CN110510619A - The preparation method of active superfine vitreous silica SILICA FUME - Google Patents
The preparation method of active superfine vitreous silica SILICA FUME Download PDFInfo
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- CN110510619A CN110510619A CN201910857981.4A CN201910857981A CN110510619A CN 110510619 A CN110510619 A CN 110510619A CN 201910857981 A CN201910857981 A CN 201910857981A CN 110510619 A CN110510619 A CN 110510619A
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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
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a kind of preparation method of active superfine vitreous silica SILICA FUME, including step A, by purity fused raw material after evenly mixing, grinding aid is added and is put into ball milling in ball mill, slurry is made；B, the slurry high-speed stirred that will be prepared in step A, and it is warming up to 850~1000 DEG C simultaneously, spraying machine sprays into modified additive, and quickly active slurry process is made in stirring；C, the active slurry process prepared in step B is dried in vacuo；D, the silicon powder being prepared in step C is crushed, is sieved, obtain the fine silica powder that granularity is 0.1~0.15 μm；E, fine silica powder obtained in step D is subjected to magnetic point, removes magnetisable material therein to get to required active superfine vitreous silica SILICA FUME, the present invention is with simple process, the beneficial effect that production cost is low, SILICA FUME partial size is small, activity is high.
Description
Technical field
The present invention relates to the preparations of SILICA FUME, it is more particularly related to a kind of micro- silicon of active superfine vitreous silica
The preparation method of powder.
Background technique
SILICA FUME is commonly called as silicon ash, is in smelt iron and industrial silicon, after the silicon steam oxidation being discharged by flue, through gathering dust
Device collects unformed, powdery the silica fine particle obtained after processing purification, and the main chemical compositions of SILICA FUME are
Silica, content are generally 85%~95%, simultaneously containing di-iron trioxide, calcium oxide, potassium oxide, sodium oxide molybdena, magnesia,
Carbon etc..SILICA FUME is since with stronger corrosion resistance, granularity is small, higher activity, biggish specific surface area and relatively strong
Hydrophily, be widely used in aerospace, construction material, fine chemistry industry, optical fiber cable, high technology ceramics, defence engineering etc. neck
Domain.The preparation method of SILICA FUME mainly includes ball-milling method, ball roller method, mill method and rushes rotation method at present, but generally existing production
Energy consumption is high for process, high production cost, active low problem, it is difficult to meet market-oriented demand.
Summary of the invention
It is an object of the invention to solve at least the above problems, a kind of system of active superfine vitreous silica SILICA FUME is provided
Preparation Method improves the activity and quality of SILICA FUME to reduce production cost.
In order to solve the above technical problems, the present invention adopts the following technical scheme: a kind of micro- silicon of active superfine vitreous silica
The preparation method of powder, comprising the following steps:
A, the grinding aid that mass fraction is 1%~3% after evenly mixing by purity fused raw material, is added, is put into
12~18h of ball milling in ball mill, is made slurry, and the mass ratio of the purity fused raw material and grinding aid is 3:1~5:
1；
B, the slurry prepared in step A is put into high-speed mixer with 1200~1800r/min, 2~4h of high-speed stirred,
And be rapidly heated simultaneously to 850~1000 DEG C, after keeping the temperature 30~60min, stop heating, spraying machine sprays into modified additive, continues
Quickly active slurry process is made in 1~2h of stirring, and wherein modified additive quality accounts for the 0.1%~1.5% of active slurry process；
C, by the active slurry process prepared in step B, dry 1~3h obtains dry silicon powder in vacuum drier, described true
The vacuum degree of empty drying machine is -0.095Mpa~0.001Mpa；
D, it by after the silicon powder prepared in step C crushing crusher machine, is then sieved with vibrating screen, obtaining granularity is
0.1~0.15 μm of fine silica powder；
E, fine silica powder obtained in step D is subjected to magnetic point, removes magnetisable material therein to get required ultra-fine work is arrived
Property vitreous silica SILICA FUME.
Preferably, wherein dioxide-containing silica >=99.9% of purity fused raw material, granularity are 1~3 μm.
Preferably, wherein part includes following ingredient to grinding aid by weight: 20~30 parts of isoamyl alcohol, dehydrated alcohol 1~
6 parts, 2~5 parts of butyric acid, 1~8 part of epoxy resin, 0.1~1 part of enuatrol, 2~5 parts of cycloalkylsulfonic acid sodium, talcum powder 0.01~
0.05 part, 0.3~0.7 part of amyl acetate, 0.01~0.03 part of manganese dioxide.
Polycondensation reaction, while epoxy occur for isoamyl alcohol in grinding aid, the carboxyl in terminal hydroxy group and butyric acid in dehydrated alcohol
The synergistic effect of resin, cycloalkylsulfonic acid sodium epoxy group and naphthenic base promotes grinding aid chemistry in the form of polymolecular layer to inhale
It is attached to silica flour particle surface, improves the mobility of silica flour, prevents the reunion of ultrafine quartz powder, so that in mechanical milling process
Quartzy powder particles develop to smaller granularity direction, meanwhile, the use of grinding aid can significantly reduce the energy consumption of mechanical milling process, drop
Low production cost.
Preferably, wherein grinding aid the preparation method is as follows: by isoamyl alcohol, epoxy resin, enuatrol, naphthenic base sulphur
Sour sodium, talcum powder, amyl acetate, manganese dioxide are dissolved in dehydrated alcohol, are heated to 30~40 DEG C after mixing evenly, slowly add
Continue 10~20min of heating after entering butyric acid, stop heating, be cooled to room temperature, filters, grinding aid described in drying to obtain.
Preferably, wherein being rapidly heated, the specific steps are elder generations to be warming up to 550~600 DEG C from room temperature with 20 DEG C/s, then
850~1000 DEG C are warming up to 60 DEG C/s.
Preferably, wherein modified additive is the ethanol solution for mixing coupling agent, wherein mixing coupling agent is silane
Coupling agent and aluminate coupling agent mixture.
Preferably, wherein silane coupling agent includes acetyl group triethoxysilane, acetyl group trimethoxy silane, γ-
Aminopropyl trimethoxysilane, 3- aminopropyl trimethoxysilane, in 3- glycidyl ether oxypropyltrimethoxysilane
At least one, the aluminate coupling agent include at least one of LS-62, LS-821, LT-1.
Preferably, wherein the mass ratio that coupling agent and dehydrated alcohol are mixed in the modified additive is 1.3:2~1:2,
The mass ratio of silane coupling agent described in the mixing coupling agent and aluminate coupling agent is 1.5:1.7~2.1:2.9；
Alkoxy C H in modified additive in silane coupling agent3O- hydrolysis generates hydroxyl, and the hydroxyl hydrolyzed participates in silicon
Alkane self-condensation reaction, with silica flour surface react and with the C in Aluminate3H7The reaction of O-, silica flour particle surface quilt
Silanol group or silicon ether cladding, these chemical groups are acted on the surface energy for reducing quartzy powder by adsorption, improve quartz
The activity of powder.
Preferably, wherein pulverizer is to rush rotary type pulverizer.
It rushes rotary type pulverizer and prepares SILICA FUME by establishing different energy range in pulverizer, so that raw material obtains different journeys
The impact strength of degree, due to not receiving the compacted effect of compulsory external force, silicon powder internal organizational structure becomes loose, compared to ball
Mill method, ball roller method, mill method are more advantageous to the basis for constructing silica flour high activity.
Preferably, wherein the rate quickly stirred is 2000~2800r/min.
The present invention is include at least the following beneficial effects: (1) living using the superfine active SILICA FUME purity is high of this method preparation
Property it is strong, do not use strong acid, highly basic, realize the free of contamination advantage of preparation process safety and environmental protection, the SILICA FUME activity of preparation is big, purity
Height is the good filler of the industries such as silicon rubber, military project, space flight, medicine；(2) association of silane coupling agent and aluminate coupling agent
The surface energy that SILICA FUME can be significantly reduced with fit effect, improves the specific surface area of SILICA FUME, improves the activity of SILICA FUME, together
When, the use of the mixing coupling agent enhances the compatibility on SILICA FUME surface, makes up SILICA FUME and be not easy the shortcomings that dispersing, widen micro-
The application field of silicon powder；(3) rush rotary type pulverizer using punching press crushing by the way of and grinding aid effect so that preparation grain
Diameter is small and production process low energy consumption, reduce the production cost of SILICA FUME, improve the product quality of SILICA FUME.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments, to enable those skilled in the art referring to specification
Text can be implemented accordingly.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of a other elements or combinations thereof.
Embodiment 1
A kind of preparation method of active superfine vitreous silica SILICA FUME, comprising the following steps:
A, the grinding aid that mass fraction is 1% after evenly mixing by purity fused raw material, is added, is put into ball mill
Middle ball milling 12h, is made slurry, and the mass ratio of the purity fused raw material and grinding aid is 3:1；
Wherein, the dioxide-containing silica 99.99% of purity fused raw material, granularity are 1 μm；
Wherein, part includes following ingredient to grinding aid by weight: 20 parts of isoamyl alcohol, 3 parts of dehydrated alcohol, and 2 parts of butyric acid, epoxy
1 part of resin, 0.1 part of enuatrol, 2 parts of cycloalkylsulfonic acid sodium, 0.01 part of talcum powder, 0.3 part of amyl acetate, manganese dioxide 0.01
Part.
Wherein, grinding aid the preparation method is as follows: by epoxy resin, enuatrol, cycloalkylsulfonic acid sodium, talcum powder, acetic acid
Pentyl ester, manganese dioxide are dissolved in dehydrated alcohol, are heated to 30 DEG C after mixing evenly, continue to heat after being slowly added to butyric acid
10min stops heating, is cooled to room temperature, and filters, grinding aid described in drying to obtain.
B, the slurry prepared in step A is put into high-speed mixer with 1200r/min high-speed stirred 2h, and simultaneously quickly
850 DEG C are warming up to, after keeping the temperature 30min, stops heating, spraying machine sprays into modified additive, continues quickly stirring 1h and active material is made
Slurry；The rate quickly stirred is 2000r/min.
Wherein, modified additive quality accounts for the 0.1% of active slurry process.
Wherein, being rapidly heated, the specific steps are elder generations to be warming up to 600 DEG C from room temperature with 20 DEG C/s, is then warming up to 60 DEG C/s
1000℃。
Wherein, modified additive is the ethanol solution for mixing coupling agent, and mixing coupling agent is silane coupling agent and aluminic acid
Ester is coupled agent composition.
Wherein, silane coupling agent is acetyl group triethoxysilane, 3- aminopropyl trimethoxysilane, γ-aminopropyl three
The mixture of methoxy silane, the mixture of aluminate coupling agent LS-62, LT-1.
Wherein, the mass ratio that coupling agent and dehydrated alcohol are mixed in modified additive is 1:2, is mixed silane coupled in coupling agent
The mass ratio of agent and aluminate coupling agent is 1.5:1.7；
C, by the active slurry process prepared in step B, dry 1h obtains dry silicon powder, the vacuum in vacuum drier
The vacuum degree of drying machine is -0.095Mpa；
D, it after the silicon powder being prepared in step C being crushed crusher machine, is then sieved with vibrating screen, obtaining granularity is
0.1~0.15 μm of fine silica powder；Wherein pulverizer is to rush rotary type pulverizer；
E, fine silica powder obtained in step D is subjected to magnetic point, removes magnetisable material therein to get required ultra-fine work is arrived
Property vitreous silica SILICA FUME.
Embodiment 2
It is essentially identical with the raw material and technique of embodiment 1, only difference is that, silane coupling agent is 3- aminopropyl three
Methoxy silane, aluminate coupling agent LT-1；
Embodiment 3
It is essentially identical with the raw material and technique of embodiment 1, only difference is that, silane coupling agent is γ-aminopropyl
Trimethoxy silane, aluminate coupling agent LS-62；
Comparative example 1
Process conditions and raw material are consistent substantially with embodiment 1 in the present embodiment, only difference is that, do not add
Add modified additive.
Comparative example 2
Process conditions and raw material are consistent substantially with embodiment 1 in the present embodiment, only difference is that, it is modified
Auxiliary agent is single silane coupling agent or aluminate coupling agent.
Comparative example 3
Process conditions and raw material are consistent substantially with embodiment 1 in the present embodiment, only difference is that, do not add
Add and helps the agent that rubs.
The ultra-fine melting activity SILICA FUME the performance test results of embodiment 1-3 and comparative example 1-3 preparation are as follows；
| Specific surface area (m2/g) | Partial size (μm) | |
| Embodiment 1 | 46.0163 | 0.1280 |
| Embodiment 2 | 47.7539 | 0.1189 |
| Embodiment 3 | 46.9289 | 0.1345 |
| Comparative example 1 | 39.7376 | 0.1214 |
| Comparative example 2 | 38.7846 | 0.1258 |
| Comparative example 3 | 46.0418 | 0.1789 |
Embodiment 1-3 compared with comparative example 1-2, prepared by the active SILICA FUME of melting specific surface area by 38.7846
~39.7376m2/ g rises to 46.0163~47.7539m2/ g, this shows silane coupling agent and Aluminate idol in modified additive
The synergistic effect for joining agent, can significantly improve the activity of SILICA FUME, principle is as follows: the alkoxy C H in silane coupling agent3O- water
Solution generates hydroxyl, the hydroxyl that hydrolyzes participate in the reaction of silane self-condensation, with silica flour surface react and and Aluminate
In C3H7The reaction of O- improves the activity of quartzy powder to significantly reduce the surface energy of quartzy powder.
Embodiment 1-3, comparative example 1-2 are compared with comparative example 3, and partial size drops to 0.11-0.12 μm by 0.1789 μm, i.e.,
The partial size of superfine active SILICA FUME prepared by addition grinding aid is significantly less than the SILICA FUME for not adding grinding aid in comparative example 3
Partial size, grinding aid are chemisorbed on silica flour particle surface by way of polymolecular layer to improve the mobility of silica flour, hindered
The only reunion of ultrafine quartz powder accelerates the mechanical milling process of quartzy powder, so that quartzy powder particles are to smaller granularity direction
Development, is conducive to the preparation of ultra-fine vitreous silica SILICA FUME.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein are not precluded one or more
The presence or addition of a other elements or combinations thereof.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details.
Claims (10)
1. a kind of preparation method of active superfine vitreous silica SILICA FUME, which comprises the following steps:
After evenly mixing by purity fused raw material, the grinding aid that mass fraction is 1%~3% is added, is put into ball mill
Middle 12~18h of ball milling, is made slurry, and the mass ratio of the purity fused raw material and grinding aid is 3:1~5:1；
The slurry prepared in step A is put into high-speed mixer with 1200~1800r/min, 2~4h of high-speed stirred, and simultaneously
It is rapidly heated to 850~1000 DEG C, after keeping the temperature 30~60min, stops heating, spraying machine sprays into modified additive, and continuation is quickly stirred
It mixes 1~2h and active slurry process is made, wherein the modified additive quality accounts for the 0.1%~1.5% of active slurry process；
By the active slurry process prepared in step B, dry 1~3h obtains dry silicon powder, the vacuum drying in vacuum drier
The vacuum degree of machine is -0.095Mpa~0.001Mpa；
By the silicon powder prepared in step C with crush crusher machine after, then sieved with vibrating screen, obtain granularity be 0.1~
0.15 μm of fine silica powder；
Fine silica powder obtained in step D is subjected to magnetic point, magnetisable material therein is removed and is melted to get to required superfine active
Quartzy SILICA FUME.
2. the preparation method of active superfine vitreous silica SILICA FUME according to claim 1, which is characterized in that described high-purity
Dioxide-containing silica >=99.9% of vitreous silica raw material is spent, granularity is 1~3 μm.
3. the preparation method of active superfine vitreous silica SILICA FUME according to claim 1, which is characterized in that the grinding aid
Part includes following ingredient by weight for agent: 20~30 parts of isoamyl alcohol, 1~6 part of dehydrated alcohol, and 2~5 parts of butyric acid, epoxy resin 1~
8 parts, 0.1~1 part of enuatrol, 2~5 parts of cycloalkylsulfonic acid sodium, 0.01~0.05 part of talcum powder, 0.3~0.7 part of amyl acetate,
0.01~0.03 part of manganese dioxide.
4. the preparation method of active superfine vitreous silica SILICA FUME according to claim 3, which is characterized in that the grinding aid
Agent the preparation method is as follows: by isoamyl alcohol, epoxy resin, enuatrol, cycloalkylsulfonic acid sodium, talcum powder, amyl acetate, titanium dioxide
Manganese is dissolved in dehydrated alcohol, is heated to 30~40 DEG C after mixing evenly, continues 10~20min of heating after being slowly added to butyric acid,
Stop heating, be cooled to room temperature, filters, grinding aid described in drying to obtain.
5. the preparation method of active superfine vitreous silica SILICA FUME according to claim 1, which is characterized in that described quick
Heating up, the specific steps are elder generations to be warming up to 550~600 DEG C from room temperature with 20 DEG C/s, is then warming up to 850~1000 DEG C with 60 DEG C/s.
6. the preparation method of active superfine vitreous silica SILICA FUME according to claim 1, which is characterized in that the modification
Auxiliary agent is the ethanol solution for mixing coupling agent, wherein the mixing coupling agent is silane coupling agent and aluminate coupling agent
Mixture.
7. the preparation method of active superfine vitreous silica SILICA FUME according to claim 6, which is characterized in that the silane
Coupling agent includes acetyl group triethoxysilane, acetyl group trimethoxy silane, γ-aminopropyltrimethoxysilane, 3- ammonia third
Base trimethoxy silane, at least one of 3- glycidyl ether oxypropyltrimethoxysilane, the aluminate coupling agent
Including at least one of LS-62, LS-821, LT-1.
8. the preparation of active superfine vitreous silica SILICA FUME according to claim 6, feature exist, in the modified additive
The mass ratio for mixing coupling agent and dehydrated alcohol is 1.3:2~1:2, silane coupling agent and aluminic acid described in the mixing coupling agent
The mass ratio of ester coupling agent is 1.5:1.7~2.1:2.9.
9. the preparation of active superfine vitreous silica SILICA FUME according to claim 1, which is characterized in that the pulverizer is
Rush rotary type pulverizer.
10. the preparation of active superfine vitreous silica SILICA FUME according to claim 1, which is characterized in that described quickly to stir
The rate mixed is 2000~2800r/min.
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| CN114656804A (en) * | 2022-03-03 | 2022-06-24 | 江苏圣天新材料有限公司 | Preparation method of soft composite silicon micro powder for copper-clad plate |
| CN114918024A (en) * | 2022-04-16 | 2022-08-19 | 吉安豫顺新材料有限公司 | Process method for grinding silicon micropowder by airflow |
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| CN114918024A (en) * | 2022-04-16 | 2022-08-19 | 吉安豫顺新材料有限公司 | Process method for grinding silicon micropowder by airflow |
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Application publication date: 20191129 |