CN106865992A - Boron aluminosilicate glass bead and preparation method thereof - Google Patents
Boron aluminosilicate glass bead and preparation method thereof Download PDFInfo
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- CN106865992A CN106865992A CN201710143416.2A CN201710143416A CN106865992A CN 106865992 A CN106865992 A CN 106865992A CN 201710143416 A CN201710143416 A CN 201710143416A CN 106865992 A CN106865992 A CN 106865992A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title abstract 4
- 239000005354 aluminosilicate glass Substances 0.000 title abstract 4
- 229910052796 boron Inorganic materials 0.000 title abstract 4
- 239000011324 bead Substances 0.000 title abstract 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 17
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 13
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims abstract description 10
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 10
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 10
- 229910052810 boron oxide Inorganic materials 0.000 claims abstract description 9
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000292 calcium oxide Substances 0.000 claims abstract description 9
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 9
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004327 boric acid Substances 0.000 claims abstract description 7
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 7
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001948 sodium oxide Inorganic materials 0.000 claims abstract description 7
- 159000000007 calcium salts Chemical class 0.000 claims abstract description 5
- 239000011521 glass Substances 0.000 claims description 70
- 238000000034 method Methods 0.000 claims description 24
- 239000000843 powder Substances 0.000 claims description 23
- 239000005368 silicate glass Substances 0.000 claims description 20
- 238000002844 melting Methods 0.000 claims description 15
- 230000008018 melting Effects 0.000 claims description 15
- 230000008569 process Effects 0.000 claims description 14
- 102220043159 rs587780996 Human genes 0.000 claims description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- 238000005187 foaming Methods 0.000 claims description 10
- 238000010791 quenching Methods 0.000 claims description 9
- 230000000171 quenching effect Effects 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 230000004083 survival effect Effects 0.000 claims description 8
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 6
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 239000006063 cullet Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 3
- 239000000428 dust Substances 0.000 claims description 3
- 230000006835 compression Effects 0.000 abstract description 22
- 238000007906 compression Methods 0.000 abstract description 22
- 238000005188 flotation Methods 0.000 abstract description 9
- 238000007667 floating Methods 0.000 abstract description 3
- 239000004005 microsphere Substances 0.000 abstract description 2
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 abstract 1
- 239000006229 carbon black Substances 0.000 abstract 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 238000005245 sintering Methods 0.000 description 14
- 239000011805 ball Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000001694 spray drying Methods 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000006260 foam Substances 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011806 microball Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 238000005352 clarification Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 238000012803 optimization experiment Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 238000001238 wet grinding Methods 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- -1 as shown in Table 1 Chemical compound 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/107—Forming hollow beads
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Glass Compositions (AREA)
Abstract
The invention provides a boron aluminosilicate glass bead, which comprises the following components in percentage by mass: 50-58% of silicon dioxide, 3-8% of boron oxide, 5-10% of aluminum oxide, 12-18% of sodium oxide, 8-15% of calcium oxide and 0-1.5% of magnesium oxide; the invention also provides a preparation method of the boron aluminosilicate glass beads, which comprises the steps of preparing raw materials; the raw materials comprise the following raw material components in parts by weight: 2.6-2.7 parts of white carbon black, 0.7-0.9 part of boric acid, 2-2.3 parts of calcium salt, 1.6-1.8 parts of sodium nitrate, 2.5-2.8 parts of aluminum nitrate, 0.2-0.4 part of magnesium nitrate and 0-0.1 part of aluminum silicate. The boron aluminosilicate glass microspheres prepared by the invention have high yield, are not subjected to water flotation, and have a floating rate of more than or equal to 99 percent; high compression strength, stable quality, high density and high compression strength uniformity.
Description
Technical field
The present invention provides a kind of boroalumino silicate glasses microballon and preparation method thereof, belongs to Inorganic Non-metallic Materials technology neck
Domain.
Background technology
Hollow glass micropearl is a kind of small hollow glass spheroid of size, with light weight, low heat conduction, resistance to compression, high dispersive,
The good advantage of sound insulation, electrical insulating property and heat endurance, is developed in recent years a kind of widely used, excellent performance new
Light material.
Hollow glass micropearl is prepared, typically using two methods：Soft chemical method and solid phase powder method.
Chinese patent（Publication No. CN102583973A）Disclose a kind of soft chemical preparation process of hollow glass micro-ball and
Made hollow glass micro-ball and its application, its production method are soft chemical method, its hollow glass micro-ball for preparing, alumina content
0-5%, density 0.1-0.7g/cm3, compression strength 1-50Mpa, its floatability >=90%, 600-1100 DEG C of sintering temperature.
The shortcoming of the patent is that the compression strength of glass microballoon is low, and cenosphere is easily broken, and causes additive effect to be failed to understand
It is aobvious, do not have the effect for reducing density.When being applied in deep well cementing cement or deep-sea floating body material, it is difficult to reach using will
Ask.
Conventional solid powder method is usually after raw material is mixed, by high temperature melting（This step includes clarifying process）、
Water quenching, drying, crushing, classification obtain the glass dust of appropriate particle size；
Chinese patent CN101638295A discloses a kind of hollow glass micropearl and its production method, is given " the original for mixing
Material is founded and can be produced cullet 100kg after being clarified, the glass melting temperature that uses and corresponding clarifying temp for：Found temperature
1400-1550 DEG C of degree, clarifying temp is 1580 DEG C "；The defect of the patent is to found and clarifying process, and time-consuming, the sky of preparation
Heart glass microballoon compression strength is small.
Chinese patent（Publication No. CN102320743A）Disclose high strength aluminosilicate hollow glass microsphere and its system
Preparation Method, its production method is solid phase glass powder method；Its hollow glass micropearl for preparing, alumina content 10-15%, density
0.2-0.6 g/cm3, resistance to compression 3-130Mpa, its floatability >=95%（After water flotation）, 1250-1450 DEG C of sintering temperature, softening temperature
≥750℃。
The shortcoming of the patent is that this glass formula fusing point is high, needs thermal-flame ability sinter molding, high energy consumption.Melting time
Long, melting time is 5-8 hours, and actually most of time is all consumption in clarifying process, because glass solution viscosity is big, exclusion
Bubble is slow, and its foaming in addition is the SO by dissolving in glass3Used as foamed gas, gas release is limited, and balling ratio is low, floating through water
>=95% its floatability is can be only achieved after choosing, waste material is more, high cost.
In sum, existing solid phase powder method prepares glass microballoon, there is following defect：
（1）Its floatability of product is low.A small amount of SO of the glass metal after clarifying cooling only by dissolving in glass3As foaming
Agent, makes glass dust be expanded to glass envelope in sintering, and gas release is limited, causes medicine ball occur, it is necessary to by water flotation ability
The product after hollow product, and water flotation is obtained, its its floatability can be only achieved more than 95%, the ball for sinking under water is waste material,
Cannot function as hollow ball to use, waste material is more, high cost.If processed without water flotation, its floatability of the product of preparation is only
70-75%。
（2）During preparing glass microballoon, if removal clarifying process, bubble can be caused in glass metal more and bubble
Size is uneven, the unstable product quality of preparation.
（3）The compression strength of product is low.
（4）Melting time is long, and sintering temperature is high, high energy consumption.
The content of the invention
The present invention is solution the deficiencies in the prior art, there is provided a kind of boroalumino silicate glasses microballon and preparation method thereof, with
Realize following goal of the invention：
（1）Boroalumino silicate glasses microballon prepared by the present invention, high yield rate, without water flotation, its floatability >=99%；Resistance to compression
Intensity is high；
（2）Boroalumino silicate glasses microballon prepared by the present invention, steady quality, bubble are uniform, density, compression strength uniformity
It is high；
（3）The preparation method of glass microballoon of the present invention, melting time is short, and sintering temperature is low, and energy consumption is low.
In order to solve the above technical problems, the technical scheme that the present invention takes is as follows：
A kind of boroalumino silicate glasses microballon, the glass microballoon, the mass ratio of each composition is：
Silica 50-58%
Boron oxide 3-8%
Aluminum oxide 5-10%
Sodium oxide molybdena 12-18%
Calcium oxide 8-15%
Magnesia 0-1.5%.
The following is the further improvement to above-mentioned technical proposal：
The glass microballoon, the mass ratio of each composition is preferably：
Silica 55-58%
Boron oxide 3-8%
Aluminum oxide 7.5-8.5%
Sodium oxide molybdena 16-17.5%
Calcium oxide 9.5-13.7%
Magnesia 0.5-1.4%.
A kind of preparation method of boroalumino silicate glasses microballon, methods described, including prepare raw material；The raw material, with weight
Amount part meter, including following raw material components：
White carbon 2.6-2.7 parts, boric acid 0.7-0.9 parts, calcium salt 2-2.3 parts, sodium nitrate 1.6-1.8 parts, aluminum nitrate 2.5-2.8
Part, magnesium nitrate 0.2-0.4 parts, alumina silicate 0-0.1 parts.
The calcium salt is the mixture of one or both in calcium carbonate, calcium nitrate；
The preparation method, also including founding；Described to found, glass melting temperature is 700-1000 DEG C, and melting time is 20-
120min；
The melting time, preferably 30min.
The preparation method, also including grinding；The grinding, by the cullet and water after water quenching together by sand mill,
Ball mill grinding is to 5-80 microns, D50=35-40 microns.
The preparation method, also including pressure treatment；The pressure treatment, by by the presoma glass of spray drying treatment
Glass powder is first processed 30 minutes under 0.5MPa, then boosts to 1MPa, is processed 5 minutes, then with the speed of 0.1MPa/min
- 0.1Mpa is reduced to, is processed 5 minutes.
The spray drying, condition is 300-400 DEG C of inlet temperature, and 110-150 DEG C of outlet temperature is spray-dried to obtain
Presoma glass powder.
The preparation method, also including secondary milled processed；The secondary milled processed, by before after pressure treatment
Body glass powder is driven, is added in vibromill, the aciculiform mill of a diameter of 5mm of filling is situated between in mill, under the frequency of 4000rpm, place
Reason 2 hours so that the particle diameter of glass powder is D50=25-30 microns.
It is the abrasive media that draw ratio is 3 that described aciculiform mill is situated between.
The preparation method, also including foaming nodularization；The foaming nodularization, nodularization temperature control is at 800-1200 DEG C.
The nodularization temperature is preferably 850-900 DEG C.
The glass microballoon, product cut size 7-80 microns, D50=30-43 microns；Density 0.5-0.55g/cm3, its floatability
97.2-99%, compression strength（80% survival content）It is 135-140MPa.
Directly it is collected by after the cooling of balling furnace cooling section by the glass powder of hollow nodularization, obtains glass microballoon
Finished product.
Compared with prior art, beneficial effects of the present invention are as follows：
（1）Boroalumino silicate glasses microballon prepared by the present invention, its floatability is high, and without water flotation, its floatability is 97-99%；Save
The subsequent treatment process gone after separating product through water flotation, it is to avoid subsequent treatment is impacted to product index；Its floatability is right
The maximum index of using effect influence, it is all very big improvement to improve several percentage points.
（2）Glass microballoon prepared by the present invention, steady quality, bubble is more uniform in microballon, density, compression strength uniformity
It is high；The glass microballoon, product cut size 7-80 microns, D50=30-43 microns；Density 0.5-0.55g/cm3, compression strength（80%
Survival content）It is 135-140MPa.
（3）Preparation method of the present invention, glass melting temperature is low, and melting time is short, and sintering temperature is low, and energy consumption is low, glass melting temperature drop
Low is 700-1000 DEG C, and melting time shortens to 20-120min, preferably 30min by 5-8 hours of the prior art, sintering
Temperature is 800-1200 DEG C, preferably 850-900 DEG C, substantially reduces production cost.
（4）Glass microballoon prepared by the present invention, softening temperature >=700 DEG C, refractoriness >=1100 DEG C.
Specific embodiment
The preferred embodiments of the present invention are illustrated below, it should be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
A kind of preparation method of boroalumino silicate glasses microballon of embodiment 1
Comprise the following steps：
（1）Weigh raw material
Weigh white carbon 2.6Kg, boric acid 0.9 Kg, calcium carbonate 2Kg, sodium nitrate 1.6 Kg, aluminum nitrate 2.5Kg, magnesium nitrate
0.4kg。
（2）Found
During the raw material for mixing is put into glass melter 30min is founded with 900 DEG C.
（3）Water quenching
Then the glass metal water quenching that will be melted.
（4）Wet grinding
By the cullet and water after water quenching together by sand mill, ball mill grinding is to 5-80 microns, D50=35-40 microns.
（5）Spray drying
It is spray-dried to obtain presoma glass powder.
（6）Pressure treatment
To first be processed 30 minutes under 0.5MPa by the presoma glass powder of dried process, then boost to 1MPa, treatment 5
Minute, -0.1Mpa is then reduced to the speed of 0.1MPa/min, process 5 minutes.
（7）Secondary milled processed
By by the presoma glass powder after pressure treatment, it is added in vibromill, the aciculiform mill of a diameter of 5mm of filling in mill
It is situated between, under the frequency of 4000rpm, processes 2 hours so that the particle diameter of glass powder is D50=25-30 microns；Described aciculiform mill
It is the abrasive media that draw ratio is 3 to be situated between.
（8）Foaming nodularization
Then in presoma being sent into nodularization flame with the speed of 20Kg/h by powder feeding equipment, temperature control is on 900 DEG C of left sides
The right side, the nodularization time is 1-2s, and powder foams nodularization in flame.
（9）Finished product
Cooling shaping is directly entered collection system after going out flame, obtains glass microballoon finished product,
Product cut size 8-75 microns for obtaining, D50=30-40 microns；Density 0.55g/cm3, its floatability 97.2%, compression strength
（80% survival content）It is 135MPa.
Silica 55.9% after sintering, boron oxide 7.42%, sodium oxide molybdena 17.04%, magnesia 1.38%, aluminum oxide 7.52%,
Calcium oxide 10.37%.
A kind of preparation method of boroalumino silicate glasses microballon of embodiment 2
Comprise the following steps：
（1）Weigh raw material
Weigh white carbon 2.7Kg, the Kg of boric acid 0.9, the Kg of calcium nitrate 2, the Kg of sodium nitrate 1.8, the Kg of magnesium nitrate 0.2, aluminum nitrate
2.8kg, alumina silicate 0.1Kg.
（2）Found
During the raw material for mixing is put into glass melter 30min is founded with 1000 DEG C.
（3）Water quenching
Then the glass metal water quenching that will be melted.
（4）Wet grinding
By the cullet and water after water quenching together by sand mill, ball mill grinding is to 5-80 microns, D50=35-40 microns.
（5）Spray drying
Presoma glass powder is obtained by spray drying.
（6）Pressure treatment
To first be processed 30 minutes under 0.5MPa by the presoma glass powder of dried process, then boost to 1MPa, treatment 5
Minute, -0.1Mpa is then reduced to the speed of 0.1MPa/min, process 5 minutes.
（7）Secondary milled processed
By by the presoma glass powder after pressure treatment, it is added in vibromill, the aciculiform mill of a diameter of 5mm of filling in mill
It is situated between, under the frequency of 4000rpm, processes 2 hours so that the particle diameter of glass powder is D50=25-30 microns.Described aciculiform mill
It is the abrasive media that draw ratio is 3 to be situated between.
（8）Foaming nodularization
Then in presoma being sent into nodularization flame with the speed of 20Kg/h by powder feeding equipment, temperature control is on 950 DEG C of left sides
The right side, the nodularization time is 1-2s, and powder foams nodularization in flame,
（9）Finished product
Go out cooling shaping after flame, be directly entered collection system, glass microballoon finished product is obtained.
Collection obtains product cut size 7-80 microns, D50=35-43 microns.
Density 0.50g/cm3, its floatability 99%, compression strength（80% survival content）It is 140MPa.
Silica 57.22% after sintering, boron oxide 6.81%, sodium oxide molybdena 17.21%, magnesia 0.63%, aluminum oxide
8.28%, calcium oxide 9.84%.
The raw material proportioning optimization experiment of embodiment 3
On the basis of embodiment 1, only change white carbon, boric acid, the mass ratio of calcium carbonate, prepare glass microballoon, determine anti-
Compressive Strength（80% survival content）, specifically it is shown in Table 1.
Added in raw material after boric acid, calcium carbonate prepare sintering and respectively obtain boron oxide, calcium oxide；Raw material white carbon is final to be obtained
To be silica, as shown in Table 1, boron oxide, calcium oxide and silica can play synergy, and glass is increased jointly
The compression strength of microballon.
The sodium nitrate of embodiment 4, aluminum nitrate addition it is preferred
On the basis of embodiment 1, only change sodium nitrate, the addition of aluminum nitrate, specific change is shown in Table 2, and the glass of preparation is micro-
Pearl, detects compression strength（80% survival content）.
The addition optimization experiment of the sodium nitrate of table 2, aluminum nitrate
Sodium nitrate and aluminum nitrate are used as foaming agent, the size of the proportioning influence foaming of sodium nitrate and aluminum nitrate, bigger, the glass of foaming
The compression strength of microballon is smaller, foams too small, and the density of glass microballoon is again too big.As shown in Table 2, group 4 and group 8 are excellent
Select embodiment.
The sintering temperature of embodiment 5 is preferred
On the basis of embodiment 1, only change step（8）Sintering temperature in foaming nodularization, changes such as table 3 below.
The sintering temperature of table 3 is preferred
Found through overtesting, group 15 and group 16 are preferred embodiments, i.e. sintering temperature is preferably 850-900 DEG C.
Documents 1
On the basis of embodiment 1, remove step（6）With（7）, remaining carries out experiment and prepares glass microballoon with embodiment 1, right
The technique that ratio 1 prepares glass microballoon with prior art is compared, and eliminates clarification steps.
It was found that the glass microballoon for preparing, without water flotation, its floatability is up to 95%；But particle size range, density range, resistance to compression
Strength range is wider, and particle diameter is 8-120 microns, and density is 0.19-0.45g/cm3, compression strength（80% survival content）For
30.7-130.5MPa。
From the result of comparative example 1, it is seen then that if simply using removal clarification steps, although the product its floatability for obtaining is obtained
Certain raising, but the product for preparing are arrived, particle size range, density range, compression strength scope are wider, particularly compression strength
Low value can not reach the requirement of high compressive strength of the present invention.
Unless otherwise indicated, the percentage employed in the present invention is percetage by weight, ratio of the present invention,
It is mass ratio.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although being described in detail to the present invention with reference to the foregoing embodiments, for a person skilled in the art, it still may be used
Modified with to the technical scheme described in foregoing embodiments, or equivalent is carried out to which part technical characteristic.
All any modification, equivalent substitution and improvements within the spirit and principles in the present invention, made etc., should be included in of the invention
Within protection domain.
Claims (10)
1. a kind of boroalumino silicate glasses microballon, it is characterised in that：The glass microballoon, the mass ratio of each composition is：
Silica 50-58%
Boron oxide 3-8%
Aluminum oxide 5-10%
Sodium oxide molybdena 12-18%
Calcium oxide 8-15%
Magnesia 0-1.5%.
2. a kind of boroalumino silicate glasses microballon according to claim 1, it is characterised in that：The glass microballoon, each group
Into mass ratio be preferably：
Silica 55-58%
Boron oxide 3-8%
Aluminum oxide 7.5-8.5%
Sodium oxide molybdena 16-17.5%
Calcium oxide 9.5-13.7%
Magnesia 0.5-1.4%.
3. a kind of preparation method of boroalumino silicate glasses microballon, it is characterised in that：Methods described, including prepare raw material；It is described
Raw material, in parts by weight, including following raw material components：
White carbon 2.6-2.7 parts, boric acid 0.7-0.9 parts, calcium salt 2-2.3 parts, sodium nitrate 1.6-1.8 parts, aluminum nitrate 2.5-2.8
Part, magnesium nitrate 0.2-0.4 parts, alumina silicate 0-0.1 parts；
The calcium salt is the mixture of one or both in calcium carbonate, calcium nitrate.
4. the preparation method of a kind of boroalumino silicate glasses microballon according to claim 3, it is characterised in that：The preparation
Method, also including founding；Described to found, glass melting temperature is 700-1000 DEG C, and melting time is 20-120min.
5. according to a kind of preparation method of boroalumino silicate glasses microballon according to claim 3, it is characterised in that：It is described
Preparation method, also including grinding；The grinding, by the cullet and water after water quenching together by sand mill, ball mill grinding is arrived
5-80 microns, D50=35-40 microns.
6. according to a kind of preparation method of boroalumino silicate glasses microballon according to claim 3, it is characterised in that：It is described
Preparation method, also including pressure treatment；The pressure treatment, will be first in 0.5MPa by the presoma glass powder of dried process
Lower treatment 30 minutes, then boosts to 1MPa, processes 5 minutes, is then reduced to -0.1Mpa with the speed of 0.1MPa/min, locates
Reason 5 minutes.
7. according to a kind of preparation method of boroalumino silicate glasses microballon according to claim 3, it is characterised in that：It is described
Preparation method, also including secondary milled processed；The secondary milled processed, by by the presoma glass dust after pressure treatment
End, is added in vibromill, and the aciculiform mill of a diameter of 5mm of filling is situated between in mill, under the frequency of 4000rpm, processes 2 hours, makes
The particle diameter for obtaining glass powder is D50=25-30 microns；It is the abrasive media that draw ratio is 3 that described aciculiform mill is situated between.
8. according to a kind of preparation method of boroalumino silicate glasses microballon according to claim 3, it is characterised in that：It is described
Preparation method, also including foaming nodularization；The foaming nodularization, nodularization temperature control is at 800-1200 DEG C.
9. according to a kind of preparation method of boroalumino silicate glasses microballon according to claim 8, it is characterised in that：It is described
Nodularization temperature is preferably 850-900 DEG C.
10. according to a kind of preparation method of boroalumino silicate glasses microballon according to claim 3, it is characterised in that：Institute
State glass microballoon, product cut size 7-80 microns, D50=30-43 microns；Density 0.5-0.55g/cm3, its floatability 97.2-99%, resist
Compressive Strength（80% survival content）It is 135-140MPa.
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| CN109554158A (en) * | 2018-12-04 | 2019-04-02 | 北京市捷瑞特弹性阻尼体技术研究中心 | A kind of clay and its preparation method and application |
| CN113336446A (en) * | 2021-05-28 | 2021-09-03 | 安徽壹石通材料科学研究院有限公司 | Metal-plated glass bead and preparation method thereof |
| CN114105481A (en) * | 2021-12-28 | 2022-03-01 | 内蒙古工业大学 | Monodisperse high-silicon microsphere and preparation method thereof |
| CN117772382A (en) * | 2024-02-28 | 2024-03-29 | 中科雅丽科技有限公司 | Fine control adjustment method for fineness of glass microsphere grinding powder |
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| CN117772382A (en) * | 2024-02-28 | 2024-03-29 | 中科雅丽科技有限公司 | Fine control adjustment method for fineness of glass microsphere grinding powder |
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