CN102795630A - Method for preparing silicon dioxide by using reverse micro-emulsion method - Google Patents
Method for preparing silicon dioxide by using reverse micro-emulsion method Download PDFInfo
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- CN102795630A CN102795630A CN2011101350418A CN201110135041A CN102795630A CN 102795630 A CN102795630 A CN 102795630A CN 2011101350418 A CN2011101350418 A CN 2011101350418A CN 201110135041 A CN201110135041 A CN 201110135041A CN 102795630 A CN102795630 A CN 102795630A
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- deionized water
- tween60
- span60
- span80
- tween80
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 22
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 11
- 238000000593 microemulsion method Methods 0.000 title description 2
- 239000004530 micro-emulsion Substances 0.000 claims abstract description 31
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 11
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 229920000136 polysorbate Polymers 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims description 100
- 229910021641 deionized water Inorganic materials 0.000 claims description 100
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 30
- HVUMOYIDDBPOLL-XGKPLOKHSA-N [2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XGKPLOKHSA-N 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- 230000015556 catabolic process Effects 0.000 claims description 9
- 239000000839 emulsion Substances 0.000 claims description 9
- 229960001866 silicon dioxide Drugs 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000009987 spinning Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000010533 azeotropic distillation Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims description 2
- 238000007701 flash-distillation Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 238000010980 drying distillation Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 description 17
- 239000011164 primary particle Substances 0.000 description 15
- 239000000843 powder Substances 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 5
- 229920005591 polysilicon Polymers 0.000 description 5
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 4
- 239000006229 carbon black Substances 0.000 description 4
- 239000013543 active substance Substances 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000009434 installation Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000007086 side reaction Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- DUIOKRXOKLLURE-UHFFFAOYSA-N 2-octylphenol Chemical compound CCCCCCCCC1=CC=CC=C1O DUIOKRXOKLLURE-UHFFFAOYSA-N 0.000 description 1
- 229910003902 SiCl 4 Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- -1 polyoxyethylene nonylphenol Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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Abstract
The invention provides a method for preparing silicon dioxide by using silicon tetrachloride. The method comprises the following steps of: (1) providing a reverse micro-emulsion system compounded by using an NP series, a TX series or a Span series and a Tween series; (2) performing micro-emulsion treatment on the reverse micro-emulsion system in the (1); (3) adding silicon tetrachloride serving as a raw material into the reverse micro-emulsion system in the (2); (4) after the reaction in the (3), performing demulsification on the reverse micro-emulsion system in the (3); and (5) drying a reaction product in the (4).
Description
Technical field
The present invention relates to a kind of preparation method of silicon-dioxide, relate in particular to the preparation method of micron or nano level monodisperse silica.
Background technology
Silicon tetrachloride is as the main by product of producing polysilicon; Because of its corrodibility strong; Inconvenience storage and transportation; Volatile, thus to the safety in production and environment protection produced great pressure, how to utilize, digest the extremely urgent problem that this by product has become China's organosilicon and polysilicon industry.At present, main both at home and abroad through two kinds of method processing silicon chloride, a kind of is to adopt vapor phase process to produce WHITE CARBON BLACK, but the required production cost of this method is higher; Another kind method is to adopt hydro-reduction technology preparation trichlorosilane, but its transformation efficiency is low and dangerous big.
In view of this, in actual production, need a kind of method for preparing silicon-dioxide, especially monodisperse silica with silicon tetrachloride really.
Summary of the invention
The object of the invention is intended to solve the problems referred to above of existing in the prior art and at least one aspect of defective.
Correspondingly, one of the object of the invention provides and a kind ofly prepares silicon-dioxide with silicon tetrachloride, especially the method for monodisperse silica.
One of the object of the invention is to adopt a kind of eco-friendly method in the preparation monodisperse silica, has eliminated side reaction product in the polysilicon preparation to the disadvantageous effect of environment, has reduced the high problem of prior art cost simultaneously.
One of the object of the invention provides a kind of method for preparing the littler monodisperse silica powder of primary particle size.
Term described herein " the single dispersion " is meant that some parameters of material have homogeneous character, is meant particle size pattern basically identical particularly, is uniformly dispersed, and particle disperses each other.
In one aspect, provide a kind of and prepared silicon-dioxide with silicon tetrachloride, the method for monodisperse silica especially, it may further comprise the steps:
(1) NP (polyoxyethylene nonylphenol) series, TX (octyl phenol Soxylat A 25-7) series or Span (sapn) the series reverse microemulsion system with Tween (tween) is provided;
(2) the reverse microemulsion system in the step (1) being carried out microemulsified handles;
(3) the raw material silicon tetrachloride is joined in the reverse microemulsion system in the step (2);
(4) treat that reaction in the step (3) is carried out after, the reverse microemulsion system in the step (3) is carried out breakdown of emulsion handles; With
(5) reaction product in the drying step (4).
In one embodiment, in step (4) afterwards, carry out the step of the reaction product in the washing step (4).
In one embodiment, the reverse microemulsion system of said NP system comprises NP-5-hexanaphthene-deionized water, NP-5-normal heptane-deionized water, NP-5-normal hexane-deionized water, NP-5-octane-deionized water or NP-5-Skellysolve A-deionized water.
In one embodiment, said TX-100 series reverse microemulsion system comprises TX-100-hexanaphthene-deionized water, TX-100-normal heptane-deionized water, TX-100-normal hexane-deionized water, TX-100-octane-deionized water, TX-100-Skellysolve A-deionized water.
In one embodiment, the reverse microemulsion system of said Span series and Tween comprises Span60+Tween60-hexanaphthene-deionized water, Span60+Tween60-normal heptane-deionized water, Span60+Tween60-normal hexane-deionized water, Span60+Tween60-octane-deionized water, Span60+Tween60-Skellysolve A-deionized water, Span60+Tween80-hexanaphthene-deionized water, Span60+Tween80-normal heptane-deionized water, Span60+Tween80-normal hexane-deionized water, Span60+Tween80-octane-deionized water, Span60+Tween80-Skellysolve A-deionized water, Span80+Tween60-hexanaphthene-deionized water, Span80+Tween60-normal heptane-deionized water, Span80+Tween60-normal hexane-deionized water, Span80+Tween60-octane-deionized water, Span80+Tween60-Skellysolve A-deionized water, Span80+Tween80-hexanaphthene-deionized water, Span80+Tween80-normal heptane-deionized water, Span80+Tween80-normal hexane-deionized water, Span80+Tween80-octane-deionized water or Span80+Tween80-Skellysolve A-deionized water.
In one embodiment, the microemulsified in the said step (2) is treated to the said reverse microemulsion system that stirs.
In one embodiment, the breakdown of emulsion in the said step (4) is handled and is to use the mixing solutions of acetone and water to carry out breakdown of emulsion.
In one embodiment, the washing step in the said step (2) is after the reaction product in the step with centrifugal separation (3), uses the absolute ethyl alcohol centrifuge washing.
In one embodiment, the drying step in the said step (5) is common drying meanss such as vacuum-drying, spraying drying, azeotropic distillation drying, flash distillation.
Detailed description through hereinafter of the present invention can be known, under identical condition, adopts SiCl
4For the WHITE CARBON BLACK primary particle size of feedstock production is little than tetraethoxy (TEOS), and distribution uniform.So,, can obtain the better monodisperse silica of quality adopting under the situation of silicon tetrachloride as raw material.Simultaneously, owing to be to utilize silicon tetrachloride, eliminated the disadvantageous effect that silicon tetrachloride causes environment as the side reaction product of producing polysilicon, and then made that the preparation method of monodisperse silica of the present invention is eco-friendly.
In addition, monodisperse silica all is widely used at aspects such as coating, catalyzer, chromatograph packing material and high-performance ceramics.In the common methods of preparation monodisperse silica, raw material adopts tetraethyl silicate, uses silicon tetrachloride to replace tetraethyl silicate to be raw material, can reduce raw materials cost.
Description of drawings
These and/or other aspect of the present invention and advantage are from obviously with easily understanding below in conjunction with becoming the accompanying drawing description of preferred embodiments, wherein:
Fig. 1 is the sem photograph under 50000 times of magnifications of the monodisperse silica powder that obtained according to embodiments of the invention one;
Fig. 2 is the primary particle size distribution plan of the monodisperse silica powder that obtained according to embodiments of the invention one;
Fig. 3 is the sem photograph under 50000 times of magnifications of the monodisperse silica powder that obtained according to embodiments of the invention two;
Fig. 4 is the primary particle size distribution plan of the monodisperse silica powder that obtained according to embodiments of the invention two;
Fig. 5 is the sem photograph under 50000 times of magnifications of the monodisperse silica powder that obtained according to embodiments of the invention three; With
Fig. 6 is the primary particle size distribution plan of the monodisperse silica powder that obtained according to embodiments of the invention three.
Embodiment
Further specify embodiment of the present invention below in conjunction with embodiment.
Embodiment one:
With NP-5-normal heptane-deionized water is the reverse microemulsion system; The NP-5 (for example 12 grams) and the oil phase (for example 8 grams) (for example normal heptane) of certain mass are mixed in the container (for example round-bottomed flask); With whipping appts (as; Constant temperature blender with magnetic force) evenly stir certain hour (as 10 minutes), the deionized water (for example 2.4 grams) with certain mass under agitation slowly is added drop-wise in the said vesse again, dropwises continued stirring certain hour (as 20 minutes) and makes it to disperse evenly; After treating the complete microemulsified of above-mentioned system, take by weighing the SiCl of certain mass (for example 2.3 grams)
4Stirring simultaneously; Join gradually in the microemulsion system of above-mentioned complete microemulsified, add the continued stirring certain hour (for example 30 minutes) that finishes and make it to react completely, carry out deemulsification with breakdown of emulsion liquid (the for example mixing solutions of 60ml acetone and water (volume ratio of acetone and water is 3: 1)) and handle; Carrying out spinning afterwards handles; After the spinning with absolute ethyl alcohol centrifuge washing for several times (for example 2-10 time); At a certain temperature (for example put into drying installation (for example vacuum drying oven) again; 10-100 ℃; Be preferably 80 ℃) vacuum-drying certain hour (for example 10 minutes to 50 hours, be preferably 4 hours), obtain the SiO of average primary particle diameter 22.8nm
2Powder.
The mass ratio of normal heptane and NP-5 is 2: 3, the mol ratio R=4 of deionized water and tensio-active agent, and the mol ratio H=10 of deionized water and silicon tetrachloride, the temperature that reaction is carried out is 15 ℃.
Visible by Fig. 1 and 2; The primary particle of the silica product that embodiment one is obtained is the regular spheroidal particle of dispersive, is the monodisperse silica particle, through statistical study; The median size of primary particle is 22.8nm; Wherein the particle of 10-20nm granularity accounts for 33.3% of sum, and the particle of 20-30nm accounts for 59.6% of sum, and the above particle of 30nm accounts for 7.1%.
Be appreciated that above-mentioned test conditions can carry out same ratio ground convergent-divergent as required, to satisfy different needs of production.
Embodiment two:
Is the reverse microemulsion system with NP-5-hexanaphthene-de-ionized as water; (for example the NP-5 of (for example 10 grams) and oil phase (for example 6 grams) (for example hexanaphthene) are mixed in the container (for example round-bottomed flask) with certain mass; With whipping appts (as; Constant temperature blender with magnetic force) evenly stir certain hour (as 10 minutes), the deionized water (for example 3 grams) with certain mass under agitation slowly is added drop-wise in the said vesse again, dropwises continued stirring certain hour (as 20 minutes) and makes it to disperse evenly; After treating the complete microemulsified of above-mentioned system, take by weighing the SiCl of certain mass (for example 7.08 grams)
4Stirring simultaneously; Join gradually in the microemulsion system of above-mentioned complete microemulsified, add the continued stirring certain hour (for example 30 minutes) that finishes and make it to react completely, carry out deemulsification with breakdown of emulsion liquid (the for example mixing solutions of 60ml acetone and water (volume ratio of acetone and water is 3: 1)) and handle; Carrying out spinning afterwards handles; After the spinning with absolute ethyl alcohol centrifuge washing for several times (for example 2-10 time); At a certain temperature (for example put into drying installation (for example vacuum drying oven) again; 10-100 ℃; Be preferably 80 ℃) vacuum-drying certain hour (for example 10 minutes to 50 hours, be preferably 4 hours), obtain the SiO of average primary particle diameter 5.74nm
2Powder.
Wherein the mass ratio of hexanaphthene and NP-5 is 3: 5, the mol ratio R=6 of deionized water and tensio-active agent, and the mol ratio H=4 of deionized water and silicon tetrachloride, the temperature that reaction is carried out is 15 ℃.
By Fig. 3 and 4 visible; Silicon tetrachloride is that the primary particle size of feedstock production silicon-dioxide is the regular spheroidal particle of dispersive, is the monodisperse silica particle, through statistical study; The median size of primary particle is 5.74nm; Wherein the particle of 1-5nm granularity accounts for 61.4% of sum, and the particle of 5-10nm accounts for 29.5% of sum, and the above particle of 10nm accounts for 9.1%.
Embodiment three:
Is the reverse microemulsion system with NP-5-hexanaphthene-de-ionized as water; The NP-5 (for example 10 grams) and the oil phase (for example 6 grams) (for example hexanaphthene) of certain mass are mixed in the container (for example round-bottomed flask); With whipping appts (as; Constant temperature blender with magnetic force) evenly stir certain hour (as 10 minutes), the deionized water with certain mass (for example 3 grams) under agitation slowly is added drop-wise in the said vesse again, dropwises continued stirring certain hour (as 20 minutes) and makes it to disperse evenly; After treating the complete microemulsified of above-mentioned system; Take by weighing the tetraethoxy of certain mass (for example 8.69 grams),, join gradually in the microemulsion system of above-mentioned complete microemulsified stirring simultaneously; Add the continued stirring certain hour (for example 30 minutes) that finishes and make it to react completely, carry out deemulsification with breakdown of emulsion liquid (the for example mixing solutions of 60ml acetone and water (volume ratio of acetone and water is 3: 1)) and handle; Carrying out spinning afterwards handles; After the spinning with absolute ethyl alcohol centrifuge washing for several times (for example 2-10 time); At a certain temperature (for example put into drying installation (for example vacuum drying oven) again; 10-100 ℃; Be preferably 80 ℃) vacuum-drying certain hour (for example 10 minutes to 50 hours, be preferably 4 hours), obtain the SiO of average primary particle diameter 18.6nm
2Powder.
Wherein the mass ratio of hexanaphthene and NP-5 is 3: 5, the mol ratio R=6 of deionized water and tensio-active agent, and the mol ratio H=4 of deionized water and tetraethoxy, the temperature that reaction is carried out is 15 ℃.
By Fig. 5 and 6 visible; TEOS is that the primary particle of feedstock production WHITE CARBON BLACK is the regular spheroidal particle of dispersive, and through statistical study, the median size of primary particle is 18.6nm; Wherein the particle of 10-15nm granularity accounts for 23.5% of sum; The particle of 15-20nm accounts for 43.1% of sum, and the particle of 20-25nm accounts for 29.5% of sum, and the above particle of 25nm accounts for 3.9%.
Comparison through embodiment two and embodiment three can know that (except having adopted different raw materials, embodiment two adopts silicon tetrachloride particularly, and embodiment three adopts tetraethoxy) adopted SiCl under identical condition
4For the WHITE CARBON BLACK primary particle size of feedstock production is little than tetraethoxy (TEOS), and distribution uniform.So,, can obtain the better silicon-dioxide of quality adopting under the situation of silicon tetrachloride as raw material.Simultaneously, owing to be to utilize silicon tetrachloride, eliminated the disadvantageous effect that silicon tetrachloride causes as the side reaction product of producing polysilicon, to environment, and then made that the preparation method of silicon-dioxide of the present invention is eco-friendly.
Those skilled in the art are appreciated that similar reverse microemulsion system (for example NP series, TX is serial or the compound system of Span series and Tween series) also can use.Particularly, the reverse microemulsion system of said NP system comprises NP-5-hexanaphthene-deionized water, NP-5-normal heptane-deionized water, NP-5-normal hexane-deionized water, NP-5-octane-deionized water or NP-5-Skellysolve A-deionized water.Said TX-100 series reverse microemulsion system comprises TX-100-hexanaphthene-deionized water, TX-100-normal heptane-deionized water, TX-100-normal hexane-deionized water, TX-100-octane-deionized water, TX-100-Skellysolve A-deionized water.Said Span series and the composite reverse microemulsion system of Tween comprise Span60+Tween60-hexanaphthene-deionized water; Span60+Tween60-normal heptane-deionized water; Span60+Tween60-normal hexane-deionized water; Span60+Tween60-octane-deionized water; Span60+Tween60-Skellysolve A-deionized water; Span60+Tween80-hexanaphthene-deionized water; Span60+Tween80-normal heptane-deionized water; Span60+Tween80-normal hexane-deionized water; Span60+Tween80-octane-deionized water; Span60+Tween80-Skellysolve A-deionized water; Span80+Tween60-hexanaphthene-deionized water; Span80+Tween60-normal heptane-deionized water; Span80+Tween60-normal hexane-deionized water; Span80+Tween60-octane-deionized water; Span80+Tween60-Skellysolve A-deionized water; Span80+Tween80-hexanaphthene-deionized water; Span80+Tween80-normal heptane-deionized water; Span80+Tween80-normal hexane-deionized water; Span80+Tween80-octane-deionized water; Or Span80+Tween80-Skellysolve A-deionized water.Therefore, those skilled in the art can select suitable above-mentioned microfacies reaction system as required.
Though describe the present invention in conjunction with accompanying drawing, disclosed embodiment is intended to the preferred embodiment for the present invention is carried out exemplary illustration in the accompanying drawing, and can not be interpreted as a kind of restriction of the present invention.
Though some embodiment of this present general inventive concept are shown and explain; Those skilled in the art will appreciate that; Under the situation of principle that does not deviate from this present general inventive concept and spirit, can make a change these embodiment, scope of the present invention limits with claim and their equivalent.
Claims (9)
1. one kind prepares the method for silicon-dioxide with silicon tetrachloride, and it may further comprise the steps:
First step: NP series, the reverse microemulsion system that TX is serial or Span is serial and Tween series is composite are provided;
Second step: the reverse microemulsion system in the first step is carried out microemulsified handle;
Third step: the raw material silicon tetrachloride is joined in the reverse microemulsion system in second step;
The 4th step: after treating that reaction in the third step is carried out, the reverse microemulsion system in the third step is carried out breakdown of emulsion handle; With
The 5th step: the reaction product in dry the 4th step.
2. method according to claim 1 is characterized in that, after the 4th step, washs the step of the reaction product in the 4th step.
3. method according to claim 1; It is characterized in that the reverse microemulsion system of said NP system comprises NP-5-hexanaphthene-deionized water, NP-5-normal heptane-deionized water, NP-5-normal hexane-deionized water, NP-5-octane-deionized water or NP-5-Skellysolve A-deionized water.
4. method according to claim 1; It is characterized in that said TX-100 series reverse microemulsion system comprises TX-100-hexanaphthene-deionized water, TX-100-normal heptane-deionized water, TX-100-normal hexane-deionized water, TX-100-octane-deionized water, TX-100-Skellysolve A-deionized water.
5. method according to claim 1; It is characterized in that the reverse microemulsion system of said Span series and Tween comprises Span60+Tween60-hexanaphthene-deionized water, Span60+Tween60-normal heptane-deionized water, Span60+Tween60-normal hexane-deionized water, Span60+Tween60-octane-deionized water, Span60+Tween60-Skellysolve A-deionized water, Span60+Tween80-hexanaphthene-deionized water, Span60+Tween80-normal heptane-deionized water, Span60+Tween80-normal hexane-deionized water, Span60+Tween80-octane-deionized water, Span60+Tween80-Skellysolve A-deionized water, Span80+Tween60-hexanaphthene-deionized water, Span80+Tween60-normal heptane-deionized water, Span80+Tween60-normal hexane-deionized water, Span80+Tween60-octane-deionized water, Span80+Tween60-Skellysolve A-deionized water, Span80+Tween80-hexanaphthene-deionized water, Span80+Tween80-normal heptane-deionized water, Span80+Tween80-normal hexane-deionized water, Span80+Tween80-octane-deionized water or Span80+Tween80-Skellysolve A-deionized water.
6. method according to claim 1 is characterized in that, the microemulsified in said second step is treated to the said reverse microemulsion system that stirs.
7. method according to claim 1 is characterized in that, the breakdown of emulsion in said the 4th step is handled and is to use the mixing solutions of acetone and water to carry out breakdown of emulsion.
8. method according to claim 2 is characterized in that, the washing step in said second step is after the reaction product in the spinning third step, uses the absolute ethyl alcohol centrifuge washing.
9. method according to claim 1 is characterized in that, the drying step in said the 5th step is vacuum-drying, spraying drying, azeotropic distillation drying or flash distillation.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103880021A (en) * | 2014-04-02 | 2014-06-25 | 北京化工大学 | Method for preparing white carbon black in reverse micro-emulsion system |
| CN106629741A (en) * | 2015-10-30 | 2017-05-10 | 中石化石油工程技术服务有限公司 | Nanometer silica preparation method |
| CN107973301A (en) * | 2017-12-12 | 2018-05-01 | 河北科技大学 | One kind is based on T-shaped microreactor controllable preparation Nano-meter SiO_22Method |
| CN110523400A (en) * | 2018-05-25 | 2019-12-03 | 中科院大连化学物理研究所淮安化工新材料研究中心 | Microemulsion method synthesized silicon rubber chromatograph packing material |
| CN112194142A (en) * | 2019-07-08 | 2021-01-08 | 新疆硅基新材料创新中心有限公司 | Method for preparing high-purity spherical silicon dioxide and high-purity spherical silicon dioxide |
| CN113731415A (en) * | 2021-09-28 | 2021-12-03 | 江苏金聚合金材料有限公司 | Preparation method and application of ethylene glycol catalyst |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993086A (en) * | 2010-12-20 | 2011-03-30 | 纪志勇 | Preparation method of mono-disperse silicon dioxide micro-spheres |
-
2011
- 2011-05-24 CN CN201110135041.8A patent/CN102795630B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993086A (en) * | 2010-12-20 | 2011-03-30 | 纪志勇 | Preparation method of mono-disperse silicon dioxide micro-spheres |
Non-Patent Citations (2)
| Title |
|---|
| 张香兰 等: "四氯化硅为原料制备二氧化硅粉体的研究", 《有机硅材料》 * |
| 范艳玲 等: "硅酸乙酯为原料反相微乳液法制备纳米二氧化硅", 《化学工业与工程》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103880021A (en) * | 2014-04-02 | 2014-06-25 | 北京化工大学 | Method for preparing white carbon black in reverse micro-emulsion system |
| CN103880021B (en) * | 2014-04-02 | 2016-03-30 | 北京化工大学 | A kind of method preparing white carbon black in anti-microemulsion system |
| CN106629741A (en) * | 2015-10-30 | 2017-05-10 | 中石化石油工程技术服务有限公司 | Nanometer silica preparation method |
| CN107973301A (en) * | 2017-12-12 | 2018-05-01 | 河北科技大学 | One kind is based on T-shaped microreactor controllable preparation Nano-meter SiO_22Method |
| CN110523400A (en) * | 2018-05-25 | 2019-12-03 | 中科院大连化学物理研究所淮安化工新材料研究中心 | Microemulsion method synthesized silicon rubber chromatograph packing material |
| CN112194142A (en) * | 2019-07-08 | 2021-01-08 | 新疆硅基新材料创新中心有限公司 | Method for preparing high-purity spherical silicon dioxide and high-purity spherical silicon dioxide |
| CN112194142B (en) * | 2019-07-08 | 2023-06-30 | 新疆硅基新材料创新中心有限公司 | Method for preparing high-purity spherical silicon dioxide and high-purity spherical silicon dioxide |
| CN113731415A (en) * | 2021-09-28 | 2021-12-03 | 江苏金聚合金材料有限公司 | Preparation method and application of ethylene glycol catalyst |
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| CN102795630B (en) | 2015-01-28 |
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