CN105366944B - A kind of preparation method of reflective glass beads - Google Patents
A kind of preparation method of reflective glass beads Download PDFInfo
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- CN105366944B CN105366944B CN201510780841.3A CN201510780841A CN105366944B CN 105366944 B CN105366944 B CN 105366944B CN 201510780841 A CN201510780841 A CN 201510780841A CN 105366944 B CN105366944 B CN 105366944B
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Abstract
The invention discloses a kind of preparation methods of reflective glass beads, including：Aluminum nitrate, zirconium nitrate, cerous nitrate and magnesium nitrate are dissolved in water to obtain mixed solution, sodium hydroxide solution is added dropwise, filtering, cleaning, which is placed in water, carries out ultrasonic disperse, heating water bath, and nitric acid, which is added dropwise, during heating water bath obtains the first colloidal sol；Ethyl orthosilicate plus ethyl alcohol are dissolved to obtain the second colloidal sol, water is added dropwise and the first colloidal sol obtains third colloidal sol；Ethyl acetoacetate is added into ethyl alcohol, adds tetrabutyl titanate and obtains the 4th colloidal sol；Zinc nitrate, chromic nitrate and boric acid are added into ethyl alcohol and obtains the 5th solution；5th solution is added dropwise in the 4th colloidal sol, water is added, is stirred, standing obtains the 6th colloidal sol；Third colloidal sol is stirred, the 6th colloidal sol is added dropwise in whipping process and water obtains the 7th colloidal sol；Paraffin oil containing sapn is subjected to heating water bath, the 7th colloidal sol is then added dropwise and enters paraffin oil, stirs, filtering is dried to obtain gel particle；Gel particle is sintered, cooling obtains reflective glass beads.
Description
Technical field
The present invention relates to glass microballoon technical field more particularly to a kind of preparation methods of reflective glass beads.
Background technology
Glass microballoon is a kind of a kind of new material widely used, performance is special developed in recent years, is a kind of
The small hollow glass sphere of size belongs to inorganic non-metallic material.Glass microballoon is the primary raw material for manufacturing reflectorized material, can be with
It is widely used in the reflectorized material of the fields such as highway, railway, airport, harbour, sea transport, mine, tunnel, fire-fighting, urban construction.With
Increasing of the China to infrastructure construction dynamics of investment, the demand of glass microballoon is increasing, while to the property of glass microballoon
It can require also higher and higher.China only has the production technology that a small number of producers grasp high refractive index glass micro pearl, and its product at present
Performance is very unstable, and actual demand is still not achieved in reflective function, cannot be satisfied market demands.
Invention content
Technical problems based on background technology, the present invention propose a kind of preparation method of reflective glass beads, institute
It is preferable to obtain glass microballoon translucency, compact structure, internal pore-free, refractive index is 1.8~1.9, and reflecting effect is good.
A kind of preparation method of reflective glass beads proposed by the present invention, includes the following steps：
A, after mixing aluminum nitrate, zirconium nitrate, cerous nitrate and magnesium nitrate, it is added to the water dissolving and obtains mixed solution, then
Sodium hydroxide solution is added dropwise, filter cake cleaning is placed in water and carries out ultrasonic disperse, then heating water bath by filtering, heating water bath
Nitric acid is added dropwise in the process to pH=3~4, obtains the first colloidal sol；
B, dissolving in ethyl alcohol is added in ethyl orthosilicate and obtains the second colloidal sol, water is then added dropwise into the second colloidal sol, then adjust
PH value is saved to 3~4, third colloidal sol is obtained after stirring, the first colloidal sol is added dropwise in whipping process；
C, it after addition ethyl acetoacetate stirs evenly into ethyl alcohol, adds tetrabutyl titanate and is once stirred to get
4th colloidal sol；It is added into ethyl alcohol after zinc nitrate, chromic nitrate and boric acid are mixed uniformly and obtains the 5th solution；5th solution is added dropwise to
In 4th colloidal sol, secondary agitation is then carried out, adds water, then triple mixing, standing obtains the 6th colloidal sol；
D, third colloidal sol is stirred, the 6th colloidal sol is added dropwise in whipping process and water obtains the 7th colloidal sol；Department will be contained
The paraffin oil of disk 60 carries out heating water bath, and the 7th colloidal sol is then added dropwise and enters paraffin oil, then stirs, filters, is dried to obtain gel
Particle；
E, gel particle is sintered, cooling obtains reflective glass beads.
Preferably, in step a, aluminum nitrate, zirconium nitrate, cerous nitrate and magnesium nitrate molar ratio be 35~38：26~30：6
~9：2~4.
Preferably, in step a, the time of ultrasonic disperse is 15~20min, and the power of ultrasonic disperse is 400~500w, is surpassed
The frequency of sound dispersion is 30~45kHz.
Preferably, in step a, the temperature of heating water bath is 75~85 DEG C.
Preferably, in step b, the volume ratio of ethyl orthosilicate and ethyl alcohol is 21~22：6~9.
Preferably, in step b, the molar ratio of ethyl orthosilicate and water is 9~12：1~3.
Preferably, in step b, the weight ratio of the second colloidal sol and the first colloidal sol is 50~60：15~18.
Preferably, in step c, tetrabutyl titanate, zinc nitrate, chromic nitrate and boric acid molar ratio be 52~55：5~8：2
~3：1~3.
Preferably, in step c, the time once stirred is 2.3~2.6h.
Preferably, in step c, the time of secondary agitation is 0.6~0.9h.
Preferably, in step c, the time of triple mixing is 20~22h.
Preferably, in step c, the time of standing is 25~28h.
Preferably, in step d, the weight ratio of third colloidal sol, the 6th colloidal sol and water is 50~60：15~18：5~8.
Preferably, in step d, the temperature of heating water bath is 52~55 DEG C.
Preferably, in step d, drying temperature is 65~75 DEG C, and drying time is 18~20h.
Preferably, in step e, the concrete operations of sintering are：150~170 DEG C are warming up to, 1~1.5h is kept the temperature, then with 1
The heating rate of~2 DEG C/min is warming up to 650~680 DEG C, keeps the temperature 40~60min, then heats to 760~790 DEG C, heat preservation 20
~25min.
Using water or ethyl alcohol as solvent in the present invention, does not interfere with reaction and generate, there is no need to limited amounts.
Acetylacetone,2,4-pentanedione alleviates the hydrolysis rate of butyl titanate as buffer in the present invention, without limited amount.
The paraffin oil containing sorbester p18 is not necessarily to limited amount as flotation agent in the present invention.
The present invention prepares SiO by raw material of ethyl orthosilicate2Colloidal sol, by the volume ratio for limiting ethyl orthosilicate and ethyl alcohol
It is 21~22：6~9, make SiO2Collosol concentration is larger, prevent in the subsequent sintering process microballon volume contraction cause in microballon greatly
There is stomata generation in portion；The present invention is using aluminum nitrate, zirconium nitrate, cerous nitrate and magnesium nitrate as raw material, and after lye is added, it is respectively right to be formed
The hydroxide sediment answered, after cleaning, carrying out ultrasonic disperse makes hydroxide sediment be uniformly distributed in water, is then added dropwise
Nitric acid forms the first colloidal sol；First colloidal sol is added dropwise in third colloidal sol, make teos hydrolysis polycondensation process be complexed aluminium,
Zirconium, cerium, magnesium ion；And using butyl titanate as raw material, zinc nitrate, chromic nitrate and boric acid is added in cooperation, and then hydrolysis obtains
TiO2Colloidal sol, by TiO2Colloidal sol, which is added third colloidal sol and is stirred, to be made silester be fully hydrolyzed and be complexed with butyl titanate to be
Glass network structure；7th colloidal sol is instilled in paraffin oil, colloidal sol becomes ball in paraffin oil due to the effect of surface tension
Shape shortens transformation time of the colloidal sol to gel in 52~55 DEG C of stirred in water bath, using sorbester p18 as dispersant, makes spherical molten
Glue hardly happens reunion in paraffin oil and granularity difference is smaller, and then filtration drying obtains gel microballon；Due to coagulating for acquisition
Glue particle surface still has paraffin oil, is first warming up to 150~170 DEG C, 1~1.5h is to remove paraffin oil for heat preservation, prevents paraffin oil from rising
Fire and keep sample temperature excessively high and burst, then slowly heating prevents organic principle in gel microballon from volatilizing too fast and causing micro-
Stomata is destroyed or generated inside pearl；The present invention introduces aluminium oxide, zirconium oxide, cerium oxide, magnesia, oxygen in glass microballoon
Change zinc, chromium oxide and boron oxide to cooperate, improve the chemical stability of glass microballoon, makes glass microballoon obtained by the present invention
Compact structure, translucency is preferable, and refractive index is up to 1.8~1.9.
Specific implementation mode
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of reflective glass beads proposed by the present invention, includes the following steps：
A, molar part is pressed by after 35 parts of aluminum nitrates, 30 parts of zirconium nitrates, 6 parts of cerous nitrates and 4 parts of magnesium nitrates mixing, is added to the water
Dissolving obtains mixed solution, and sodium hydroxide solution is then added dropwise, and filters, and filter cake cleaning is placed in water and carries out ultrasonic disperse,
The time of ultrasonic disperse is 15min, and the power of ultrasonic disperse is 500w, and the frequency of ultrasonic disperse is 30kHz, and then water-bath adds
The temperature of heat, heating water bath is 85 DEG C, and nitric acid is added dropwise during heating water bath to pH=3~4, obtains the first colloidal sol；
B, dissolving in ethyl alcohol is added in ethyl orthosilicate and obtains the second colloidal sol, water, positive silicon are then added dropwise into the second colloidal sol
The volume ratio of acetoacetic ester and ethyl alcohol is 7：3, the molar ratio of ethyl orthosilicate and water is 3：1, then pH value is adjusted to 3~4, after stirring
Third colloidal sol is obtained, is added dropwise the first colloidal sol in whipping process, the weight ratio of the second colloidal sol and the first colloidal sol is 25：9；
C, it is added into ethyl alcohol by molar part after ethyl acetoacetate stirs evenly, adds 52 parts of tetrabutyl titanates and carry out
The 4th colloidal sol once is stirred to get, the time once stirred is 2.6h；5 parts of zinc nitrates, 3 parts of chromic nitrates and 1 are added into ethyl alcohol
Part boric acid obtains the 5th solution after mixing uniformly；5th solution is added dropwise in the 4th colloidal sol, secondary agitation is then carried out, it is secondary to stir
The time mixed is 0.9h, adds water, then triple mixing, and the time of triple mixing is 20h, stands 28h and obtains the 6th colloidal sol；
D, 50 parts of third colloidal sols are stirred by weight, 18 part of the 6th colloidal sol and 5 parts of water is added dropwise in whipping process
Obtain the 7th colloidal sol；Paraffin oil containing sorbester p18 is subjected to heating water bath, the temperature of heating water bath is 52 DEG C, is then added dropwise the 7th
Colloidal sol enters paraffin oil, then stirs, and filtering, 75 DEG C of dry 18h obtain gel particle；
E, gel particle is warming up to 170 DEG C, keeps the temperature 1h, be then warming up to 650 DEG C with the heating rate of 2 DEG C/min, protected
Warm 60min then heats to 760 DEG C, keeps the temperature 25min, and cooling obtains reflective glass beads.
Embodiment 2
A kind of preparation method of reflective glass beads proposed by the present invention, includes the following steps：
A, molar part is pressed by after 38 parts of aluminum nitrates, 26 parts of zirconium nitrates, 9 parts of cerous nitrates and 2 parts of magnesium nitrates mixing, is added to the water
Dissolving obtains mixed solution, and sodium hydroxide solution is then added dropwise, and filters, and filter cake cleaning is placed in water and carries out ultrasonic disperse,
The time of ultrasonic disperse is 20min, and the power of ultrasonic disperse is 400w, and the frequency of ultrasonic disperse is 45kHz, and then water-bath adds
The temperature of heat, heating water bath is 75 DEG C, and nitric acid is added dropwise during heating water bath to pH=3~4, obtains the first colloidal sol；
B, dissolving in ethyl alcohol is added in ethyl orthosilicate and obtains the second colloidal sol, water, positive silicon are then added dropwise into the second colloidal sol
The volume ratio of acetoacetic ester and ethyl alcohol is 11：3, the molar ratio of ethyl orthosilicate and water is 12：1, then pH value is adjusted to 3~4, it stirs
After obtain third colloidal sol, be added dropwise the first colloidal sol in whipping process, the weight ratio of the second colloidal sol and the first colloidal sol is 4：1；
C, it is added into ethyl alcohol by molar part after ethyl acetoacetate stirs evenly, adds 55 parts of tetrabutyl titanates and carry out
The 4th colloidal sol once is stirred to get, the time once stirred is 2.3h；8 parts of zinc nitrates, 2 parts of chromic nitrates and 3 are added into ethyl alcohol
Part boric acid obtains the 5th solution after mixing uniformly；5th solution is added dropwise in the 4th colloidal sol, secondary agitation is then carried out, it is secondary to stir
The time mixed is 0.6h, adds water, then triple mixing, and the time of triple mixing is 22h, stands 25h and obtains the 6th colloidal sol；
D, 60 parts of third colloidal sols are stirred by weight, 15 part of the 6th colloidal sol and 8 parts of water is added dropwise in whipping process
Obtain the 7th colloidal sol；Paraffin oil containing sorbester p18 is subjected to heating water bath, the temperature of heating water bath is 55 DEG C, is then added dropwise the 7th
Colloidal sol enters paraffin oil, then stirs, and filtering, 65 DEG C of dry 20h obtain gel particle；
E, gel particle is warming up to 150 DEG C, keeps the temperature 1.5h, is then warming up to 680 DEG C with the heating rate of 1 DEG C/min,
40min is kept the temperature, then heats to 790 DEG C, keeps the temperature 20min, cooling obtains reflective glass beads.
Embodiment 3
A kind of preparation method of reflective glass beads proposed by the present invention, includes the following steps：
A, molar part is pressed by after 36 parts of aluminum nitrates, 29 parts of zirconium nitrates, 7 parts of cerous nitrates and 3.5 parts of magnesium nitrates mixing, and water is added
Middle dissolving obtains mixed solution, and sodium hydroxide solution is then added dropwise, filtering, and filter cake cleaning is placed in water and carries out ultrasound point
It dissipates, the time of ultrasonic disperse is 16min, and the power of ultrasonic disperse is 480w, and the frequency of ultrasonic disperse is 35kHz, then water-bath
The temperature of heating, heating water bath is 82 DEG C, and nitric acid is added dropwise during heating water bath to pH=3~4, obtains the first colloidal sol；
B, dissolving in ethyl alcohol is added in ethyl orthosilicate and obtains the second colloidal sol, water, positive silicon are then added dropwise into the second colloidal sol
The volume ratio of acetoacetic ester and ethyl alcohol is 21.3：8, the molar ratio of ethyl orthosilicate and water is 10：2.3, then adjust pH value to 3~4,
Third colloidal sol is obtained after stirring, is added dropwise the first colloidal sol in whipping process, and the weight ratio of the second colloidal sol and the first colloidal sol is 54：17；
C, it is added into ethyl alcohol by molar part after ethyl acetoacetate stirs evenly, adds 53 parts of tetrabutyl titanates and carry out
The 4th colloidal sol once is stirred to get, the time once stirred is 2.5h；Into ethyl alcohol be added 6 parts of zinc nitrates, 2.8 parts of chromic nitrates and
1.5 parts of boric acid obtain the 5th solution after mixing uniformly；5th solution is added dropwise in the 4th colloidal sol, then carries out secondary agitation, two
The time of secondary stirring is 0.8h, adds water, then triple mixing, and time of triple mixing is 20.5h, stands 27h and obtains the
Six colloidal sols；
D, 52 parts of third colloidal sols are stirred by weight, 17 part of the 6th colloidal sol and 6 parts of water is added dropwise in whipping process
Obtain the 7th colloidal sol；Paraffin oil containing sorbester p18 is subjected to heating water bath, the temperature of heating water bath is 53 DEG C, is then added dropwise the 7th
Colloidal sol enters paraffin oil, then stirs, and filtering, 72 DEG C of dry 19h obtain gel particle；
E, gel particle is warming up to 160 DEG C, keeps the temperature 1.2h, is then warming up to 660 with the heating rate of 1.5 DEG C/min
DEG C, 55min is kept the temperature, then heats to 770 DEG C, keeps the temperature 22min, cooling obtains reflective glass beads.
Embodiment 4
A kind of preparation method of reflective glass beads proposed by the present invention, includes the following steps：
A, molar part is pressed by after 37 parts of aluminum nitrates, 27 parts of zirconium nitrates, 8 parts of cerous nitrates and 2.5 parts of magnesium nitrates mixing, and water is added
Middle dissolving obtains mixed solution, and sodium hydroxide solution is then added dropwise, filtering, and filter cake cleaning is placed in water and carries out ultrasound point
It dissipates, the time of ultrasonic disperse is 18min, and the power of ultrasonic disperse is 450w, and the frequency of ultrasonic disperse is 40kHz, then water-bath
The temperature of heating, heating water bath is 78 DEG C, and nitric acid is added dropwise during heating water bath to pH=3~4, obtains the first colloidal sol；
B, dissolving in ethyl alcohol is added in ethyl orthosilicate and obtains the second colloidal sol, water, positive silicon are then added dropwise into the second colloidal sol
The volume ratio of acetoacetic ester and ethyl alcohol is 21.7：7, the molar ratio of ethyl orthosilicate and water is 11：1.5, then adjust pH value to 3~4,
Third colloidal sol is obtained after stirring, is added dropwise the first colloidal sol in whipping process, and the weight ratio of the second colloidal sol and the first colloidal sol is 58：16；
C, it is added into ethyl alcohol by molar part after ethyl acetoacetate stirs evenly, adds 54 parts of tetrabutyl titanates and carry out
The 4th colloidal sol once is stirred to get, the time once stirred is 2.4h；Into ethyl alcohol be added 7 parts of zinc nitrates, 2.5 parts of chromic nitrates and
2.5 parts of boric acid obtain the 5th solution after mixing uniformly；5th solution is added dropwise in the 4th colloidal sol, then carries out secondary agitation, two
The time of secondary stirring is 0.7h, adds water, then triple mixing, and the time of triple mixing is 21h, stands 26h and obtains the 6th
Colloidal sol；
D, 56 parts of third colloidal sols are stirred by weight, 16 part of the 6th colloidal sol and 7 parts of water is added dropwise in whipping process
Obtain the 7th colloidal sol；Paraffin oil containing sorbester p18 is subjected to heating water bath, the temperature of heating water bath is 54 DEG C, is then added dropwise the 7th
Colloidal sol enters paraffin oil, then stirs, and filtering, 68 DEG C of dry 19.6h obtain gel particle；
E, gel particle is warming up to 155 DEG C, keeps the temperature 1.4h, is then warming up to 670 with the heating rate of 1.2 DEG C/min
DEG C, 45min is kept the temperature, then heats to 780 DEG C, keeps the temperature 21min, cooling obtains reflective glass beads.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of reflective glass beads, which is characterized in that include the following steps：
A, after mixing aluminum nitrate, zirconium nitrate, cerous nitrate and magnesium nitrate, it is added to the water dissolving and obtains mixed solution, be then added dropwise
Filter cake cleaning is placed in water and carries out ultrasonic disperse, then heating water bath by sodium hydroxide solution, filtering, heating water bath process
Middle dropwise addition nitric acid obtains the first colloidal sol to pH=3~4；
B, dissolving in ethyl alcohol is added in ethyl orthosilicate and obtains the second colloidal sol, water is then added dropwise into the second colloidal sol, then adjust pH
Value obtains third colloidal sol, the first colloidal sol is added dropwise in whipping process to 3~4 after stirring；
C, it after addition ethyl acetoacetate stirs evenly into ethyl alcohol, adds tetrabutyl titanate progress and once stirs to get the 4th
Colloidal sol；It is added into ethyl alcohol after zinc nitrate, chromic nitrate and boric acid are mixed uniformly and obtains the 5th solution；5th solution is added dropwise to the 4th
In colloidal sol, secondary agitation is then carried out, adds water, then triple mixing, standing obtains the 6th colloidal sol；
D, third colloidal sol is stirred, the 6th colloidal sol is added dropwise in whipping process and water obtains the 7th colloidal sol；Sorbester p18 will be contained
Paraffin oil carry out heating water bath, then be added dropwise the 7th colloidal sol enter paraffin oil, then stir, filter, be dried to obtain gel particle；
E, gel particle is sintered, cooling obtains reflective glass beads.
2. the preparation method of reflective glass beads according to claim 1, which is characterized in that in step a, aluminum nitrate, nitric acid
The molar ratio of zirconium, cerous nitrate and magnesium nitrate is 35~38：26~30：6~9：2~4.
3. the preparation method of reflective glass beads according to claim 1 or claim 2, which is characterized in that in step a, ultrasonic disperse
Time be 15~20min, the power of ultrasonic disperse is 400~500w, and the frequency of ultrasonic disperse is 30~45kHz.
4. the preparation method of reflective glass beads according to claim 1 or claim 2, which is characterized in that in step a, heating water bath
Temperature be 75~85 DEG C.
5. the preparation method of reflective glass beads according to claim 1 or claim 2, which is characterized in that in step b, positive silicic acid second
The volume ratio of ester and ethyl alcohol is 21~22：6~9.
6. the preparation method of reflective glass beads according to claim 1 or claim 2, which is characterized in that in step b, positive silicic acid second
The molar ratio of ester and water is 9~12：1~3.
7. the preparation method of reflective glass beads according to claim 1 or claim 2, which is characterized in that in step b, the second colloidal sol
Weight ratio with the first colloidal sol is 50~60：15~18.
8. the preparation method of reflective glass beads according to claim 1 or claim 2, which is characterized in that in step c, the positive fourth of metatitanic acid
Ester, zinc nitrate, chromic nitrate and boric acid molar ratio be 52~55：5~8：2~3：1~3；Preferably, primary to stir in step c
Time be 2.3~2.6h；Preferably, in step c, the time of secondary agitation is 0.6~0.9h；Preferably, in step c, three
The time of secondary stirring is 20~22h；Preferably, in step c, the time of standing is 25~28h.
9. the preparation method of reflective glass beads according to claim 1 or claim 2, which is characterized in that in step d, third colloidal sol,
The weight ratio of 6th colloidal sol and water is 50~60：15~18：5~8；Preferably, in step d, the temperature of heating water bath is 52~
55℃；Preferably, in step d, drying temperature is 65~75 DEG C, and drying time is 18~20h.
10. the preparation method of reflective glass beads according to claim 1 or claim 2, which is characterized in that in step e, the tool of sintering
Gymnastics conduct：It is warming up to 150~170 DEG C, keeps the temperature 1~1.5h, then 650 are warming up to the heating rate of 1~2 DEG C/min~
680 DEG C, 40~60min is kept the temperature, then heats to 760~790 DEG C, keeps the temperature 20~25min.
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| CN107365084A (en) * | 2017-07-18 | 2017-11-21 | 合肥鼎亮光学科技有限公司 | A kind of sol-gal process prepares the process of magnetic reflective glass beads |
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| CN1575262A (en) * | 2001-10-24 | 2005-02-02 | 3M创新有限公司 | Glass beads and uses thereof |
| CN101890326A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing TiO2/SiO2 composite microspheres |
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| CN1575262A (en) * | 2001-10-24 | 2005-02-02 | 3M创新有限公司 | Glass beads and uses thereof |
| CN101890326A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing TiO2/SiO2 composite microspheres |
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