CN106744997B - Adulterate the preparation method of the acidic silicasol of heterogeneous element - Google Patents
Adulterate the preparation method of the acidic silicasol of heterogeneous element Download PDFInfo
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 230000002378 acidificating effect Effects 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000010703 silicon Substances 0.000 claims abstract description 18
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 13
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 12
- 239000012456 homogeneous solution Substances 0.000 claims abstract description 12
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims abstract description 5
- BWOAAAYNOWWMHL-UHFFFAOYSA-K trichloroyttrium;hydrate Chemical compound O.[Cl-].[Cl-].[Cl-].[Y+3] BWOAAAYNOWWMHL-UHFFFAOYSA-K 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 150000004760 silicates Chemical class 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 37
- 239000000243 solution Substances 0.000 description 21
- 239000002245 particle Substances 0.000 description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 229910052782 aluminium Inorganic materials 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000004411 aluminium Substances 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 5
- 239000000443 aerosol Substances 0.000 description 5
- 235000013339 cereals Nutrition 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005498 polishing Methods 0.000 description 5
- 229910052726 zirconium Inorganic materials 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 125000005909 ethyl alcohol group Chemical group 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 229910052746 lanthanum Inorganic materials 0.000 description 4
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 238000010183 spectrum analysis Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910052727 yttrium Inorganic materials 0.000 description 4
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- 238000005352 clarification Methods 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910009523 YCl3 Inorganic materials 0.000 description 2
- 239000006061 abrasive grain Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- NZSLBYVEIXCMBT-UHFFFAOYSA-N chloro hypochlorite;zirconium Chemical compound [Zr].ClOCl NZSLBYVEIXCMBT-UHFFFAOYSA-N 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000011978 dissolution method Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- PCMOZDDGXKIOLL-UHFFFAOYSA-K yttrium chloride Chemical compound [Cl-].[Cl-].[Cl-].[Y+3] PCMOZDDGXKIOLL-UHFFFAOYSA-K 0.000 description 2
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- WZFUQSJFWNHZHM-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)N1CC2=C(CC1)NN=N2 WZFUQSJFWNHZHM-UHFFFAOYSA-N 0.000 description 1
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 241000219000 Populus Species 0.000 description 1
- 229910006251 ZrOCl2.8H2O Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 description 1
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- -1 metallurgy Substances 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/145—Preparation of hydroorganosols, organosols or dispersions in an organic medium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of the acidic silicasol of doping heterogeneous element, and using chloride hydrate yttrium, eight water of zirconium oxychloride or six water of aluminium chloride as heterogeneous element, positive quanmethyl silicate is that silicon source follows the steps below successively using hydrochloric acid solution as catalyst：It is 2.8~3.2 that hydrochloric acid solution, which is added in solvent to pH value, is stirring uniformly to obtain transparent clear solution；Stirring to heterogeneous element is added into transparent clear solution in heterogeneous element to dissolve, obtains homogeneous solution；At a temperature of stirring condition, 20~80 DEG C, positive quanmethyl silicate is added dropwise in homogeneous solution, time for adding is 10~20 minutes；Subsequent continuous 2.5~3.5h of insulated and stirred is added dropwise, the acidic silicasol of heterogeneous element must be adulterated.
Description
Technical field
The present invention relates to a kind of preparation methods of the acidic silicasol of doping heterogeneous element, and in particular to a kind of to be urged with hydrochloric acid
Turn to the preparation method that sol gel reaction prepares the acidic silicasol of doping heterogeneous element.
Background technology
Ludox also known as silica sol or silica hydrosol, are amorphous SiO2Colloidal particles be dispersed in water
The colloidal solution of formation.Ludox have stronger adsorptivity, larger specific surface area, excellent insulating properties and caking property and
Good reactivity, to the mankind and it is environmentally friendly the features such as, in coating, binder, metallurgy, essence casting, refractory material, weaving, system
The fields such as medicine have broad application prospects, therefore, also more and more extensive to the requirement of product category both at home and abroad.Nineteen sixty-eight,
Stober and Fink etc. using ammonia-catalyzed tetraethyl orthosilicate hydrolyze it is final obtain monodisperse Ludox, this method find with
Come, has numerous scholars and it is furtherd investigate.But the more alkaline particle absorption of acid monodisperse nano silicon dioxide particle
Can be more superior, also have wide practical use.Wang Shaoming etc. thinks that the stability of pH and Ludox has direct relation, Jia Guangyao etc.
Mentioning collosol and gel dynamics can be taking human as control.Perhaps read it is strong etc. think, only work as SiO2When the grain size of particle is relatively small, silicon
The stability of colloidal sol is just by electrolytic salinity large effect, with SiO2Grain size increases, and electrolytic salinity is molten to silicon
The stability influence of glue weakens.When the salt content in Ludox is reduced to certain value, electrolytic salinity is to a certain extent
The major influence factors for preparing acidic silicasol will not be constituted.Yang Jing etc. is in the type, reaction temperature, reaction for having studied catalyst
The impact effect of electrolytes is analyzed when influence of the factors such as time, additive to Ludox performance.
At present both at home and abroad in the doping Ludox of patent and paper report the element that adulterates mainly have boron, phosphorus, aluminium, magnesium, iron,
Four kinds of elements such as lanthanum, wherein aluminium, magnesium, iron, lanthanum metallic elements adulterate the production that Ludox are mainly used in polishing fluid, use these
On the one hand the Ludox polishing device of metallic element doping improves removal rate, on the other hand reduce the coarse of device surface
Degree.The instruction of poplar in 2014 at et al. silica flour, aluminium powder reacted with sodium hydroxide using metal simple-substance dissolution method synthesized a kind of aluminium and change
Property Ludox has simultaneously applied for patent.The thunder of Shanghai University in 2015 is red et al. combine coprecipitation and ion-exchange by magnesium, iron,
Lanthanum mixes by a certain percentage to be synthesized polishing fluid and has successfully applied for 3 patents in Ludox, wherein three kinds of magnesium, iron, lanthanum elements can
To improve the chemical action of abrasive grain, and the removal rate of polishing speed and material can be improved in the chemical action of abrasive grain.
Although metallic element doping Ludox prepared by above method all has good performance, all exist centainly
The energy consumption of defect, metal simple-substance dissolution method is big, and reaction condition is harsher, and the production procedure of ion-exchange is complicated, production effect
Rate is low, and the purity of modification sol is insufficient.
Invention content
The technical problem to be solved in the present invention is to provide a kind of preparation methods of the acidic silicasol of doping heterogeneous element, should
The Ludox that method prepares doping heterogeneous element under acid condition improves Ludox to reduce the use cost of Ludox
Dispersibility and stability.
In order to solve the above technical problem, the present invention provides a kind of preparation sides of the acidic silicasol of doping heterogeneous element
Method, with chloride hydrate yttrium (YCl3·6H2O), eight water (ZrOCl of zirconium oxychloride2.8H2) or six water (AlCl of aluminium chloride O3.6H2O) it is
Heterogeneous element (that is, for source of heterogeneous element), positive quanmethyl silicate are that silicon source carries out successively using hydrochloric acid solution as catalyst
Following steps：
1) it is that 2.8~3.2 (preferable pH value is, at room temperature, hydrochloric acid solution to be added in the solvent of 10ml to pH value
3), uniform stirring (mixing time is about 5~15min), obtains transparent clear solution；
2), by (1~1.1) × 10-3The heterogeneous element of mol be added into the transparent clear solution obtained by step 1) stir to
Heterogeneous element dissolves, and obtains homogeneous solution；
The step 2) is also to carry out at room temperature；
3), at a temperature of stirring condition, 20~80 DEG C (preferably 20~60 DEG C), by the positive silicic acid tetramethyls of 1.0~2.0mL
Ester be added dropwise to (with buret be slowly added to) in homogeneous solution obtained by step 2), time for adding is 10~20 minutes；It is added dropwise
After continue (20~80 DEG C) 2.5~3.5h of stirring (be, for example, 3h) of heat preservation, the acidic silicasol of heterogeneous element must be adulterated.
Remarks explanation：The acidic silicasol of the doping heterogeneous element is sealed in container in 5~20 DEG C of preservations；Sealing is anti-
Only Ludox is by external environmental, and 5~20 DEG C to be that temperature is excessively high the reason of preservation make Ludox that gel easily occur to go bad.
The improvement of the preparation method of the acidic silicasol of doping heterogeneous element as the present invention：The solvent is deionization
The volume ratio of the mixture of water and absolute ethyl alcohol, deionized water and absolute ethyl alcohol is 1：0.1~4.0.
The improvement of the preparation method of the acidic silicasol of doping heterogeneous element as the present invention：The hydrochloric acid solution it is dense
Degree is 0.1mol/L.
The acidic silicasol being prepared using the method for the present invention, the grain size of Ludox is in 50~500nm, size uniformity,
Heterogeneous element is evenly distributed.The content of heterogeneous element can be 10%~20% (for the molar content of opposite Ludox).
The method of the present invention is to add positive silicon in mixed solution to hydrochloric acid, containing heterogeneous element salt deionized water and ethyl alcohol
Sour four methyl esters.Present invention employs the acidic silicasols that sol-gal process prepares doping heterogeneous element, by adjusting concentration of hydrochloric acid
And addition, the addition of the positive quanmethyl silicate of silicon source, heterogeneous element source yttrium chloride, zirconium oxychloride or aluminium chloride addition and
The ratio of water and ethyl alcohol obtains the uniform of the grain size of required Ludox, the pattern of Ludox and heterogeneous element in solvent
Distribution.
The present invention prepares three kinds of aluminium, zirconium, yttrium metallic elements using sol-gel method and adulterates Ludox, is catalyzed by improving
The modes such as agent addition and alcohol water ratio, control presoma drop rate, use positive quanmethyl silicate for presoma, instead of positive silicic acid
Tetra-ethyl ester, further improves the solid concentration of Ludox, and with easy to operate, and reaction condition requires low, and energy consumption is few, production
A variety of advantages such as gained colloidal sol purity is high, and metallic element and Ludox are tightly combined, are evenly distributed, and aerosol particle size is adjustable, not only
There is good application prospect in polishing industry, and can be used for preparing the raw material of composite aerogel.
In conclusion the present invention provides a kind of acidic silicasol materials of doping heterogeneous element, and can be with Effective Regulation
The grain size and pattern of Ludox, the Ludox of preparation can effectively widen the application field of Ludox, reduce Ludox
Application cost improves the dispersibility and stability of Ludox.
Specific implementation mode
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This.
(stirring of step 1~step 3) carries out under the rotating speed of 200~300r/min in following embodiment.
Embodiment 1, a kind of preparation method of the acidic silicasol of doping heterogeneous element, with chloride hydrate yttrium (YCl3·
6H2O) it is heterogeneous element source, positive quanmethyl silicate is silicon source, and the hydrochloric acid solution of a concentration of 0.1mol/L is catalyst；Successively
It follows the steps below：
1), using the mixed solution of 9mL water and 1mL absolute ethyl alcohols as solvent；
At room temperature, by hydrochloric acid solution be added into above-mentioned solvent until pH value be 3, stir 10min after, obtain transparent clarification
Solution；
2), by 1.055 × 10-3Mol (about 0.32g) chloride hydrate yttrium is added into the transparent clear solution obtained by step 1)
Stirring obtains homogeneous solution to dissolving；
3), at a temperature of stirring condition, 60 DEG C, the positive quanmethyl silicates of 1.0mL are slowly added to buret to step
2) in the homogeneous solution obtained by, time for adding is 10 minutes (that is, drop rate about 0.1mL/min), and subsequent continuation of insurance is added dropwise
Temperature stirring 3h, must adulterate the acidic silicasol of heterogeneous element.
In 5~20 DEG C of preservations after the acidic silicasol sealing of the doping heterogeneous element.
Laser particle analyzer test result shows silicon, yttrium colloidal sol even particle size distribution, concentrates near 500nm.Transmission electron microscope
EDS energy spectrum analysis shows that silicon, yttrium are evenly distributed in sample.The silica sol gel time is about 30 days, and stability is good.
That is, the aerosol particle size is 500nm, yttrium is evenly distributed, and stability is good.
Embodiment 2, a kind of preparation method of the acidic silicasol of doping heterogeneous element, with six water of aluminium chloride
(AlCl3.6H2O) it is heterogeneous element source, positive quanmethyl silicate (TMOS) is silicon source, and the hydrochloric acid solution of a concentration of 0.1mol/L is
Catalyst；It follows the steps below successively：
1), using the mixed solution of 5mL water and 5mL absolute ethyl alcohols as solvent,
At room temperature, by above-mentioned hydrochloric acid solution be added into solvent until pH value be 3, stir 10min after, obtain transparent clarification
Solution；
2), by 1.077 × 10-3Six water of mol aluminium chloride, which is added into the transparent clear solution obtained by step 1), to be stirred to molten
Solution, obtains homogeneous solution；
3), at a temperature of stirring condition, 50 DEG C, the positive quanmethyl silicates of 1.5mL are slowly added to buret to step
2) in the homogeneous solution obtained by, time for adding is 15 minutes (that is, drop rate about 0.1mL/min), and subsequent continuation of insurance is added dropwise
Temperature stirring 3h, must adulterate the acidic silicasol of heterogeneous element.
In 5~20 DEG C of preservations after the acidic silicasol sealing of the doping heterogeneous element.
Laser particle analyzer test result shows silicon, Aluminum sol even particle size distribution, concentrates near 300nm.Transmission electron microscope
EDS energy spectrum analysis shows that silicon, aluminium element are evenly distributed in sample.The silica sol gel time is about 30 days, and stability is good.
Embodiment 3, a kind of preparation method of the acidic silicasol of doping heterogeneous element, with eight water of zirconium oxychloride
(ZrOCl2.8H2O) it is heterogeneous element source, positive quanmethyl silicate is silicon source, and the hydrochloric acid solution of a concentration of 0.1mol/L is catalysis
Agent；It follows the steps below successively：
1), using the mixed solution of 2mL water and 8mL absolute ethyl alcohols as solvent；
At room temperature, by hydrochloric acid solution be added into above-mentioned solvent until pH value be 3, stir 10min after, obtain transparent clarification
Solution；
2), by 1.055 × 10-3Eight water of mol zirconium oxychlorides be added into the transparent clear solution obtained by step 1) stir to
Dissolving, obtains homogeneous solution；
3), at a temperature of stirring condition, 20 DEG C, the positive quanmethyl silicates of 2.0mL are slowly added to step 2) with buret
In the homogeneous solution of gained, time for adding is 20 minutes (rate about 0.1mL/min), and subsequent continuous insulated and stirred 3h is added dropwise,
The acidic silicasol of heterogeneous element must be adulterated.
In 5~20 DEG C of preservations after the acidic silicasol sealing of the doping heterogeneous element.
Laser particle analyzer test result shows silicon, zirconium colloidal sol even particle size distribution, concentrates near 150nm.Transmission electron microscope
EDS energy spectrum analysis shows that silicon, zr element are evenly distributed in sample.The silica sol gel time is about 30 days, and stability is good.
Solvent in 3 step 1) of embodiment is changed to 10mL absolute ethyl alcohols by comparative example 1, remaining is equal to embodiment 3, most
Whole methyl orthosilicate can not hydrolyze, and no silica sol particle occurs.
Comparative example 2, by the mole of eight water of zirconium oxychloride in 3 step 2) of embodiment by 1.055 × 10-3Mol makes 0.3 into ×
10-3mol；Remaining is equal to embodiment 3.
Transmission electron microscope EDS energy spectrum analysis shows that silicon, zr element are unevenly distributed in sample, and zr element is significantly built up.Silicon is molten
Glue grain shape is irregular, and testing graininess result shows that silica sol granule is obviously uneven.
Comparative example 3, the tetraethyl orthosilicate that the positive quanmethyl silicate of 2.0ml in embodiment 3 is made into 2.0ml, remaining etc.
It is same as embodiment 3.Acquired results are：The aerosol particle size is 800nm, and zirconium is evenly distributed, and stability is slightly not so good as embodiment 3.
Comparative example 4-1, by " be added hydrochloric acid solution " in 3 step 1) of embodiment until pH value is 3 to make into until pH value is
4, remaining is equal to embodiment 3.Acquired results are：The aerosol particle size is 700nm, and zirconium is evenly distributed, and stability is slightly not so good as to implement
Example 3.
Comparative example 4-2, by " be added hydrochloric acid solution " in 3 step 1) of embodiment until pH value is 3 to make into until pH value is
2, remaining is equal to embodiment 3.Acquired results are：The aerosol particle size is 800nm, and zirconium is evenly distributed, and stability is slightly not so good as to implement
Example 3.
Finally, it should also be noted that it is listed above be only the present invention several specific embodiments.Obviously, this hair
Bright to be not limited to above example, acceptable there are many deformations.Those skilled in the art can be from present disclosure
All deformations for directly exporting or associating, are considered as protection scope of the present invention.
Claims (2)
1. the preparation method of the acidic silicasol of heterogeneous element is adulterated, it is characterized in that：With chloride hydrate yttrium, eight water of zirconium oxychloride or
Six water of aluminium chloride is heterogeneous element, and positive quanmethyl silicate is that silicon source follows the steps below successively using hydrochloric acid solution as catalyst：
1) it is 2.8~3.2, at room temperature, hydrochloric acid solution to be added in the solvent of 10ml to pH value, and uniform stirring obtains
Bright clear solution；
The solvent is the mixture of deionized water and absolute ethyl alcohol, and the volume ratio of deionized water and absolute ethyl alcohol is 1：0.1~
4.0；
2), by (1~1.1) × 10-3The heterogeneous element of mol, which is added into the transparent clear solution obtained by step 1), to be stirred to heterogeneous
Element dissolves, and obtains homogeneous solution；
3), at a temperature of stirring condition, 20~80 DEG C, the positive quanmethyl silicates of 1.0~2.0mL are added dropwise to obtained by step 2)
In homogeneous solution, time for adding is 10~20 minutes；Subsequent continuous 2.5~3.5h of insulated and stirred is added dropwise, heterogeneous member must be adulterated
The acidic silicasol of element.
2. the preparation method of the acidic silicasol of doping heterogeneous element according to claim 1, it is characterised in that：
A concentration of 0.1mol/L of the hydrochloric acid solution.
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