CN106745009A - A kind of monodispersed submicron grade silicon dioxide microballoon and preparation method thereof - Google Patents
A kind of monodispersed submicron grade silicon dioxide microballoon and preparation method thereof Download PDFInfo
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- CN106745009A CN106745009A CN201611114914.6A CN201611114914A CN106745009A CN 106745009 A CN106745009 A CN 106745009A CN 201611114914 A CN201611114914 A CN 201611114914A CN 106745009 A CN106745009 A CN 106745009A
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- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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Abstract
The invention provides a kind of monodispersed submicron grade silicon dioxide microballoon and preparation method thereof, comprise the following steps：End silicone based polyether is dissolved in the ethanol solution of ammoniacal liquor; add positive esters of silicon acis and stir; reacted at 100~120 DEG C using hydro-thermal method; obtain monodispersed submicron grade silicon dioxide microballoon dispersion liquid; by dispersion liquid under the protection of inert atmosphere; fired under the conditions of 650~700 DEG C, that is, obtain the monodispersed submicron grade silicon dioxide microballoon.The method has the advantages that reaction condition is simple, reaction raw materials are easy to get.Monodispersed submicron grade silicon dioxide microballoon prepared by the method, the monodispersed submicron grade silicon dioxide microballoon has the advantages that good dispersion, is difficult reunion, uniform particle sizes, and its particle size range is 0.5~15 micron, is sub-micron rank.
Description
Technical field
The present invention relates to earth silicon material preparing technical field, in particular to a kind of monodispersed submicron level two
Silicon oxide microsphere and preparation method thereof.
Background technology
SiO2It is a kind of nontoxic, tasteless, free of contamination nonmetallic materials.Nano-meter SiO_22Due to the miniaturization of particle size, than
Surface area is sharply increased so that SiO2Nano-particle has the performance of many uniquenesses and is widely applied prospect, such as special light
Point special efficacy, Magnetoresistance Phenomena high, nonlinear resistance phenomenon, the features such as still there is tough and good stability high under high temperature.Obtain property high
Can SiO2The premise of dispersion is to prepare single scattered SiO2Microballoon.Monodisperse superfine SiO2Microballoon catalyst, ceramics,
Application in chromatogram filling is widely.Spherical SiO2Due to dielectric high, moisture-proof heat-resisting, high high, high filler loading capacity, low bulk
The superior function such as property, low stress, low impurity, low-friction coefficient, can be used for multiple fields.
However, in the existing method for preparing monodisperse nano silicon dioxide microballoon, based on sol-gel process, using just
Tetraethyl orthosilicate SiO pure with analysis2It is raw material, made silicon dioxide microsphere is the silicon dioxide microsphere of Nano grade.So
And, if necessary to big particle diameter silicon dioxide microsphere when, such as micron level or during sub-micron rank, the above method can not be obtained
To the silicon dioxide microsphere of corresponding particle diameter.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of preparation method of monodispersed submicron grade silicon dioxide microballoon, to solve
Certainly existing sol-gel process prepares the problem of the bad dispersibility of monodisperse silica microspheres, described monodispersed submicron level
The preparation method of silicon dioxide microsphere, it is raw material to use positive esters of silicon acis, end silicone based polyether, is led in the ethanol solution of ammoniacal liquor
Hydro-thermal method is crossed, the dispersion liquid of monodispersed submicron grade silicon dioxide microballoon is prepared, then monodispersed submicron is obtained by firing
Grade silicon dioxide microballoon.Have the advantages that reaction condition is simple, reaction raw materials are easy to get.
The second object of the present invention is to provide a kind of preparation side of described monodispersed submicron grade silicon dioxide microballoon
Monodispersed submicron grade silicon dioxide microballoon prepared by method, the monodispersed submicron grade silicon dioxide microballoon, with dispersiveness
Well, the advantages of being difficult reunion, uniform particle sizes, its particle size range can reach 0.5~15 micron.
In order to realize above-mentioned purpose of the invention, spy uses following technical scheme：
A kind of preparation method of monodispersed submicron grade silicon dioxide microballoon, comprises the following steps：
End silicone based polyether is dissolved in the ethanol solution of ammoniacal liquor, positive esters of silicon acis is added and is stirred, using water
Hot method is reacted at 100~120 DEG C, monodispersed submicron grade silicon dioxide microballoon dispersion liquid is obtained, by dispersion liquid in indifferent gas
Under the protection of atmosphere, fired under the conditions of 650~700 DEG C, that is, obtain the monodispersed submicron grade silicon dioxide microballoon.
In the application, it is raw material to use positive esters of silicon acis, end silicone based polyether, and hydro-thermal is passed through in the ethanol solution of ammoniacal liquor
Method, prepares the dispersion liquid of monodispersed submicron grade silicon dioxide microballoon, then obtains monodispersed submicron level dioxy by firing
SiClx microballoon.Hold the end group of silicone based polyether similar to positive silicate structure, easily produce absorption, two are prepared in hydro-thermal reaction
Play a part of nucleator and template during silicon oxide microsphere.It is when the high temperature of more than cloud point is reached in pelletizing shape from water
It is separated out, is dispersed in water, the silicon that the silanol and positive silicic acid ester hydrolysis of generation are generated is hydrolyzed by holding siloxy group
Alcohol is combined into core by condensation reaction, and then positive esters of silicon acis hydrolysate is constantly deposited on core, and then greatly submicron order long
Silicon dioxide microsphere.Therefore, during using end silicone based polyether as nucleator and template, prepared silicon dioxide microsphere can
To reach sub-micron rank.The method has the advantages that reaction condition is simple, reaction raw materials are easy to get.
Preferably, the concentration of the ammoniacal liquor is 5%~10%.
Ammoniacal liquor as positive silicic acid ester hydrolysis catalyst, its concentration difference can cause changing for positive esters of silicon acis hydrolysis rate
Become.Ammonia concn is excessive, makes reaction speed too fast, and the silicon dioxide microsphere for obtaining is reuniting；Concentration is too small, reaction speed mistake
Slowly.
Preferably, the positive esters of silicon acis is the one kind in methyl silicate or tetraethyl orthosilicate.
Preferred positive esters of silicon acis is the ester that positive silicic acid and straight-chain fatty alcohol reaction are obtained, the chain length of fatty alcohol be difficult it is long,
Influence hydrolysis rate.It is optimal with fatty alcohol methyl esters or fatty alcohol ethyl ester.
Preferably, the structure of the end silicone based polyether is：
OrIn
It is a kind of；
Wherein, n >=2, R is with a kind of oxirane, the ring as initiator in ethylene glycol, glycerine or tetrahydrofuran
Ethylene Oxide homopolymers or copolymer.
Preferably, the mean molecule quantity of the end silicone based polyether is 200~20000.
Preferably, the preparation method of the end silicone based polyether, specifically includes following steps：
End hydroxy polyether is dissolved in organic solvent, is made with chloropropene reaction under catalyst action and is obtained end-allyl group
Polyethers, allyl-terminated polyether is issued with trimethoxy hydrogen silane or triethoxy hydrogen silane in chloroplatinic acid catalyst effect again
Raw hydrosilylation is made end silicone based polyether；
It is furthermore preferred that the organic solvent is the one kind in ethylene glycol, glycerine or tetrahydrofuran；
It is furthermore preferred that the catalyst is the one kind in TBAB or potassium hydroxide.
Hold the structure and preferred molecular weight and preparation method of silicone based polyether as described above.End siloxy group gathers
Ether is a kind of high molecular type surfactant.End silicone based polyether has water-soluble and oil-soluble concurrently, and can easily be accommodated, and it both had
Every excellent properties of traditional siloxane class product, such as high-low temperature resistant, anti-aging, hydrophobic, electric insulation, low surface tension, together
When there is the special natures such as lubrication, soft effect, good spreadability and emulsion stability that polyether segment provides again.
Preferably, the time of the reaction is 1~1.5 hour.
Preferably, the inert atmosphere is the one kind in nitrogen, argon gas or helium.
Preferably, the time of the firing is 3~3.5 hours.
Monodispersed submicron level prepared by the preparation method of monodispersed submicron grade silicon dioxide microballoon as described above
Silicon dioxide microsphere.
Monodispersed submicron level prepared by the preparation method of monodispersed submicron grade silicon dioxide microballoon as described above
Silicon dioxide microsphere, good dispersion, uniform particle sizes, particle size range is between 0.5~15 micron.
Compared with prior art, beneficial effects of the present invention are：
(1) preparation method of monodispersed submicron grade silicon dioxide microballoon provided herein, using positive esters of silicon acis, end
Silicone based polyether is raw material, by hydro-thermal method in the ethanol solution of ammoniacal liquor, prepares monodispersed submicron grade silicon dioxide micro-
The dispersion liquid of ball, then obtains monodispersed submicron grade silicon dioxide microballoon by firing.The method have reaction condition it is simple,
The advantages of reaction raw materials are easy to get.
(2) single dispersing prepared by the preparation method of monodispersed submicron grade silicon dioxide microballoon provided herein is sub-
Micron silica microballoon, during using end silicone based polyether as nucleator and template, prepared silicon dioxide microsphere
Sub-micron rank can be reached, there is good dispersion, reunion, uniform particle sizes are difficult, its particle size range is 0.5~15
Micron, is sub-micron rank.
Brief description of the drawings
In order to illustrate more clearly of the specific embodiment of the invention or technical scheme of the prior art, below will be to specific
The accompanying drawing to be used needed for implementation method or description of the prior art is briefly described, it should be apparent that, in describing below
Accompanying drawing is some embodiments of the present invention, for those of ordinary skill in the art, before creative work is not paid
Put, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 is the monodispersed submicron grade silicon dioxide microballoon electron lens photo that the embodiment of the present invention 3 is provided.
Specific embodiment
Technical scheme is clearly and completely described below in conjunction with the drawings and specific embodiments, but
It is it will be understood to those of skill in the art that following described embodiment is a part of embodiment of the invention, rather than whole
Embodiment, is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.Based on the embodiment in the present invention, ability
The every other embodiment that domain those of ordinary skill is obtained under the premise of creative work is not made, belongs to guarantor of the present invention
The scope of shield.Unreceipted actual conditions person in embodiment, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same
Or the unreceipted production firm person of instrument, it is the conventional products that can be obtained by commercially available purchase.
In the description of the invention, it is necessary to explanation, term " " center ", " on ", D score, "left", "right", " vertical ",
The orientation or position relationship of the instruction such as " level ", " interior ", " outward " be based on orientation shown in the drawings or position relationship, merely to
Be easy to the description present invention and simplify describe, rather than indicate imply signified device or element must have specific orientation,
With specific azimuth configuration and operation, therefore it is not considered as limiting the invention.Additionally, term " first ", " second ",
" the 3rd " is only used for describing purpose, and it is not intended that indicating or implying relative importance.
In the description of the invention, it is necessary to illustrate, unless otherwise clearly defined and limited, term " installation ", " phase
Company ", " connection " should be interpreted broadly, for example, it may be being fixedly connected, or being detachably connected, or be integrally connected；Can
Being to mechanically connect, or electrically connect；Can be joined directly together, it is also possible to be indirectly connected to by intermediary, Ke Yishi
Two connections of element internal.For the ordinary skill in the art, with concrete condition above-mentioned term can be understood at this
Concrete meaning in invention.
Embodiment 1
The preparation method of monodispersed submicron grade silicon dioxide microballoon provided herein, specifically includes following steps：
(1) end hydroxy polyether, is dissolved in tetrahydrofuran, end alkene is made with chloropropene reaction under TBAB effect
There is hydrosilylation under chloroplatinic acid catalyst effect with trimethoxy hydrogen silane again in propyl group polyethers, allyl-terminated polyether,
End silicone based polyether is made, molecular weight is 200.
(2), the end silicone based polyether in step (1) is dissolved in the ethanol solution of the ammoniacal liquor that concentration is 5%, is added
Methyl silicate simultaneously stirs, and is reacted 1 hour at 120 DEG C using hydro-thermal method, obtains monodispersed submicron grade silicon dioxide
Microballoon dispersion liquid；
(3), the dispersion liquid for obtaining step (2) is under the protection of nitrogen atmosphere, fires 3 hours under the conditions of 650 DEG C, i.e.,
Obtain the monodispersed submicron grade silicon dioxide microballoon.
Embodiment 2
The preparation method of monodispersed submicron grade silicon dioxide microballoon provided herein, specifically includes following steps：
(1) end hydroxy polyether, is dissolved in tetrahydrofuran, end-allyl group is made with chloropropene reaction under potassium hydroxide effect
There is hydrosilylation in polyethers, allyl-terminated polyether, be made with triethoxy hydrogen silane under chloroplatinic acid catalyst effect again
End silicone based polyether, molecular weight is 20000.
(2), the end silicone based polyether in step (1) is dissolved in the ethanol solution of the ammoniacal liquor that concentration is 15%, then is added
Enter tetraethyl orthosilicate and stir, reacted 1.5 hours at 100 DEG C using hydro-thermal method, obtain monodispersed submicron level dioxy
SiClx microballoon dispersion liquid；
(3), the dispersion liquid for obtaining step (2) is fired 3.5 hours under the protection of helium atmosphere under the conditions of 700 DEG C,
Obtain the monodispersed submicron grade silicon dioxide microballoon.
Embodiment 3
The preparation method of monodispersed submicron grade silicon dioxide microballoon provided herein, specifically includes following steps：
(1) end hydroxy polyether, is dissolved in tetrahydrofuran, end alkene is made with chloropropene reaction under TBAB effect
There is hydrosilylation under chloroplatinic acid catalyst effect with trimethoxy hydrogen silane again in propyl group polyethers, allyl-terminated polyether,
End silicone based polyether is made, molecular weight is 2000.
(2), the end silicone based polyether in step (1) is dissolved in the ethanol solution of the ammoniacal liquor that concentration is 10%, then is added
Enter tetraethyl orthosilicate and stir, reacted 1 hour at 110 DEG C using hydro-thermal method, obtain monodispersed submicron level titanium dioxide
Silicon microballoon dispersion liquid；
(3), the dispersion liquid for obtaining step (2) is under the protection of argon gas atmosphere, fires 3 hours under the conditions of 680 DEG C, i.e.,
Obtain the monodispersed submicron grade silicon dioxide microballoon.
Embodiment 4
(1) end hydroxy polyether, is dissolved in tetrahydrofuran, end alkene is made with chloropropene reaction under TBAB effect
There is hydrosilylation under chloroplatinic acid catalyst effect with triethoxy hydrogen silane again in propyl group polyethers, allyl-terminated polyether,
End silicone based polyether is made, molecular weight is 3000.
(2), the end silicone based polyether in step (1) is dissolved in the ethanol solution of the ammoniacal liquor that concentration is 8%, is added
Tetraethyl orthosilicate simultaneously stirs, and is reacted 1 hour at 110 DEG C using hydro-thermal method, obtains monodispersed submicron grade silicon dioxide
Microballoon dispersion liquid；
(3), the dispersion liquid for obtaining step (2) is under the protection of argon gas atmosphere, fires 3 hours under the conditions of 690 DEG C, i.e.,
Obtain the monodispersed submicron grade silicon dioxide microballoon.
Embodiment 5
(1), end silicone based polyether is dissolved in the ethanol solution of the ammoniacal liquor that concentration is 12%, methyl silicate is added
And stir, reacted 1 hour at 110 DEG C using hydro-thermal method, obtain monodispersed submicron grade silicon dioxide microballoon dispersion liquid；
Wherein, the structure of end silicone based polyether is：
N >=2, R is the oxirane homopolymerization with ethylene glycol as initiator
Thing, end silicone based polyether molecular weight is 5000
(2), the dispersion liquid for obtaining step (1) is under the protection of nitrogen atmosphere, fires 3 hours under the conditions of 650 DEG C, i.e.,
Obtain the monodispersed submicron grade silicon dioxide microballoon.
Embodiment 6
(2), end silicone based polyether is dissolved in the ethanol solution of the ammoniacal liquor that concentration is 13%, tetraethyl orthosilicate is added
And stir, reacted 1 hour at 110 DEG C using hydro-thermal method, obtain monodispersed submicron grade silicon dioxide microballoon dispersion liquid；
Wherein, the structure of end silicone based polyether is：
N >=2, R is the propylene oxide copolymer with glycerine as initiator
Thing, end silicone based polyether molecular weight is 10000.
(2), the dispersion liquid for obtaining step (1) is fired 3.5 hours under the protection of argon gas atmosphere under the conditions of 680 DEG C,
Obtain the monodispersed submicron grade silicon dioxide microballoon.
Embodiment 7
(1) end hydroxy polyether, is dissolved in tetrahydrofuran, end alkene is made with chloropropene reaction under TBAB effect
There is hydrosilylation under chloroplatinic acid catalyst effect with trimethoxy hydrogen silane again in propyl group polyethers, allyl-terminated polyether,
End silicone based polyether is made, molecular weight is 15000.
(2), the end silicone based polyether in step (1) is dissolved in the ethanol solution of the ammoniacal liquor that concentration is 13%, then is added
Enter tetraethyl orthosilicate and stir, reacted 1 hour at 120 DEG C using hydro-thermal method, obtain monodispersed submicron level titanium dioxide
Silicon microballoon dispersion liquid；
(3), the dispersion liquid for obtaining step (2) is under the protection of helium atmosphere, fires 3 hours under the conditions of 670 DEG C, i.e.,
Obtain the monodispersed submicron grade silicon dioxide microballoon.
Experimental example monodispersed submicron grade silicon dioxide microspherulite diameter is tested
The pattern and granularity of the monodispersed submicron grade silicon dioxide microballoon provided for the embodiment of the present application 1~7 are used
Transmission electron microscope (TEM, H-800) is characterized.
Experimental result is as shown in table 1.Wherein, the TEM photos of embodiment 3 are as shown in Figure 1.
The monodispersed submicron grade silicon dioxide microspherulite diameter test result of table 1
| Embodiment | Particle diameter (micron) |
| 1 | 0.54 |
| 2 | 13.5 |
| 3 | 1.1 |
| 4 | 2.5 |
| 5 | 3.4 |
| 6 | 5.8 |
| 7 | 7.6 |
Test result indicate that, monodispersed submicron grade silicon dioxide microballoon provided herein provided herein
Monodispersed submicron grade silicon dioxide microballoon prepared by preparation method, the monodispersed submicron grade silicon dioxide microballoon, has
Good dispersion, be difficult to reunite, the advantages of particle diameter is small, its particle size range is 0.5~15 micron, is sub-micron rank.
In sum, the preparation of monodispersed submicron grade silicon dioxide microballoon provided herein provided herein
Method, it is raw material to use positive esters of silicon acis, end silicone based polyether, by hydro-thermal method in the ethanol solution of ammoniacal liquor, prepares single point
The dispersion liquid of submicron silica powder microballoon is dissipated, then monodispersed submicron grade silicon dioxide microballoon is obtained by firing.Should
Method has the advantages that reaction condition is simple, reaction raw materials are easy to get.Monodispersed submicron grade silicon dioxide prepared by the method
Microballoon, the monodispersed submicron grade silicon dioxide microballoon has the advantages that good dispersion, is difficult reunion, uniform particle sizes, its particle diameter
Scope is 0.5~15 micron, is sub-micron rank.
Although illustrate and describing the present invention with specific embodiment, but will be appreciated that various embodiments above is only used
To illustrate technical scheme, rather than its limitations；It will be understood by those within the art that：Without departing substantially from this hair
In the case of bright spirit and scope, the technical scheme described in foregoing embodiments can be modified, or to wherein
Some or all of technical characteristic carries out equivalent；And these modifications or replacement, do not make the essence of appropriate technical solution
Depart from the scope of various embodiments of the present invention technical scheme；It is, therefore, intended that including belonging to the present invention in the following claims
In the range of all these substitutions and modifications.
Claims (10)
1. a kind of preparation method of monodispersed submicron grade silicon dioxide microballoon, it is characterised in that comprise the following steps：
End silicone based polyether is dissolved in the ethanol solution of ammoniacal liquor, positive esters of silicon acis is added and is stirred, using hydro-thermal method
Reacted at 100~120 DEG C, monodispersed submicron grade silicon dioxide microballoon dispersion liquid is obtained, by dispersion liquid in inert atmosphere
Under protection, fired under the conditions of 650~700 DEG C, that is, obtain the monodispersed submicron grade silicon dioxide microballoon.
2. the preparation method of monodispersed submicron grade silicon dioxide microballoon according to claim 1, it is characterised in that described
The concentration of ammoniacal liquor is 5%~10%.
3. the preparation method of monodispersed submicron grade silicon dioxide microballoon according to claim 1, it is characterised in that described
Positive esters of silicon acis is the one kind in methyl silicate or tetraethyl orthosilicate.
4. the preparation method of monodispersed submicron grade silicon dioxide microballoon according to claim 1, it is characterised in that described
Hold silicone based polyether structure be：
OrIn one kind；
Wherein, n >=2, R is with a kind of oxirane, the epoxy third as initiator in ethylene glycol, glycerine or tetrahydrofuran
Alkane homopolymers or copolymer.
5. the preparation method of monodispersed submicron grade silicon dioxide microballoon according to claim 4, it is characterised in that described
The mean molecule quantity for holding silicone based polyether is 200~20000.
6. the preparation method of monodispersed submicron grade silicon dioxide microballoon according to claim 5, it is characterised in that described
The preparation method of silicone based polyether is held, following steps are specifically included：
End hydroxy polyether is dissolved in tetrahydrofuran solution, is made with chloropropene reaction under catalyst action and is obtained end-allyl group
Polyethers, allyl-terminated polyether is issued with trimethoxy hydrogen silane or triethoxy hydrogen silane in chloroplatinic acid catalyst effect again
Raw hydrosilylation is made end silicone based polyether；
Preferably, the catalyst is the one kind in TBAB or potassium hydroxide.
7. the preparation method of monodispersed submicron grade silicon dioxide microballoon according to claim 1, it is characterised in that described
The time of reaction is 1~1.5 hour.
8. the preparation method of monodispersed submicron grade silicon dioxide microballoon according to claim 1, it is characterised in that described
Inert atmosphere is the one kind in nitrogen, argon gas or helium.
9. the preparation method of monodispersed submicron grade silicon dioxide microballoon according to claim 1, it is characterised in that described
The time of firing is 3~3.5 hours.
10. prepared by the preparation method of the monodispersed submicron grade silicon dioxide microballoon according to claim any one of 1-9
Monodispersed submicron grade silicon dioxide microballoon.
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| CN109593204A (en) * | 2018-12-14 | 2019-04-09 | 浙江开化合成材料有限公司 | A kind of application method reducing the secondary addition by-product of hydrogen silicon |
| CN112176720A (en) * | 2020-09-28 | 2021-01-05 | 安徽瑜合警用装备有限公司 | Photoluminescent finishing agent based on silica microspheres, preparation method and application thereof |
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| CN106745009B (en) | 2018-08-17 |
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