CN106517221B - A kind of silica and the preparation method and application thereof with high dispersion stability - Google Patents
A kind of silica and the preparation method and application thereof with high dispersion stability Download PDFInfo
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- CN106517221B CN106517221B CN201610993128.1A CN201610993128A CN106517221B CN 106517221 B CN106517221 B CN 106517221B CN 201610993128 A CN201610993128 A CN 201610993128A CN 106517221 B CN106517221 B CN 106517221B
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- silica
- dispersion stability
- high dispersion
- microcrystalline cellulose
- sand milling
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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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Silicon Compounds (AREA)
- Colloid Chemistry (AREA)
- Paints Or Removers (AREA)
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Abstract
The silica surface modified method with high dispersion stability that the invention discloses a kind of, the step of preparation method are as follows: add a certain proportion of microcrystalline cellulose into the aqueous solution of silica, high speed is sanded, and then spray drying obtains modified silica flatting silica.Microcrystalline cellulose is added in the aqueous solution of silica in the present invention, carry out high speed sand milling, on the one hand reduce the partial size of silica and microcrystalline cellulose itself, on the other hand silica is made to be combined with each other well with microcrystalline cellulose, to guaranteeing that silica is well dispersed in water solution system, last spray-drying process can keep the pore structure of silica script, and no change has taken place.
Description
Technical field
The present invention relates to a kind of silica and the preparation method and application thereof, in particular to a kind of to have high dispersion stability
Silica and the preparation method and application thereof.
Background technique
Vapor phase method and the precipitation method are the important methods of current domestic manufacture nano silica, and vapor phase method prepares product purity
Height, dispersion degree is high, and particle carefully forms spherical shape, and surface hydroxyl is few, thus has excellent reinforcing property.But it is raw materials used expensive, if
Standby to require height, technology is complicated, limits application and popularization.
And the precipitation method have become domestic manufacture nano-silica since the requirement to raw material and equipment is low compared with vapor phase method
The main method of SiClx, but in current manufacturing process from the point of view of, there is also processing step is more, reaction is not easy to control, quality compared with
The defects of difference, technological parameter is unstable, and product dispersibility in subsequent applications is poor, cannot reach related request.
Precipitated silica occupies staple market at present, and increasing market part is occupied in all kinds of flatting silica specific gravity
Volume, but at present the country be mainly used in solvent type and UV type coating, most of silica products in water environment dispersibility compared with
Difference, and sinking speed is very fast, limits its application in water paint, the above problem is urgently to be resolved.
Summary of the invention
The present invention provides a kind of silica and the preparation method and application thereof with high dispersion stability, solves existing skill
Art silica product dispersibility in water environment is poor, and sinking speed is very fast, limits its application in water paint
Problem.
In order to achieve the above object, the present invention is achieved by the following technical solutions:
The present invention provides a kind of silica surface modified method with high dispersion stability, comprising the following steps:
(1) silica slurry is prepared；
(2) add microcrystalline cellulose: microcrystalline cellulose is added in the silica slurry that the step (1) is prepared, then
It is configured to lotion；
(3) it is sanded: the lotion in step (2) is sanded；
(4) be spray-dried: the slurry after step (3) are sanded is spray-dried, and be can be obtained and is stablized with high dispersive
The silica of property.
Preferably, the concentration that silica slurry is prepared in the step (1) is 1%-9%.
Preferably, the microcrystalline cellulose that the step (2) is added is 1%-15% relative to the amount of silica.
Preferably, it is sanded in the step (3) using zirconium ball.
Preferably, it is 0.1mm-2mm that zirconium bulb diameter, which is sanded,.
Preferably, the sand milling time of the step (3) is 30-120 minutes, and sand milling revolving speed is 4000-6000r/min, is made
Be sanded it is more uniform sufficiently, effect is good.
Preferably, the slurry after sand milling is done by spraying under 50-150r/min stirring condition in the step (4)
Dry, spray drying inlet temperature is 150-250 DEG C.
The present invention also provides it is a kind of by preparation method described above be prepared it is surface-modified have high dispersive it is steady
Qualitative silica.
The present invention also provides a kind of application of surface-modified silica with high dispersion stability described above,
Application of the surface-modified silica with high dispersion stability in aqueous systems.
The present invention for silica settled under the conditions of aqueous solvent it is too fast improve, mainly by silica with it is micro-
Interaction between crystalline cellulose, and reduce composite-grain diameter by being sanded to extend dispersion of the silica in aqueous systems
Time
Preferably: application of the surface-modified silica with high dispersion stability in water paint.
The advantages and beneficial effects of the present invention are: the present invention relates to a kind of silicon dioxide meters with high dispersion stability
Surface modification process, by adding a certain proportion of microcrystalline cellulose into the aqueous solution of silica, high speed is sanded, and is then done by spraying
It is dry to obtain modified silica flatting silica.Microcrystalline cellulose is added in the present invention in the aqueous solution of silica, carries out high speed sand
On the one hand mill reduces the partial size of silica and microcrystalline cellulose itself, on the other hand makes silica and microcrystalline cellulose very
Good is combined with each other, to guarantee that silica is well dispersed in water solution system, last spray-drying process can be kept
No change has taken place for the pore structure of silica script.
Present invention preparation has the silica simple process of high dispersion stability, raw materials used to be easy purchase in the market,
And it is cheap, environmental protection, solve prior art silica product in water environment dispersibility it is poor, and sinking speed compared with
Fastly, the problem of limiting its application in water paint, the silica prepared by the present invention with high dispersion stability can quilt
It is widely used in water paint.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other drawings based on these drawings.
Fig. 1 is that unmodified silica and the modified sample of embodiment 1-5 are made into certain density solution dispersion
Effect contrast figure.
Specific embodiment
With reference to the accompanying drawings and examples, further description of the specific embodiments of the present invention.Following embodiment is only
For clearly illustrating technical solution of the present invention, and not intended to limit the protection scope of the present invention.
The present invention provides a kind of silica surface modified method with high dispersion stability, comprising the following steps:
(1) silica slurry is prepared, the concentration for preparing silica slurry is 1%-9%；
(2) add microcrystalline cellulose: microcrystalline cellulose is added in the silica slurry that the step (1) is prepared, then
It is configured to lotion, the microcrystalline cellulose of addition is 1%-15% relative to the amount of silica；
(3) it is sanded: the lotion in step (2) being sanded using zirconium ball, sand milling zirconium bulb diameter is 0.1mm-2mm, when sand milling
Between be 30-120 minute, sand milling revolving speed be 4000-6000r/min；
(4) it is spray-dried: step (3) is done the slurry after sand milling by spraying under 50-150r/min stirring condition
Dry, spray drying inlet temperature is 150-250 DEG C, and the silica with high dispersion stability can be obtained.
Embodiment 1:
50g silica is added in the reactor, 0.5g (solid content) microcrystalline cellulose is then added, 500ml is added and goes
Ionized water stirs, and the zirconium ball of 0.1mm diameter is added in the lotion stirred evenly, using the speed of 5000r/min
It is sanded, it is 1 hour that the time, which is sanded, the liquid after sand milling is spray-dried under 100r/min stirring condition, temperature
It is 200 DEG C, product is made into certain density solution, after standing 1 day, it is as shown in Figure 1 to overturn 20 results.
Embodiment 2:
30g silica is added in the reactor, 1.0g (solid content) microcrystalline cellulose is then added, 500ml is added and goes
Ionized water stirs, and the zirconium ball of 0.7mm diameter is added in the lotion stirred evenly, using the speed of 5000r/min
It is sanded, the sand milling time is 30min, the liquid after sand milling is spray-dried under 100r/min stirring condition, temperature
It is 150 DEG C, product is made into certain density solution, after standing 1 day, it is as shown in Figure 1 to overturn 20 results.
Embodiment 3:
45g silica is added in the reactor, 0.5g (solid content) microcrystalline cellulose is then added, 500ml is added and goes
Ionized water stirs, and the zirconium ball of 0.1mm diameter is added in the lotion stirred evenly, using the speed of 5000r/min
It is sanded, the sand milling time is 50min, the liquid after sand milling is spray-dried under 100r/min stirring condition, temperature
It is 180 DEG C, product is made into certain density solution, after standing 1 day, it is as shown in Figure 1 to overturn 20 results.
Embodiment 4:
10g silica is added in the reactor, 1.0g (solid content) microcrystalline cellulose is then added, 500ml is added and goes
Ionized water stirs, and the zirconium ball of 1.2mm diameter is added in the lotion stirred evenly, using the speed of 5000r/min
It is sanded, the sand milling time is 90min, the liquid after sand milling is spray-dried under 100r/min stirring condition, temperature
It is 240 DEG C, product is made into certain density solution, after standing 1 day, it is as shown in Figure 1 to overturn 20 results.
Embodiment 5:
In the reactor be added 5g silica, then be added 0.8g (solid content) microcrystalline cellulose, be added 500ml go from
Sub- water stirs, and the zirconium ball of 2mm diameter is added in the lotion stirred evenly, is carried out using the speed of 5000r/min
It is sanded, the sand milling time is 120min, the liquid after sand milling is spray-dried under 100r/min stirring condition, temperature is
210 DEG C, product is made into certain density solution, after standing 1 day, it is as shown in Figure 1 to overturn 20 results.
Fig. 1 is by the left-to-right production for being followed successively by unmodified embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5
Product are made into certain density solution, overturn 20 comparative result figures, as seen from Figure 1, non-modified titanium dioxide after standing 1 day
The clarification of silicon solution, poor dispersion, the product of embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 after modified
It is made into the white muddy shape of certain density solution, good dispersion.The present invention settles under the conditions of aqueous solvent for silica
It is too fast to improve, the main interaction by between silica and microcrystalline cellulose, and reduce composite-grain diameter to prolong
Jitter time of the long silica in aqueous systems.
The present invention is by compound with silica after addition microcrystalline cellulose, and making product, jitter time lengthens in water；Into
Row is sanded, and reduces silica and the compound grain diameter of microcrystalline cellulose, it is steady to further increase the dispersion of product in water
It is qualitative；Spray drying keeps the pore structure of silica script.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of silica surface modified method with high dispersion stability, it is characterised in that: the following steps are included:
(1) silica slurry is prepared；
(2) add microcrystalline cellulose: microcrystalline cellulose is added in the silica slurry that the step (1) is prepared, then prepares
At lotion, the microcrystalline cellulose is 1%-15% relative to the amount of silica；
(3) it is sanded: the lotion in step (2) is sanded；
(4) be spray-dried: the slurry after step (3) are sanded is spray-dried, and can be obtained with high dispersion stability
Silica；
The sand milling time of the step (3) is 30-120 minutes, and sand milling revolving speed is 4000-6000r/min.
2. a kind of silica surface modified method with high dispersion stability according to claim 1, feature exist
In the concentration for preparing silica slurry in the step (1) is 1%-9%.
3. a kind of silica surface modified method with high dispersion stability according to claim 1, feature exist
In using zirconium ball sand milling in the step (3).
4. a kind of silica surface modified method with high dispersion stability according to claim 3, feature exist
In sand milling zirconium bulb diameter is 0.1mm-2mm.
5. a kind of silica surface modified method with high dispersion stability according to claim 1, feature exist
In, the slurry after sand milling is spray-dried under 50-150r/min stirring condition in the step (4), be spray-dried into
Mouth temperature is 150-250 DEG C.
6. it is a kind of by preparation method of any of claims 1-5 be prepared it is surface-modified have high dispersive it is steady
Qualitative silica.
7. the application of the surface-modified silica with high dispersion stability according to claim 6, feature exist
In: application of the surface-modified silica with high dispersion stability in aqueous systems.
8. the application of the surface-modified silica with high dispersion stability according to claim 7, feature exist
In: application of the surface-modified silica with high dispersion stability in water paint.
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| CN201610993128.1A CN106517221B (en) | 2016-11-11 | 2016-11-11 | A kind of silica and the preparation method and application thereof with high dispersion stability |
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| CN201610993128.1A CN106517221B (en) | 2016-11-11 | 2016-11-11 | A kind of silica and the preparation method and application thereof with high dispersion stability |
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| CN106517221B true CN106517221B (en) | 2019-04-05 |
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| CN111282698A (en) * | 2020-02-21 | 2020-06-16 | 江苏海格新材料有限公司 | Preparation method of electronic-grade superfine silica micropowder for copper-clad plate |
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| DE10337198A1 (en) * | 2003-08-13 | 2005-03-17 | Degussa Ag | Carriers based on granules produced from pyrogenically prepared silicon dioxides |
| DE102006039273A1 (en) * | 2006-08-22 | 2008-02-28 | Evonik Degussa Gmbh | Pyrogenic silica for use as adjuvant in pharmaceutical and cosmetic compositions |
| CN101723388A (en) * | 2008-10-15 | 2010-06-09 | 赢创德固赛有限责任公司 | Silica granules prepared on basis of pyrolysis and preparation method and app {} lication thereof |
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Effective date of registration: 20191220 Address after: 336000 Yichun Economic and Technological Development Zone Yiwei Road, Yichun City, Jiangxi Province Patentee after: Jiangxi Baohong Nano Technology Co., Ltd Address before: 334202 sulfur chemical industry park, Dexing Tuen Shangrao eco industrial park, Jiangxi, China Patentee before: Jiangxi Dehong New Material Co., Ltd. |
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