following steps: mixing ethyl orthosilicate, deionized water and 3% ammonia water solution, and stirring for 1-3 hours at 40-60 ℃ to prepare a mixed solution a; dissolving sucrose in deionized water to prepare a mixed solution b; slowly dripping the mixed solution b into the mixed solution a for 1-3 hours; after the dropwise addition is finished, stirring for 5-8 hours, wherein the stirring reaction temperature is 85-90 ℃; after stirring, standing for 10-20 hours at the temperature of 30-40 ℃; preparing SiC sol; the volume ratio of the ethyl orthosilicate, the deionized water and the 10% ammonia water solution in the mixed solution a is as follows: (30-40) mL, (10-20) mL; the mass volume ratio of the sucrose to the deionized water in the mixed solution b is as follows: 1g to (2-4) mL.
5. The method of claim 1, wherein the composite ceramic fiber is prepared by the following steps: the SiO2Sol, Al2O3The volume ratio of the sol to the SiC sol is as follows: (40-60): (10-20).
6. The composite ceramic fiber for building concrete is characterized by being prepared by the preparation method of the composite ceramic fiber for building concrete according to any one of claims 1 to 5.
CN201911335181.2A 2019-12-23 2019-12-23 Composite ceramic fiber for building concrete and preparation method thereof Pending CN110981499A (en)

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