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CN109626831A - A method of reducing residual microbubbles in electronic glass fibers - Google Patents

A method of reducing residual microbubbles in electronic glass fibers Download PDF

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Publication number
CN109626831A
CN109626831A CN201910039253.2A CN201910039253A CN109626831A CN 109626831 A CN109626831 A CN 109626831A CN 201910039253 A CN201910039253 A CN 201910039253A CN 109626831 A CN109626831 A CN 109626831A
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glass
particle
raw material
tail gas
glass metal
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Inventor
宁祥春
李伟
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Henan Guangyuan New Materials Ltd By Share Ltd
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Henan Guangyuan New Materials Ltd By Share Ltd
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Priority to CN201910039253.2A priority Critical patent/CN109626831A/en
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C13/00Fibre or filament compositions
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01Manufacture of glass fibres or filaments
    • C03B37/02Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
    • C03B37/022Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from molten glass in which the resultant product consists of different sorts of glass or is characterised by shape, e.g. hollow fibres, undulated fibres, fibres presenting a rough surface
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B5/00Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
    • C03B5/16Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
    • C03B5/18Stirring devices; Homogenisation
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B5/00Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
    • C03B5/16Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
    • C03B5/225Refining
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C1/00Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/004Refining agents

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

Abstract

The invention discloses a kind of methods for reducing residual microbubbles in electronic glass fibers, including glass raw material prepares, glass raw material is melted, glass metal defoaming, tail gas clean-up, the defoaming of glass metal vacuum, glass metal cools down and glass metal molding;The method of this kind reduction residual microbubbles in electronic glass fibers, pass through the specified particle size gradation of glass raw material particle, in i.e. same raw particles, proportion optimizing between different-grain diameter particle, realize optimal melted effect, reduce bubbles number and bubble diameter, by further being defoamed using the method for vacuum defoaming again after clarifying agent defoams, two kinds of debubbling methods combine, so as to reach good defoaming effect, advantageously reduce residual microbubbles in electronic glass fibers, improve the quality of electronic-grade glass, by being purified to the tail gas during defoaming, remove the nitrogen oxides and SO in tail gas2, so that final vent gas meet the requirement of environmental protection, is conducive to protect environment.

Description

A method of reducing residual microbubbles in electronic glass fibers
Technical field
It is the present invention relates to glass fibre technical field of producing, in particular to residual in a kind of reduction electronic-grade glass The method for staying microbubble.
Background technique
Glass fibre, English original name are glass fiber, are a kind of inorganic non-metallic materials haveing excellent performance, type is numerous It is more, have many advantages, such as that good insulating, heat resistance are strong, corrosion resistance is good, high mechanical strength.Using glass fibre as the circuit board of substrate It is that performance is best in current various circuit boards, with good insulation preformance, dielectric constant is low, dielectric loss is small, mechanical performance is excellent The development of the series of advantages such as good, especially current electronic product is getting faster, and the application of fiberglass circuit board is also increasingly Extensively, correspondingly also higher and higher to the performance requirement of fiberglass circuit board.Circuit board in the fabrication process, need drill and Spraying plating in hole.If the hole bored is communicated with this microbubble, plating solution or lead liquid will penetrate into what this microbubble was formed In cavity, decline circuit board electrical insulation capability, forms abnormal circuit to generate short circuit, reduce the performance of circuit board so that making Circuit board is scrapped, therefore the quantity and size of microbubble are remained in glass fibre, is the electricity for determining manufacture fiberglass circuit board The key technical index of sub- level fiberglass quality.
But due to being limited by preparation process, glass is in melting process, it will usually incorporate part bubble, lead to glass It is easy the various bubbles of residual in limit, affects the quality of glass fibre.At present in the base glass of electronic-grade glass Such as reinforcement stirring has been used in production technology, is improved stove, is improved composition of raw materials, from a series of reduction bubbles of tank bottom bubbling Measure, but more bubble is still remained in base glass, seriously affect the quality of electronic-grade glass.
Summary of the invention
The main purpose of the present invention is to provide a kind of methods for reducing residual microbubbles in electronic glass fibers, can be with Effectively solve the problems in background technique.
To achieve the above object, the invention provides the following technical scheme: being remained in a kind of reduction electronic-grade glass micro- The method of bubble, including glass raw material prepare, glass raw material be melted, glass metal defoaming, tail gas clean-up, glass metal vacuum defoam, Glass metal cooling and glass metal molding, steps are as follows for specific method:
Glass raw material prepares: glass raw material particle being rinsed using pure water or deionized water, then, is dried in the air naturally It does or is dried up by large-scale fan, and according to feldspar, the quartz sand, lime in certain second fraction glazing raw particles Stone, dolomite, soda ash and saltcake;
Glass raw material is melted: glass raw material particle being placed in kiln, rises to 1600~1700 DEG C by room temperature, and keep the temperature 2 Glass metal is made in~3h;
Glass metal defoaming: appropriate clarifying agent is added in 1600~1650 DEG C of glass metal, it is total that clarifying agent accounts for glass raw material The 1-3.5% of amount, settling time are 90~180 minutes, and clarifying agent generates the gas being largely dissolved in glass metal at high temperature, It is permeated to the bubble remained in glass metal, to take away the micro-bubble in glass metal;
Tail gas clean-up: the tail gas generated in defoaming process is collected using hood, and is sent tail gas to denitration using blower Purified treatment is carried out in device, is discharged into atmosphere again after purified tail gas cooling;
The defoaming of glass metal vacuum: being placed under vacuum environment progress vacuum defoaming for glass metal, and pressure maintaining 5-30 minutes, by can The vacuum degree of control promotes high-temperature glass liquid to escape due to pressure, improves the discharge ability of bubble;
Glass metal cooling: the temperature of the glass metal after clarification is down to 1610 DEG C, and keeps the temperature 1.5~2h;
Glass metal molding: wire-drawing shape is carried out to glass metal using bushing at a temperature of 1610 DEG C, E-glass is made Fiber.
Preferably, in the glass raw material preparation process, feldspar, quartz sand, lime stone, white clouds in glass raw material particle Stone, soda ash and saltcake are allocated according to following particle size fraction: feldspar, and partial size is the total feldspar amount of feldspar particle Zhan of 0.1-0.25mm 70-75wt%, partial size be 0.4-0.55mm the total feldspar amount of feldspar particle Zhan 25-30wt%;Quartz sand, partial size 0.1- The quartz sand particle of 1mm accounts for the 85-90wt% of quartz sand total amount, and it is total that partial size is that the quartz sand particle of 0.05-0.1mm accounts for quartz sand The 10-15wt% of amount;Lime stone, partial size are that the limestone particle of 0.08-0.15mm accounts for the 15-20wt% of lime stone total amount, grain Diameter is that the limestone particle of 2.5-3.0mm accounts for the 80-85wt% of lime stone total amount;Dolomite, partial size are the white of 0.05-0.2mm Dolomite particles account for the 15-20wt% of dolomite total amount, and partial size is that the dolomite particles of 2.0-2.5mm account for the 80- of dolomite total amount 85wt%;Soda ash, partial size are that the soda ash particle of 0.1-1mm accounts for the 70-75wt% of soda ash total amount, and partial size is pure for 0.05-0.1mm's Alkali particle accounts for the 25-30wt% of soda ash total amount;Saltcake, partial size are that the saltcake particle of 0.1-1mm accounts for the 85- of saltcake total amount 90wt%, partial size are that the saltcake particle of 0.08-0.1mm accounts for the 10-15wt% of saltcake total amount.
Preferably, in the glass raw material melting step, appropriate boric acid is added and fluorite makees fluxing agent.
Preferably, in the glass raw material melting step, 3~5 DEG C/min of heating rate.
Preferably, in the tail gas clean-up step, denitrification apparatus sprays into NH into tail gas3, tail gas and NH3After mixing Together by SCR reactor, under the action of catalyst, by NOxIt is reduced into harmless N2And H2O reaches good clean-up effect, The SCR reactor is to be filled with catalyst (such as V2O5-TiO2) reactor, for by the nitrogen oxides and ammonia in tail gas It is catalytically converted into nontoxic gas.
Preferably, in the tail gas clean-up step, the temperature for controlling tail gas is about 280~420 DEG C.
Preferably, in the glass metal cooling step, rate of temperature fall is 1~3 DEG C/min.
Compared with prior art, the invention has the following beneficial effects:
1), incomplete and glass is reacted in the fusing due to the presence of Bubbles in Glass mainly by batch in melting process Caused by glass liquid homogenizing is insufficient, and the granularity of glass raw material then influences the fusing and homogenizing of glass, the grain of glass raw material To spend smaller, the contact area between raw material is bigger, and reaction surface is also bigger, so that the reaction speed between raw material is also bigger, On the contrary, the speed to react between raw material is slower when raw material granularity is bigger than normal, so that burn-off rate is slack-off, but if raw material grain It spends small, is then easy to produce and flies upward and agglomerate, while the lesser raw material of granularity can prematurely participate in reacting, batch is caused to be melted Layering also will affect being melted for glass, be unfavorable for the homogenizing of glass;By the specified particle size gradation of glass raw material particle, i.e., together In a kind of raw particles, the proportion optimizing between different-grain diameter particle realizes optimal melted effect, reduces bubbles number and bubble Diameter;
2), glass metal is defoamed by using clarifying agent, while again using vacuum defoaming after clarifying agent defoaming Method is further defoamed, and two kinds of debubbling methods combine, and so as to reach good defoaming effect, advantageously reduces electricity Microbubble is remained in sub- level fiberglass, improves the quality of electronic-grade glass;
3), by purifying to the tail gas during defoaming, the nitrogen oxides and SO in tail gas are removed2, using ammonia and Selective reduction reaction makes conversion of nitrogen oxides N to tail gas under the action of catalyst2And H2O achievees the effect that purification, has The characteristics of purification efficiency is high, good purification, so that final vent gas meet the requirement of environmental protection, is conducive to protect environment.
Specific embodiment
To be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, below with reference to Specific embodiment, the present invention is further explained.
A method of residual microbubbles in electronic glass fibers being reduced, including glass raw material prepares, glass raw material is molten System, glass metal defoaming, tail gas clean-up, the defoaming of glass metal vacuum, glass metal cooling and glass metal molding, specific method step is such as Under:
Glass raw material prepares: glass raw material particle being rinsed using pure water or deionized water, then, is dried in the air naturally It does or is dried up by large-scale fan, and according to feldspar, the quartz sand, lime in certain second fraction glazing raw particles Stone, dolomite, soda ash and saltcake;
Glass raw material is melted: glass raw material particle being placed in kiln, rises to 1600~1700 DEG C by room temperature, and keep the temperature 2 Glass metal is made in~3h;
Glass metal defoaming: appropriate clarifying agent is added in 1600~1650 DEG C of glass metal, it is total that clarifying agent accounts for glass raw material The 1-3.5% of amount, settling time are 90~180 minutes, and clarifying agent generates the gas being largely dissolved in glass metal at high temperature, It is permeated to the bubble remained in glass metal, to take away the micro-bubble in glass metal;
Tail gas clean-up: the tail gas generated in defoaming process is collected using hood, and is sent tail gas to denitration using blower Purified treatment is carried out in device, is discharged into atmosphere again after purified tail gas cooling;
The defoaming of glass metal vacuum: being placed under vacuum environment progress vacuum defoaming for glass metal, and pressure maintaining 5-30 minutes, by can The vacuum degree of control promotes high-temperature glass liquid to escape due to pressure, improves the discharge ability of bubble;
Glass metal cooling: the temperature of the glass metal after clarification is down to 1610 DEG C, and keeps the temperature 1.5~2h;
Glass metal molding: wire-drawing shape is carried out to glass metal using bushing at a temperature of 1610 DEG C, E-glass is made Fiber.
Feldspar, quartz sand, lime stone, dolomite, soda ash and awns in glass raw material preparation process, in glass raw material particle Nitre is allocated according to following particle size fraction: feldspar, and partial size is the 70- of the total feldspar amount of feldspar particle Zhan of 0.1-0.25mm 75wt%, partial size are the 25-30wt% of the total feldspar amount of feldspar particle Zhan of 0.4-0.55mm;Quartz sand, partial size are 0.1-1mm's Quartz sand particle accounts for the 85-90wt% of quartz sand total amount, and partial size is that the quartz sand particle of 0.05-0.1mm accounts for quartz sand total amount 10-15wt%;Lime stone, partial size are that the limestone particle of 0.08-0.15mm accounts for the 15-20wt% of lime stone total amount, and partial size is The limestone particle of 2.5-3.0mm accounts for the 80-85wt% of lime stone total amount;Dolomite, partial size are the dolomite of 0.05-0.2mm Particle accounts for the 15-20wt% of dolomite total amount, and partial size is that the dolomite particles of 2.0-2.5mm account for the 80- of dolomite total amount 85wt%;Soda ash, partial size are that the soda ash particle of 0.1-1mm accounts for the 70-75wt% of soda ash total amount, and partial size is pure for 0.05-0.1mm's Alkali particle accounts for the 25-30wt% of soda ash total amount;Saltcake, partial size are that the saltcake particle of 0.1-1mm accounts for the 85- of saltcake total amount 90wt%, partial size are that the saltcake particle of 0.08-0.1mm accounts for the 10-15wt% of saltcake total amount.
In glass raw material melting step, appropriate boric acid is added and fluorite makees fluxing agent.
In glass raw material melting step, 3~5 DEG C/min of heating rate.
In tail gas clean-up step, denitrification apparatus sprays into NH into tail gas3, tail gas and NH3Pass through SCR together after mixing Reactor, under the action of catalyst, by NOxIt is reduced into harmless N2And H2O, reaches good clean-up effect, and SCR reactor is It is filled with catalyst (such as V2O5-TiO2) reactor, for by tail gas nitrogen oxides and ammonia be catalytically converted into nontoxic nothing Evil gas.
In tail gas clean-up step, the temperature for controlling tail gas is about 280~420 DEG C.
In glass metal cooling step, rate of temperature fall is 1~3 DEG C/min.
Embodiment 1
A method of residual microbubbles in electronic glass fibers being reduced, including glass raw material prepares, glass raw material is molten System, glass metal defoaming, tail gas clean-up, the defoaming of glass metal vacuum, glass metal cooling and glass metal molding, specific method step is such as Under:
Glass raw material prepares: glass raw material particle being rinsed using pure water or deionized water, then, is dried in the air naturally It does or is dried up by large-scale fan, and be allocated feldspar, quartz sand, stone in glass raw material particle according to following particle size fraction Lime stone, dolomite, soda ash and saltcake;Feldspar, partial size are the 75wt% of the total feldspar amount of feldspar particle Zhan of 0.1-0.25mm, partial size For the 25wt% of the total feldspar amount of feldspar particle Zhan of 0.4-0.55mm;Quartz sand, partial size are that the quartz sand particle of 0.1-1mm accounts for stone The 85wt% of sand total amount, partial size are that the quartz sand particle of 0.05-0.1mm accounts for the 15wt% of quartz sand total amount;Lime stone, partial size The 15wt% of lime stone total amount is accounted for for the limestone particle of 0.08-0.15mm, partial size is that the limestone particle of 2.5-3.0mm accounts for stone The 85wt% of lime stone total amount;Dolomite, partial size are that the dolomite particles of 0.05-0.2mm account for the 20wt% of dolomite total amount, partial size The 80wt% of dolomite total amount is accounted for for the dolomite particles of 2.0-2.5mm;Soda ash, partial size account for pure for the soda ash particle of 0.1-1mm The 70wt% of alkali total amount, partial size are that the soda ash particle of 0.05-0.1mm accounts for the 30wt% of soda ash total amount;Saltcake, partial size 0.1- The saltcake particle of 1mm accounts for the 85wt% of saltcake total amount, and partial size is that the saltcake particle of 0.08-0.1mm accounts for the 15wt% of saltcake total amount;
Glass raw material is melted: glass raw material particle being placed in kiln, appropriate boric acid is added and fluorite makees fluxing agent, with 5 DEG C/heating rate of min rises to 1650 DEG C by room temperature, and keeps the temperature 2h, glass metal is made;
Glass metal defoaming: appropriate clarifying agent is added in 1650 DEG C of glass metal, clarifying agent accounts for glass raw material total amount 1%, settling time is 100 minutes, and clarifying agent generates at high temperature is largely dissolved in gases in glass metal, to remaining on glass Bubble in liquid is permeated, to take away the micro-bubble in glass metal;
Tail gas clean-up: the tail gas generated in defoaming process is collected using hood, and is sent tail gas to denitration using blower Purified treatment is carried out in device, the temperature for controlling tail gas is about 300 DEG C, and denitrification apparatus sprays into NH into tail gas3, tail gas and NH3It is mixed Together by SCR reactor after closing uniformly, under the action of catalyst, by NOxIt is reduced into harmless N2And H2O reaches good net Change effect, the SCR reactor is to be filled with catalyst (such as V2O5-TiO2) reactor, for by the nitrogen oxides in tail gas It is catalytically converted into nontoxic gas with ammonia, is discharged into atmosphere again after purified tail gas cooling;
The defoaming of glass metal vacuum: glass metal being placed under vacuum environment and carries out vacuum defoaming, and pressure maintaining 15 minutes, by controllable Vacuum degree promote high-temperature glass liquid to escape due to pressure, improve the discharge ability of bubble;
Glass metal cooling: the temperature of the glass metal after clarification is down to 1610 DEG C with the rate of temperature fall of 3 DEG C/min, and keeps the temperature 2h;
Glass metal molding: wire-drawing shape is carried out to glass metal using bushing at a temperature of 1610 DEG C, E-glass is made Fiber.
Embodiment 2
A method of residual microbubbles in electronic glass fibers being reduced, including glass raw material prepares, glass raw material is molten System, glass metal defoaming, tail gas clean-up, the defoaming of glass metal vacuum, glass metal cooling and glass metal molding, specific method step is such as Under:
Glass raw material prepares: glass raw material particle being rinsed using pure water or deionized water, then, is dried in the air naturally It does or is dried up by large-scale fan, and be allocated feldspar, quartz sand, stone in glass raw material particle according to following particle size fraction Lime stone, dolomite, soda ash and saltcake;Feldspar, partial size are the 75wt% of the total feldspar amount of feldspar particle Zhan of 0.1-0.25mm, partial size For the 25wt% of the total feldspar amount of feldspar particle Zhan of 0.4-0.55mm;Quartz sand, partial size are that the quartz sand particle of 0.1-1mm accounts for stone The 85wt% of sand total amount, partial size are that the quartz sand particle of 0.05-0.1mm accounts for the 15wt% of quartz sand total amount;Lime stone, partial size The 15wt% of lime stone total amount is accounted for for the limestone particle of 0.08-0.15mm, partial size is that the limestone particle of 2.5-3.0mm accounts for stone The 85wt% of lime stone total amount;Dolomite, partial size are that the dolomite particles of 0.05-0.2mm account for the 20wt% of dolomite total amount, partial size The 80wt% of dolomite total amount is accounted for for the dolomite particles of 2.0-2.5mm;Soda ash, partial size account for pure for the soda ash particle of 0.1-1mm The 70wt% of alkali total amount, partial size are that the soda ash particle of 0.05-0.1mm accounts for the 30wt% of soda ash total amount;Saltcake, partial size 0.1- The saltcake particle of 1mm accounts for the 85wt% of saltcake total amount, and partial size is that the saltcake particle of 0.08-0.1mm accounts for the 15wt% of saltcake total amount;
Glass raw material is melted: glass raw material particle being placed in kiln, appropriate boric acid is added and fluorite makees fluxing agent, with 5 DEG C/heating rate of min rises to 1650 DEG C by room temperature, and keeps the temperature 2h, glass metal is made;
Glass metal defoaming: appropriate clarifying agent is added in 1650 DEG C of glass metal, clarifying agent accounts for glass raw material total amount 2%, settling time is 100 minutes, and clarifying agent generates at high temperature is largely dissolved in gases in glass metal, to remaining on glass Bubble in liquid is permeated, to take away the micro-bubble in glass metal;
Tail gas clean-up: the tail gas generated in defoaming process is collected using hood, and is sent tail gas to denitration using blower Purified treatment is carried out in device, the temperature for controlling tail gas is about 300 DEG C, and denitrification apparatus sprays into NH into tail gas3, tail gas and NH3It is mixed Together by SCR reactor after closing uniformly, under the action of catalyst, by NOxIt is reduced into harmless N2And H2O reaches good net Change effect, the SCR reactor is to be filled with catalyst (such as V2O5-TiO2) reactor, for by the nitrogen oxides in tail gas It is catalytically converted into nontoxic gas with ammonia, is discharged into atmosphere again after purified tail gas cooling;
The defoaming of glass metal vacuum: glass metal being placed under vacuum environment and carries out vacuum defoaming, and pressure maintaining 15 minutes, by controllable Vacuum degree promote high-temperature glass liquid to escape due to pressure, improve the discharge ability of bubble;
Glass metal cooling: the temperature of the glass metal after clarification is down to 1610 DEG C with the rate of temperature fall of 3 DEG C/min, and keeps the temperature 2h;
Glass metal molding: wire-drawing shape is carried out to glass metal using bushing at a temperature of 1610 DEG C, E-glass is made Fiber.
Embodiment 3
A method of residual microbubbles in electronic glass fibers being reduced, including glass raw material prepares, glass raw material is molten System, glass metal defoaming, tail gas clean-up, the defoaming of glass metal vacuum, glass metal cooling and glass metal molding, specific method step is such as Under:
Glass raw material prepares: glass raw material particle being rinsed using pure water or deionized water, then, is dried in the air naturally It does or is dried up by large-scale fan, and be allocated feldspar, quartz sand, stone in glass raw material particle according to following particle size fraction Lime stone, dolomite, soda ash and saltcake;Feldspar, partial size are the 75wt% of the total feldspar amount of feldspar particle Zhan of 0.1-0.25mm, partial size For the 25wt% of the total feldspar amount of feldspar particle Zhan of 0.4-0.55mm;Quartz sand, partial size are that the quartz sand particle of 0.1-1mm accounts for stone The 85wt% of sand total amount, partial size are that the quartz sand particle of 0.05-0.1mm accounts for the 15wt% of quartz sand total amount;Lime stone, partial size The 15wt% of lime stone total amount is accounted for for the limestone particle of 0.08-0.15mm, partial size is that the limestone particle of 2.5-3.0mm accounts for stone The 85wt% of lime stone total amount;Dolomite, partial size are that the dolomite particles of 0.05-0.2mm account for the 20wt% of dolomite total amount, partial size The 80wt% of dolomite total amount is accounted for for the dolomite particles of 2.0-2.5mm;Soda ash, partial size account for pure for the soda ash particle of 0.1-1mm The 70wt% of alkali total amount, partial size are that the soda ash particle of 0.05-0.1mm accounts for the 30wt% of soda ash total amount;Saltcake, partial size 0.1- The saltcake particle of 1mm accounts for the 85wt% of saltcake total amount, and partial size is that the saltcake particle of 0.08-0.1mm accounts for the 15wt% of saltcake total amount;
Glass raw material is melted: glass raw material particle being placed in kiln, appropriate boric acid is added and fluorite makees fluxing agent, with 5 DEG C/heating rate of min rises to 1650 DEG C by room temperature, and keeps the temperature 2h, glass metal is made;
Glass metal defoaming: appropriate clarifying agent is added in 1650 DEG C of glass metal, clarifying agent accounts for glass raw material total amount 3%, settling time is 100 minutes, and clarifying agent generates at high temperature is largely dissolved in gases in glass metal, to remaining on glass Bubble in liquid is permeated, to take away the micro-bubble in glass metal;
Tail gas clean-up: the tail gas generated in defoaming process is collected using hood, and is sent tail gas to denitration using blower Purified treatment is carried out in device, the temperature for controlling tail gas is about 300 DEG C, and denitrification apparatus sprays into NH into tail gas3, tail gas and NH3It is mixed Together by SCR reactor after closing uniformly, under the action of catalyst, by NOxIt is reduced into harmless N2And H2O reaches good net Change effect, the SCR reactor is to be filled with catalyst (such as V2O5-TiO2) reactor, for by the nitrogen oxides in tail gas It is catalytically converted into nontoxic gas with ammonia, is discharged into atmosphere again after purified tail gas cooling;
The defoaming of glass metal vacuum: glass metal being placed under vacuum environment and carries out vacuum defoaming, and pressure maintaining 30 minutes, by controllable Vacuum degree promote high-temperature glass liquid to escape due to pressure, improve the discharge ability of bubble;
Glass metal cooling: the temperature of the glass metal after clarification is down to 1610 DEG C with the rate of temperature fall of 3 DEG C/min, and keeps the temperature 2h;
Glass metal molding: wire-drawing shape is carried out to glass metal using bushing at a temperature of 1610 DEG C, E-glass is made Fiber.
Embodiment 4
A method of residual microbubbles in electronic glass fibers being reduced, including glass raw material prepares, glass raw material is molten System, glass metal defoaming, tail gas clean-up, the defoaming of glass metal vacuum, glass metal cooling and glass metal molding, specific method step is such as Under:
Glass raw material prepares: glass raw material particle being rinsed using pure water or deionized water, then, is dried in the air naturally It does or is dried up by large-scale fan, and be allocated feldspar, quartz sand, stone in glass raw material particle according to following particle size fraction Lime stone, dolomite, soda ash and saltcake;Feldspar, partial size are the 75wt% of the total feldspar amount of feldspar particle Zhan of 0.1-0.25mm, partial size For the 25wt% of the total feldspar amount of feldspar particle Zhan of 0.4-0.55mm;Quartz sand, partial size are that the quartz sand particle of 0.1-1mm accounts for stone The 85wt% of sand total amount, partial size are that the quartz sand particle of 0.05-0.1mm accounts for the 15wt% of quartz sand total amount;Lime stone, partial size The 15wt% of lime stone total amount is accounted for for the limestone particle of 0.08-0.15mm, partial size is that the limestone particle of 2.5-3.0mm accounts for stone The 85wt% of lime stone total amount;Dolomite, partial size are that the dolomite particles of 0.05-0.2mm account for the 20wt% of dolomite total amount, partial size The 80wt% of dolomite total amount is accounted for for the dolomite particles of 2.0-2.5mm;Soda ash, partial size account for pure for the soda ash particle of 0.1-1mm The 70wt% of alkali total amount, partial size are that the soda ash particle of 0.05-0.1mm accounts for the 30wt% of soda ash total amount;Saltcake, partial size 0.1- The saltcake particle of 1mm accounts for the 85wt% of saltcake total amount, and partial size is that the saltcake particle of 0.08-0.1mm accounts for the 15wt% of saltcake total amount;
Glass raw material is melted: glass raw material particle being placed in kiln, appropriate boric acid is added and fluorite makees fluxing agent, with 5 DEG C/heating rate of min rises to 1650 DEG C by room temperature, and keeps the temperature 2h, glass metal is made;
Glass metal defoaming: appropriate clarifying agent is added in 1650 DEG C of glass metal, clarifying agent accounts for glass raw material total amount 3.5%, settling time is 100 minutes, and clarifying agent generates at high temperature is largely dissolved in gases in glass metal, to remaining on glass Bubble in glass liquid is permeated, to take away the micro-bubble in glass metal;
Tail gas clean-up: the tail gas generated in defoaming process is collected using hood, and is sent tail gas to denitration using blower Purified treatment is carried out in device, the temperature for controlling tail gas is about 300 DEG C, and denitrification apparatus sprays into NH into tail gas3, tail gas and NH3It is mixed Together by SCR reactor after closing uniformly, under the action of catalyst, by NOxIt is reduced into harmless N2And H2O reaches good net Change effect, the SCR reactor is to be filled with catalyst (such as V2O5-TiO2) reactor, for by the nitrogen oxides in tail gas It is catalytically converted into nontoxic gas with ammonia, is discharged into atmosphere again after purified tail gas cooling;
The defoaming of glass metal vacuum: glass metal being placed under vacuum environment and carries out vacuum defoaming, and pressure maintaining 30 minutes, by controllable Vacuum degree promote high-temperature glass liquid to escape due to pressure, improve the discharge ability of bubble;
Glass metal cooling: the temperature of the glass metal after clarification is down to 1610 DEG C with the rate of temperature fall of 3 DEG C/min, and keeps the temperature 2h;
Glass metal molding: wire-drawing shape is carried out to glass metal using bushing at a temperature of 1610 DEG C, E-glass is made Fiber.
Table 1 is that the seed concentration in the glass fibre obtained using the method for embodiment 1-4 is compared:
Project Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4
Seed concentration (a seed/m) 0.72-0.84 0.36-0.59 0.08-0.25 0.07-0.20
As shown in Table 1, by controlling the additional amount of clarifying agent, and the dwell time for controlling vacuum defoaming can reduce seed Concentration, therefore, using clarifying agent defoaming and vacuum defoaming method combine and can effectively reduce in electronic-grade glass Residual microbubble.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its Equivalent thereof.

Claims (7)

1. a kind of method for reducing residual microbubbles in electronic glass fibers, which is characterized in that prepare including glass raw material, glass Glass raw material is melted, glass metal defoaming, tail gas clean-up, the defoaming of glass metal vacuum, glass metal cools down and glass metal molding, specific method Steps are as follows:
Glass raw material prepares: glass raw material particle is rinsed using pure water or deionized water, then, naturally dry or Person passes through large-scale fan drying, and according in certain second fraction glazing raw particles feldspar, quartz sand, lime stone, Dolomite, soda ash and saltcake;
Glass raw material is melted: glass raw material particle is placed in kiln, rises to 1600~1700 DEG C by room temperature, and keep the temperature 2~3h, Glass metal is made;
Glass metal defoaming: appropriate clarifying agent is added in 1600~1650 DEG C of glass metal, clarifying agent accounts for glass raw material total amount 1-3.5%, settling time are 90~180 minutes, and clarifying agent generates at high temperature is largely dissolved in gases in glass metal, to residual The bubble in glass metal is stayed to be permeated, to take away the micro-bubble in glass metal;
Tail gas clean-up: the tail gas generated in defoaming process is collected using hood, and is sent tail gas to denitrification apparatus using blower Middle carry out purified treatment is discharged into atmosphere again after purified tail gas cooling;
The defoaming of glass metal vacuum: glass metal being placed under vacuum environment and carries out vacuum defoaming, and pressure maintaining 5-30 minutes, by controllable Vacuum degree promotes high-temperature glass liquid to escape due to pressure, improves the discharge ability of bubble;
Glass metal cooling: the temperature of the glass metal after clarification is down to 1610 DEG C, and keeps the temperature 1.5~2h;
Glass metal molding: wire-drawing shape is carried out to glass metal using bushing at a temperature of 1610 DEG C, electronic-grade glass is made.
2. a kind of method for reducing residual microbubbles in electronic glass fibers according to claim 1, which is characterized in that In the glass raw material preparation process, feldspar, quartz sand, lime stone, dolomite, soda ash and saltcake in glass raw material particle are pressed Be allocated according to following particle size fraction: feldspar, partial size are the 70-75wt% of the total feldspar amount of feldspar particle Zhan of 0.1-0.25mm, grain Diameter is the 25-30wt% of the total feldspar amount of feldspar particle Zhan of 0.4-0.55mm;Quartz sand, partial size are the quartz sand of 0.1-1mm Grain accounts for the 85-90wt% of quartz sand total amount, and partial size is that the quartz sand particle of 0.05-0.1mm accounts for the 10- of quartz sand total amount 15wt%;Lime stone, partial size are that the limestone particle of 0.08-0.15mm accounts for the 15-20wt%, partial size 2.5- of lime stone total amount The limestone particle of 3.0mm accounts for the 80-85wt% of lime stone total amount;Dolomite, partial size are the dolomite particles of 0.05-0.2mm The 15-20wt% of dolomite total amount is accounted for, partial size is that the dolomite particles of 2.0-2.5mm account for the 80-85wt% of dolomite total amount;It is pure Alkali, partial size are that the soda ash particle of 0.1-1mm accounts for the 70-75wt% of soda ash total amount, and partial size is that the soda ash particle of 0.05-0.1mm accounts for The 25-30wt% of soda ash total amount, saltcake, partial size are that the saltcake particle of 0.1-1mm accounts for the 85-90wt% of saltcake total amount, and partial size is The saltcake particle of 0.08-0.1mm accounts for the 10-15wt% of saltcake total amount.
3. a kind of method for reducing residual microbubbles in electronic glass fibers according to claim 1, which is characterized in that In the glass raw material melting step, appropriate boric acid is added and fluorite makees fluxing agent.
4. a kind of method for reducing residual microbubbles in electronic glass fibers according to claim 1, which is characterized in that In the glass raw material melting step, 3~5 DEG C/min of heating rate.
5. a kind of method for reducing residual microbubbles in electronic glass fibers according to claim 1, which is characterized in that In the tail gas clean-up step, denitrification apparatus sprays into NH into tail gas3, tail gas and NH3It is reacted together by SCR after mixing Device, under the action of catalyst, by NOxIt is reduced into harmless N2And H2O, reaches good clean-up effect, and the SCR reactor is It is filled with catalyst (such as V2O5-TiO2) reactor, for by tail gas nitrogen oxides and ammonia be catalytically converted into nontoxic nothing Evil gas.
6. a kind of method for reducing residual microbubbles in electronic glass fibers according to claim 1, which is characterized in that In the tail gas clean-up step, the temperature for controlling tail gas is about 280~420 DEG C.
7. a kind of method for reducing residual microbubbles in electronic glass fibers according to claim 1, which is characterized in that In the glass metal cooling step, rate of temperature fall is 1~3 DEG C/min.
CN201910039253.2A 2019-01-16 2019-01-16 A method of reducing residual microbubbles in electronic glass fibers Pending CN109626831A (en)

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