CN115924923A - High-purity spherical silica sol and preparation method thereof - Google Patents
High-purity spherical silica sol and preparation method thereof 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 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000003756 stirring Methods 0.000 claims abstract description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- -1 silicate ester Chemical class 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 28
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 9
- 239000012498 ultrapure water Substances 0.000 claims description 9
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 229910021645 metal ion Inorganic materials 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 238000005341 cation exchange Methods 0.000 claims description 3
- 150000007529 inorganic bases Chemical class 0.000 claims description 3
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 claims description 2
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims description 2
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 40
- 238000009826 distribution Methods 0.000 abstract description 18
- 239000000377 silicon dioxide Substances 0.000 description 19
- 239000000243 solution Substances 0.000 description 13
- 235000012239 silicon dioxide Nutrition 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 9
- 238000011056 performance test Methods 0.000 description 8
- 239000002994 raw material Substances 0.000 description 5
- 230000035040 seed growth Effects 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 3
- 238000004100 electronic packaging Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000011863 silicon-based powder Substances 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
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- 239000000463 material Substances 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
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- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
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- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
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- 239000008393 encapsulating agent Substances 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
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Abstract
The invention relates to a high-purity spherical silica sol and a preparation method thereof, which relate to the field of silica microspheres and comprise the following steps: step 1: preparing the following component A and component B according to the weight percentage: the component A consists of 3 to 27 weight percent of purified silicate ester and 1.5 to 12 weight percent of low molecular alcohol; the component B consists of 12 to 45 weight percent of water, 40 to 80 weight percent of low molecular alcohol and 0.05 to 5 weight percent of catalyst; step 2: stirring and atomizing the component A, continuously stirring the component B, adding the atomized component A into the component B, and continuously stirring at constant temperature until the high-purity spherical silica sol is obtained. Provides a high-purity spherical silica sol which has low cost, large grain diameter and sharp grain size distribution and is applied to industry.
Description
Technical Field
The invention relates to the field of silica microspheres, in particular to a high-purity spherical silica sol and a preparation method thereof.
Background
The silicon dioxide microspheres as an important inorganic raw material have multiple unique performances of high temperature resistance, high strength, high toughness, small thermal expansion coefficient, low dielectric constant, good stability and the like, and are widely applied to the fields of catalysis, pigments, chromatographic analysis, semiconductors and the like. Particularly, the silicon micro powder can reduce the thermal expansion coefficient of the plastic package material, reduce the internal stress, improve the insulation strength, reduce the dielectric constant, increase the strength of the plastic package material, resist flame, meet the environmental protection requirement and prevent moisture absorption in electronic packaging. This makes high purity silica microspheres an alternative to making epoxy-type encapsulants (BMCs).
At present, the method for preparing the silicon dioxide microspheres at home and abroad mainly comprises a silicon powder hydrolysis method, a seed growth method, an ion exchange method and a sol-gel method. Patent CN1699165A uses silicon powder as a raw material, and reacts with water under the catalytic action of alkali to obtain a reaction solution, the reaction solution is filtered by a filter press, a filtrate is a silica sol finished product, filter residue obtained by filtering the reaction solution is washed and filtered by water to obtain a silica sol finished product, and the filter residue obtained by filtering the reaction solution contains silicon powder in the preparation process by the method, so that the actual recycling rate is low, and adverse effects are generated on the environment. The patent US15219533 uses monodisperse spherical silica sol with the particle size of 20nm-30nm as seed crystal, seed crystal and active silicic acid are dripped into a reaction system by adopting a seed growth method, the liquid level is kept constant, meanwhile, inorganic base is dripped until the pH value of the system is 9.5-10, the system is kept alkaline, and the silica sol is obtained after heat preservation reaction for a period of time and cooling. However, the silica sol obtained by this method has a wide particle size distribution, and it is difficult to prepare a monodisperse silica sol. Patent CN106276927a adds silicon halide into fluorine-containing ion solution to produce silicon dioxide precipitate and silicon dioxide suspension, and then filters and washes to obtain silicon dioxide filter cake, and dries to obtain powder, but the purity of silica sol obtained by this method is low, and ionic impurities are difficult to remove. In patent CN105283413A, alkoxysilane is continuously or indirectly added to a mixture of water and an organic solvent mixed in a certain proportion, after a reaction at a temperature above 60 ℃ for a period of time, an organic base compound is added thereto, heated to the boiling point of the solvent, and cooled to room temperature, to obtain silica sol. The silicate ester used as the raw material for preparing the silica sol by the method is not purified, the purity is not high, and the high-purity silica sol is difficult to prepare industrially; CN104003409A discloses a method for preparing controllable monodisperse spherical large-particle-size nano-silica, which is based on a sol-gel method, wherein tetraethoxysilane is hydrolyzed to obtain ortho-silicic acid, and the silica is obtained by dehydration condensation through a method of intermittently supplementing tetraethoxysilane.
In view of the above, a method for preparing a high purity spherical silica sol having a large particle size, a sharp particle size distribution, and uniform dispersion, which is industrially applicable at low cost, is provided to overcome the above technical problems.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-purity spherical silica sol and a preparation method thereof. Aims to provide a high-purity spherical silica sol which is applied to industry and has low cost, large grain diameter and sharp grain size distribution.
In order to solve the above technical problems, a first object of the present invention is to provide a method for preparing a high purity spherical silica sol, comprising the steps of:
step 1: preparing the following component A and component B according to the weight percentage:
the component A consists of purified silicate ester with the weight percentage of 3 to 27 percent and low molecular alcohol with the weight percentage of 1.5 to 12 percent; the component B consists of 12 to 45 weight percent of water, 40 to 80 weight percent of low molecular alcohol and 0.05 to 5 weight percent of catalyst;
and 2, step: stirring and atomizing the component A, continuously stirring the component B, adding the atomized component A into the component B, and continuously stirring at constant temperature until the high-purity spherical silica sol is obtained.
The invention has the beneficial effects that: the preparation method comprises the steps of mixing purified silicate ester with a small part of low-molecular alcohol to form a component A, then placing the rest low-molecular alcohol, water and a catalyst in a reaction container according to a certain proportion to form a component B, placing the component A in a liquid storage tank, atomizing the component A into fine droplets at a certain flow rate and pressure, adding the fine droplets into the reactor, and simultaneously mixing and stirring to enable the component A and the component B to be capable of instantly colliding and reacting, so that the generated silica sol has narrower particle size distribution, the whole process is simple and convenient to operate, and the prepared silica sol has large particle size, sharp particle size distribution, uniform dispersion and low metal ion content. The preparation method has the advantages of simple and feasible process, environmental protection and high efficiency, and the obtained silica sol has high purity, large particle size and uniform particle size distribution.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, in the step 1, the component A consists of 7 to 9 weight percent of purified silicate and 1.6 to 2 weight percent of low molecular alcohol; the component B consists of 12.5 to 14 weight percent of water, 70 to 80 weight percent of low molecular alcohol and 1 to 4 weight percent of catalyst.
Further, the specific purification process of the silicate ester in the step 1 is to firstly carry out rectification to remove organic impurities, and then to exchange and remove dissolved inorganic metal impurity ions by adopting a cation exchange column to obtain the high-purity silicate ester.
The beneficial effect of adopting the further scheme is that: the purified ethyl silicate raw material can be used for preparing the silica sol with higher purity, and the total amount of metal ions of the silica sol is less than 5ppm.
Further, the silicate in step 1 is one or a mixture of two or more of methyl silicate, ethyl silicate, propyl silicate and butyl silicate, preferably ethyl silicate.
Further, the water in step 1 is distilled water, deionized water or ultrapure water, preferably ultrapure water.
Further, the low molecular alcohol in the step 1 is alcohol with 1-4 carbon atoms; the catalyst in the step 1 is inorganic base.
Further, the low molecular alcohol is a mixture of one or more than two of methanol, ethanol, propanol, isopropanol and n-butanol, preferably ethanol; the catalyst is one or a mixture of more than two of sodium hydroxide, potassium hydroxide and ammonia water, and preferably the ammonia water.
Further, step 2 specifically comprises: at 25-80 deg.c, the component A may be heated in water bath to stir and atomize while stirring the component B, and the atomized component A is added into the component B and stirred at constant temperature of 25-80 deg.c to obtain high purity spherical silica sol.
Further, the stirring of the component a and the component B in the step 2 is performed by using a flap paddle stirrer (shanghai zhiwei electric appliance ltd, D2010W); the stirring speed of the continuous stirring in the step 2 is 200-800r/min, and the stirring time of the continuous stirring in the step 2 is 1-4h.
The second purpose is to provide a high-purity spherical silica sol, which is prepared by the preparation method of the high-purity spherical silica sol, wherein the particle size of the high-purity spherical silica sol is 80-500nm, and the total amount of metal ions is less than 5ppm.
The preparation method of the high-purity spherical silica sol with large particle size and sharp particle size distribution provided by the invention has the advantages of simple and feasible preparation process, environmental protection and high efficiency, and the obtained silica sol has high purity, large particle size and uniform particle size distribution. The high-purity spherical silica sol with large particle size and sharp particle size distribution for electronic packaging of integrated circuits has good application prospect.
Drawings
FIG. 1 is TEM images of silica sols prepared under different conditions according to the present invention, wherein FIGS. a-h are TEM images of silica sols S1-S8 prepared in examples 1-8, respectively.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Example 1:
the preparation method of the high-purity spherical silica sol comprises the following steps:
(1) Preparing the following component A and component B according to the weight percentage:
the component A comprises: 7.45 percent of ethyl silicate
Ethanol 1.65%
And B component: 12.9% of ultrapure water
75.5 percent of ethanol
2.5 percent of ammonia water
(2) And (3) carrying out water bath at 30 ℃, atomizing the component A while continuously stirring the component B of the solution at the speed of 460r/min, adding the atomized component A into the stirred component B, and continuously stirring for 3 hours at the constant temperature of 30 ℃ at the speed of 460r/min after the addition is finished to obtain the silica sol S1. The results of the silica sol performance test are shown in table 1 and fig. 1, respectively.
Example 2:
the preparation method of the high-purity spherical silica sol comprises the following steps:
(1) Preparing the following component A and component B according to the weight percentage:
the component A comprises: 7.45 percent of ethyl silicate
Ethanol 1.65%
And B component: 12.9% of ultrapure water
75.5 percent of ethanol
2.5 percent of ammonia water
(2) And (3) carrying out water bath at 40 ℃, atomizing the component A while continuously stirring the solution B at the speed of 460r/min, adding the atomized component A into the stirred component B, and continuously stirring for 3 hours at the constant temperature of 40 ℃ at the speed of 460r/min after the addition is finished to obtain the silica sol S2. The silica sol performance test results are shown in table 1 and fig. 1, respectively.
Example 3:
this example was substantially the same in composition and procedure as examples 1 and 2, except that the water bath temperature in step (2) in example 3 was 50 ℃ to obtain silica sol S3. The silica sol performance test results are shown in table 1 and fig. 1, respectively.
Example 4:
this example was substantially the same in composition and procedure as examples 1, 2 and 3 except that the water bath temperature in step (2) of example 3 was 60 ℃ to obtain silica sol S4. The silica sol performance test results are shown in table 1 and fig. 1, respectively.
Example 5:
the preparation method of the high-purity spherical silica sol comprises the following steps:
(1) Preparing the following component A and component B according to the weight percentage:
and (2) component A: ethyl silicate 7.62%
Ethanol 1.69%
And B component: 13.19 percent of ultrapure water
75.5 percent of ethanol
2.0 percent of ammonia water
(2) And (3) carrying out water bath at 30 ℃, atomizing the component A while continuously stirring the solution B at the speed of 460r/min, adding the atomized component A into the stirred component B, and continuously stirring for 3 hours at the constant temperature of 30 ℃ at the speed of 460r/min after the addition is finished to obtain the silica sol S5. The results of the silica sol performance test are shown in table 1 and fig. 1, respectively.
Example 6:
the preparation method of the high-purity spherical silica sol comprises the following steps:
(1) Preparing the following component A and component B according to the weight percentage:
and (2) component A: ethyl silicate 7.28%
Ethanol 1.61%
And B component: 12.61% of ultrapure water
75.5 percent of ethanol
Ammonia water 3.0%
(2) And (3) carrying out water bath at 30 ℃, atomizing the component A while continuously stirring the solution B at the speed of 460r/min, adding the atomized component A into the stirred component B, and continuously stirring for 3 hours at the constant temperature of 30 ℃ at the speed of 460r/min after the addition is finished to obtain the silica sol S6. The silica sol performance test results are shown in table 1 and fig. 1, respectively.
Example 7: comparative example
The embodiment is a preparation method for preparing high-purity spherical silica sol by adopting a seed growth method, which comprises the following steps:
(1) Preparing the following component A and component B according to the weight percentage:
the component A comprises: ethyl silicate 7.62%
Ethanol 1.69%
And B component: 13.19 percent of ultrapure water
51.1 percent of ethanol
24.43 percent of silicon dioxide seed liquid
2.0 percent of ammonia water
(2) And (3) carrying out water bath at 30 ℃, continuously stirring the solution B at the speed of 460r/min, simultaneously atomizing the component A, adding the atomized component A into the component B containing the silicon dioxide seed solution in stirring, and continuously stirring for 3 hours at the constant temperature of 30 ℃ at the speed of 460r/min after the addition is finished to obtain the silica sol S7. The results of the silica sol performance test are shown in table 1 and fig. 1, respectively.
Example 8: comparative example
The embodiment is a preparation method for preparing high-purity spherical silica sol by adopting a seed growth method, and the preparation method comprises the following steps:
(1) Preparing the following component A and component B according to the weight percentage:
the component A comprises: ethyl silicate 7.28%
Ethanol 1.61%
And B component: 12.61% of ultrapure water
51.1 percent of ethanol
24.61 percent of silicon dioxide seed liquid
3.0 percent of ammonia water
(2) And (3) carrying out water bath at 30 ℃, continuously stirring the solution B at the speed of 460r/min, simultaneously atomizing the component A, adding the atomized component A into the component B containing the silicon dioxide seed solution in stirring, and continuously stirring for 3 hours at the constant temperature of 30 ℃ at the speed of 460r/min after the addition is finished to obtain the silica sol S8. The results of the silica sol performance test are shown in table 1 and fig. 1, respectively.
TABLE 1 EXAMPLES 1-6 preparation of silica sols having a particle size table obtained under different conditions
The mechanism of the invention is that the purified silicate reacts with water in low molecular alcohol solvent under the action of catalyst, and the particle size and particle size distribution of the final product, namely the silica sol, are controlled by controlling the adding mode and flow of the silicate, the shape and speed of a stirrer, the reaction temperature and the content of the catalyst. Wherein, the silicate ester is subjected to rectification and cation exchange column to remove organic and inorganic impurities in the raw materials respectively, thereby improving the purity of the silicate ester. The mixture of silicate ester and low molecular alcohol is added into a container in an atomization mode, and after the mixture is stirred by a flap paddle stirrer, the component A and the component B are instantaneously collided to react, so that spheres are more uniformly grown, and the generated silicon dioxide has narrower particle size distribution.
As is clear from the data in Table 1, the silica sols S1 to S6 obtained in examples 1 to 6 by the sol-gel process of the present invention had particle diameters of 443nm, 162.2nm, 128.8nm, 80.3nm, 242.4nm and 282.5nm, respectively, and their PDI values were all less than 0.07, indicating that the obtained silica sols had sharp particle size distributions. The TEM' S of a to f in FIG. 1 show that the resulting silica sols S1 to S6 are all smooth spheres and do not agglomerate. In contrast, the particle sizes of the silica sols S7 and S8 obtained in examples 7 to 8 by the seed growth method were 340.0nm and 184.1nm, respectively, and the particle size distributions were 0.1669 and 0.417, respectively, indicating that the particle size distributions were not uniform, as can be further confirmed from the TEM images of g to h in FIG. 1.
The silica sol S1 sample prepared in example 1 was analyzed by inductively coupled plasma emission spectrometer model PQ9000 from analytikjena, germany. Firstly preparing a standard solution, then measuring the energy released by the sample when the sample returns to a stable state from an excited state, and then comparing the energy with the specific spectral lines and intensities of different elements in the prepared standard solution so as to analyze the types and the contents of the elements in the sample. The content of each metal ion in the silica sol S1 is shown in table 2. As can be seen from the data in Table 2, the total metal ion content in the prepared sol was 3.59. Mu.g/ml.
TABLE 2 table of contents of respective ions in silica sol S1
In conclusion, the preparation method of the high-purity spherical silica sol with large particle size and sharp particle size distribution provided by the invention has the advantages of simple and feasible preparation process, environmental protection and high efficiency, and the obtained silica sol has high purity, large particle size and uniform particle size distribution. Therefore, the obtained high-purity spherical silica sol used for integrated circuit electronic packaging has a good application prospect, and has large particle size and sharp particle size distribution.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A preparation method of high-purity spherical silica sol is characterized by comprising the following steps:
step 1: preparing the following component A and component B according to the weight percentage:
the component A consists of purified silicate ester with the weight percentage of 3 to 27 percent and low molecular alcohol with the weight percentage of 1.5 to 12 percent; the component B consists of 12 to 45 weight percent of water, 40 to 80 weight percent of low molecular alcohol and 0.05 to 5 weight percent of catalyst;
step 2: stirring and atomizing the component A, continuously stirring the component B, adding the atomized component A into the component B, and continuously stirring at constant temperature until the high-purity spherical silica sol is obtained.
2. The method for preparing a high purity spherical silica sol according to claim 1, wherein in the step 1, the component A is composed of 7 to 9% by weight of purified silicate and 1.6 to 2% by weight of low molecular alcohol; the component B consists of 12.5 to 14 weight percent of water, 70 to 80 weight percent of low molecular alcohol and 1 to 4 weight percent of catalyst.
3. The method for preparing a high purity spherical silica sol according to claim 1 or 2, wherein the specific purification process of the silicate in step 1 is rectification followed by exchange and removal using a cation exchange column to obtain the high purity silicate.
4. The method for preparing a high purity spherical silica sol according to claim 1, wherein the silicate used in the step 1 is a mixture of one or more of methyl silicate, ethyl silicate, propyl silicate and butyl silicate.
5. The method for preparing a highly pure spherical silica sol according to claim 1, wherein the water used in step 1 is distilled water, deionized water or ultrapure water.
6. The method for preparing a highly pure spherical silica sol according to claim 1, wherein the low molecular alcohol in the step 1 is an alcohol having 1 to 4 carbon atoms; the catalyst in the step 1 is inorganic base.
7. The method for preparing a high-purity spherical silica sol according to claim 6, wherein the low-molecular alcohol is a mixture of one or more of methanol, ethanol, propanol, isopropanol and n-butanol; the catalyst is one or a mixture of more than two of sodium hydroxide, potassium hydroxide and ammonia water.
8. The method for preparing a high-purity spherical silica sol according to claim 1, wherein the step 2 specifically comprises: stirring and atomizing the component A at 25-80 ℃, continuously stirring the component B, adding the atomized component A into the component B, and continuously stirring at a constant temperature of 25-80 ℃ until high-purity spherical silica sol is obtained.
9. The method for preparing a high purity spherical silica sol according to claim 1, wherein the stirring of the A-component and the B-component in the step 2 is performed by a flap paddle type stirrer; the stirring speed of the continuous stirring in the step 2 is 200-800r/min, and the stirring time of the continuous stirring in the step 2 is 1-4h.
10. A high purity spherical silica sol according to any one of claims 1 to 9, which has a particle size of 80 to 500nm and a total amount of metal ions of less than 5ppm.
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| CN107934975A (en) * | 2017-12-14 | 2018-04-20 | 青岛大学 | A kind of preparation method of nano silicon dioxide |
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| CN107934975A (en) * | 2017-12-14 | 2018-04-20 | 青岛大学 | A kind of preparation method of nano silicon dioxide |
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| Title |
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| 于遵宏: "《化工过程开发》", 31 December 1996, 华东理工大学出版社, pages: 292 - 293 * |
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