CN108751204A - A kind of preparation method of submicron silicon dioxide dispersion liquid - Google Patents
A kind of preparation method of submicron silicon dioxide dispersion liquid Download PDFInfo
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- CN108751204A CN108751204A CN201810454019.1A CN201810454019A CN108751204A CN 108751204 A CN108751204 A CN 108751204A CN 201810454019 A CN201810454019 A CN 201810454019A CN 108751204 A CN108751204 A CN 108751204A
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- dispersion liquid
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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
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- 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
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Abstract
The present invention is a kind of preparation method of submicron silicon dioxide dispersion liquid, filtrate and filter cake are obtained by primary grinding and centrifugal classification, by the step both obtained granularity close to sub-micron high solids content dispersion liquid, the purity of silica in dispersion liquid is in turn ensured simultaneously, again by D50=0.7-0.8 μm of filtrate fine gtinding, dispersant, modifying agent, anti-settling agent, mould inhibitor are sequentially added, the good sub-micron titanium dioxide method dispersion liquid of high solids content, good dispersion, stability is obtained.Present invention process is simple, at low cost, highly filled, high-purity, good dispersion, stability are good, not only it had produced submicron silicon dioxide but also had solved the problems, such as that submicron silica powder dispersibility, product can be widely used for the fields such as water paint, Aqueous Adhesives, polishing.
Description
Technical field
The present invention relates to non-metal ore advanced processing technical area, especially a kind of preparation of submicron silicon dioxide dispersion liquid
Method.
Background technology
The scratch resistance of coating is very important index such as automobile finish, furniture lacquer, floor paint etc. in certain fields.?
The silica filler that high rigidity is added in coating is to improve paint film modulus, to improve the common of scratch resistance and wear resistance
Method.But some undesirable influences can be then brought on the performance of paint film using conventional micron particles, it such as reduces gloss, increase
Add the flexibility etc. of the transparency and film of mist shadow, reduction varnish.But the use of suitable sub-micron filler is not in these
Problem.Because（1）The gloss of paint film and surface it is coarse related, grain size is smaller, and roughness is smaller, and gloss is higher；（2）Film
Mist shadow and the particle on film surface layer, particle index of refraction difference and the quantity of particle it is related.The grain size of particle is smaller, refractive power
The difference of rate is smaller（The index of refraction of usual resin is 1.5 or so, and the index of refraction of crystalline silica is 1.54, and the two ten taps
Closely）, particle content is lower, and mist shadow is smaller；（3）The transparency of film and the particle grain size contained by film, particle index of refraction and tree
The difference of the index of refraction of fat and the quantity of particle are related, and the grain size of particle is smaller, and the difference of index of refraction is smaller, and particle content is lower,
Transparency is better.
Submicron silicon dioxide dispersibility, granularity and purity influence application performance most important.
In existing patent：The patent of patent No. CN 103627215 passes through using crystal quartz sand or vitreous silica as raw material
Micron silicon powder is made in dry grinding, then reuses sand mill wet grinding to granularity to submicron order, is obtained by press filtration
Sub-micron silicon powder filter cake.
For the patent of patent No. CN103466645 using micron silica as raw material, water is decentralized medium, first passes through sand mill
D50=1.5 μm are ground to, D50=500nm is then ground to by sand mill again, are finally ground to nano-silica by sand mill
SiClx.
For the patent of patent No. CN104693849 using gas phase silica flour as raw material, deionized water is decentralized medium, is added six partially
Silica dispersions are made in sodium phosphate, the high-speed stirred dispersion of acetic acid elder generation, then sand mill grinding, are then adjusted and are disperseed with ammonium hydroxide again
The PH of liquid has obtained silica dispersions to neutrality.
The patent of patent No. CN1675128 is using pyrogenic silica as raw material, to be dissolved with polyvalent cation compound
For decentralized medium, preservative is added and obtains average secondary particle grain size < 200nm, the aqueous titanium dioxide that solid content 10-60% stablizes
Silicon dispersion liquid.
The patent of patent No. CN1678525 is using silicon-metal mix powder as raw material, after being handled using acid, is prepared into solid
The dispersion liquid of content 10-70%, 200 nanometers of mean aggregate diameter <.
For the patent of patent No. CN105567193 using micro- silicon as raw material, distilled water is decentralized medium, addition surface capping agents,
Polyanion dispersant, stabilizer, PH conditioning agents are prepared into solid content 30-60%, the dispersion of average grain diameter < 200nm silica
Liquid.
The patented product of patent CN 103627215 is sub-micron filter cake, and when use needs ultrasonic wave to be disperseed, simultaneously
The handicraft product is raw material dry grinding to micron order using quartz, then is sanded to submicron order, product purity is not high.
Micron silica is directly ground to nanometer grade silica needs by patent CN103466645 by sand mill
The time of grinding is long, and grinding efficiency is low, process of lapping induces one, and impurity is more, and purity is relatively low, in addition, solid contents≤35%, Gu
Body object content is relatively low, and the application of product is also restrained.
Patent CN105567193, CN1675128, CN1678525 are using chemically synthesized nano silicon dioxide as raw material
It being prepared, raw material prepares complexity, and technique is not easy to control, and processing cost is higher, further, since raw material specific surface area is larger,
Needing to be added a large amount of auxiliary agents could be fully dispersed, and auxiliary agent is affected to properties of product, and products application is also restrained.
For patent CN105567193 using micro- silicon as raw material, technique is big with this process variations, and it is more that raw material contains impurity, application
It is limited in scope.
Invention content
The technical problem to be solved by the present invention is in view of the problems of the existing technology, provide a kind of simple for process, production
Product solid content is high, purity is high, the preparation method of good dispersion submicron silicon dioxide dispersion liquid.
The technical problem to be solved by the present invention is to what is realized by technical solution below, the present invention is a kind of sub-micro
The preparation method of rice silica dispersions, its main feature is that：Its step are as follows：
（1）Primary grinding：Progress primary in ball mill is added in crystal quartz sand or tekite sand, silicon ball, deionized water to grind
Mill.
（2）Centrifugal classification：Slurry after grinding is obtained into filtrate and filter cake by sedimentation centrifugal classification.
（3）Fine gtinding：Sedimentation centrifugal classification is obtained into filtrate addition sand mill and is ground to D50=0.7-0.8 μm, successively
Dispersant, modifying agent, anti-settling agent, antimildew disinfectant is added and continues to be ground to granularity to sub-micron.
Wherein filter cake can be used instead of quartz sand as feedstock circulation.
In the preparation method of submicron silicon dioxide dispersion liquid of the present invention：Step（1）The liner of middle ball mill is
Polyurethane or silica, mill are situated between for quartzy silicon ball.
In the preparation method of submicron silicon dioxide dispersion liquid of the present invention：Step（1）Middle quartz sand, deionization
Water, silicon ball mass ratio be 1:0.5:2-1:1:4, it is ground to -5.5 μm of slurry granularity D50=3.5 μm.
In the preparation method of submicron silicon dioxide dispersion liquid of the present invention：Step（2）It is middle to use sedimentation centrifuge
Carry out sedimentation centrifugal classification, maximum separation factor >=946.
In the preparation method of submicron silicon dioxide dispersion liquid of the present invention：Step（2）Middle centrifugal sedimentation is classified
The filtrate solid contents 35%-55% arrived, -2.0 μm of granularity D50=1.0 μm.
In the preparation method of submicron silicon dioxide dispersion liquid of the present invention：Step（3）Middle dispersant is polypropylene
Sour sodium, additive amount are the 0.5%-2.0% of slurry weight；The modifying agent is in silane coupling agent KBM603, KBM903, KBE903
One or more of water-soluble modified doses, additive amount is the 0.2%-1.0% of slurry weight.
In the preparation method of submicron silicon dioxide dispersion liquid of the present invention：Step（3）Middle anti-settling agent is that grain size is
The aerosil of 10 nm -50nm, additive amount are the 1%-3% of slurry weight；The antimildew disinfectant is anti-for Kathon CG anti-corrosion
Mould dose, additive amount is slurry weight 0.2%-0.6%
In the preparation method of submicron silicon dioxide dispersion liquid of the present invention：Step（3）Described in sand mill liner be poly-
Urethane, silicon carbide or zirconium oxide, it is zirconium oxide or silicon nitride, a diameter of 0.2 ㎜ -0.8 ㎜ of mill Jie that mill, which is situated between,.
In the preparation method of submicron silicon dioxide dispersion liquid of the present invention：Step（3）In be finely ground to slurry
D50=0.1-0.6 μm of granularity, D100≤1.0 μm, purity >=98.0% of silica after drying.
The preparation method of submicron silica powder dispersion liquid described in any of the above described one dispersion liquid product obtained exists
Water paint, Aqueous Adhesives, polishing liquid for metal surface, aqueous polyurethane varnish, water soluble acrylic acid varnish, water-base epoxy are clear
The anti scuffing for improving paint film in paint, aqueous UV varnish, improves the purposes of hardness of paint film.
Dispersion liquid shelf life of products is 6 months.
The present invention is obtained by primary grinding and centrifugal classification compared with filtrate and filter cake, and it is close both to have obtained granularity by the step
The high solids content dispersion liquid of sub-micron, while in turn ensuring the purity of silica in dispersion liquid, it sequentially adds dispersant, change
Property agent, anti-settling agent, mould inhibitor carry out fine gtinding, obtain the good submicron silicon dioxide of high solids content, good dispersion, stability
Dispersion liquid.
Compared with prior art, present invention process is simple, at low cost, highly filled, high-purity, good dispersion, stabilization
Property it is good, not only produced submicron silicon dioxide but solve the problems, such as submicron silica powder dispersibility, product can be extensive
For fields such as water paint, Aqueous Adhesives, polishings.
Specific implementation mode
The specific technical solution of the present invention described further below, in order to which those skilled in the art is further understood that
The present invention, without constituting the limitation to its right.
Embodiment 1, a kind of preparation method of submicron silicon dioxide dispersion liquid, its step are as follows：
（1）Primary grinding：Progress primary in ball mill is added in crystal quartz sand or tekite sand, silicon ball, deionized water to grind
Mill, is ground to -5.5 μm of slurry granularity D50=3.5 μm, wherein quartz sand, deionized water, silicon ball mass ratio be 1:
0.5:2-1:1:4, the liner of ball mill is polyurethane or silica, and mill is situated between for quartzy silicon ball.
（2）Centrifugal classification：Slurry after grinding is subjected to sedimentation centrifugal classification, maximum separation factor by sedimentation centrifuge
>=946, sedimentation centrifugal classification obtains filtrate and filter cake, filtrate solid contents 35%-55%, -2.0 μm of granularity D50=1.0 μm.
（3）Fine gtinding：Sedimentation centrifugal classification is obtained into filtrate addition sand mill and is ground to certain particle size, sand mill liner
For polyurethane, silicon carbide or zirconium oxide, it is zirconium oxide or silicon nitride that mill, which is situated between, and a diameter of 0.2-0.8 ㎜ of mill Jie sequentially add dispersion
Agent, modifying agent, anti-settling agent, antimildew disinfectant continue to be ground to granularity to sub-micron, i.e. D50=0.1-0.6 μm of slurry granularity,
D100≤1.0 μm, purity >=98.0% of silica after drying, you can；Wherein dispersant is Sodium Polyacrylate, and additive amount is
The 0.5%-2.0% of slurry weight, modifying agent are silane coupling agent KBM603, KBM903, KBE903 etc. one or more of water-soluble
Modifying agent, additive amount are the 0.2%-1.0% of slurry weight, and anti-settling agent is aerosil, and additive amount is the 1%- of slurry weight
3%.Antimildew disinfectant is Kathon CG Antisepticize and mildew preventive, and additive amount is slurry weight 0.2%-0.6%
Embodiment 2, a kind of preparation method of submicron silicon dioxide dispersion liquid, its step are as follows：By 20 ㎏, 4-40 purposes are high-purity
The ball mill that high-purity silicon ball of crystal quartz sand sand, 13kg deionized waters and a diameter of 2-4cm of 65 ㎏ is put into 100L carries out primary
The frequency of grinding, ball mill is 50 hertz, and inner liner of bowl mill is silica.When being ground to D50=3.5-4.0 μm of slurry granularity, it will starch
Material is classified to obtain filtrate solid content 40-45% by the progress centrifugal sedimentation of the sedimentation centrifuge of φ 1m, D50=1.0-1.3 μm of granularity,
5L vertical grinding machine fine gtindings are added in filtrate, sand mill liner is zirconium oxide, and it is silicon nitride, mill Jie's diameter 0.2- that mill, which is situated between,
0.4mm after being ground to D50=0.7-0.8 μm of slurry granularity, sequentially adds the Sodium Polyacrylate dipersant of slurry weight 1.0%,
The KBM603 modifying agent of slurry weight 0.4%, the aerosil anti-settling agent of slurry weight 1.0%, 0.3% Kathon CG anti-corrosion are anti-
Mould dose, continuing to be ground to D50=0.2-0.4 μm of slurry, this product can be used in waterborne UV coating, raising hardness of paint film,
Improve paint film anti scuffing, salt spray resistance and alcohol resistance energy.
Embodiment 3, a kind of preparation method of submicron silicon dioxide dispersion liquid, its step are as follows：By 20 ㎏, 4-40 purposes
The ball mill that high-purity silicon ball of high-purity tekite sand, 11kg deionized waters and 65 ㎏, a diameter of 2-4cm is put into 100L carries out just
The frequency of grade grinding, ball mill is 50 hertz, and inner liner of bowl mill is silica.It, will when being ground to D50=5.0-5.5 μm of slurry granularity
Slurry carries out centrifugal sedimentation by the sedimentation centrifuge of φ 1m and is classified to obtain filtrate solid content 45-50%, granularity D50=1.4-1.7 μ
Filtrate addition 5L vertical grinding machines are ground by m, and sand mill liner is polyurethane, and it is zirconium oxide that mill, which is situated between, and mill is situated between a diameter of
0.4-0.6 mm are ground to D50=0.7-0.8 μm of slurry granularity, sequentially add the polyacrylic acid sodium salt dispersion of slurry weight 1.0%
Agent, the KBE903 modifying agent of slurry weight 0.5%, the aerosil anti-settling agent of slurry weight 1.5%, 0.3% Kathon CG anti-corrosion
Mould inhibitor continues to be ground to D50=0.4-0.6 μm of slurry, this product can be used for aqueous woodware paint, and can to improve paint film hard
Degree improves paint film anti scuffing, salt spray resistance and alcohol resistance energy；For can improve in Aqueous Adhesives product adhesion strength and
Durability.
Claims (10)
1. a kind of preparation method of submicron silicon dioxide dispersion liquid, which is characterized in that its step are as follows：
(1) primary grinding：Progress primary in ball mill is added in crystal quartz sand or tekite sand, silicon ball, deionized water to grind
Mill；
(2) centrifugal classification：Slurry after grinding is obtained into filtrate and filter cake by sedimentation centrifugal classification；
(3) fine gtinding：Sedimentation centrifugal classification is obtained into filtrate addition sand mill and is ground to D50=0.7-0.8 μm, is sequentially added
Dispersant, modifying agent, anti-settling agent, antimildew disinfectant continue to be ground to granularity to sub-micron.
2. the preparation method of submicron silicon dioxide dispersion liquid according to claim 1, it is characterised in that：Step（1）In
The liner of ball mill is polyurethane or silica, and mill is situated between for quartzy silicon ball.
3. requiring a kind of preparation method of submicron silica powder dispersion liquid according to right 1, it is characterised in that：Step
Suddenly（1）Middle quartz sand, deionized water, silicon ball mass ratio be 1:0.5:2-1:1:4, it is ground to slurry granularity D50=3.5 μm-
5.5μm。
4. requiring a kind of preparation method of submicron silica powder dispersion liquid according to right 1, it is characterised in that：Step
（2）It is middle to carry out sedimentation centrifugal classification, maximum separation factor >=946 using sedimentation centrifuge.
5. requiring a kind of preparation method of submicron silica powder dispersion liquid according to right 1, it is characterised in that：Step
（2）The filtrate solid contents 35%-55% that middle centrifugal sedimentation is classified, -2.0 μm of granularity D50=1.0 μm.
6. requiring a kind of preparation method of submicron silica powder dispersion liquid according to right 1, it is characterised in that：Step
（3）Middle dispersant is Sodium Polyacrylate, and additive amount is the 0.5%-2.0% of slurry weight；The modifying agent is silane coupling agent
Water-soluble modified dose of one or more of KBM603, KBM903, KBE903, additive amount are the 0.2%-1.0% of slurry weight.
7. requiring a kind of preparation method of submicron silica powder dispersion liquid according to right 1, it is characterised in that：Step
（3）Middle anti-settling agent is that grain size is 10 nm -50nm aerosils, and additive amount is the 1%-3% of slurry weight；It is described mould proof to kill
Microbial inoculum is Kathon CG Antisepticize and mildew preventive, and additive amount is slurry weight 0.2%-0.6%.
8. requiring a kind of preparation method of submicron silica powder dispersion liquid according to right 1, it is characterised in that：Step
（3）Described in sand mill liner be polyurethane, silicon carbide or zirconium oxide, mill be situated between be zirconium oxide or silicon nitride, mill be situated between it is a diameter of
0.2-0.8㎜。
9. requiring a kind of preparation method of submicron silica powder dispersion liquid according to right 1, it is characterised in that：Step
（3）In be finely ground to D50=0.1-0.6 μm of slurry granularity, D100≤1.0 μm, the purity of silica after drying >=
98.0%。
10. dispersion liquid made from the preparation method of the submicron silica powder dispersion liquid described in claim 1-9 any one
Product is in water paint, Aqueous Adhesives, polishing liquid for metal surface, aqueous polyurethane varnish, water soluble acrylic acid varnish, aqueous ring
The anti scuffing for improving paint film in oxygen varnish, aqueous UV varnish, improves the purposes of hardness of paint film.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110079128A (en) * | 2019-04-29 | 2019-08-02 | 江苏辉迈粉体科技有限公司 | A kind of Submicron spherical silica micropowder organic dispersions and preparation method thereof |
| CN111073350A (en) * | 2019-12-25 | 2020-04-28 | 中建材蚌埠玻璃工业设计研究院有限公司 | Preparation method of submicron active silica micropowder |
| CN112374504A (en) * | 2020-11-05 | 2021-02-19 | 黄运雷 | Process for manufacturing nano silicon dioxide by physical method |
| CN113755032A (en) * | 2020-12-16 | 2021-12-07 | 安徽进化硅纳米材料科技有限公司 | Method for refining silicon dioxide, ultrafine silicon dioxide powder and use |
| CN114085566A (en) * | 2021-12-07 | 2022-02-25 | 安徽进化硅纳米材料科技有限公司 | Aqueous silicon dioxide suspension, preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110079128A (en) * | 2019-04-29 | 2019-08-02 | 江苏辉迈粉体科技有限公司 | A kind of Submicron spherical silica micropowder organic dispersions and preparation method thereof |
| CN111073350A (en) * | 2019-12-25 | 2020-04-28 | 中建材蚌埠玻璃工业设计研究院有限公司 | Preparation method of submicron active silica micropowder |
| CN112374504A (en) * | 2020-11-05 | 2021-02-19 | 黄运雷 | Process for manufacturing nano silicon dioxide by physical method |
| CN112374504B (en) * | 2020-11-05 | 2023-01-24 | 黄运雷 | Process for manufacturing nano silicon dioxide by physical method |
| CN113755032A (en) * | 2020-12-16 | 2021-12-07 | 安徽进化硅纳米材料科技有限公司 | Method for refining silicon dioxide, ultrafine silicon dioxide powder and use |
| CN114085566A (en) * | 2021-12-07 | 2022-02-25 | 安徽进化硅纳米材料科技有限公司 | Aqueous silicon dioxide suspension, preparation method and application thereof |
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