CN106145125A - A kind of titanium modified silicasol and preparation method thereof - Google Patents
A kind of titanium modified silicasol and preparation method thereof Download PDFInfo
- Publication number
- CN106145125A CN106145125A CN201610496508.4A CN201610496508A CN106145125A CN 106145125 A CN106145125 A CN 106145125A CN 201610496508 A CN201610496508 A CN 201610496508A CN 106145125 A CN106145125 A CN 106145125A
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- CN
- China
- Prior art keywords
- titanium
- modified silicasol
- preparation
- ludox
- chelating agent
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- 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
- C01B33/146—After-treatment of sols
- C01B33/148—Concentration; Drying; Dehydration; Stabilisation; Purification
- C01B33/1485—Stabilisation, e.g. prevention of gelling; Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Catalysts (AREA)
Abstract
A kind of titanium modified silicasol of the present invention and preparation method thereof, its formula includes: silica flour 15 35g；NaOH 0‑2g；Titanium salt 5 50g；Chelating agent 10 250g；H2O 50 200g, will can effectively reduce silica sol particle surface hydroxyl (OH) number, stops the reunion of sol particles to be reunited, obtains the modified silicasol of " stablizing ".Compared with prior art, the advantage that the present invention is the most prominent is that technique is simple, and modified effect is good.
Description
Technical field
The present invention relates to a kind of titanium modified silicasol and preparation method thereof.
Background technology
Its internal siloxane bond (-Si-O-Si-) of Ludox, covers at micelle surface silica alcohol radical (-SiOH) and hydroxyl
Metal ion in (-OH) and solution has collectively constituted diffused electric doublet layer structure, therefore, exists undersaturated on Ludox surface
Residual bond and different keys and the hydroxyl of state, the structure of Ludox as shown in Figure 1.
Owing to Ludox surface exists hydroxyl, adjacent hydroxyl groups is each other with hydrogen bonded, the hydrogen atom electropositive of isolated hydroxyl
By force, easily adsorbing with electronegative atom, with hydroxy-containing compounds generation dehydration condensation, therefore, it is non-that Ludox is in thermodynamics
Stable state, it is easy to reunite together, form larger-size aggregate, and after Ludox agglomerates into gel, can not
By heating, add other reagent or other conditions are allowed to again become colloidal sol.
The most how to prepare the Ludox of " the stablizing " of even particle size distribution, be a focal issue of application, so far
Till the present, although have a lot of surface modification of silica technique, but all there is respective drawback.As: silane coupled
Although the modified method of agent is simple, but expensive due to silane coupler, unsuitable large-scale production；Enter with polymer
The method of row modification of graft, owing to there is homopolymerization, percent grafting is relatively low, and the mechanical property of material is produced certain shadow
Ring；The shortcoming of esterification reaction method is that ester group is susceptible to hydrolysis, and its heat stability is poor.
Summary of the invention
Instant invention overcomes shortcoming of the prior art, it is provided that a kind of titanium modified silicasol and preparation method thereof, its system
Standby technique is simple, Ludox stable system, and the particle diameter of Ludox is controlled between 200-800nm.
In order to solve above-mentioned technical problem, the present invention is achieved by the following technical solutions:
A kind of titanium modified silicasol, its formula includes: silica flour 15-35g；NaOH 0-2g；Titanium salt 5-50g；Chelating agent 10-
250g；H2O 50-200g。
Further, described titanium salt is butyl titanate, tetraisopropyl titanate, titanium sulfate any one.
Further, any one during described chelating agent is hydrogen peroxide, ethanol, diethanolamine.
The preparation method of a kind of titanium modified silicasol, comprises the following steps:
(1) press formula, water adds silica flour, stirs；
(2) addition NaOH is as catalyst, stirring, is placed in constant temperature bath insulation, prepares unmodified Ludox,
(3) titanium salt and chelating agent are pressed formula hydrolysis, obtains Ti (OH)4；
(4) titanium salt hydrolyzate Ti (OH) that will prepare in (3)4It is slowly added to unmodified Ludox described in (2)
In, stirring, and be incubated；
(5) stopping heating, stop stirring, reaction system is down to room temperature naturally；
(6) filter, separate, i.e. can get the Ludox that titanium is modified.
Further, in step (2), the temperature of constant temperature bath controls between 50-90 DEG C.
Further, in step (2), the time of constant temperature controls between 3-9h.
Further, in step (2), the ratio (amount of material) of catalyst n aOH and silica flour controls between 1:10 25.
Further, in step (3), the ratio (amount of material) of titanium salt and chelating agent controls between 1:1 30.
Further, the temperature in step (4) controls between 50-90 DEG C.
Compared with prior art, the invention has the beneficial effects as follows:
A kind of titanium modified silicasol of the present invention and preparation method thereof will can effectively reduce silica sol particle surface hydroxyl
Base (-OH) number, stops the reunion of sol particles to be reunited, obtains the modified silicasol of " stablizing ".Compared with prior art, this
The most prominent bright advantage is that technique is simple, and modified effect is good.
Accompanying drawing explanation
Accompanying drawing is used for providing a further understanding of the present invention, is used for together with embodiments of the present invention explaining the present invention,
It is not intended that limitation of the present invention, in the accompanying drawings:
Fig. 1 is the structural representation of Ludox.
Detailed description of the invention
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are illustrated, it will be appreciated that preferred reality described herein
Execute example be merely to illustrate and explain the present invention, be not intended to limit the present invention.
The present invention utilizes the hydrolyzate Ti (OH) of titanium salt4The hydroxyl (-OH) of (-OH) and nano-silica surface send out
Raw condensation reaction, is modified nano-silica surface, and reaction principle is as follows:
By above-mentioned dehydration condensation, will can effectively reduce silica sol particle surface hydroxyl (-OH) number, stop
The reunion of sol particles is reunited, and obtains the modified silicasol of " stablizing ".
Embodiment 1
(1) in 200g water, add 25g silica flour, stir；
(2) 0.4g NaOH catalyst is added, stirring, it is placed in insulation 3h in constant temperature bath (90 DEG C), prepares unmodified
Ludox；
(3) 50g butyl titanate and 35g diethanolamine are added to the water, hydrolysis, obtain Ti (OH)4；
(4) the titanium salt hydrolyzate prepared in (3) is slowly added in the Ludox system described in (2), stirring, and
20min it is incubated at 60 DEG C；
(5) stopping heating, stop stirring, reaction system is down to room temperature naturally；
(6) filter, separate, i.e. can get the Ludox that titanium is modified.
Using laser particle analyzer S3500 to test this Ludox sample, result shows: the granularity of this Ludox exists
About 507nm, and distribution is the most uniform.
Embodiment 2
(1) in 200g water, add 25g silica flour, stir；
(2) 0.2g NaOH catalyst is added, stirring, it is placed in insulation 6h in constant temperature bath (80 DEG C), prepares unmodified
Ludox；
(3) 24g titanium sulfate is added the H of 217g2O2In, hydrolysis, obtain Ti (OH)4；
(4) the titanium salt hydrolyzate prepared in (3) is slowly added in the Ludox system described in (2), stirring, and
20min it is incubated at 60 DEG C；
(5) stopping heating, stop stirring, reaction system is down to room temperature naturally；
(6) filter, separate, i.e. can get the Ludox that titanium is modified.
Using laser particle analyzer S3500 to test this Ludox sample, result shows: the granularity of this Ludox exists
About 275nm, and distribution is the most uniform.
Embodiment 3
(1) in 200g water, add 25g silica flour, stir；
(2) 0.3g NaOH catalyst is added, stirring, it is placed in insulation 9h in constant temperature bath (60 DEG C), prepares unmodified
Ludox；
(3) 50g tetraisopropyl titanate and 25g ethanol are added to the water, hydrolysis, obtain Ti (OH)4；
(4) the titanium salt hydrolyzate prepared in (3) is slowly added in the Ludox system described in (2), stirring, and
25min it is incubated at 60 DEG C；
(5) stopping heating, stop stirring, reaction system is down to room temperature naturally；
(6) filter, separate, i.e. can get the Ludox that titanium is modified.
Using laser particle analyzer S3500 to test this Ludox sample, result shows: the granularity of this Ludox exists
About 689nm, and distribution is the most uniform.
Finally it is noted that these are only the preferred embodiments of the present invention, it is not limited to the present invention, although
Being described in detail the present invention with reference to embodiment, for a person skilled in the art, it still can be to aforementioned
Technical scheme described in each embodiment is modified, or wherein portion of techniques feature carries out equivalent, but all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included in the protection of the present invention
Within the scope of.
Claims (9)
1. a titanium modified silicasol, it is characterised in that its formula includes: silica flour 15-35g；NaOH 0-2g；Titanium salt 5-50g；
Chelating agent 10-250g；H2O 50-200g。
A kind of titanium modified silicasol, it is characterised in that described titanium salt is butyl titanate, metatitanic acid
Four isopropyl esters, titanium sulfate any one.
A kind of titanium modified silicasol, it is characterised in that described chelating agent be hydrogen peroxide, ethanol,
Any one in diethanolamine.
The preparation method of a kind of titanium modified silicasol, it is characterised in that comprise the following steps:
(1) press formula, water adds silica flour, stirs；
(2) addition NaOH is as catalyst, stirring, is placed in constant temperature bath insulation, prepares unmodified Ludox,
(3) titanium salt and chelating agent are pressed formula hydrolysis, obtains Ti (OH)4；
(4) titanium salt hydrolyzate Ti (OH) that will prepare in (3)4It is slowly added to described in (2) in unmodified Ludox, stirs
Mix, and be incubated；
(5) stopping heating, stop stirring, reaction system is down to room temperature naturally；
(6) filter, separate, i.e. can get the Ludox that titanium is modified.
The preparation method of a kind of titanium modified silicasol, it is characterised in that constant temperature bath in step (2)
Temperature control between 50-90 DEG C.
The preparation method of a kind of titanium modified silicasol, it is characterised in that constant temperature in step (2)
Time controls between 3-9h.
The preparation method of a kind of titanium modified silicasol, it is characterised in that catalyst in step (2)
The ratio (amount of material) of NaOH and silica flour controls between 1:10 25.
A kind of preparation method of titanium modified silicasol, it is characterised in that in step (3) titanium salt with
The ratio (amount of material) of chelating agent controls between 1:1 30.
The preparation method of a kind of titanium modified silicasol, it is characterised in that the temperature in step (4)
Control between 50-90 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610496508.4A CN106145125B (en) | 2016-06-27 | 2016-06-27 | A kind of titanium modified silicasol and preparation method thereof |
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| CN201610496508.4A CN106145125B (en) | 2016-06-27 | 2016-06-27 | A kind of titanium modified silicasol and preparation method thereof |
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| CN106145125A true CN106145125A (en) | 2016-11-23 |
| CN106145125B CN106145125B (en) | 2018-05-01 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110105490A (en) * | 2019-06-04 | 2019-08-09 | 中科广化（重庆）新材料研究院有限公司 | Preparation and application containing reactive Ti-Si sol and its modification (methyl) acrylic ester polymerization lotion |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003026417A (en) * | 2001-07-13 | 2003-01-29 | Catalysts & Chem Ind Co Ltd | Method of manufacturing silica sol and silica-base multiple oxide sol |
| CN104588568A (en) * | 2014-11-21 | 2015-05-06 | 广东惠和硅制品有限公司 | Preparation method of aluminum modified silica sol |
| CN104785276A (en) * | 2015-03-16 | 2015-07-22 | 中科合成油技术有限公司 | Fischer-Tropsch synthesis catalyst prepared by using composite sol as silicon source, and preparation method and application thereof |
-
2016
- 2016-06-27 CN CN201610496508.4A patent/CN106145125B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003026417A (en) * | 2001-07-13 | 2003-01-29 | Catalysts & Chem Ind Co Ltd | Method of manufacturing silica sol and silica-base multiple oxide sol |
| CN104588568A (en) * | 2014-11-21 | 2015-05-06 | 广东惠和硅制品有限公司 | Preparation method of aluminum modified silica sol |
| CN104785276A (en) * | 2015-03-16 | 2015-07-22 | 中科合成油技术有限公司 | Fischer-Tropsch synthesis catalyst prepared by using composite sol as silicon source, and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 田华等: ""单质硅溶解法制备硅溶胶的研究"", 《辽宁化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110105490A (en) * | 2019-06-04 | 2019-08-09 | 中科广化（重庆）新材料研究院有限公司 | Preparation and application containing reactive Ti-Si sol and its modification (methyl) acrylic ester polymerization lotion |
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| CN106145125B (en) | 2018-05-01 |
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