CN107365084A - A kind of sol-gal process prepares the process of magnetic reflective glass beads - Google Patents
A kind of sol-gal process prepares the process of magnetic reflective glass beads Download PDFInfo
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- CN107365084A CN107365084A CN201710586950.0A CN201710586950A CN107365084A CN 107365084 A CN107365084 A CN 107365084A CN 201710586950 A CN201710586950 A CN 201710586950A CN 107365084 A CN107365084 A CN 107365084A
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- Prior art keywords
- sol
- magnetic
- glass beads
- reflective glass
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Classifications
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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
- C03C12/02—Reflective beads
-
- 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
-
- 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
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- 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)
- Colloid Chemistry (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses the process that a kind of sol-gal process prepares magnetic reflective glass beads, the present invention by using tetraethyl orthosilicate as silicon source, butyl titanate is titanium source, add iron chloride alcoholic solution and obtain the mixed sols system of doping iron, it is added drop-wise in certain temperature paraffin and disperses, colloidal sol disperses under surface tension effects and preferably obtains SiO as roundness2‑TiO2Glass microballoon spheroid；On the other hand can be by controlling the addition of iron chloride alcoholic solution, while ensureing that glass microballoon has good refractive index, the certain magnetic of glass microballoon is imparted, can carry out planting pearl processing by magnetic fields, make the product of preparation there is magnetic, strengthen its performance.
Description
Technical field
The present invention relates to reflectorized material technical field, and in particular to a kind of manufacturing process side of magnetic reflective glass beads
Method.
Background technology
In the preparation method of glass microballoon, blowing process production glass microballoon technique is simple, beading efficiency high, cost are low, its shortcoming
It is that microballon roundness is poor, is sometimes prone to the defects of " small tail ", " wire drawing cotton " occur, need to be by adjusting flame temperature and air-flow
To solve such defect, but its optical quality is preferable；Interleaving agent method bead yield rate is high, and product roundness is good, can produce plurality of specifications
Glass microballoon, its shortcoming is that produced glass microballoon surface is stained with graphite powder, it is more difficult to washes clean, is also easy to produce the glass of devitrification
Glass microballon.
Sol-gel process is to use liquid or the mixture of easy mixing liquid as reactant, because raw material uniformly mixes
In the low-viscosity (mobile) liquid of molecular level and complex reaction occurs, prepares multicomponent glass, the glass of high purity glass and high homogeneity
Glass ceramics.It can be retrofited using sol-gel process in the case of composition is not changed by polymer network by molecular structure,
That is the kinetics such as control hydrolysis, cohesion obtains the microstructure oxygen different with property to change the polymer architecture of gel
Compound glass.Additionally, due to colloid sheet as network body, the sintering temperature of glass or glass ceramics substantially reduces, largely
Reduce production cost.
The content of the invention
The invention provides a kind of method of manufacturing technology of magnetic reflective glass beads, is ensureing that it is good that glass microballoon has
While refractive index, assign glass microballoon certain magnetic.
The present invention is achieved by the following technical solutions：
A kind of sol-gel process prepares the process of magnetic reflective glass beads, including step in detail below：
（1）The preparation of miscellaneous ferrotitanium colloidal sol：
20-40 parts by weight butyl titanates are slowly dropped in 240-480 parts absolute ethyl alcohol/water mixed liquid, add 0.03-
For 0.1 part of acetylacetone,2,4-pentanedione as hydrolysis inhibitor, regulation pH values are 3.2-4.0, add 10-20 parts 20-40%FeCl afterwards3Alcohol is molten
Liquid, it is well mixed；
（2）Prepare Ludox：
Under intense agitation, 60-80 parts tetraethyl orthosilicate is added in 250-400 part deionized waters, while uses 0.5M
Hydrochloric acid solution adjusts sol system pH value in 2.8-3.4；
（3）Hydrolysis：
Treat step（2）When Ludox produces into transparence and leaving no air bubbles inside, step is slowly dropped into（1）Uniform doping ferrotitanium
Colloidal sol, ultrasonic disperse 15-30 minutes, at a temperature of stirring with 0 DEG C, 70-140 part distilled water, stirring are added dropwise into mixed sols
1.5-3 hour；
（4）Then while stirring by step（3）Mixed sols is slowly added dropwise in atoleine, is placed in 40-50 DEG C of thermostatted water
In bath, it is in uniform colloidal sol droplet to stir to colloidal dispersion in atoleine, as the volatilization of solvent obtains wet gel microballon,
Dried 1-4 days in 55-65 DEG C of vacuum constant temperature；
（5）Sintering：
Microballon obtained above is positioned in corundum crucible, is placed in vacuum sintering furnace after vacuumizing, is filled with nitrogen protection,
Begun to warm up with 1-2 DEG C/min speed from room temperature, be incubated 0.4-1 hours at 130-160 DEG C, continue to be heated to 280-320 DEG C
Insulation 1 hour, 600 DEG C of insulation 1-2 hours are warming up to 2-4 DEG C/min afterwards, after furnace cooling, takes out and produces.
Wherein, the step（1）Both volume ratios are 5-8 in absolute ethyl alcohol/water mixed liquid:1.
Wherein, the step（4）The usage amount of middle atoleine is 2 times of mixed sols volume.
Wherein, the step（4）Middle mixing speed is 200-400r/min.
Compared with prior art, the present invention by using tetraethyl orthosilicate as silicon source, butyl titanate as titanium source, addition chlorination
Iron alcoholic solution obtains the mixed sols system of doping iron, is added drop-wise in certain temperature paraffin and divides while stirring before colloidal sol gelling
Dissipate, colloidal sol disperses under surface tension effects and preferably obtains SiO as roundness2-TiO2Glass microballoon spheroid, through drying
Slowly heating sintering, drying time are grown, prevent from, because the too high moisture evaporation of drying temperature is too fast, cracking vapor solidifying as far as possible afterwards
Glue and the shape for destroying microballon, obtain glass microballoon close structure；On the other hand can be by controlling adding for iron chloride alcoholic solution
Dosage, while ensureing that glass microballoon has good refractive index, the certain magnetic of glass microballoon is imparted, can be made by magnetic field
Handled with plant pearl is carried out, make the product of preparation there is magnetic, strengthen its performance.
Embodiment
A kind of sol-gel process prepares the process of magnetic reflective glass beads, including step in detail below：
（1）The preparation of miscellaneous ferrotitanium colloidal sol：
30 parts by weight butyl titanates are slowly dropped in 420 parts of absolute ethyl alcohol/water mixed liquids, add 0.08 part of acetylacetone,2,4-pentanedione
As hydrolysis inhibitor, regulation pH values are 3.8, add 10 parts of 30%FeCl afterwards3Alcoholic solution, it is well mixed；
（2）Prepare Ludox：
Under intense agitation, 60 parts of tetraethyl orthosilicates are added in 320 parts of deionized waters, while uses 0.5M hydrochloric acid solutions
Sol system pH value is adjusted 3.2；
（3）Hydrolysis：
Treat step（2）When Ludox produces into transparence and leaving no air bubbles inside, step is slowly dropped into（1）Uniform doping ferrotitanium
Colloidal sol, ultrasonic disperse 20 minutes, at a temperature of stirring with 0 DEG C, 90 parts of distilled water are added dropwise into mixed sols, stir 2 hours；
（4）Then while stirring by step（3）Mixed sols is slowly added dropwise in 2 times of volume of liquid paraffin, is placed in 45 DEG C of perseverances
In warm water bath, stirred with 300r/min rotating speed, in atoleine be in uniform colloidal sol droplet to colloidal dispersion, with solvent
Volatilization obtain wet gel microballon, dried 2 days in 50 DEG C of vacuum constant temperatures；
（5）Sintering：
Microballon obtained above is positioned in corundum crucible, is placed in vacuum sintering furnace after vacuumizing, is filled with nitrogen protection,
Begun to warm up with 2 DEG C/min speed from room temperature, 1 hour is incubated at 150 DEG C, continued to be heated to 300 DEG C and be incubated 1 hour, afterwards
600 DEG C are warming up to 4 DEG C/min and is incubated 1 hour, after furnace cooling, are taken out and are produced.
Wherein, the step（1）Both volume ratios are 5 in absolute ethyl alcohol/water mixed liquid:1.
Claims (4)
1. a kind of sol-gel process prepares the process of magnetic reflective glass beads, it is characterised in that including walking in detail below
Suddenly：
（1）The preparation of miscellaneous ferrotitanium colloidal sol：
20-40 parts by weight butyl titanates are slowly dropped in 240-480 parts absolute ethyl alcohol/water mixed liquid, add 0.03-
For 0.1 part of acetylacetone,2,4-pentanedione as hydrolysis inhibitor, regulation pH values are 3.2-4.0, add 10-20 parts 20-40%FeCl afterwards3Alcohol is molten
Liquid, it is well mixed；
（2）Prepare Ludox：
Under intense agitation, 60-80 parts tetraethyl orthosilicate is added in 250-400 part deionized waters, while uses 0.5M
Hydrochloric acid solution adjusts sol system pH value in 2.8-3.4；
（3）Hydrolysis：
Treat step（2）When Ludox produces into transparence and leaving no air bubbles inside, step is slowly dropped into（1）Uniform doping ferrotitanium
Colloidal sol, ultrasonic disperse 15-30 minutes, at a temperature of stirring with 0 DEG C, 70-140 part distilled water, stirring are added dropwise into mixed sols
1.5-3 hour；
（4）Then while stirring by step（3）Mixed sols is slowly added dropwise in atoleine, is placed in 40-50 DEG C of thermostatted water
In bath, it is in uniform colloidal sol droplet to stir to colloidal dispersion in atoleine, as the volatilization of solvent obtains wet gel microballon,
Dried 1-4 days in 55-65 DEG C of vacuum constant temperature；
（5）Sintering：
Microballon obtained above is positioned in corundum crucible, is placed in vacuum sintering furnace after vacuumizing, is filled with nitrogen protection,
Begun to warm up with 1-2 DEG C/min speed from room temperature, be incubated 0.4-1 hours at 130-160 DEG C, continue to be heated to 280-320 DEG C
Insulation 1 hour, 600 DEG C of insulation 1-2 hours are warming up to 2-4 DEG C/min afterwards, after furnace cooling, takes out and produces.
2. the method for manufacturing technology of a kind of magnetic reflective glass beads according to claims 1, it is characterised in that described
Step（1）Both volume ratios are 5-8 in absolute ethyl alcohol/water mixed liquid:1.
3. the method for manufacturing technology of a kind of magnetic reflective glass beads according to claims 1, it is characterised in that described
Step（4）The usage amount of middle atoleine is 2 times of mixed sols volume.
4. the method for manufacturing technology of a kind of magnetic reflective glass beads according to claims 1, it is characterised in that described
Step（4）Middle mixing speed is 200-400r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710586950.0A CN107365084A (en) | 2017-07-18 | 2017-07-18 | A kind of sol-gal process prepares the process of magnetic reflective glass beads |
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| CN201710586950.0A CN107365084A (en) | 2017-07-18 | 2017-07-18 | A kind of sol-gal process prepares the process of magnetic reflective glass beads |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108943235A (en) * | 2018-07-20 | 2018-12-07 | 广西大学 | One kind preparing Fe in wood surface3+Adulterate TiO2/SiO2The method of composite membrane |
| CN112192914A (en) * | 2020-10-13 | 2021-01-08 | 黄山市亿华装饰材料有限公司 | Mould-proof antibacterial flame-retardant composite wallpaper |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6259553A (en) * | 1985-09-06 | 1987-03-16 | Agency Of Ind Science & Technol | Porous spherical glass and production thereof |
| CN103007957A (en) * | 2012-11-21 | 2013-04-03 | 嘉兴学院 | Method for preparing modified hollow glass beads with magnetism and photocatalytic activity |
| CN103833222A (en) * | 2014-01-14 | 2014-06-04 | 杭州电子科技大学 | Multifunctional quantum dot glass material doped with Fe nano-particles and preparation method thereof |
| CN105366944A (en) * | 2015-11-12 | 2016-03-02 | 合肥安奎思成套设备有限公司 | Preparation method of reflective glass beads |
-
2017
- 2017-07-18 CN CN201710586950.0A patent/CN107365084A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6259553A (en) * | 1985-09-06 | 1987-03-16 | Agency Of Ind Science & Technol | Porous spherical glass and production thereof |
| CN103007957A (en) * | 2012-11-21 | 2013-04-03 | 嘉兴学院 | Method for preparing modified hollow glass beads with magnetism and photocatalytic activity |
| CN103833222A (en) * | 2014-01-14 | 2014-06-04 | 杭州电子科技大学 | Multifunctional quantum dot glass material doped with Fe nano-particles and preparation method thereof |
| CN105366944A (en) * | 2015-11-12 | 2016-03-02 | 合肥安奎思成套设备有限公司 | Preparation method of reflective glass beads |
Non-Patent Citations (1)
| Title |
|---|
| 黄希风: "高折射玻璃微珠的溶胶-凝胶法制备研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108943235A (en) * | 2018-07-20 | 2018-12-07 | 广西大学 | One kind preparing Fe in wood surface3+Adulterate TiO2/SiO2The method of composite membrane |
| CN112192914A (en) * | 2020-10-13 | 2021-01-08 | 黄山市亿华装饰材料有限公司 | Mould-proof antibacterial flame-retardant composite wallpaper |
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Application publication date: 20171121 |