CN115924920B - Preparation method of neutral silica sol - Google Patents
Preparation method of neutral silica sol Download PDFInfo
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- CN115924920B CN115924920B CN202310003356.XA CN202310003356A CN115924920B CN 115924920 B CN115924920 B CN 115924920B CN 202310003356 A CN202310003356 A CN 202310003356A CN 115924920 B CN115924920 B CN 115924920B
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- silica sol
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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 68
- 230000007935 neutral effect Effects 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011347 resin Substances 0.000 claims abstract description 35
- 229920005989 resin Polymers 0.000 claims abstract description 35
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 230000002378 acidificating effect Effects 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000003381 stabilizer Substances 0.000 claims abstract description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 13
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 230000008929 regeneration Effects 0.000 claims description 8
- 238000011069 regeneration method Methods 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- QNGQBCXQVIHJEM-UHFFFAOYSA-N 2-dodecyl-2-methyl-1,3,5,7,9,11-hexaoxa-2,4,6,8,10,12-hexasilacyclododecane Chemical compound CCCCCCCCCCCC[Si]1(C)O[SiH2]O[SiH2]O[SiH2]O[SiH2]O[SiH2]O1 QNGQBCXQVIHJEM-UHFFFAOYSA-N 0.000 claims description 6
- 229910021538 borax Inorganic materials 0.000 claims description 5
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 5
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 abstract description 10
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000377 silicon dioxide Substances 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 235000019353 potassium silicate Nutrition 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention belongs to the field of nano material preparation, and particularly relates to a preparation method of neutral silica sol. The preparation method is realized by the following steps: adding alkaline silica sol into the regenerated resin, starting stirring, and exchanging to obtain acidic silica sol; adding a stabilizer and ammonia water into the acidic silica sol, and heating and stirring to obtain neutral silica sol. In the preparation process, the space stability among the particles in the silica sol is increased by adding the stabilizer, the prepared silica sol has good stability, and the zata potential of the prepared silica sol is improved.
Description
Technical Field
The invention belongs to the field of nano material preparation, and particularly relates to a preparation method of neutral silica sol.
Background
The silica sol is a nano material with excellent performance, is a colloidal solution formed by uniformly dispersing amorphous silica particles in water or an organic solvent, and is an inorganic high polymer material with wider application. The center of the micelle of the silica sol is a micelle core, which is a compact polymer composed of thousands of molecules. The surface layer of the silica sol is covered by siloxy groups and hydroxyl groups, and the electrostatic interaction between particles plays an important role in stabilizing the colloidal solution. Currently, silica sols are mainly used in the fields of electronics industry, textile industry, paint, refractory materials, etc.
The preparation of neutral silica sol is always a research hot spot, in the prior art, the ion exchange method is mature, sodium ions and other cationic impurities in water glass are removed by taking water glass as a main raw material and using strong acid type cation exchange resin; however, the method has to strictly control the concentration of each reactant, and the stability is required to be improved; among other methods, such as elemental silicon stage dissolution methods, most of the particles formed by this method are non-spherical and cannot be controlled in shape effectively. Therefore, developing a preparation method that can control the reaction process and effectively control the particle shape is a problem to be solved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of neutral silica sol, which is simple and has strong controllability, can effectively control the shape and the size of particles, and has uniform size.
The technical scheme adopted by the invention for achieving the purpose is as follows:
the invention provides a preparation method of neutral silica sol, which comprises the following steps:
(1) Resin regeneration: soaking weak acid exchange resin in acid solution for a period of time, and cleaning the resin;
(2) Adding alkaline silica sol into the regenerated resin, starting stirring, and exchanging to obtain acidic silica sol;
(3) Adding a stabilizer and ammonia water into the acidic silica sol, and heating and stirring to obtain neutral silica sol.
Further, in the step (1), the acid solution is sulfuric acid solution with the mass concentration of 2-4%; the pH of the soaked resin is 5.0-6.0.
Further, in the step (2), the pH of the acidic silica sol is 5.0-7.0.
Further, in the step (3), the addition amount of the stabilizer accounts for 0.1-8% of the mass of the acidic silica sol; the addition amount of the ammonia water accounts for 1.5-2% of the mass of the acidic silica sol.
In the step (3), the stabilizer is composed of dodecyl-methyl-cyclohexasiloxane, propylene glycol and sodium borate according to a mass ratio of 1:0.5:0.2.
Further, in the step (3), the heating and stirring are performed by heating to 40-55 ℃ and stirring for 50min, and then heating to 80-90 ℃ and stirring for 2h.
The alkaline silica sol used in the invention has the particle size of 8-25 nanometers, the pH value of 8.5-10 and the silica content of 30-35 percent.
The beneficial effects of the invention are as follows:
(1) According to the preparation method provided by the invention, the prepared silica sol has uniform particle size and uniform dispersion;
(2) In the preparation process, the space stability among the particles in the silica sol is improved by adding the stabilizer, the prepared silica sol has good stability, the zata potential of the prepared silica sol is improved, and the heat stability is excellent.
Drawings
FIG. 1 is a transmission electron microscope image of the neutral silica sol prepared in example 1.
Detailed Description
The technical scheme of the invention is further explained and illustrated by specific examples.
Example 1
(1) Resin regeneration: soaking the weak acid exchange resin in 4% sulfuric acid for 60min, and cleaning the resin;
(2) Adding alkaline silica sol into the regenerated resin, starting stirring, and exchanging to obtain acidic silica sol;
(3) Adding 1% of stabilizer (composed of dodecyl methyl cyclohexasiloxane, propylene glycol and sodium borate according to the mass ratio of 1:0.5:0.2) and 2% of ammonia water into the acidic silica sol, firstly heating to 45 ℃ and stirring for 50min, then heating to 90 ℃ and stirring for 2h to obtain the neutral silica sol.
FIG. 1 is a transmission electron microscope image of a neutral silica sol, and it can be seen from the image that the prepared silica sol has uniform particles and good dispersibility; the pH value of the prepared neutral silica sol is 7-7.5.
Example 2
(1) Resin regeneration: soaking the weak acid exchange resin in 4% sulfuric acid for 60min, and cleaning the resin;
(2) Adding alkaline silica sol into the regenerated resin, starting stirring, and exchanging to obtain acidic silica sol;
(3) Adding 0.25% of stabilizer (composed of dodecyl methyl cyclohexasiloxane, propylene glycol and sodium borate according to the mass ratio of 1:0.5:0.2) and 1.5% of ammonia water into the acidic silica sol, firstly heating to 50 ℃, stirring for 50min, then heating to 90 ℃, and stirring for 2h to obtain the neutral silica sol.
Example 3
(1) Resin regeneration: soaking the weak acid exchange resin in 4% sulfuric acid for 60min, and cleaning the resin;
(2) Adding alkaline silica sol into the regenerated resin, starting stirring, and exchanging to obtain acidic silica sol;
(3) Adding 6% of stabilizer (composed of dodecyl methyl cyclohexasiloxane, propylene glycol and sodium borate according to the mass ratio of 1:0.5:0.2) and 2% of ammonia water into the acidic silica sol, firstly heating to 50 ℃, stirring for 50min, then heating to 90 ℃, and stirring for 2h to obtain the neutral silica sol.
Comparative example 1
(1) Resin regeneration: soaking the weak acid exchange resin in 4% sulfuric acid for 60min, and cleaning the resin;
(2) Adding alkaline silica sol into the regenerated resin, starting stirring, and exchanging to obtain acidic silica sol;
(3) Adding 1% of stabilizer dodecyl methyl cyclohexasiloxane and 2% of ammonia water into the acidic silica sol, firstly heating to 45 ℃ and stirring for 50min, then heating to 90 ℃ and stirring for 2h to obtain neutral silica sol.
Comparative example 2
(1) Resin regeneration: soaking the weak acid exchange resin in 4% sulfuric acid for 60min, and cleaning the resin;
(2) Adding alkaline silica sol into the regenerated resin, starting stirring, and exchanging to obtain acidic silica sol;
(3) 1% of stabilizer (the composition is the same as in example 1) is added into the acidic silica sol, and the acidic silica sol is stirred for 3 hours at the temperature of 90 ℃ to obtain the neutral silica sol.
Comparative example 3
(1) Resin regeneration: soaking the weak acid exchange resin in 4% sulfuric acid for 60min, and cleaning the resin;
(2) Adding alkaline silica sol into the regenerated resin, starting stirring, and exchanging to obtain acidic silica sol;
(3) Adding 2% ammonia water into the acidic silica sol, heating to 45 ℃ and stirring for 50min, heating to 90 ℃ and stirring for 2h to obtain neutral silica sol.
Effect examples
The initial alkaline silica sols used in examples and comparative examples had a Zata potential of-34 mv, and the neutral silica sols prepared in examples 1 to 3 and comparative examples 1 to 3 were examined for Zata potential by a Zata tester, and the specific results are shown in Table 1.
TABLE 1
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Zata potential | -18 | -20 | -23 | -24 | -26 | -27 |
(II) stability detection is carried out on the neutral silica sol prepared in the example 1 and the comparative examples 1-3, and the detection method is as follows: the measurement was carried out by heating, 50g of silica sol was weighed and placed in a clean container, then the container was capped and sealed and placed in an incubator at 40℃and 65℃and 70℃with no flow at 45℃being inclined as a gel point, and the whole gel time was recorded, and the specific results are shown in Table 2.
TABLE 2
Claims (5)
1. The preparation method of the neutral silica sol is characterized by comprising the following steps of:
(1) Resin regeneration: soaking weak acid exchange resin in acid solution for a period of time, and cleaning the resin;
(2) Adding alkaline silica sol into the regenerated resin, starting stirring, and exchanging to obtain acidic silica sol;
(3) Adding a stabilizer and ammonia water into the acidic silica sol, heating and stirring to obtain neutral silica sol, wherein the stabilizer consists of dodecyl-methyl-cyclohexasiloxane, propylene glycol and sodium borate according to a mass ratio of 1:0.5:0.2.
2. The method according to claim 1, wherein in the step (1), the acid solution is a sulfuric acid solution having a mass concentration of 2 to 4%; the pH of the soaked resin is 5.0-6.0.
3. The method according to claim 1, wherein in the step (2), the acidic silica sol has a pH of 5.0 to 7.0.
4. A method according to any one of claims 1 to 3, wherein in step (3), the stabilizer is added in an amount of 0.1 to 8% by mass of the acidic silica sol; the addition amount of the ammonia water accounts for 1.5-2% of the mass of the acidic silica sol.
5. The method according to claim 4, wherein in the step (3), the heating and stirring are performed by heating to 40-55deg.C for 50min, and then heating to 80-90deg.C for 2h.
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| CN202310003356.XA CN115924920B (en) | 2023-01-03 | 2023-01-03 | Preparation method of neutral silica sol |
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| CN115924920B true CN115924920B (en) | 2024-01-26 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644498A (en) * | 2004-12-16 | 2005-07-27 | 章浩龙 | Method for preparing stable silica sol |
| CN102391688A (en) * | 2011-08-23 | 2012-03-28 | 南通海迅天恒纳米科技有限公司 | Formulation type stabilizer of acid silica sol |
| CN107253726A (en) * | 2017-05-18 | 2017-10-17 | 江苏天恒纳米科技股份有限公司 | A kind of preparation technology of polymer modification Ludox |
| CN111017935A (en) * | 2019-12-18 | 2020-04-17 | 上海新安纳电子科技有限公司 | Preparation method of silica sol and application of silica sol in ceramic coating |
| CN113880095A (en) * | 2020-07-03 | 2022-01-04 | 青岛海湾精细化工有限公司 | Preparation method of acidic silica sol and acidic silica sol |
| CN113896204A (en) * | 2021-11-29 | 2022-01-07 | 苏州西丽卡电子材料有限公司 | Preparation method of ultra-high purity silica sol |
-
2023
- 2023-01-03 CN CN202310003356.XA patent/CN115924920B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1644498A (en) * | 2004-12-16 | 2005-07-27 | 章浩龙 | Method for preparing stable silica sol |
| CN102391688A (en) * | 2011-08-23 | 2012-03-28 | 南通海迅天恒纳米科技有限公司 | Formulation type stabilizer of acid silica sol |
| CN107253726A (en) * | 2017-05-18 | 2017-10-17 | 江苏天恒纳米科技股份有限公司 | A kind of preparation technology of polymer modification Ludox |
| CN111017935A (en) * | 2019-12-18 | 2020-04-17 | 上海新安纳电子科技有限公司 | Preparation method of silica sol and application of silica sol in ceramic coating |
| CN113880095A (en) * | 2020-07-03 | 2022-01-04 | 青岛海湾精细化工有限公司 | Preparation method of acidic silica sol and acidic silica sol |
| CN113896204A (en) * | 2021-11-29 | 2022-01-07 | 苏州西丽卡电子材料有限公司 | Preparation method of ultra-high purity silica sol |
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