CN1371878A - Method and apparatus for producing high-refraction glass bead - Google Patents
Method and apparatus for producing high-refraction glass bead Download PDFInfo
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- CN1371878A CN1371878A CN 01103988 CN01103988A CN1371878A CN 1371878 A CN1371878 A CN 1371878A CN 01103988 CN01103988 CN 01103988 CN 01103988 A CN01103988 A CN 01103988A CN 1371878 A CN1371878 A CN 1371878A
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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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
- C03C17/30—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
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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
- C03C12/00—Powdered glass; Bead compositions
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Abstract
The molten lead silicate glass is passed through heat-insulating furnace and material conveying pipe, and fed into centrifugal plate atomization production equipment to make atomization, the atomized glass microbead is moistened with organic solution containing hydrogen-bearing silicon oil, and heated to remove solvent and coated with organosilicon hydrophobic film. The centrifugal plate atomization production equipment is formed from atomization plate, electromagnetic induction heating coil, auxiliary support, extended shaft, high-speed motor, base seat, flange, cooling water jacket, main machine cover and fastener.
Description
The present invention relates to a kind of production method and production equipment of high-refraction glass bead, especially adopt the centrifugal pan atomizing to produce the production method and the corresponding centrifugal pan atomizing production equipment of high-refraction glass bead.
High-refraction glass bead is used as the raw material of light reflecting material in material and production field widespread uses such as tapetum lucidum, reflective tape, refletorized paints.E.I.Du Pont Company in producing the reflective fiber fabric with resin spinning such as glass microballon and fused polyester nylon, directly be made into reflective fabric, replace the fabric that fluorescence vest and glass microballon apply, as the safe clothes at transportation work personnel, cyclist and pedestrian night.The glass microballon that is used for light reflecting material for pursuing good regression reflecting effect, needs high refractive index, (N
d〉=1.9).For the glass microballon that adopts in tapetum lucidum, licence plate, the highway refletorized paint, still needing possesses the characteristics that particle is thin, particle size distribution range is narrow, and the particle diameter of the glass microballon that is adopted mainly is distributed in 10～200 μ m; Glass microballon in highway refletorized paint and the reflective tape also should possess resistance to soiling and rainy day, greasy weather without water stained on its surface, keeps good reflecting effect, and the modified glass microballon of existing surface coatings occurs in this respect.
The high-refraction glass bead of producing can be divided into titanium barium base and plumbous system according to its composition at present; Titanium barium base mainly is titanium dioxide-barium oxide, if plumbous owner's silicon-dioxide-plumbous oxide.The high-refraction glass bead of titanium barium base of being produced and plumbous system, the interpolation rare earth oxide that has is to improve the specific refractory power of product.The production method of high-refraction glass bead is divided into once moulding method and post forming method; Once moulding method is that material is melt into glass melt, and glass melt is dispersed into liquid droplet in a certain way, utilizes its surface tension to make drop be shrunk to pearl, and cooling is collected again; The post forming method is to make desired glass earlier, then glass is pulverized, and screening obtains required glass powder, again powder is heated into pearl with certain sample presentation, type of heating in Cheng Zhulu, cooling, collection.
The post forming method also comprises passes through chemical reaction earlier, forms precipitation or gel, and drying is made powder, again powder is heated into this method of pearl with certain sample presentation, type of heating in Cheng Zhulu.
Once moulding method is dispersed into the means difference that fine droplet adopts according to it with glass melt, is divided into blowing process, centrifuging, electromagnetic method, wire drawing scorification, impeller dispersion method.Blowing process is to utilize the high speed hot gas flow that glass melt is blown out liquid droplet, and drop is shrunk to pearl under self surface tension effects; Centrifuging is to adopt the firing tray of high speed rotating, and glass melt is thrown away into droplet-like, and drop is shrunk to pearl under self surface tension effects; These two kinds of methods can be produced product in enormous quantities, and optical property is good, and particle is thinner, but have hangover and wire drawing phenomenon, have a large amount of glass fibre to produce, and particle size distribution range is wide, and yield rate is low, and yield rate can reach 75～80% in the world.Centrifuging and blowing process contain the high-refraction glass bead of Zr, Ti, Pb, rare-earth oxide for production, because its tendency towards devitrification is bigger, based on these two kinds of methods because the crystallization phenomenon is few.Electromagnetic method be mobile high temp glass liquation under the effect of alternating magnetic field, be dispersed into drop, nodularization Cheng Zhu; The wire drawing scorification is first with the glass melt wire drawing, in the descending process of glass yarn, makes it become drop with flame heating, nodularization Cheng Zhu; The impeller dispersion method is to utilize impeller with holes, under certain speed conditions, the glass melt fluid that falls is dispersed into drop, nodularization Cheng Zhu.The grain roundness of electromagnetic method, wire drawing scorification is greatly improved, but yields poorly, and particle median size 〉=500 μ m can not be used for the production of tapetum lucidum, and added value of product is not high; The product particle of impeller dispersion method is bigger, and also has conditions of streaking to exist, and the work-ing life of impeller is not long, the frequent adhesion of blade and glass melt, and this method is eliminated in developed country.
The post forming method mainly contains separant method, molten metal method, flame smelting method, flame floating method, flame spray gun method.The separant method is to adopt Graphite Powder 99, magnesia powder, silicon dioxide powder as separant, mixes with glass powder, is heated into pearl in the Cheng Zhulu that rolls, and collects, cleans separation, drying; The glass microballon surface quality that this method is produced is poor, and has the pollution and the recovery problem of separant, only is fit to make the glass microballon of particle diameter 〉=500 μ m, and added value is low.The molten metal method is to utilize molten metal proportion bigger than glass, and the molten metal heat transfer evenly, makes glass powder swim in the molten metal surface and nodularization; This method is with high costs, can't continuous production.The flame smelting method is to be raw material with glass stick, glass yarn, utilizes flame that gas-fired produces that it moltenly is cut to drop, nodularization Cheng Zhu in the decline process; This method can only be produced the macrobead glass microballon.Flame floating method, flame spray gun method all are to utilize the high temperature of flame to make the glass powder surface melting and nodularization Cheng Zhu.The flame floating method is present the most frequently used post forming method, and it is floating that patent 861107294,95219672 all is based on the glass micro mist, and the high temperature that produces with coal gas, combustion of natural gas makes the glass powder surface melting and nodularization Cheng Zhu; 00102868 of patent changes type of heating into electrically heated; Shanghai Inst. of Silicate, Chinese Academy of Sciences is a high-refraction glass bead at the titanium oxide-barium oxide with acetylene-oxygen flame spray gun production interpolation small amounts lanthanum in 1989, but productive rate is low; The grain roundness of the glass microballon that above-mentioned flame floating method, flame spray gun method are produced is greatly improved, but has energy consumption height, complex process and crystallization phenomenon, and is with high costs.
At the shortcoming that occurs in the existing high-refraction glass bead production method, the centrifugal pan of be intended to release that a kind of technology is simple, energy consumption is low, the centrifugal pan atomizing of no crystallization phenomenon, yield rate height, the modification of glass microballon surface-coated molecular film being produced the method for high-refraction glass bead and the realized this method production equipment that atomizes.
The present invention is achieved in that
Adopt lead silicate for making the main body composition of high-refraction glass bead,, be easy to realize the centrifugal pan atomization process because lead silicate glass melt viscosity in high refracting glass is lower; Add rare earth oxide to improve specific refractory power and the color of improving glass microballon, add a small amount of rare earth fluorine, be convenient to atomizing and reduce hangover and wire drawing phenomenon, the raising yield rate to reduce the viscosity of glass melt; And to the glass microballon that atomizes out after screening, handle with the organic solution of containing hydrogen silicone oil, heating evaporation organic solvent and condensation are reclaimed, and make the glass microballon surface form transparent, hydrophobic organosilicon molecular film.
Glass raw material can be a main body with quartz sand, plumbous oxide, also can adopt industrial lead bisilicate (containing plumbous oxide 63%～67%) or single lead silicate (containing plumbous oxide 78%～85%), prepares in proportion with rare earth oxide and rare earth fluorine then.When adopting quartz sand and plumbous oxide, the melt raw material time is longer, and plumbous oxide volatilization phenomenon under the high temperature is arranged, and adopt condensate recovery system to pollute to reduce; When adopting lead bisilicate or single lead silicate, fusing is fast, and basically eliminate plumbous oxide volatilization phenomenon, but the material cost expense slightly increases, and ferric oxide impurity is wayward in the starting material, and ferric oxide can make glass microballon darken, and produces increased devitrification resistance.
Rare earth oxide not only can improve glass refraction, and the high cerium of oxidation (IV) makes iron be high valence state, improves the transparency of glass, and Neodymium trioxide, Praseodymium trioxide can be adjusted the color of glass; Rare earth oxide can increase the melt viscosity of glass, controls its total add-on in 5%.
Rare earth fluorine reduces the melt viscosity of lead silicate glass rapidly, to improve the manufacturability of centrifugal atomizing, can not cause the loss of specific refractory power, as lead silicate glass (the plumbous oxide content 60%) melt that adds 1% lanthanum fluoride is 1200～1300cp in the time of 850 ℃, be convenient to atomizing, but the add-on increase will influence the chemical stability of glass microballon, and its add-on is controlled in 2%.
Glass raw material is fused into glass melt, and material conveying tube enters the centrifugal atomizing dish of high speed rotating under the warp, and glass melt is atomized into pearl.Wherein glass melt can not be lower than 800 ℃ in the temperature that arrives the atomizing disk ingress, otherwise a large amount of wire drawing phenomenons will occur.In this way make high-refraction glass bead,, also be the especially particular design of centrifugal atomizing dish of centrifugal atomization apparatus, to guarantee good atomizing effect except the liquation of high refracting glass possesses lower viscosity to guarantee the aerosolizable manufacturability.
Centrifugal atomization apparatus adopts three phase squirrel cage frequency modulation high-speed electric expreess locomotive to drive, because the rotating speed of centrifugal atomizing dish is all more than 3000rpm during atomizing, produces the suitable accordingly rotating speed of 200～400 purpose glass microballons more than 12000rpm, and common electric machine is difficult to be competent at; Connect with extension shaft between motor and the centrifugal atomizing dish, and extension shaft is cooled off, the high temperature when guaranteeing atomizing disk work does not influence the works better of motor; And to extension shaft interpolation supplemental support, to guarantee atomisation unit stability under high speed rotating; Extension shaft, motor, atomizing disk structurally will guarantee right alignment, guarantee the life-time service life-span of centrifugal atomization apparatus.
The structure design of centrifugal atomizing dish must guarantee that the time that glass melt stops is short as far as possible in atomizing disk, possessing good stream shape is evenly dispersed to guarantee glass melt, and for fluidic radial motion does not have mechanical resistance link, because the time greater than 12000rpm, glass melt feeding quantity with 3～5kg/min, several microns approximately of the dispersion thickness of glass melt in atomizing disk, when atomizing disk did not have heat supplement, its speed of cooling was about 10
5℃/sec, if 3～4 milliseconds of times that glass melt stops in atomizing disk cause nearly 300～400 ℃ of cooling, and when being lower than 650 ℃, a large amount of wire drawings and tadpole shape (seeing figure (1)) will appear in the atomizing of lead silicate glass liquation, and easily cause the spout obstruction; Figure (1) is that the lead silicate glass liquation is when the temperature that arrives the atomizing disk ingress still remains on 850～900 ℃, when adopting the resistance furnace of 10kw to carry out radiation heating (position of the electromagnetic induction heating circle of figure (3) be the resistance furnace of each 5kw) up and down to atomizing disk, the result of lead silicate glass liquation atomizing; Must guarantee to replenish rapidly the atomizing disk heat that quilt loses with gas current friction through the air-flow and the atomizing disk surface of atomizing disk inside under high speed rotating, reduce glass melt cooling degree, be added with induction heating circle in both sides up and down at atomizing disk, and consider that in acceptable cost scope and from the maturity of technology induction heating is the unique type of heating of calorific loss that replenishes the atomizing disk of high speed rotating rapidly; The induction heating of atomizing disk is controlled with infrared sensor, and heating and temperature control is between 800～1000 ℃, to guarantee atomization process; In design, to guarantee that also glass melt should be along the radially ejection of atomizing disk, its radial velocity V
rTangential velocity V with the atomizing disk rotation
nForm maximum sum velocity V
t, see figure (2), thereby best crushing effect arranged when guaranteeing the glass melt of ejection and air friction that because under the certain condition of viscosity, proportion, the surface tension of gas density, pressure, liquid, the diameter behind the liquid crushing and its travelling speed are inversely proportional to.Atomizing disk since long term operation in the condition of high temperature, fused lead silicate has very strong corrodibility, its material should adopt heat-resistance stainless steel.
Have very strong aggressiveness and oxidisability owing to contain the lead silicate glass melt of fluorochemical, the smelting furnace that is contacted in glass melting and the glass melt course of conveying, the body of heater material and the blanking transfer line material of holding furnace are good with zircon corundum all, and white fused alumina and red corundum easily are etched.But also can with thin platinum liner.Following material conveying tube adopts hollow Si-Mo rod or electromagnetic induction heating, and the control Heating temperature guarantees that the lead silicate glass melt has good flowability between 850～1000 ℃.
Feature of the present invention is:
1, adopt rare earth fluorine to reduce the viscosity of the lead silicate glass liquation that adds rare earth oxide, the addition of rare earth fluorine is no more than 2%, and the addition of rare earth oxide is no more than 5%.Wherein the wt% of various components is: plumbous oxide 55%～68% silicon-dioxide 28%～43% rare earth oxide 1%～5% rare earth fluorine 0.5%～2%
Rare earth oxide can adopt lanthanum trioxide or based on the mixed rare-earth oxide of lanthanum trioxide, if in starting material plumbous oxide or single lead silicate, lead bisilicate ferric oxide (Fe
2O
3) content surpass 5ppm, must contain high cerium of oxidation and Neodymium trioxide in the added rare earth oxide, mend the glass light transmission that causes because of ferric oxide to transfer.
Rare earth fluorine can adopt lanthanum fluoride or based on the mixed rare earth fluoride of lanthanum fluoride.
Form the plumbous oxide of lead silicate glass and the starting material of silica composition and preferably adopt single lead silicate and lead bisilicate, be aided with a spot of silica powder with the suitable ratio of furnishing.All raw material (comprising rare earth oxide and rare earth fluorine) all should mix before adding smelting furnace, in order to avoid evenly need to prolong fusing, reaction times for asking to reach to spread in the heavy-gravity glass melt.
2, adopt the organic solution of containing hydrogen silicone oil to handle glass microballon, the concentration of containing hydrogen silicone oil solution is advisable 5%～10%, and concentration Tai Gaoyi causes the waste of containing hydrogen silicone oil, and the too rare meeting of concentration can not be covered the glass microballon surface fully by the containing hydrogen silicone oil molecule.Heating evaporation organic solvent and condensation are reclaimed, and containing hydrogen silicone oil then forms one deck organosilicon molecular film on the glass microballon surface.Play hydrophobic, antifouling effect, and improved the chemical stability of lead silicate glass to a certain extent.The hydrogen content of containing hydrogen silicone oil should be suitable at glass surface to be cross-linked to form molecular film between 0.3%～0.7%.In the heat-processed, the glass microballon temperature should not be above 120 ℃.
The solvent that organic solution adopted of containing hydrogen silicone oil can be dimethylbenzene, toluene, benzene, ethylene dichloride, chloroform, hexane, hexanaphthene equal solvent, but their water content must be less than 0.2%, otherwise crosslinking polymerization can take place in containing hydrogen silicone oil katalysis because of water under heating condition, can not form effective hydrophobic molecule film on the glass microballon surface.Be easy to that condensation is reclaimed and security consideration during heating from solvent, be advisable with ethylene dichloride, chloroform.
3, realize the centrifugal pan atomisation unit (seeing figure (3)) of centrifugal pan atomization production high-refraction glass bead, constitute main body by atomizing disk 1, atomizing disk spout 2, electromagnetic induction heating circle 3a and 3b, infrared temperature probe 3c, supplemental support 5, extension shaft 9, three phase squirrel cage frequency modulation high-speed electric expreess locomotive 13, motor base 14; Atomizing disk 1 connects with extension shaft 9 by clamping pad 21 and holding bolt 22, extension shaft 9 connects with three phase squirrel cage frequency modulation high-speed electric expreess locomotive 13, three phase squirrel cage frequency modulation high-speed electric expreess locomotive 13 is installed on the motor base 14, motor base 14 is fixed on the pedestal flange 16, extension shaft 9 between atomizing disk 1 and the three phase squirrel cage frequency modulation high-speed electric expreess locomotive 13 is added with supplemental support 5, supplemental support 5 becomes 6 welding of the uniform supplemental support bearing of 120 degree with three, be fixed on the supplemental support flange 8 with supplemental support holding bolt 20, with the fixing middle flange 18 of three phase squirrel cage frequency modulation high-speed electric expreess locomotive 13,6 uniform fastening screws 10 of motor base 14 usefulness pass positioning pipe 19, following positioning pipe 11 is fixed as one; The lower end of screw rod is screwed among the fixing threaded hole of motor base, and the upper end is fastening with nut 7; 12 uniform holding bolts 17 of main frame cover 12 lower liner circles, 15 usefulness are fixed on the pedestal flange; The upper end of main frame cover 12 has the centre hole greater than the atomizing disk diameter, is convenient to dismounting; In the upper surface of main frame cover 12 built-up type watercooling jacket 4 is installed, the heat that produces with blocking-up electromagnetic induction heating circle 3a and 3b is to the influence of supplemental support 5 and three phase squirrel cage frequency modulation high-speed electric expreess locomotive 13, and extension shaft 9 cooled off, built-up type watercooling jacket 4 is less than 5 millimeters with the gap of extension shaft 9, to guarantee cooling performance; During running, feed liquid by the upper end edge A of atomizing disk to entering atomizing disk, from the uniform radially B ejection atomizing of spout 2 of atomizing disk.
Wherein atomizing disk 1 is by coiling 23 (seeing figure (4)), atomizing disk mid-game 24 (seeing figure (5), vertical view), atomizing disk lower wall 25 (seeing figure (6)) and atomizing disk blade 26 (see figure (7-1) and (7-2)) on the atomizing disk with bolted together.The awl that coils 23 (seeing figure (4)) on the atomizing disk is to excessive to employing camber line structure with level, to reduce fluid resistance; Rounding is adopted in the corner of coiling on the atomizing disk, the corner burn-off phenomenon that produces during with the minimizing electromagnetic induction heating, and for same reason, the rounding structure is also adopted in the corner of the lower wall 25 of atomizing disk (seeing figure (6)).Coil the right alignment of 23 (seeing figure (4)), atomizing disk mid-game 24 (seeing figure (5), vertical view), atomizing disk lower wall 25 (seeing figure (6)) palpus assurance processing on the atomizing disk.The blade 26 of atomizing disk (see figure (7-1) and (7-2)) constitute atomizing disk spout 2, width of jet is 2 (D
2-D
1), be no less than 3 millimeters, otherwise be unfavorable for cleaning; The blade 26 of atomizing disk is (R along the radical length of sense of rotation
1-R
5), should be greater than the radical length (R of its back
1-R
4); Screw location α, the β of the blade 26 of atomizing disk, R
3, must guarantee that the screw periphery partly is no less than 3 millimeters width from blade edge, otherwise be difficult to guarantee the physical strength under the hot working conditions.The spout 2 of uniform atomizing disk can adopt 6～24, under the condition that the power of motor of three phase squirrel cage frequency modulation high-speed electric expreess locomotive 13 can guarantee, adopts more spout as far as possible, to enhance productivity; But adopt more spout meaning will adopt than long radius R
1The atomizing disk 1 of (seeing figure (3), figure (6) and figure (7-1)) just needs great start-up current, and power of motor increases; Figure (4), (5), (6), (7-1), (7-2) are the atomizing disk schemas of 12 spouts.Coil the side bumper thickness (R that 23 (seeing figure (4)) and atomizing disk lower wall 25 (seeing figure (6)) and atomizing disk blade 26 (seeing figure (7-1)) are complementary on the atomizing disk of atomizing disk 1
1-R
2) be no less than 4 millimeters, to guarantee the physical strength under the hot working conditions.Atomizing disk 1 adopts key connecting with extension shaft 9, and guaranteeing right alignment, the key connection structure of key connection structure of atomizing disk lower wall 25 (seeing figure (6a)) and extension shaft 9 (see figure (8) and (8a)) is complementary.
4, built-up type watercooling jacket 4 is seen figure (9a), (9b), form by two semicircle water jackets, two semicircle water jackets are twisted through screw 27 with screw and are closed, and when sandwiching mica with the assurance electromagnetic induction heating between two semicircle water jackets, do not make watercooling jacket 4 form eddy current; Each semicircle water jacket has two water hole interfaces 28, as cooling water intakeoutfall; Each semicircle water jacket all has two fixing feet 29, is screwed on main frame cover 12.
5, the lead silicate glass liquation that melts through smelting furnace, pour holding furnace 31 (seeing figure (10)) into, holding furnace places on the insulation bearing 32, the furnace temperature of holding furnace maintains 1000～1100 ℃, blanking hole 36 diameters of holding furnace are between 5～10 millimeters, lead silicate glass liquation 30 enters down material conveying tube 35 through blanking hole 36, enters atomizing disk 1 behind outlet 37 (diameter is between 1～8 millimeter) the reducing adjusting flow by following material conveying tube and atomizes.Following material conveying tube 35 is made by zircon corundum, will descend the material conveying tube heating with hollow Si-Mo rod 34 and silicon molybdenum process furnace 33, keeps its temperature between 850～1000 ℃, guarantees the flowability of lead silicate glass liquation.
Embodiment: one, produce the batching of lead silicate glass: sequence number starting material wt%1, single lead silicate (containing plumbous oxide 85%) 76.5%2, quartz sand (100 order) 18.5%3, lanthanum trioxide 2.5%4, lanthanum fluoride 1%5, Neodymium trioxide 1%6, contain Fe in the wherein single lead silicate of the high cerium 0.5% of oxidation
2O
3Be 5.6ppm.Two, consisting of of Dui Ying lead silicate high-refraction glass bead: sequence number starting material wt%1, plumbous oxide 65%2, silicon-dioxide 30%3, rare earth oxide 4%4, rare earth fluorine (lanthanum fluoride) 1% 3, technology
Raw material mixes, 1350～1400 ℃ melted 6 hours in the zircon corundum electric smelter, pour the holding furnace 31 (temperature control point is 1050 ℃) that furnace temperature maintains 1000～1100 ℃ into, lead silicate glass liquation 30 is that 8 millimeters blanking holes 36 enter down material conveying tube 35 through the diameter of holding furnace, following material conveying tube 35 usefulness silicon molybdenum process furnace 33 and hollow Si-Mo rod 34 will descend material conveying tube 35 heating to keep its temperature (temperature control point is 950 ℃) between 950～1000 ℃, the discharge hole diameter of following material conveying tube 35 is 3.5 millimeters, and discharging speed is 4～5kg/min.Lead silicate glass liquation 30, through the discharge hole diameter is 3.5 millimeters following material conveying tubes 35, enter and be heated in 850～900 ℃ (temperature control point of infrared temperature probe 3c is 850 ℃) and the atomizing disk 1 (spout of atomizing disk 1 is 12) atomizing production high-refraction glass bead with electromagnetic induction heating collar 3a and 3b with the 15000rpm rotation.
The spherical rate of high-refraction glass bead of producing that atomizes is that 92%, 200 mesh standard sieve screen underflow is 83%.With the glass microballon sub-sieve, the undersized glass microballons at different levels of 200 mesh standard sieves, (hydrogen content is 0.7%) containing hydrogen silicone oil chloroformic solution with 8% is in the ratio of 400 liters of glass microballons per ton, wetting glass microballon, heating evaporation and reclaim solvent chloroform (rate of recovery is 82%) under slowly stirring stops heating, to apply the organosilicon molecular film when glass microballon is warming up to 110 ℃, after the cooling, weigh, packing, labelled and trade mark.Its Photomicrograph of high-refraction glass bead product that the following 250 mesh standard sieves sieve of 200 mesh standard sieves sieve is gone up this one-level is seen figure (11).
Every index of the coating organosilicon molecular film high-refraction glass bead of being produced:
1, specific refractory power N
d=1.97
2, spherical rate 92%
3, devitrification rate (being commonly called as dead pearl rate)≤0.1%
4, the crystallization phenomenon does not have
Claims (25)
1. the production method of a high-refraction glass bead and realize the device of this method, it is lead silicate glass liquation with the smelting furnace fusing, through holding furnace, following material conveying tube enters the centrifugal pan atomizing production equipment that the atomizing disk centrifugal atomizing is produced the production method of high-refraction glass bead and realized this method; Wherein the wt% of various components is in the high-refraction glass bead:
Plumbous oxide 55%～68%,
Silicon-dioxide 28%～43%,
Rare earth oxide 1%～5%,
Rare earth fluorine 0.5%～2%;
What corresponding centrifugal pan atomized production equipment is to be made of atomizing disk 1, atomizing disk spout 2, electromagnetic induction heating circle 3a and 3b, infrared temperature probe 3c, supplemental support 5, supplemental support bearing 6, supplemental support flange 8, extension shaft 9, three phase squirrel cage frequency modulation high-speed electric expreess locomotive 13, middle flange 18, motor base 14, pedestal flange 16, built-up type watercooling jacket 4, clamping pad 21, main frame cover 12 and fastening piece; Atomizing disk 1 connects with extension shaft 9 by clamping pad 21 and holding bolt 22, extension shaft 9 connects with three phase squirrel cage frequency modulation high-speed electric expreess locomotive 13, three phase squirrel cage frequency modulation high-speed electric expreess locomotive 13 is installed on the motor base 14, motor base 14 is fixed on the pedestal flange 16,9 of extension shafts between atomizing disk 1 and the three phase squirrel cage frequency modulation high-speed electric expreess locomotive 13 are supplemental support 5, supplemental support 5 becomes 6 welding of the uniform supplemental support bearing of 120 degree with three, be fixed on the supplemental support flange 8 with supplemental support holding bolt 20, with the fixing middle flange 18 of three phase squirrel cage frequency modulation high-speed electric expreess locomotive 13,6 uniform fastening screws 10 of motor base 14 usefulness pass positioning pipe 19, following positioning pipe 11 is fixed as one; The lower end of screw rod is screwed among the fixing threaded hole of motor base, and the upper end is fastening with nut 7; 12 uniform holding bolts 17 of main frame cover 12 lower liner circles, 15 usefulness are fixed on the pedestal flange; In the upper surface of main frame cover 12 built-up type watercooling jacket 4 is installed.
2. the production method of high-refraction glass bead according to claim 1 is characterized in that described rare earth oxide is a lanthanum trioxide.
3. the production method of high-refraction glass bead according to claim 1 is characterized in that described rare earth oxide is the mixed rare-earth oxide based on lanthanum trioxide.
4. the production method of high-refraction glass bead according to claim 1 is characterized in that described rare earth oxide is high cerium of oxidation and Neodymium trioxide.
5. the production method of high-refraction glass bead according to claim 1 is characterized in that described rare earth fluorine is a lanthanum fluoride.
6. the production method of high-refraction glass bead according to claim 1 is characterized in that described rare earth fluorine is the rare earth mixed fluoride thing based on lanthanum fluoride.
7, the centrifugal pan of production high-refraction glass bead according to claim 1 atomizing production equipment, it is characterized in that described atomizing disk 1 be by coil 23 on the atomizing disk, atomizing disk mid-game 24, atomizing disk lower wall 25 be in the same place with atomizing disk blade 26 usefulness bolted.
8, according to the centrifugal pan atomizing production equipment of claim 1,7 described production high-refraction glass beads, the awl that it is characterized in that dish 23 on the described atomizing disk is to excessive to employing camber line structure with level.
9,, it is characterized in that the corner rounding of dish 23 on the described atomizing disk according to the centrifugal pan atomizing production equipment of claim 1,7 described production high-refraction glass beads.
10,, it is characterized in that the corner rounding of the lower wall 25 of described atomizing disk according to the centrifugal pan atomizing production equipment of claim 1,7 described production high-refraction glass beads.
11, the centrifugal pan of claim 1,7 described production high-refraction glass beads atomizing production equipment is characterized in that dish 23 and atomizing disk lower wall 25 side bumper thickness are no less than 4 millimeters on the atomizing disk of described atomizing disk 1.
12, according to the centrifugal pan of claim 1,7 described production high-refraction glass beads atomizing production equipment, the blade 26 that it is characterized in that described atomizing disk is a radical length greater than its back along the radical length of sense of rotation.
13, according to the centrifugal pan atomizing production equipment of claim 1,7 described production high-refraction glass beads, the spout that it is characterized in that described atomizing disk is uniform 6～24.
14, require the centrifugal pan atomizing production equipment of 1,7,13 described production high-refraction glass beads, it is characterized in that the width of described atomizing disk spout is no less than 3 millimeters.
15, the production method of high-refraction glass bead according to claim 1, it is characterized in that the fusing of described lead silicate glass and carrying the body of heater material of used smelting furnace, holding furnace and blanking transfer line material is zircon corundum.
16, the production method of high-refraction glass bead according to claim 1, it is characterized in that the fusing of described lead silicate glass and carrying the furnace lining material of used smelting furnace, holding furnace and blanking transfer line inner lining material is platinum.
17,, it is characterized in that blanking hole 36 diameters of described holding furnace are 5～10 millimeters according to the production method of claim 1,15,16 described high-refraction glass beads.
18, according to the production method of claim 1,15,16 described high-refraction glass beads, the working temperature that it is characterized in that described holding furnace is 1000～1100 ℃.
19, the production method of high-refraction glass bead according to claim 1 is characterized in that described material conveying tube 35 down is to place among hollow Si-Mo rod 34 and the silicon molybdenum process furnace 33.
20,, it is characterized in that the described diameter of the outlet 37 of material conveying tube 35 down is 1～8 millimeter according to the production method of the described high-refraction glass bead of claim 1.
21, the production method of high-refraction glass bead according to claim 1 is characterized in that the described working temperature of material conveying tube 35 down is between 850～1000 ℃.
22, the production method of high-refraction glass bead according to claim 1, the working temperature that it is characterized in that described atomizing disk 1 are 800～1000 ℃.
23, the production method of the described high-refraction glass bead of claim 1 is characterized in that described high refracting glass is a glass microballon wetting in the organic solution of 5%～10% containing hydrogen silicone oil with concentration, that be lower than 120 ℃ of desolventizings.
24, the production method of high-refraction glass bead according to claim 23, the solvent that it is characterized in that the organic solution of described 5%～10% containing hydrogen silicone oil are that water content is less than a kind of of 0.2% dimethylbenzene, toluene, benzene, ethylene dichloride, chloroform, hexane, hexanaphthene.
25, the production method of high-refraction glass bead according to claim 23, the hydrogen content that it is characterized in that described containing hydrogen silicone oil is 0.3%～0.7%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01103988 CN1371878A (en) | 2001-02-19 | 2001-02-19 | Method and apparatus for producing high-refraction glass bead |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01103988 CN1371878A (en) | 2001-02-19 | 2001-02-19 | Method and apparatus for producing high-refraction glass bead |
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| CN1371878A true CN1371878A (en) | 2002-10-02 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781083A (en) * | 2009-12-21 | 2010-07-21 | 浙江通达实业有限公司 | Hydrophobic hollow glass microsphere preparation method and prepared hydrophobic hollow glass microsphere thereof |
| CN102849955A (en) * | 2012-10-21 | 2013-01-02 | 道明光学股份有限公司 | Invisible anti-counterfeiting glass bead |
| CN104451621A (en) * | 2014-12-04 | 2015-03-25 | 苏州润佳工程塑料股份有限公司 | Preparation method of silver-coated silicon dioxide composite powder |
| CN108975663A (en) * | 2018-08-13 | 2018-12-11 | 北京科技大学 | A kind of method that cinder from refuse incineration collaboration cullet prepares glass microballoon |
| CN112223798A (en) * | 2020-09-28 | 2021-01-15 | 徐君东 | Reflective film production device and production method |
-
2001
- 2001-02-19 CN CN 01103988 patent/CN1371878A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781083A (en) * | 2009-12-21 | 2010-07-21 | 浙江通达实业有限公司 | Hydrophobic hollow glass microsphere preparation method and prepared hydrophobic hollow glass microsphere thereof |
| CN101781083B (en) * | 2009-12-21 | 2011-12-28 | 浙江通达机械有限公司 | Hydrophobic hollow glass microsphere preparation method and prepared hydrophobic hollow glass microsphere thereof |
| CN102849955A (en) * | 2012-10-21 | 2013-01-02 | 道明光学股份有限公司 | Invisible anti-counterfeiting glass bead |
| CN104451621A (en) * | 2014-12-04 | 2015-03-25 | 苏州润佳工程塑料股份有限公司 | Preparation method of silver-coated silicon dioxide composite powder |
| CN108975663A (en) * | 2018-08-13 | 2018-12-11 | 北京科技大学 | A kind of method that cinder from refuse incineration collaboration cullet prepares glass microballoon |
| CN112223798A (en) * | 2020-09-28 | 2021-01-15 | 徐君东 | Reflective film production device and production method |
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