High-strength and high-modulus inorganic mineral fiber prepared from water-quenched slag and preparation method of high-strength and high-modulus inorganic mineral fiber

Abstract

The invention belongs to the technical field of inorganic mineral fiber preparation, and provides a high-strength and high-modulus inorganic mineral fiber prepared from water-quenched slag and a preparation method of the high-strength and high-modulus inorganic mineral fiber. Firstly, the chemical purity of raw materials is improved through density separation and acid pickling, meanwhile, Na2CO3 and Fe2O3 are added, the tendency of crystal precipitation is reduced, and the vitrification characteristic of water-quenched slag is improved; secondly, the composite oxide modifier further optimizes the structure of the glass network, and B2O3 enhances the chemical stability of the glass network and reduces the melt viscosity by forming a B-O-Si bond; y2O3 provides high electric field intensity, inhibits crystal precipitation and enhances the crosslinking degree of a network; v2O5 provides a redox buffer function through a variable valence state, so that the chemical environment in the melting process is optimized, and the creep resistance is improved; and finally, a compact Al2O3 coating is formed on the surface of the fiber, so that the mechanical strength, the oxidation resistance, the corrosion resistance and the high-temperature stability of the fiber are improved.

Description

Technical Field

[0001] The present invention belongs to the technical field of inorganic mineral fiber preparation, and relates to a method for preparing high-strength and high-modulus inorganic mineral fibers from water-quenched slag and its preparation method. Background Art

[0002] Quenched slag is an important solid waste generated in the process of metallurgical industry production, and is a special material formed by the rapid cooling of high-temperature molten slag after metal smelting. Its production process mainly originates from steel smelting. By quickly contacting the high-temperature molten slag with a large amount of cold water, it is rapidly cooled and solidified to form an amorphous vitreous solid material. The chemical composition of water-quenched slag is complex, mainly including silicon dioxide, calcium oxide, aluminum oxide, magnesium oxide and other trace oxides. This material has an amorphous structure. Due to the rapid cooling to form a vitreous solid, it has a large surface area, high chemical activity and uniform microstructure. Water-quenched slag has important resource utilization value in industrial production and can be widely used in fields such as cement production, civil engineering, and subgrade materials. Its unique chemical composition and physical structure make it a very potential industrial by-product.

[0003] However, in the process of preparing water-quenched slag into inorganic mineral fibers, the most important problem is that during the high-temperature heat treatment stage, the components in the water-quenched slag are extremely prone to crystal phase precipitation. This crystal phase precipitation phenomenon will seriously affect the microstructure of the fibers, resulting in the formation of a large number of crystal nuclei inside the fibers, significantly reducing the overall strength of the fibers. Crystal phase precipitation not only makes the internal structure of the fibers uneven, but also forms stress concentration areas in the fibers, fundamentally weakening the mechanical properties of the fibers and making it difficult to meet the technical requirements of high strength and high modulus. Therefore, it is necessary to suppress the crystal phase precipitation during the preparation of water-quenched slag, maintain the amorphous structure of the fibers, and improve the performance of inorganic mineral fibers. Summary of the Invention

[0004] Aiming at the deficiencies of the existing technology, the purpose of the present invention is to provide a method for preparing high-strength and high-modulus inorganic mineral fibers from water-quenched slag and its preparation method. By performing density separation, pickling purification and high-temperature calcination on water-quenched slag, introducing fluxing agents Na2CO3 and Fe2O3, optimizing its chemical composition, and enhancing its vitrification ability, a composite modification system composed of B2O3, Y2O3 and V2O5 is used to improve the uniformity, chemical stability and processing performance of the melt through enhancing network cross-linking, inhibiting crystal precipitation and redox buffering effects respectively. A dense Al2O3 coating is deposited and calcined on the fiber surface to significantly improve the high-temperature resistance, chemical corrosion resistance and matrix interface bonding performance of the fiber, so as to meet the actual production needs.

[0005] To achieve this purpose, the present invention adopts the following technical solutions: In a first aspect, the present invention provides a preparation method for preparing high-strength and high-modulus inorganic mineral fibers using water-quenched slag, and the preparation method is as follows: Step S1: Put the water-quenched slag raw material into a vibrating screen for particle grading, retain the medium particle part, pour the medium particle part of the water-quenched slag into a lithium chloride solution, collect the floating part, filter and wash it, then dry it thoroughly at a first temperature. Place the dried floating water-quenched slag in a hydrochloric acid solution, stir it thoroughly at room temperature, filter and wash it, and then dry it thoroughly at the first temperature to obtain pickled water-quenched slag particles. Crush the pickled water-quenched slag particles to below the target particle size, then mix them with Na2CO3 and Fe2O3, raise the temperature to a second temperature and continue calcining. After the calcining is completed, cool it to room temperature to obtain high-temperature sintered water-quenched slag; Step S2: Mix a boric acid solution and a yttrium nitrate solution to obtain a mixed solution. Then dissolve vanadium pentoxide in ammonia water and add it to the above mixed solution. Stir it evenly and then use ammonia water to adjust the pH to 8 - 8.5. Keep stirring to complete the precipitation reaction, filter and wash it, and then dry it at a third temperature to obtain a wet powder precursor. Then mix H3BO3, Y2O3 and V2O5 to obtain a mixture. Put the mixture and the wet powder precursor into a ball mill and add ethanol. After ball milling, calcine it at a second temperature to obtain a composite oxide modifier; Step S3: Mix the high-temperature sintered water-quenched slag, the composite oxide modifier and borax, and obtain a mixed material after ball milling. Heat the mixed material to a fourth temperature, and use a fiber blowing device to draw the molten material into fibers. Then place the fibers in an argon atmosphere and perform annealing treatment at a fifth temperature to obtain annealed fibers; Step S4: Immerse the annealed fibers in absolute ethanol, ultrasonically clean to remove surface contaminants, and then dry them at a first temperature. Dissolve aluminum nitrate in deionized water, stir until dissolved, then add an ammonia water solution to adjust the pH to 7.5 to obtain an Al(OH)3 suspension. Immerse the dried annealed fibers in the Al(OH)3 suspension, take out the annealed fibers after a certain time, and calcine them at a second temperature to obtain high-strength and high-modulus inorganic mineral fibers prepared using water-quenched slag.

[0006] Water quenched slag is a complex solid waste, usually composed of various silicates, aluminosilicates, oxides and a small amount of metal elements. Its main components include: amorphous silicate glass phase, such as SiO2 - Al2O3 - CaO system; crystalline phase impurities, such as calcium oxide CaO, magnesium oxide MgO, unreacted metallic iron Fe, etc.; unreacted light components, such as porous amorphous materials or low - density vitreous particles. By placing the water quenched slag in a lithium chloride solution, the lower - density particles (such as particles containing amorphous light silicates) will float on the surface of the solution, while the higher - density particles (such as metal oxides and unreacted metals) will sink to the bottom of the solution. The high - density particles in water quenched slag usually contain metallic iron, which may cause difficulties in uniform melting during the fiber preparation process. High - density residues (such as unreacted metals or metal oxides) may introduce defects and reduce the mechanical properties of the fibers. The floating part is mainly low - density amorphous silicate particles, which are the core raw materials for fiber preparation. Amorphous silicate particles have a high glass - forming ability and can form uniform vitreous fibers during high - temperature melting. In contrast, the crystalline components in high - density impurities tend to crystallize more at high temperatures, resulting in grain boundaries within the material and reducing the strength and modulus of the fibers. The flotation process removes high - density impurities. If these high - density particles are not separated, non - uniform melts may be generated during the subsequent melting process, leading to non - uniform phases during the fiberization process; introducing brittle impurities, forming stress concentration points, and reducing the mechanical properties of the fibers; causing the fiber surface to be rough and affecting the final modulus and strength.

[0007] The amorphous silicate in water-quenched slag is a substance that does not form a crystal structure under rapid cooling. Its molecular structure is a disordered silicon-oxygen network. This network structure has a high vitrification ability and is the core material for fiber preparation. The key properties of the amorphous state lie in the disorder and uniformity of its structure. This disorder endows it with good mechanical properties and thermal stability. However, crystalline impurities such as CaO, MgO, and unreacted silicates in water-quenched slag often exist in the form of local crystal phases or weakly bonded phases, distributed in the amorphous matrix. Their presence will cause the material to form crystallization phases (such as CaSiO3) at high temperatures. These crystallization phases destroy the uniformity of the glassy state, thereby reducing the strength and modulus of the fiber. Under high-temperature conditions, the crystalline impurities will chemically react with silicon oxides (SiO2) or aluminosilicates (Al2O3·SiO2) in the amorphous matrix to generate new crystal phases. For example, the reaction of CaO with SiO2 forms calcium silicate crystals. CaO is a basic oxide that will react with SiO2 in the amorphous silicate matrix at high temperatures to form CaSiO3 crystals. CaSiO3 is a crystallization phase, and its crystal structure destroys the original continuous network structure. The reaction of MgO with SiO2 forms magnesium silicate crystals (MgSiO3), which also destroys the uniformity of the network. In the amorphous structure, atoms such as Si, O, and Al are arranged in a disordered manner to form a continuous silicon-oxygen network. The crystallization phases (such as CaSiO3, MgSiO3) have a highly ordered crystal structure. The formation of these crystal phases will cause local phase separation in the matrix, that is, an interface is formed between the crystal phase and the amorphous matrix. The interface between the crystal phase and the matrix cannot withstand high-intensity mechanical stress, reducing the strength of the material. The formation of the crystal phase destroys the continuity of the network, resulting in uneven stress distribution at the microscale of the material. At the same time, the thermal expansion coefficients of the crystallization phase and the amorphous matrix are different (for example, the thermal expansion coefficient of CaSiO3 is higher than that of the amorphous silicate matrix). Thermal stress will be introduced during temperature changes. The grain boundary is a stress concentration point and is prone to forming microcracks and expanding under external forces, ultimately leading to a reduction in the strength of the material. The crystalline impurities will chemically react with the amorphous matrix at high temperatures to generate crystallization phases that destroy the uniformity of the material and introduce grain boundaries, thereby causing stress concentration and crack propagation paths inside the material. The formation of the crystallization phase directly weakens the integrity of the network, reducing the strength and modulus of the material.

[0008] One of the cores of preparing inorganic mineral fiber materials from water quenched slag is the silicon-oxygen network. Its molecular structure is formed by silicon atoms connected to each other by covalent bonds through oxygen atoms, forming a three-dimensional network structure. The key feature in the structure is the bridging oxygen. The bridging oxygen is an oxygen atom connecting two silicon atoms, endowing the glass network with a high degree of crosslinking and mechanical strength. The non-bridging oxygen refers to an oxygen atom that is only connected to one silicon atom and has a negative charge at the other end. The existence of non-bridging oxygen reduces the rigidity and uniformity of the network. The introduction of basic oxides will destroy the continuity of the silicon-oxygen network. At high temperatures, CaO and MgO will dissociate into Ca 2+ , Mg 2+ ions and O 2- ions. The O 2- ions react with the bridging oxygen in the silicon-oxygen network. The bridging oxygen is a symmetric covalent bond structure. The O 2- ions, due to their high electronegativity and strong electron affinity, tend to compete with oxygen atoms for the bonding ability of silicon atoms. When O 2- approaches the bridging oxygen, due to its strong electron affinity, it causes the polarization of the bridging oxygen bond. The introduction of O 2- results in the breakage of the Si-O-Si bond, and the oxygen atom changes from the bridging oxygen state to two independent non-bridging oxygens. The degree of crosslinking in the silicon-oxygen network decreases, resulting in a decrease in the mechanical properties of the material. At the same time, the uniformity of the material is destroyed. At the same time, the reduction of bridging oxygen will reduce the rigidity of the network, causing the glass transition temperature and softening point temperature of the material to decrease significantly, reducing the thermal stability of the material. After dissolving CaO and MgO with hydrochloric acid, the number of non-bridging oxygens in the silicon-oxygen network decreases, and the degree of crosslinking increases, enhancing the rigidity and strength of the material. At the same time, the removal of basic oxides and weakly bound phases at the boundary reduces the tendency of calcium silicate and magnesium silicate crystals to form during the high-temperature melting process, making the melt more likely to form an amorphous structure rather than precipitate crystals when cooled. The removal of weakly bound phases and crystal phases reduces the stress concentration points inside the material, reducing the risk of crack initiation and propagation, thereby improving the mechanical properties of the fiber.

[0009] In the borate system, boron atoms form covalent bonds with oxygen atoms to form two basic structural units, BO3 (planar triangle) and BO4 (tetrahedron). The BO3 unit is the main structural form of borate. Among them, boron atoms are connected to three oxygen atoms through three B-O bonds to form a planar triangle structure. The BO3 unit has high structural flexibility and can be embedded in the silicon-oxygen network to improve the fluidity of water quenched slag after high-temperature melting. When borate coexists with other oxides, the O 2-Ions can react with BO3 units, converting some of the BO3 into BO4 tetrahedral units. The BO4 units have a strong network bonding ability. During the melting process, the oxygen atoms of the BO4 units share with the oxygen atoms of the SiO4 units to form Si-O-B bonds. This bridge bond structure enhances the crosslinking degree of the network, improving the mechanical strength and chemical stability. When BO4 units replace some of the SiO4 units, part of the silicon-oxygen network is replaced by B-O-Si or B-O-B bridge bonds, which can optimize the elasticity and viscosity of the network, contributing to achieving a low melting temperature and high fluidity. Meanwhile, in the borosilicate system, basic oxides introduce additional O 2- , promoting the conversion of BO3 to BO4. The participation of basic oxides reduces the melting temperature while maintaining a certain network structure strength.

[0010] Y 3+ is a rare earth metal ion with a relatively small radius and a high charge density. Therefore, Y 3＋ has a strong electrostatic attraction, making Y 3+ ions prone to combine with O 2- ions to form stable oxide bonds (Y-O bonds). The bond energy of the Y-O bond is relatively high, which enables the introduction of Y 3＋ ions to improve the strength and stability of inorganic mineral fibers. In the material system, SiO2 and Al2O3 are the main network formers, and their basic units are silicon-oxygen tetrahedrons (SiO4) and aluminum-oxygen tetrahedrons (AlO4). These tetrahedrons are connected through bridging oxygen (Si-O-Si or Si-O-Al) to form a network. After introducing Y2O3, Y 3+ ions can form strong Y-O bonds with O 2- ions. Y 3+ ions are connected to SiO4 or AlO4 units through bridging oxygen to form Si-O-Y or Al-O-Y bonds. These newly formed bridge bonds increase the crosslinking degree, thus enhancing the material strength. Meanwhile, Y 3+ ions can neutralize the negative charges of AlO4 units, further improving the material stability. The introduction of Y2O3 can also inhibit the precipitation of crystals in the fiber. In the water-quenched slag melt, ions in local areas (such as Ca 2+ , Mg 2+ ) form crystal nuclei with a periodic structure through diffusion and rearrangement. The crystal nuclei continuously adsorb surrounding ions to form a long-range ordered crystal structure. Introducing Y2O3 into the water-quenched slag melt can interfere with the diffusion of ions or disrupt their ordered arrangement, then the probability of crystal nucleus formation will be significantly reduced. Even if crystal nuclei are formed, these interferences will prevent the further growth of the crystal nuclei, thus inhibiting crystal precipitation. Y 3+ ions have a high charge density, and their strong electrostatic interaction can significantly affect the distribution of surrounding ions, changing Ca 2+ and Mg2+ The migration path of the plasma in the melt makes it difficult for these ions to arrange in the periodicity required for the crystal. Y 3+ Ions can combine with SiO4 or AlO4 units in the glass network to form Si-O-Y or Al-O-Y bonds, which will introduce disorder in local areas and destroy the chemical symmetry and uniformity required for crystal formation. At the same time, Y 3+ The high electric field strength of the ions enables them to preferentially coordinate with O 2- , especially in the melt, Y 3+ has a much higher affinity for oxygen than Ca 2+ and Mg 2+ . When Y 3+ ions combine with O 2- to form Y-O bonds, Ca 2+ and Mg 2+ are repelled to other regions of the melt, resulting in uneven distribution of the ion concentration required for crystal growth, and the probability of forming crystal nuclei will be greatly reduced. And in the melt, Ca 2+ and Mg 2+ and other ions need to combine with O 2- and SiO4 and other units through diffusion to finally form a crystal structure. The introduction of Y 3+ results in an enhanced Coulomb interaction between ions in the melt, increasing the energy required for the migration of Ca 2+ and Mg 2+ , making it difficult for the ions to arrange in the direction of crystal growth in the melt. The precipitation of crystals usually reduces the high-temperature performance of the material. The introduction of Y2O3 suppresses the precipitation of crystals, enabling the fiber to exhibit better thermal stability and strength at high temperatures.

[0011] V2O5 is an oxide that is extremely easy to melt and acts as a powerful flux in the system. It can significantly reduce the melting temperature of water-quenched slag. After V2O5 is introduced, it can break some silicon-oxygen bonds by interacting with SiO2 and Al2O3, thereby reducing the viscosity of the melt. The reduction of the melting temperature reduces the energy consumption in the fiber preparation process, improves production efficiency, improves the fluidity of the melt, and reduces wire breakage or non-uniformity. Vanadium in V2O5 can exhibit two main oxidation states in the molten material, V 5+ and V 4+ , which gives it an oxidation-reduction buffering function. In an oxidizing atmosphere, V 4+ is oxidized to V 5+ to form V2O5. In a reducing atmosphere, V 5+ is partially reduced to V 4+ to form a vanadium oxide containing V 4+ (such as VO2 +), During the glass melting process, fluctuations in the redox conditions may lead to uneven distribution or precipitation of certain components. This redox balance enables the chemical environment of the melt to be dynamically adjusted, improving the uniformity of the fibers. At the same time, the redox characteristics of V2O5 enable it to capture the oxygen free radicals generated in the glass melt, effectively inhibiting the occurrence of free radical chain reactions. V 5+ By reducing to V 4+ absorbs some free electrons, reducing the concentration of free radicals, reducing the component separation and phase separation phenomena caused by free radicals in the melt, and improving the chemical uniformity of the material. And Y 3+ 's high electric field strength combined with the redox ability of V 5+ / V 4+ can further enhance the chemical stability of the glass by forming stable Y-O-V bonds with V2O5. The introduction of V2O5 significantly increases the structural rigidity of the glass network by forming strong V-O-Si, V-O-B, and V-O-Y bonds. The addition of B2O3 further improves the high-temperature toughness of the glass, while the high thermal stability of Y2O3 enhances the overall support force of the fiber at high temperatures, making the fiber exhibit a lower creep rate in a high-temperature environment.

[0012] B2O3 exists in the melt in the form of BO3 or BO4 units. Its introduction can enhance the chemical stability of the fiber and reduce the viscosity of the melt. The BO3 and BO4 units can cooperate with the SiO4 units to form a more stable borosilicate network, thereby improving the uniformity and mechanical properties of the fiber; Y2O3 forms Y-O-Si or Y-O-B bonds with the SiO4 or BO3 units, enhancing the degree of crosslinking. The high electric field strength of Y 3+ ions can inhibit the precipitation of crystals during the melting process, ensuring that the melt remains in an amorphous structure during the cooling process; the variable valence state of V2O5 provides a redox buffering effect during the melting process, dynamically adjusting the chemical environment of the glass, inhibiting crystal formation and optimizing the fluidity of the melt. At high temperatures, the mixed materials melt to form a uniform glassy melt. During the fiber drawing process, the melt is stretched into fibers through a fiber blowing device. Strong bonds (Si-O, B-O, Y-O, V-O bonds) provide the mechanical strength of the fiber. The composite oxide modifier enables the rapid cooling at high temperatures to solidify the glass melt into an amorphous structure, avoiding crystal precipitation, thereby ensuring the uniformity and toughness of the fiber. The annealing process eliminates the local internal stress generated during the drawing process by slowly releasing the residual stress in the fiber, making the fiber have higher mechanical strength and thermal stability.

[0013] The surface of the fiber is rich in a silicon-oxygen network. Some of the silicon-oxygen bonds on the fiber surface will be hydrolyzed under the action of moisture, generating reactive hydroxyl groups. Hydroxyl groups have hydrophilicity and chemical activity and are the key sites for adsorbing Al 3+ ions. Hydroxyl groups can bond with Al3+ Ions undergo a coordination reaction to form strong chemical bonds, enhancing the bonding force between the deposited layer and the fiber matrix, thereby improving the adhesion and stability of the coating. And in the suspension, dissolved Al 3+ ions combine with OH - ions to form aluminum hydroxide precipitate. The Al(OH)3 precipitate is colloidal and easily adheres to the fiber surface, resulting in good bonding performance at the interface between the coating and the matrix. The calcination process dehydrates and decomposes the deposited Al(OH)3, converting it into a dense alumina coating. High-temperature calcination densifies the Al2O3 coating on the fiber surface while retaining the strong bonding formed by chemical combination, further enhancing the bonding force between the coating and the fiber matrix. The calcined Al2O3 coating is a high-hardness and high-strength inorganic material, enhancing the tensile strength and wear resistance of the fiber and also improving the acid and alkali corrosion resistance of the fiber.

[0014] As a preferred technical solution of the present invention, in step S1, the particle size of the medium particle part is 100 - 1000 μm.

[0015] In some alternative examples, the density of the lithium chloride solution is 1.3 g / cm 3 .

[0016] In some alternative examples, the mass ratio of the medium particle part to the lithium chloride solution is 1:(5 - 6), for example, it can be 1:5.0, 1:5.1, 1:5.2, 1:5.3, 1:5.4, 1:5.5, 1:5.6, 1:5.7, 1:5.8, 1:5.9 or 1:6.0, but is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0017] In some alternative examples, the first temperature is 120 - 130 °C, for example, it can be 120.0 °C, 121.0 °C, 122.0 °C, 123.0 °C, 124.0 °C, 125.0 °C, 126.0 °C, 127.0 °C, 128.0 °C, 129.0 °C or 130.0 °C, but is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0018] In some alternative examples, the drying time of the floating part is 12 - 14 h, for example, it can be 12.0 h, 12.2 h, 12.4 h, 12.6 h, 12.8 h, 13.0 h, 13.2 h, 13.4 h, 13.6 h, 13.8 h or 14.0 h, but is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0019] In some alternative examples, the mass fraction of the hydrochloric acid solution is 3-4 wt.%, for example, it can be 3.0 wt.%, 3.1 wt.%, 3.2 wt.%, 3.3 wt.%, 3.4 wt.%, 3.5 wt.%, 3.6 wt.%, 3.7 wt.%, 3.8 wt.%, 3.9 wt.% or 4.0 wt.%, but is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0020] In some alternative examples, the solid-liquid ratio of the floating part to the hydrochloric acid solution is 1 g: 10 mL.

[0021] In some alternative examples, the stirring time at room temperature is 2-3 h, for example, it can be 2.0 h, 2.1 h, 2.2 h, 2.3 h, 2.4 h, 2.5 h, 2.6 h, 2.7 h, 2.8 h, 2.9 h or 3.0 h, but is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0022] In some alternative examples, the drying time after stirring with hydrochloric acid is 12-14 h, for example, it can be 12.0 h, 12.2 h, 12.4 h, 12.6 h, 12.8 h, 13.0 h, 13.2 h, 13.4 h, 13.6 h, 13.8 h or 14.0 h, but is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0023] In some alternative examples, the target particle size is 50 μm.

[0024] In some alternative examples, the mass of Na2CO3 is 5-10% of the mass of the pickled water-quenched slag particles, for example, it can be 5.0%, 5.5%, 6.0%, 6.5%, 7.0%, 7.5%, 8.0%, 8.5%, 9.0%, 9.5% or 10.0%, but is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0025] In some alternative examples, the mass of Fe2O3 is 2-4% of the mass of the pickled water-quenched slag particles, for example, it can be 2.0%, 2.2%, 2.4%, 2.6%, 2.8%, 3.0%, 3.2%, 3.4%, 3.6%, 3.8% or 4.0%, but is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0026] In some alternative examples, the second temperature is 850 - 950 °C. For example, it can be 850.0 °C, 860.0 °C, 870.0 °C, 880.0 °C, 890.0 °C, 900.0 °C, 910.0 °C, 920.0 °C, 930.0 °C, 940.0 °C or 950.0 °C. However, it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0027] In some alternative examples, the calcination time at the second temperature is 2 - 3 h. For example, it can be 2.0 h, 2.1 h, 2.2 h, 2.3 h, 2.4 h, 2.5 h, 2.6 h, 2.7 h, 2.8 h, 2.9 h or 3.0 h. However, it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0028] As a preferred technical solution of the present invention, in step S2, the mass ratio of boric acid to deionized water in the boric acid solution is 1:10.

[0029] In some alternative examples, in the yttrium nitrate solution, the mass ratio of yttrium nitrate hexahydrate to deionized water is 4:25.

[0030] In some alternative examples, the mass ratio of vanadium pentoxide to ammonia water is 1:15.

[0031] In some alternative examples, the mass fraction of the ammonia water is 20 wt.%.

[0032] In some alternative examples, the mass ratio of boric acid, yttrium nitrate hexahydrate, and vanadium pentoxide is 5:8:2.

[0033] In some alternative examples, the stirring reaction time is 30 - 50 min. For example, it can be 30.0 min, 32.0 min, 34.0 min, 36.0 min, 38.0 min, 40.0 min, 42.0 min, 44.0 min, 46.0 min, 48.0 min or 50.0 min. However, it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0034] In some alternative examples, the third temperature is 80 - 100 °C. For example, it can be 80.0 °C, 82.0 °C, 84.0 °C, 86.0 °C, 88.0 °C, 90.0 °C, 92.0 °C, 94.0 °C, 96.0 °C, 98.0 °C or 100.0 °C. However, it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0035] In some alternative examples, the drying time at the third temperature is 10 - 12 h. For example, it can be 10.0 h, 10.2 h, 10.4 h, 10.6 h, 10.8 h, 11.0 h, 11.2 h, 11.4 h, 11.6 h, 11.8 h or 12.0 h. However, it is not limited to the listed values, and other unlisted values within this range are equally applicable.

[0036] In some alternative examples, the mass ratio of H3BO3, Y2O3, and V2O5 is 4:3:2.

[0037] In some alternative examples, the mass ratio of the mixture to the wet powder precursor is 2:3.

[0038] In some alternative examples, the ball milling time is 2 - 3 h. For example, it can be 2.0 h, 2.1 h, 2.2 h, 2.3 h, 2.4 h, 2.5 h, 2.6 h, 2.7 h, 2.8 h, 2.9 h or 3.0 h. However, it is not limited to the listed values, and other unlisted values within this range are equally applicable.

[0039] In some alternative examples, the calcination time is 4 - 6 h. For example, it can be 4.0 h, 4.2 h, 4.4 h, 4.6 h, 4.8 h, 5.0 h, 5.2 h, 5.4 h, 5.6 h, 5.8 h or 6.0 h. However, it is not limited to the listed values, and other unlisted values within this range are equally applicable.

[0040] As a preferred technical solution of the present invention, in step S3, the mass ratio of the high-temperature sintered water quenched slag, the composite oxide modifier, and borax is (60 - 70):(20 - 30):(10 - 20).

[0041] In some alternative examples, the ball milling time is 40 - 60 min. For example, it can be 40.0 min, 42.0 min, 44.0 min, 46.0 min, 48.0 min, 50.0 min, 52.0 min, 54.0 min, 56.0 min, 58.0 min or 60.0 min. However, it is not limited to the listed values, and other unlisted values within this range are equally applicable.

[0042] In some alternative examples, the fourth temperature is 1450 - 1550 °C. For example, it can be 1450.0 °C, 1460.0 °C, 1470.0 °C, 1480.0 °C, 1490.0 °C, 1500.0 °C, 1510.0 °C, 1520.0 °C, 1530.0 °C, 1540.0 °C or 1550.0 °C. However, it is not limited to the listed values, and other unlisted values within this range are equally applicable.

[0043] In some alternative examples, the fifth temperature is 400 - 500 °C. For example, it can be 400.0 °C, 410.0 °C, 420.0 °C, 430.0 °C, 440.0 °C, 450.0 °C, 460.0 °C, 470.0 °C, 480.0 °C, 490.0 °C or 500.0 °C. However, it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0044] In some alternative examples, the heat preservation time of the annealing treatment is 60 - 80 min. For example, it can be 60.0 min, 62.0 min, 64.0 min, 66.0 min, 68.0 min, 70.0 min, 72.0 min, 74.0 min, 76.0 min, 78.0 min or 80.0 min. However, it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable. The cooling rate is 3 °C / min.

[0045] As a preferred technical solution of the present invention, in step S4, the ultrasonic cleaning time is 10 - 20 min. For example, it can be 10.0 min, 11.0 min, 12.0 min, 13.0 min, 14.0 min, 15.0 min, 16.0 min, 17.0 min, 18.0 min, 19.0 min or 20.0 min. However, it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0046] In some alternative examples, the drying time is 2 - 3 h. For example, it can be 2.0 h, 2.1 h, 2.2 h, 2.3 h, 2.4 h, 2.5 h, 2.6 h, 2.7 h, 2.8 h, 2.9 h or 3.0 h. However, it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0047] In some alternative examples, the mass ratio of aluminum nitrate to deionized water is 1:10.

[0048] In some alternative examples, the mass fraction of the ammonia water solution is 10 - 12 wt.%. For example, it can be 10.0 wt.%, 10.2 wt.%, 10.4 wt.%, 10.6 wt.%, 10.8 wt.%, 11.0 wt.%, 11.2 wt.%, 11.4 wt.%, 11.6 wt.%, 11.8 wt.% or 12.0 wt.%. However, it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0049] In some alternative examples, the holding time of immersing in the Al(OH)3 suspension is 30 - 40 min. For example, it can be 30.0 min, 31.0 min, 32.0 min, 33.0 min, 34.0 min, 35.0 min, 36.0 min, 37.0 min, 38.0 min, 39.0 min or 40.0 min. However, it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0050] In some alternative examples, the time for calcination is 2 - 3 h. For example, it can be 2.0 h, 2.1 h, 2.2 h, 2.3 h, 2.4 h, 2.5 h, 2.6 h, 2.7 h, 2.8 h, 2.9 h or 3.0 h. However, it is not limited to the listed values, and other unlisted values within this numerical range are equally applicable.

[0051] In a second aspect, the present invention provides high-strength and high-modulus inorganic mineral fibers prepared from water-quenched slag by using the preparation method described in the first aspect.

[0052] Compared with the prior art, the beneficial effects of the present invention are as follows: (1) During the high-temperature melting process, the BO3 units in B2O3 react chemically with the silicon-oxygen bonds in the SiO4 units to form new B-O-Si bonds. The formation of B-O-Si bonds significantly increases the crosslinking degree of the glass network. This crosslinking not only enhances the structural stability of the material but also improves the chemical stability and chemical erosion resistance of the melt. At the same time, the B-O-B bonds further enhance the crosslinking degree of the glass network, making the fibers denser and more uniform. (2) In Y2O3, Y 3+ By combining with the oxygen bridge bonds, it destroys the local atomic arrangement order required for crystal growth. At the same time, the high electric field strength of the ions can significantly inhibit the precipitation of crystal phases in the melt, preventing the formation and growth of crystal nuclei. At the same time, Y 3+ ions can interfere with the aggregation tendency of crystal phases in the melt, ensuring that the glass maintains an amorphous structural characteristic during the cooling process. The high electric field strength of Y 3＋ ions can form stable connections of B-O-Si and B-O-B bonds with B2O3, enhancing the crosslinking degree and at the same time reducing the tendency of crystal precipitation. (3) During the high-temperature melting process, as a transition metal oxide, V2O5, vanadium ions can be in V 5+ and V 4+There is a dynamic conversion between two oxidation states. This variable valence state enables V2O5 to act as a redox buffer in the molten glass system, regulating the redox balance in the melt by capturing or releasing electrons. The redox buffering effect reduces the phase separation phenomenon caused by excessive oxidation or reduction of components in the melt, ensuring the chemical homogeneity of the glass system. Description of the Drawings

[0053] Figure 1 SEM image of the inorganic mineral fiber prepared from water quenched slag in Example 1 of the present invention (scale bar: 20 μm); Figure 2 SEM image of the inorganic mineral fiber prepared from water quenched slag in Example 1 of the present invention (scale bar: 5 μm); Figure 3 TEM image of the inorganic mineral fiber prepared from water quenched slag in Example 1 of the present invention; Figure 4 SEM image of the composite oxide modifier in Example 1 of the present invention. Detailed Description of the Invention

[0054] The technical solution of the present invention will be described in detail below in conjunction with specific embodiments and their accompanying drawings. The embodiments described herein are specific specific embodiments of the present invention for explaining the concept of the present invention; these descriptions are all explanatory and exemplary, and should not be construed as limiting the embodiments of the present invention and the protection scope of the present invention. Except for the embodiments described herein, those skilled in the art can also adopt other obvious technical solutions based on the content disclosed in the claims and the specification of the present application. These technical solutions include technical solutions that make any obvious substitutions and modifications to the embodiments described herein.

[0055] The chemical reagents used in the examples and comparative examples of the present invention are all commercially available products without any further purification treatment.

[0056] Example 1 This example provides a preparation method for preparing high-strength and high-modulus inorganic mineral fibers using water quenched slag. The preparation method specifically includes the following steps: Step S1: Put the water-quenched slag raw material into a vibrating screen for particle sizing, retain the medium-sized particle part of 100 - 1000 μm. Pour 100 g of the medium-sized particle part of the water-quenched slag into 500 g of lithium chloride solution, collect the floating part, filter and wash it, then place it at 123 °C for full drying for 12.6 h. Put 50 g of the dried floating water-quenched slag into 500 mL of 3.3 wt.% hydrochloric acid solution, stir it fully at room temperature for 2.2 h, filter and wash it, then place it at 123 °C for full drying for 13.0 h to obtain pickled water-quenched slag particles. Crush 50 g of the pickled water-quenched slag particles to below 50 μm, then mix them with 3.5 g of Na2CO3 and 1.5 g of Fe2O3, heat up to 880 °C and continue to calcine for 2.2 h. After the calcination is completed, cool it to room temperature to obtain high-temperature sintered water-quenched slag; Step S2: Mix 55 g of 9 wt.% boric acid solution and 58 g of 13 wt.% yttrium nitrate solution to obtain a mixed solution. Then dissolve 2 g of vanadium pentoxide in 30 g of 20 wt.% ammonia water, and add it to the above mixed solution. After stirring evenly, use ammonia water to adjust the pH to 8.0, keep stirring for 35 min to complete the precipitation reaction. Filter and wash it, then place it at 85 °C for drying for 10.5 h to obtain a wet-process powder precursor. Then mix 8 g of H3BO3, 6 g of Y2O3 and 4 g of V2O5 to obtain a mixture. Put the mixture and 27 g of the wet-process powder precursor into a ball mill and add ethanol, ball mill for 2.3 h, and then place it at 850 °C for calcination for 4.2 h to obtain a composite oxide modifier; Step S3: Mix 62 g of high-temperature sintered water-quenched slag, 28 g of the composite oxide modifier and 13 g of borax, ball mill for 45 min to obtain a mixed material. Heat up the mixed material to 1500 °C, use a fiber blowing device to draw the molten material into fibers, then place the fibers in an argon atmosphere, carry out annealing treatment at 450 °C, with a holding time of 65 min and a cooling rate of 3 °C / min to obtain annealed fibers; Step S4: Immerse the annealed fibers in absolute ethanol, ultrasonically clean to remove surface contaminants, then place them at 122 °C for drying for 2.4 h. Dissolve 10 g of aluminum nitrate in 100 g of deionized water, stir until dissolved, then add 10.5 wt.% ammonia water solution to adjust the pH to 7.5 to obtain an Al(OH)3 suspension. Immerse the dried annealed fibers in the Al(OH)3 suspension, take out the annealed fibers after 33 min, and place them at 880 °C for calcination for 2.4 h to obtain a high-strength and high-modulus inorganic mineral fiber prepared from water-quenched slag.

[0057] Figure 1 This is the SEM image of the inorganic mineral fiber prepared in this example. It can be seen that the fiber surface is smooth, the diameter is uniform, and there are no obvious cracks and particle attachments; Figure 2 This is the SEM image (scale: 5 μm) of the inorganic mineral fiber prepared from water-quenched slag in Example 1 of the present invention;Figure 3 TEM image of the inorganic mineral fiber prepared from water quenched slag in Example 1 of the present invention; Figure 4 SEM image of the composite oxide modifier in Example 1 of the present invention.

[0058] Example 2 This example provides a preparation method for preparing high-strength and high-modulus inorganic mineral fibers using water quenched slag. The specific steps of the preparation method are as follows: Step S1: Put the water quenched slag raw material into a vibrating screen for particle grading, retain the medium particle part of 100 - 1000 μm. Pour 100 g of the medium particle part of the water quenched slag into 550 g of lithium chloride solution, collect the floating part, filter and wash it, then place it at 120 °C for full drying for 12.0 h. Put 60 g of the dried floating water quenched slag into 600 mL of 3.7 wt.% hydrochloric acid solution, stir well at room temperature for 2.0 h, filter and wash it, then place it at 120 °C for full drying for 12.5 h to obtain pickled water quenched slag particles. Crush 70 g of the pickled water quenched slag particles to less than 50 μm, then mix it with 5.6 g of Na2CO3 and 2.1 g of Fe2O3, heat it up to 850 °C and continue to calcine for 2.6 h. After the calcination is completed, cool it to room temperature to obtain high-temperature sintered water quenched slag; Step S2: Mix 55 g of 9 wt.% boric acid solution and 58 g of 13 wt.% yttrium nitrate solution to obtain a mixed solution. Then dissolve 2 g of vanadium pentoxide in 30 g of 20 wt.% ammonia water and add it to the above mixed solution. Stir well and use ammonia water to adjust the pH to 8.5, keep stirring for 30 min to complete the precipitation reaction. Filter and wash it, then place it at 80 °C for drying for 11.1 h to obtain a wet powder precursor. Then mix 8 g of H3BO3, 6 g of Y2O3 and 4 g of V2O5 to obtain a mixture. Put the mixture and 27 g of the wet powder precursor into a ball mill and add ethanol, ball mill for 2.6 h, and then place it at 890 °C for calcination for 4.8 h to obtain a composite oxide modifier; Step S3: Mix 67 g of high-temperature sintered water quenched slag, 30 g of the composite oxide modifier and 10 g of borax, ball mill for 50 min to obtain a mixed material. Heat the mixed material to 1450 °C, use a fiber blowing device to draw the molten material into fibers, then place the fibers in an argon atmosphere, anneal at 400 °C, the holding time is 70 min, and the cooling rate is 3 °C / min to obtain annealed fibers; Step S4, soak the annealed fibers in absolute ethanol, ultrasonically clean to remove surface contaminants, and then dry at 127 °C for 2.0 h. Dissolve 10 g of aluminum nitrate in 100 g of deionized water, stir until dissolved, and then add 11.0 wt.% ammonia water solution to adjust the pH to 7.5 to obtain an Al(OH)3 suspension. Immerse the dried annealed fibers in the Al(OH)3 suspension, take out the annealed fibers after 30 min, and calcine at 850 °C for 2.1 h to obtain a high-strength and high-modulus inorganic mineral fiber prepared from water-quenched slag.

[0059] Example 3 This example provides a preparation method for high-strength and high-modulus inorganic mineral fibers prepared from water-quenched slag. The preparation method specifically includes the following steps: Step S1, put the water-quenched slag raw material into a vibrating screen for particle classification, retain the medium particle part of 100 - 1000 μm, pour 100 g of the medium particle part of the water-quenched slag into 600 g of lithium chloride solution, collect the floating part, filter and wash, and then dry thoroughly at 126 °C for 13.4 h. Put 70 g of the dried floating water-quenched slag into 700 mL of 4.0 wt.% hydrochloric acid solution, stir thoroughly at room temperature for 2.6 h, filter and wash, and then dry thoroughly at 126 °C for 14.0 h to obtain pickled water-quenched slag particles. Crush 60 g of pickled water-quenched slag particles to less than 50 μm, and then mix with 4.2 g of Na2CO3 and 2.4 g of Fe2O3, heat up to 910 °C and continue to calcine for 2.0 h. After the calcination is completed, cool to room temperature to obtain high-temperature sintered water-quenched slag; Step S2, mix 55 g of 9 wt.% boric acid solution and 58 g of 13 wt.% yttrium nitrate solution to obtain a mixed solution. Then dissolve 2 g of vanadium pentoxide in 30 g of 20 wt.% ammonia water and add it to the above mixed solution. Stir evenly and use ammonia water to adjust the pH to 8.4, keep stirring for 50 min to complete the precipitation reaction, filter and wash, and then dry at 94 °C for 12.0 h to obtain a wet powder precursor. Then mix 8 g of H3BO3, 6 g of Y2O3 and 4 g of V2O5 to obtain a mixture. Put the mixture and 27 g of the wet powder precursor into a ball mill and add ethanol, ball mill for 2.0 h, and then calcine at 950 °C for 5.4 h to obtain a composite oxide modifier; Step S3, mix 60 g of high-temperature sintered water-quenched slag, 24 g of composite oxide modifier and 16 g of borax, ball mill for 51 min to obtain a mixed material. Heat the mixed material to 1550 °C, use a fiber blowing device to draw the molten material into fibers, and then place the fibers in an argon atmosphere and carry out annealing treatment at 410 °C, with a holding time of 71 min and a cooling rate of 3 °C / min to obtain annealed fibers; Step S4: Immerse the annealed fibers in absolute ethanol, ultrasonically clean to remove surface contaminants, and then dry at 120 °C for 2.8 h. Dissolve 10 g of aluminum nitrate in 100 g of deionized water, stir until dissolved, add 11.3 wt.% ammonia water solution to adjust the pH to 7.5 to obtain an Al(OH)3 suspension. Immerse the dried annealed fibers in the Al(OH)3 suspension, take out the annealed fibers after 36 min, and calcine at 950 °C for 2.7 h to obtain a high-strength and high-modulus inorganic mineral fiber prepared from water-quenched slag.

[0060] Example 4 This example provides a preparation method for high-strength and high-modulus inorganic mineral fibers prepared from water-quenched slag. The preparation method specifically includes the following steps: Step S1: Put the water-quenched slag raw material into a vibrating screen for particle classification, retain the medium particle part of 100 - 1000 μm. Pour 100 g of the medium particle part of the water-quenched slag into 580 g of lithium chloride solution, collect the floating part, filter and wash it, and then dry it at 130 °C for 14.0 h. Put 60 g of the dried floating water-quenched slag into 600 mL of 3.0 wt.% hydrochloric acid solution, stir well at room temperature for 3.0 h, filter and wash it, and then dry it at 130 °C for 12.7 h to obtain pickled water-quenched slag particles. Crush 50 g of pickled water-quenched slag particles to less than 50 μm, and then mix them with 5 g of Na2CO3 and 2.0 g of Fe2O3, heat up to 950 °C and continue to calcine for 3.0 h. After the calcination is completed, cool to room temperature to obtain high-temperature sintered water-quenched slag; Step S2: Mix 55 g of 9 wt.% boric acid solution and 58 g of 13 wt.% yttrium nitrate solution to obtain a mixed solution. Then dissolve 2 g of vanadium pentoxide in 30 g of 20 wt.% ammonia water and add it to the above mixed solution. Stir evenly and use ammonia water to adjust the pH to 8.3, keep stirring for 40 min to complete the precipitation reaction, filter and wash it, and then dry it at 100 °C for 10.9 h to obtain a wet-process powder precursor. Then mix 8 g of H3BO3, 6 g of Y2O3 and 4 g of V2O5 to obtain a mixture. Put the mixture and 27 g of the wet-process powder precursor into a ball mill and add ethanol, ball mill for 3.0 h, and then calcine at 910 °C for 6.0 h to obtain a composite oxide modifier; Step S3: Mix 70 g of high-temperature sintered water-quenched slag, 20 g of the composite oxide modifier and 20 g of borax, ball mill for 60 min to obtain a mixed material. Heat up the mixed material to 1490 °C, use a fiber blowing device to draw the molten material into fibers, and then place the fibers in an argon atmosphere, anneal at 500 °C, the holding time is 80 min, and the cooling rate is 3 °C / min to obtain annealed fibers; Step S4: Immerse the annealed fibers in absolute ethanol, ultrasonically clean to remove surface contaminants, and then dry at 130 °C for 3.0 h. Dissolve 10 g of aluminum nitrate in 100 g of deionized water, stir until dissolved, and then add 12.0 wt.% ammonia water solution to adjust the pH to 7.5 to obtain an Al(OH)3 suspension. Immerse the dried annealed fibers in the Al(OH)3 suspension, take out the annealed fibers after 40 min, and calcine at 910 °C for 3.0 h to obtain a high-strength and high-modulus inorganic mineral fiber prepared from water quenching slag.

[0061] Comparative Example 1 This comparative example provides a preparation method of high-strength and high-modulus inorganic mineral fiber prepared from water quenching slag. The difference from Example 1 is that the mass of H3BO3 in Step S2 is adjusted to 15 g, which is 7 g more than that in Example 1, and other process parameters and operating conditions are exactly the same as those in Example 1.

[0062] Comparative Example 2 This comparative example provides a preparation method of high-strength and high-modulus inorganic mineral fiber prepared from water quenching slag. The difference from Example 1 is that the mass of H3BO3 in Step S2 is adjusted to 1 g, which is 7 g less than that in Example 1, and other process parameters and operating conditions are exactly the same as those in Example 1.

[0063] Comparative Example 3 This comparative example provides a preparation method of high-strength and high-modulus inorganic mineral fiber prepared from water quenching slag. The difference from Example 1 is that the mass of V2O5 in Step S2 is adjusted to 7 g, which is 3 g more than that in Example 1, and other process parameters and operating conditions are exactly the same as those in Example 1.

[0064] Comparative Example 4 This comparative example provides a preparation method of high-strength and high-modulus inorganic mineral fiber prepared from water quenching slag. The difference from Example 1 is that the mass of V2O5 in Step S2 is adjusted to 1 g, which is 3 g less than that in Example 1, and other process parameters and operating conditions are exactly the same as those in Example 1.

[0065] In this invention, the test standards for the tensile strength and elastic modulus of the prepared inorganic mineral fiber are GB / T1447 - 2005. The test results are shown in Table 1.

[0066] Table 1 Test Results of High-Strength and High-Modulus Inorganic Mineral Fibers Prepared in Examples 1 - 4 and Comparative Examples 1 - 4

[0067] As can be seen from the data in the table, compared with Example 1, both the tensile strength and elastic modulus of Comparative Example 1 decreased; both the tensile strength and elastic modulus of Comparative Example 2 decreased. An appropriate amount of B2O3 can enhance the cross-linking of the network through BO3 and BO4 units. In Comparative Example 1, excessive B2O3 will cause a significant increase in the proportion of BO3 units in the glass network, and the proportion of B-O-B bonds will also increase. However, the mechanical strength of B-O-B bonds is low. At the same time, excessive B2O3 will reduce the viscosity of the melt. Although it is helpful for fiber drawing, the excessive fluidity of the melt may lead to compositional segregation or crystal precipitation in local areas. The presence of crystal precipitation will become a stress concentration point inside the fiber, reducing the tensile strength and elastic modulus. When borate coexists with other oxides, the O 2- ions can react with BO3 units to convert some BO3 into BO4 tetrahedral units. BO4 units have strong network bonding ability. During the melting process, the oxygen atoms of BO4 units share with the oxygen atoms of SiO4 units to form Si-O-B bonds. This bridge bond structure enhances the cross-linking degree of the network, improving the mechanical strength and chemical stability. In Comparative Example 2, the amount of H3BO3 is insufficient, so the tensile strength and elastic modulus of the inorganic mineral fiber decrease.

[0068] Compared with Example 1, both the tensile strength and elastic modulus of Comparative Example 3 decreased; both the tensile strength and elastic modulus of Comparative Example 4 decreased. When V2O5 is in excess, its solubility in the melt may exceed the saturation limit, which may lead to the enrichment of V2O5 in local areas and even the precipitation of vanadium oxide crystal phases (such as V2O4 or V2O5 crystals). The presence of crystals introduces defects in the fiber, thus becoming a stress concentration point and reducing the tensile strength of the fiber. Therefore, in Comparative Example 3, the tensile strength and elastic modulus decreased. V2O5 provides redox buffering through its variable valence state to keep the melt in redox balance. When the amount of V2O5 is insufficient, it may lead to an increase in the proportion of peroxides or suboxides in the melt, increasing the risk of crystal precipitation. At the same time, the proportions of V-O-Si and V-O-B decrease. Therefore, the tensile strength and elastic modulus decreased in Comparative Example 4.

[0069] The above are only the specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention fall within the protection scope and disclosure scope of the present invention.

Claims

1. A preparation method for preparing high-strength and high-modulus inorganic mineral fibers using water-quenched slag, characterized in that, The preparation method is as follows: Step S1: Classify the water-quenched slag raw material by particle size, retain the medium particle part and pour it into a lithium chloride solution, collect the floating part, place the dried floating water-quenched slag in a hydrochloric acid solution to obtain pickled water-quenched slag particles, crush the pickled water-quenched slag particles to below the target particle size, and then mix and calcine with Na2CO3 and Fe2O3 to obtain high-temperature sintered water-quenched slag; Step S2: Mix the boric acid solution and the yttrium nitrate solution to obtain a mixed solution, dissolve vanadium pentoxide in ammonia water and add it to the above mixed solution, adjust the pH to 8-8.5 to obtain a wet powder precursor, and then mix H3BO3, Y2O3 and V2O5 to obtain a mixture. The mixture is ball-milled and calcined with the wet powder precursor to obtain a composite oxide modifier; Step S3: Mix the high-temperature sintered water-quenched slag, the composite oxide modifier and borax, ball-mill and then melt and draw into fibers, and then anneal the fibers in an argon atmosphere to obtain annealed fibers; Step S4: Immerse the annealed fibers in absolute ethanol, ultrasonically clean and dry them. Dissolve aluminum nitrate in deionized water and adjust the pH to 7.5 to obtain an Al(OH)3 suspension. Immerse the dried annealed fibers in the Al(OH)3 suspension, take out the annealed fibers after a certain period of time and calcine them to obtain a high-strength and high-modulus inorganic mineral fiber prepared from water-quenched slag.

2. The preparation method of high-strength and high-modulus inorganic mineral fibers using water quenching slag according to claim 1, characterized in that, In step S1, the particle size of the medium particle part is 100-1000 μm; The density of the lithium chloride solution is 1.3 g / cm 3 .

3. The preparation method of a high-strength and high-modulus inorganic mineral fiber prepared by using water quenching slag according to claim 1, characterized in that, In step S1, the solid-liquid ratio of the floating part to the hydrochloric acid solution is 1 g: 10 mL.

4. The preparation method of a high-strength and high-modulus inorganic mineral fiber prepared by using water quenching slag according to claim 1, characterized in that, In step S1, the target particle size is 50 μm; the mass of Na2CO3 is 5-10% of the mass of the pickled water-quenched slag particles; the mass of Fe2O3 is 2-4% of the mass of the pickled water-quenched slag particles.

5. The preparation method of a high-strength and high-modulus inorganic mineral fiber prepared by using water quenching slag according to claim 1, characterized in that, In step S2, in the yttrium nitrate solution, the mass ratio of yttrium nitrate hexahydrate to deionized water is 4:25; the mass ratio of boric acid, yttrium nitrate hexahydrate and vanadium pentoxide is 5:8:

2.

6. The preparation method of a high-strength and high-modulus inorganic mineral fiber prepared by using water quenching slag according to claim 1, characterized in that, In step S2, the mass ratio of H3BO3, Y2O3 and V2O5 is 4:3:2; the mass ratio of the mixture to the wet powder precursor is 2:

3.

7. The preparation method of a high-strength and high-modulus inorganic mineral fiber prepared by using water quenching slag according to claim 1, characterized in that, In step S3, the mass ratio of the high-temperature sintered water-quenched slag, the composite oxide modifier and borax is (60-70):(20-30):(10-20); the heat preservation time of the annealing treatment is 60-80 min, and the cooling rate is 3 °C / min.

8. The preparation method of a high-strength and high-modulus inorganic mineral fiber prepared from water quenching slag according to claim 1, characterized in that, In step S4, the mass ratio of aluminum nitrate to deionized water is 1:

10.

9. The preparation method of a high-strength and high-modulus inorganic mineral fiber prepared by using water quenching slag according to claim 1, characterized in that, In step S4, the holding time of immersing in the Al(OH)3 suspension is 30-40 min; the calcination time is 2-3 h.

10. The high-strength and high-modulus inorganic mineral fiber prepared from water-quenched slag obtained by the preparation method according to any one of claims 1-9.

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