CN112341001B - High silica glass fiber, preparation method thereof and fireproof equipment - Google Patents

High silica glass fiber, preparation method thereof and fireproof equipment Download PDF

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CN112341001B
CN112341001B CN202011283216.5A CN202011283216A CN112341001B CN 112341001 B CN112341001 B CN 112341001B CN 202011283216 A CN202011283216 A CN 202011283216A CN 112341001 B CN112341001 B CN 112341001B
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oxide
glass fiber
silica glass
rare earth
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CN112341001A (en
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赵祥
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Linyi Haoquan Silicon Technology Co ltd
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Linyi Haoquan Silicon Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C13/00—Fibre or filament compositions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
    • C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
    • E—FIXED CONSTRUCTIONS
    • E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
    • E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
    • E06B5/00—Doors, windows, or like closures for special purposes; Border constructions therefor
    • E06B5/10—Doors, windows, or like closures for special purposes; Border constructions therefor for protection against air-raid or other war-like action; for other protective purposes
    • E06B5/16—Fireproof doors or similar closures; Adaptations of fixed constructions therefor
    • E—FIXED CONSTRUCTIONS
    • E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
    • E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
    • E06B9/00—Screening or protective devices for wall or similar openings, with or without operating or securing mechanisms; Closures of similar construction
    • E06B9/02—Shutters, movable grilles, or other safety closing devices, e.g. against burglary
    • E06B9/08—Roll-type closures
    • E06B9/11—Roller shutters
    • E06B9/15—Roller shutters with closing members formed of slats or the like

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Structural Engineering (AREA)
  • Materials Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Civil Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Architecture (AREA)
  • Glass Compositions (AREA)

Abstract

The invention relates to the technical field of glass fiber preparation, in particular to high-silica glass fiber and a preparation method thereof. The high-silica glass fiber is mainly composed of the following raw materials in parts by weight: 70-80 parts of silicon dioxide, 10-20 parts of silicon carbide, 2-5 parts of aluminum oxide, 5-15 parts of boron trioxide, 10-15 parts of sodium oxide and 0.05-0.1 part of rare earth oxide. The rare earth oxide is prepared from holmium oxide and niobium pentoxide according to the weight ratio of (1-3): 5, the components are mixed. According to the invention, the holmium oxide and the niobium pentoxide are introduced according to the optimized proportion, so that the high-temperature viscosity and the forming temperature of the glass are effectively reduced, the ductility of the glass material block is enhanced, and the high-strength glass fiber is obtained at relatively low melting temperature and wire drawing temperature.

Description

High silica glass fiber, preparation method thereof and fireproof equipment
Technical Field
The invention relates to the technical field of glass fiber preparation, in particular to a high silica glass fiber, a preparation method thereof and fireproof equipment.
Background
The high silica fiber is a high purity silicon oxide noncrystal continuous fiber for short, the finished product mainly comprises continuous yarn, rope belt, sleeve, net cloth and stitch-bonded product, and is mainly applied to 1000-DEG superhigh temperature fire prevention and heat insulation, the diameter of single fiber is more than 5 microns, and the high silica fiber does not contain any asbestos or ceramic cotton and is completely harmless to body health. The high silica fiber can maintain good strength and elasticity for a long time at 1000 ℃, and is an effective heat barrier for ultrahigh-temperature heat flow and jet flame and a reliable protection device for personnel facilities; the high-temperature resistant alloy has low heat conductivity coefficient, has good resistance to high-temperature impact, is inert to most chemicals, has good corrosion resistance to compounds at high temperature, corrosive minerals and weakly alkaline molten alloy, and can normally and continuously work under the conditions of high heat and strong radiation.
The high silica fiber is widely applied to the aspects of spacecraft thermal ablation prevention materials, high-temperature-resistant heat insulators, high-temperature gas dust collection, liquid filtration, metal dissolution filtration, purification and the like, and has very wide application prospect and huge market potential.
The existing high-silica glass fiber has high mechanical strength and good high-temperature performance, but the glass has high melting temperature and wire drawing temperature, high-temperature viscosity and difficulty in wire drawing.
Disclosure of Invention
The invention aims to provide high-silica glass fiber and a preparation method thereof, which overcome the defects of the prior art, effectively reduce the accommodating temperature and the wire drawing temperature and improve the high-temperature viscosity of the product on the premise of higher mechanical strength and good high-temperature performance.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the high-silica glass fiber mainly comprises the following raw materials in parts by weight: 70-80 parts of silicon dioxide, 10-20 parts of silicon carbide, 2-5 parts of aluminum oxide, 5-15 parts of boron trioxide, 10-15 parts of sodium oxide and 0.05-0.1 part of rare earth oxide.
Preferably, the material mainly comprises the following raw materials in parts by weight: 78 parts of silicon dioxide, 16 parts of silicon carbide, 3 parts of aluminum oxide, 12 parts of boron trioxide, 7 parts of sodium oxide and 0.08 part of rare earth oxide.
Preferably, the rare earth oxide is prepared from holmium oxide and niobium pentoxide according to a weight ratio of (1-3): 5.
Preferably, the rare earth oxide is prepared by mixing holmium oxide and niobium pentoxide in a weight ratio of 2: 5, the components are mixed.
A preparation method of high silica glass fiber comprises the following steps:
(1) weighing silicon dioxide, silicon carbide, aluminum oxide, boron trioxide and sodium oxide according to the specified weight parts, grinding and uniformly mixing to obtain a primary mixture, weighing rare earth oxide according to the specified weight parts after the particle size of the primary mixture reaches the nanometer level, adding the rare earth oxide into the primary mixture, and continuously mixing to form a final raw material mixture, wherein the particle size of the final raw material mixture reaches the nanometer level;
(2) placing the final raw material mixture into a corundum crucible, placing the corundum crucible into a silicon-molybdenum rod electric heating furnace, melting at the high temperature of 1200-1350 ℃ for 2-3 hours to melt the mixture, then casting and molding the melt, placing the molded glass into a muffle furnace, and carrying out phase-splitting heat treatment at the temperature of 450-480 ℃ for 12-16 hours to obtain a glass block;
(3) and (3) putting the glass block into a wire drawing furnace, and carrying out secondary melting and wire drawing at 800-.
Preferably, the rotation speed of the drawing furnace is 1000-.
The invention also discloses a fire-proof device which is a rolling door, and the surface of the rolling door is provided with the high silica glass fiber.
Preferably, the high silica glass fiber is bonded to the surface of the rolling door through aerogel.
The invention has the beneficial effects that: compared with the prior art, the high silica glass fiber and the preparation method thereof have the following advantages: the holmium oxide and the niobium pentoxide are introduced according to the optimized proportion, so that the high-temperature viscosity and the forming temperature of the glass are effectively reduced, the ductility of the glass material block is enhanced, and the high-strength glass fiber is obtained at relatively low melting temperature and wire drawing temperature.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
Fig. 2 is a schematic rear view of the present invention.
FIG. 3 is a schematic view of the internal structure of the case of the present invention.
FIG. 4 is a schematic structural view of a composite steel fireproof rolling curtain II of the present invention.
FIG. 5 is a schematic view of the roller structure of the present invention.
Fig. 6 is a schematic view of the structure of the bushing of the present invention.
FIG. 7 is a schematic view of a partially enlarged structure of the roll shaft according to the present invention.
Fig. 8 is a schematic structural diagram of the adjusting mechanism of the present invention.
Fig. 9 is a schematic view of a split structure of the sliding disk of the present invention.
Fig. 10 is a schematic structural view of a guide rail ii according to the present invention.
Illustration of the drawings: 1. rolling door main part, 2, compound steel fire prevention roll up curtain I, 3, compound steel fire prevention roll up curtain II, 4, soft coating, 5, box, 6, run-through I, 7, roller, 8, fixed bolster I, 9, motor, 10, fixed bolster II, 11, sleeve pipe, 12, arc wall, 13, lantern ring, 14, the arc, 15, adjustment mechanism, 16, limiting plate, 17, rolling disc, 18, sliding disc, 19, the guide way, 20, ring form piece, 21, the roller bearing, 22, the connection piece, 23, the card axle, 24, run-through II, 25, the support arm, 26, the baffle, 27, the draw-in groove, 28, guided way I, 29, guided way II, 30, lift spout I, 31, lift spout II, 32, the guide piece, 33, the spring.
Detailed Description
Example 1
The high silica glass fiber mainly comprises the following raw materials in parts by weight: 78 parts of silicon dioxide, 16 parts of silicon carbide, 3 parts of aluminum oxide, 12 parts of boron trioxide, 7 parts of sodium oxide and 0.08 part of rare earth oxide. The rare earth oxide is prepared from holmium oxide and niobium pentoxide in a weight ratio of 2: 5.
A preparation method of high silica glass fiber comprises the following steps:
(1) weighing silicon dioxide, silicon carbide, aluminum oxide, boron trioxide and sodium oxide according to the specified weight parts, grinding and uniformly mixing to obtain a primary mixture, weighing rare earth oxide according to the specified weight parts after the particle size of the primary mixture reaches the nanometer level, adding the rare earth oxide into the primary mixture, and continuously mixing to form a final raw material mixture, wherein the particle size of the final raw material mixture reaches the nanometer level;
(2) placing the final raw material mixture into a corundum crucible, placing the corundum crucible into a silicon-molybdenum rod electric heating furnace, melting at 1280 ℃ for 2.5 hours to melt the mixture, then casting and molding the melt, placing the molded glass into a muffle furnace, and carrying out split-phase heat treatment at 460 ℃ for 14 hours to obtain a glass material block;
(3) and (3) putting the glass material block into a wire drawing furnace, secondarily melting at 9000 ℃, and drawing wires.
The rotating speed of the wire drawing furnace is 1200 r/min.
The tensile strength of the high-silica glass fiber monofilament in the embodiment is 4969 MPa.
Example 2
The high silica glass fiber mainly comprises the following raw materials in parts by weight: 70 parts of silicon dioxide, 10 parts of silicon carbide, 2 parts of aluminum oxide, 5 parts of boron trioxide, 10 parts of sodium oxide and 0.05 part of rare earth oxide. The rare earth oxide is prepared from holmium oxide and niobium pentoxide in a weight ratio of 1: 5.
A preparation method of high silica glass fiber comprises the following steps:
(1) weighing silicon dioxide, silicon carbide, aluminum oxide, boron trioxide and sodium oxide according to the specified weight parts, grinding and uniformly mixing to obtain a primary mixture, weighing rare earth oxide according to the specified weight parts after the particle size of the primary mixture reaches the nanometer level, adding the rare earth oxide into the primary mixture, and continuously mixing to form a final raw material mixture, wherein the particle size of the final raw material mixture reaches the nanometer level;
(2) placing the final raw material mixture into a corundum crucible, placing the corundum crucible into a silicon-molybdenum rod electric heating furnace, melting at the high temperature of 1200 ℃ for 2 hours to melt the mixture, then casting and molding the melt, placing the molded glass into a muffle furnace, and carrying out phase-splitting heat treatment at the temperature of 450 ℃ for 12 hours to obtain a glass material block;
(3) and (3) putting the glass material block into a wire drawing furnace, secondarily melting at 800 ℃ and drawing wires.
The rotating speed of the wire drawing furnace is 1000 rpm.
The tensile strength of the high silica glass fiber monofilament in the embodiment is 4933 MPa.
Example 3
The high silica glass fiber mainly comprises the following raw materials in parts by weight: 80 parts of silicon dioxide, 20 parts of silicon carbide, 5 parts of aluminum oxide, 15 parts of boron trioxide, 15 parts of sodium oxide and 0.1 part of rare earth oxide. The rare earth oxide is prepared from holmium oxide and niobium pentoxide in a weight ratio of 3: 5.
A preparation method of high silica glass fiber comprises the following steps:
(1) weighing silicon dioxide, silicon carbide, aluminum oxide, boron trioxide and sodium oxide according to the specified weight parts, grinding and uniformly mixing to obtain a primary mixture, weighing rare earth oxide according to the specified weight parts after the particle size of the primary mixture reaches the nanometer level, adding the rare earth oxide into the primary mixture, and continuously mixing to form a final raw material mixture, wherein the particle size of the final raw material mixture reaches the nanometer level;
(2) placing the final raw material mixture into a corundum crucible, placing the corundum crucible into a silicon-molybdenum rod electric heating furnace, melting at 1350 ℃ for 3 hours to melt the mixture, then casting and molding the melt, placing the molded glass into a muffle furnace, and performing phase-splitting heat treatment at 480 ℃ for 16 hours to obtain a glass material block;
(3) and (3) putting the glass material block into a wire drawing furnace, secondarily melting at 1000 ℃ and drawing wires.
The rotating speed of the wire drawing furnace is 1400 revolutions per minute.
The tensile strength of the high-silica glass fiber monofilament in the embodiment is 4945 MPa.
Comparative example 1
The high silica glass fiber mainly comprises the following raw materials in parts by weight: 78 parts of silicon dioxide, 16 parts of silicon carbide, 3 parts of aluminum oxide, 12 parts of boron trioxide, 7 parts of sodium oxide and 0.08 part of rare earth oxide. The rare earth oxide consists of holmium oxide and niobium pentoxide in a weight ratio of 1: 1.
A preparation method of high silica glass fiber comprises the following steps:
(1) weighing silicon dioxide, silicon carbide, aluminum oxide, boron trioxide and sodium oxide according to the specified weight parts, grinding and uniformly mixing to obtain a primary mixture, weighing rare earth oxide according to the specified weight parts after the particle size of the primary mixture reaches the nanometer level, adding the rare earth oxide into the primary mixture, and continuously mixing to form a final raw material mixture, wherein the particle size of the final raw material mixture reaches the nanometer level;
(2) placing the final raw material mixture into a corundum crucible, placing the corundum crucible into a silicon-molybdenum rod electric heating furnace, melting at 1280 ℃ for 2.5 hours to melt the mixture, then casting and molding the melt, placing the molded glass into a muffle furnace, and carrying out split-phase heat treatment at 460 ℃ for 14 hours to obtain a glass material block;
(3) and (3) putting the glass material block into a wire drawing furnace, secondarily melting at 9000 ℃, and drawing wires.
The rotating speed of the wire drawing furnace is 1200 r/min.
The tensile strength of the high-silica glass fiber monofilament in the embodiment is 3857 MPa.
The invention also discloses a fire-proof device which is a rolling shutter door, in particular to a fire-proof rolling shutter door convenient for fire fighting, wherein the surface of the rolling shutter door is provided with the high silica glass fiber. Preferably, the high silica glass fiber is bonded to the surface of the rolling door through aerogel.
The rolling door comprises a rolling door main body 1, a composite steel fireproof rolling curtain I2, a composite steel fireproof rolling curtain II 3, a box body 5 and a motor 9, wherein the rolling door main body 1 comprises the composite steel fireproof rolling curtain I2 and the composite steel fireproof rolling curtain II 3, the composite steel fireproof rolling curtain II 3 is arranged on the left upper side of the composite steel fireproof rolling curtain I2, a connecting sheet 22 is hinged at the upper end of the composite steel fireproof rolling curtain II 3, a clamping shaft 23 is arranged on the upper side of the connecting sheet 22, the clamping shaft 23 is clamped between an arc-shaped groove 12 and an arc-shaped plate 14, when a sleeve 11 rotates along a pointer, the clamping shaft 23 can fall out of the arc-shaped groove 12 and fall downwards, the upper end of the composite steel fireproof rolling curtain II 3 falls and is folded to form an opening, the fire is conveniently extinguished and controlled from the folding opening of the composite steel fireproof rolling curtain II 3, the lower end of the composite steel fireproof rolling curtain II 3 is hinged with the composite steel fireproof rolling curtain I2, the composite steel fireproof roller shutter comprises a composite steel fireproof roller shutter I2 and a composite steel fireproof roller shutter II 3, wherein a soft coating layer 4 is arranged on the outer side of the composite steel fireproof roller shutter I2 and the outer side of the composite steel fireproof roller shutter II 3, a box body 5 for accommodating the roller shutter main body 1 is arranged on the upper side of the roller shutter main body 1, a through hole I6 is formed in the box body 5, a roller shaft 7 for rolling the composite steel fireproof roller shutter I2 and the composite steel fireproof roller shutter II 3 is arranged on the inner side of the box body 5, the upper end of the composite steel fireproof roller shutter I2 is hinged to the roller shaft 7, fixing supports I8 connected with the box body 5 are arranged at the two ends of the roller shaft 7, a motor 9 for driving the roller shaft 7 is arranged on the right side of the roller shaft 7, and a fixing support II 10 connected with the right side wall of the box body 5 is arranged on the motor 9;
the diameter of the left part of the roll shaft 7 is smaller than that of the right part, a sleeve 11 is sleeved on the left part of the roll shaft 7, a quarter position of the sleeve 11 is in an open state, an arc-shaped groove 12 is formed in the sleeve 11, a sleeve ring 13 is sleeved at the left end of the sleeve 11, an arc-shaped plate 14 is connected to the left part of the roll shaft 7, and the arc-shaped plate 14 is located in the open position of the sleeve 11;
the left side of the roller shaft 7 is provided with an adjusting mechanism 15 for adjusting the rotation of the sleeve 11, the adjusting mechanism 15 comprises a limiting plate 16, a rotating disc 17 and a sliding disc 18, the inner side of the limiting plate 16 is provided with a through opening II 24 longitudinally penetrating the limiting plate 16, a support arm 25 connected with the rotating disc 17 is arranged in the through opening II 24, the upper side of the through opening II 24 is provided with a spring 33 for elastically supporting the support arm 25, the support arm 25 is provided with a baffle 26, the baffle 26 is positioned in the through opening I6, the middle part of the limiting plate 16 is provided with the rotating disc 17, the inner wall of the rotating disc 17 is provided with three clamping grooves 27 for clamping the roller 21, the limiting plate 16 is provided with a guide groove 19 for clockwise rotation of the rotating disc 17, the inner side of the rotating disc 17 is provided with the sliding disc 18, the sliding disc 18 comprises a pair of annular sheets 20, three roller shafts 21 are connected between the annular sheets 20, so that the sliding disc 18 is in a balanced state, when the sliding disk 18 inclines to any side, the sliding disk can slide rapidly to perform balance restoration, and the lantern ring 13 is positioned between the three rollers 21 and is in contact with the rollers 21;
rolling slats door main part 1 right side is provided with and is used for leading compound steel fire prevention to roll up gliding guided way I28 of I2 lift, 1 left side of rolling slats door main part is provided with and is used for leading compound steel fire prevention to roll up curtain I2 and compound steel fire prevention to roll up II 3 guided way II 29, be provided with lift spout I30 on guided way II 29, compound steel fire prevention is rolled up curtain I2 right-hand member and compound steel fire prevention to roll up II 3 right-hand member block and is gone up and down in lift spout I30, lift spout I30 front side is provided with lift spout II 31, II 29 upsides of guided way are provided with and are used for direction card axle 23 to go into the direction piece 32 in the lift spout II 31 to the downside, the direction falls into in lift spout II 31 when making card axle 23 drop to the downside, make compound steel fire prevention roll up curtain II 3 can form fold condition fast and form the opening.
The surface of at least one of the composite steel fireproof roller shutter I and the composite steel fireproof roller shutter II is provided with a high-silica glass fiber layer, and the high-silica glass fiber layers can be arranged; certainly, other components in the fireproof rolling door can be provided according to actual needs, and a silica glass fiber layer is high and is bonded to the surface of the fireproof rolling door or the surface of each component through aerogel.
Through the card axle block between arc wall and arc, the card axle can be followed the arc wall and come out and drop to the downside when making the sleeve pipe rotate along with the pointer, makes II upper ends whereabouts of compound steel fire-resistant rolling curtain folding formation openings of falling, is convenient for stamp out the control to the conflagration from II folding openings of compound steel fire-resistant rolling curtain.
Through II direction card axial downside of guided way guide rails get into the direction piece in the lift spout II, the direction falls into in the lift spout II when making card axial downside drop, makes compound steel fire prevention shutter II can form fold condition fast and form the opening.
Three rolling shafts are connected and arranged between the annular sheets, so that the sliding disc is in a balanced state, and can quickly slide to perform balance restoration when the sliding disc inclines to any side.
The surface of at least one of the roller shutter door main body, the composite steel fireproof roller shutter I and the composite steel fireproof roller shutter II is provided with a high silica glass fiber layer. The high silica glass fiber layer has good high temperature resistance, and prevents the rolling door and parts of the rolling door from deforming at high temperature.
The aerogel used in the invention is silicon-aluminum composite aerogel, and is prepared by the following method:
step 1, pretreating fly ash;
step 2, mixing the pretreated fly ash with a hydrochloric acid solution, carrying out suction filtration on the obtained reaction liquid after boiling water bath, mixing the obtained filter residue with an alkali solution, and carrying out suction filtration to obtain an aluminosilicate solution;
step 3, performing cation resin exchange on the aluminosilicate solution obtained in the step 2, and catalyzing the obtained filtrate to obtain silicon-aluminum sol;
step 4, preparing pure aluminum sol: mixing aluminum salt and a chelating agent, and dropwise adding ethanol, water and a catalyst to react to obtain pure aluminum sol;
step 5, uniformly mixing the silicon-aluminum sol prepared in the step 3 and the pure aluminum sol obtained in the step 4 to prepare silicon-aluminum composite sol;
and 6, standing, aging and drying the silicon-aluminum composite sol to obtain the silicon-aluminum composite sol.
In one example, the following protocol was used to prepare aerogels:
the method comprises the following steps:
step 1, coal ash pretreatment: mixing fly ash and sodium carbonate according to the mass ratio of 1:1, and then carrying out high-temperature calcination, water washing and drying. The calcining temperature is 500 ℃, the calcining time is 3 hours, and the calcining temperature is 3 times, and the calcining time is 1 hour after the calcining time is 3 times and the calcining time is 150 ℃.
Step 2, mixing the pretreated fly ash and a hydrochloric acid solution according to the mass volume ratio of 1:5g/mL, and reacting in a boiling water bath for 3 hours; and after boiling water bath, carrying out suction filtration on the obtained reaction liquid, and mixing the obtained filter residue and the alkali solution according to the mass-volume ratio of 1:5g/mL for reaction for 3 h. The concentration of the hydrochloric acid solution is 3mol/L, and the concentration of the alkali solution is 15 g/L.
Step 3, performing cation resin exchange on the aluminosilicate solution obtained in the step 2, and catalyzing the obtained filtrate to obtain silicon-aluminum sol; in step 3, cation resin exchange is carried out on the aluminosilicate solution until the pH value of the solution is 2-3, the used catalyst is ammonia water, and the pH value of the solution reaction is 5-7.
Step 4, preparing pure aluminum sol: mixing aluminum isopropoxide and ethyl acetoacetate, and dropwise adding ethanol, water and ammonia water to react to obtain pure aluminum sol; the molar ratio of aluminum isopropoxide to ethyl acetoacetate to ethanol to water to ammonia water is as follows: 1:0.1:5:1:0.1.
And 5, uniformly mixing the silicon-aluminum sol prepared in the step 3 and the pure aluminum sol obtained in the step 4 according to the mass ratio of 5:1 to prepare the silicon-aluminum composite sol.
And 6, standing the silicon-aluminum composite sol for 1 hour at 60 ℃, adding an alcohol solvent for aging for 24 hours, and finally placing the silicon-aluminum gel in a drying oven at 110 ℃ for drying for 24 hours under normal pressure. The silicon-aluminum composite aerogel powder obtained by crushing and screening has the density of 0.167g/cm3, the porosity of 94.4 percent and the specific surface area of 691.7m 2/g.
In another example, aerogels were prepared using the following method:
the method comprises the following steps:
step 1, coal ash pretreatment: mixing the fly ash and sodium carbonate according to the mass ratio of 1:3, and then carrying out high-temperature calcination, washing and drying. The calcining temperature is 700 ℃, the calcining time is 1.5h, and the calcining temperature is 3 times, and the calcining time is 2h under 175 ℃.
Step 2, mixing the pretreated fly ash and a hydrochloric acid solution according to the mass volume ratio of 1:8g/mL, and reacting in a boiling water bath for 1.5 h; and after boiling water bath, carrying out suction filtration on the obtained reaction liquid, and mixing the obtained filter residue and the alkali solution according to the mass-volume ratio of 1:8g/mL for reaction for 2 h. The concentration of the hydrochloric acid solution is 3.5mol/L, and the concentration of the alkali solution is 20 g/L.
Step 3, performing cation resin exchange on the aluminosilicate solution obtained in the step 2, and catalyzing the obtained filtrate to obtain silicon-aluminum sol; in step 3, cation resin exchange is carried out on the aluminosilicate solution until the pH value of the solution is 2-3, the used catalyst is ammonia water, and the pH value of the solution reaction is 5-7.
Step 4, preparing pure aluminum sol: mixing aluminum sec-butoxide with acetylacetone, and dropwise adding ethanol, water and ammonia water to react to obtain pure aluminum sol; the molar ratio of the aluminum sec-butoxide to the acetylacetone to the ethanol to the water to the ammonia water is as follows: 1:0.3:10:2: 0.5;
step 5, uniformly mixing the silicon-aluminum sol prepared in the step 3 and the pure aluminum sol obtained in the step 4 according to the mass ratio of 6:1 to prepare silicon-aluminum composite sol;
and 6, standing the silicon-aluminum composite sol at 80 ℃ for 1-3h, and adding an alcohol solvent for aging for 24-48h for aging. Finally, the silica-alumina gel is placed in a drying oven at 105 ℃ and dried for 24 hours under normal pressure. The silicon-aluminum composite aerogel powder obtained by crushing and screening has the density of 0.163g/cm3, the porosity of 96.17 percent and the specific surface area of 679.3m 2/g.
The method effectively pretreats the fly ash, fully activates the fly ash, and removes a large amount of impurities in the original fly ash after the fly ash is exchanged by the cation resin, thereby improving the quality of sol.
The silicon-aluminum composite aerogel prepared by utilizing the fly ash has high porosity and specific surface area, and has the quality similar to that of gel obtained by compounding pure silica sol and pure aluminum sol. The invention realizes the high-efficiency resource utilization of the fly ash and reduces the production cost of enterprises.
The above embodiments are only specific examples of the present invention, and the protection scope of the present invention includes but is not limited to the product forms and styles of the above embodiments, and any suitable changes or modifications made by those skilled in the art according to the claims of the present invention shall fall within the protection scope of the present invention.

Claims (7)

1. High silica glass fiber which is characterized in that: the composite material mainly comprises the following raw materials in parts by weight: 70-80 parts of silicon dioxide, 10-20 parts of silicon carbide, 2-5 parts of aluminum oxide, 5-15 parts of boron trioxide, 10-15 parts of sodium oxide and 0.05-0.1 part of rare earth oxide; the rare earth oxide is prepared from holmium oxide and niobium pentoxide according to the weight ratio of (1-3): 5.
2. The high-silica glass fiber according to claim 1, wherein: the material mainly comprises the following raw materials in parts by weight: 78 parts of silicon dioxide, 16 parts of silicon carbide, 3 parts of aluminum oxide, 12 parts of boron trioxide, 7 parts of sodium oxide and 0.08 part of rare earth oxide.
3. The high-silica glass fiber according to claim 1, wherein: the rare earth oxide is prepared from holmium oxide and niobium pentoxide in a weight ratio of 2: 5, the components are mixed.
4. The method of preparing a high-silica glass fiber according to claim 1, wherein: the method comprises the following steps:
(1) weighing silicon dioxide, silicon carbide, aluminum oxide, boron trioxide and sodium oxide according to the specified weight parts, grinding and uniformly mixing to obtain a primary mixture, weighing rare earth oxide according to the specified weight parts after the particle size of the primary mixture reaches the nanometer level, adding the rare earth oxide into the primary mixture, and continuously mixing to form a final raw material mixture, wherein the particle size of the final raw material mixture reaches the nanometer level;
(2) placing the final raw material mixture into a corundum crucible, placing the corundum crucible into a silicon-molybdenum rod electric heating furnace, melting at the high temperature of 1200-1350 ℃ for 2-3 hours to melt the mixture, then casting and molding the melt, placing the molded glass into a muffle furnace, and carrying out phase-splitting heat treatment at the temperature of 450-480 ℃ for 12-16 hours to obtain a glass block;
(3) and (3) putting the glass block into a wire drawing furnace, and carrying out secondary melting and wire drawing at 800-.
5. The method of preparing a high-silica glass fiber according to claim 4, wherein: the rotating speed of the wire drawing furnace is 1000-1400 rpm.
6. A fire protection device, wherein the fire protection device is a roller door provided with high silica glass fibers according to any one of claims 1 to 6.
7. The fire protection device of claim 6, wherein the high silica glass fibers are bonded to the surface of the tambour door by an aerogel.
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US2444845A (en) * 1946-05-09 1948-07-06 Leeds & Northrup Co ph-responsive glass electrode
CN1926073B (en) * 2004-03-11 2010-05-12 艾利森电讯公司 Glass for optical magnifier fiber
JP6081914B2 (en) * 2010-10-18 2017-02-15 オーシーヴィー インテレクチュアル キャピタル リミテッド ライアビリティ カンパニー High refractive index glass composition
CN103896494A (en) * 2014-03-10 2014-07-02 苏州捷德瑞精密机械有限公司 Glass optical fiber and preparation method thereof
CN108423999A (en) * 2018-03-28 2018-08-21 济南大学 A kind of low dielectric glass fiber of free-floride and preparation method thereof that rare earth oxide is co-doped with
CN111747654B (en) * 2020-07-10 2022-04-01 巨石集团有限公司 High-modulus glass fiber composition, and glass fiber and composite material thereof

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Denomination of invention: A high silica glass fiber and its preparation method and fireproof equipment

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