CN106543773A - The scale surface treatment method of the superfine quartz powder of median≤2 μm - Google Patents
The scale surface treatment method of the superfine quartz powder of median≤2 μm Download PDFInfo
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- CN106543773A CN106543773A CN201610934485.0A CN201610934485A CN106543773A CN 106543773 A CN106543773 A CN 106543773A CN 201610934485 A CN201610934485 A CN 201610934485A CN 106543773 A CN106543773 A CN 106543773A
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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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
- C01P2004/61—Micrometer sized, i.e. from 1-100 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
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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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
- C01P2006/90—Other properties not specified above
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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
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Abstract
The present invention discloses a kind of scale surface treatment method of the superfine quartz powder of median≤2 μm; it is pre-dispersed by superfine quartz powder is carried out; by modifying agent hydrolysis, atomization; modification in mixer is entered after well dispersed superfine quartz powder and the modifying agent uniform contact of atomization; the present invention adopts dry modification process; process is simple; without the need for the operation such as filter, dry, break up; treating capacity is big; production efficiency is high; uniformly it is sprayed on superfine quartz powder granule after modifying agent atomization, significantly improves modification efficiency, reduces amount of modifier.
Description
Technical field
The invention belongs to a kind of surface treatment method of superfine powder, is related specifically to the ultra-fine stone of median≤2 μm
The scale surface treatment method of English powder body.
Background technology
Superfine powder is primarily referred to as the powder of D50≤2 μm, D97≤5 μm, including silicon powder, alumina powder, aluminium hydroxide
Powder etc., is mainly used in the industries such as electron and electrician, coating, special cermacis.Ultrafine quartz powder granule has higher surface energy,
There is substantial amounts of hydroxyl in grain surface, reunion is easily produced in the presence of molecular separating force.Ultrafine quartz powder reunite after, conveying and
Easily occur reuniting and clogging during feed, and there is very strong hydrophilic, the easy moisture absorption of powder body, its point when mixing with high polymer
Scattered property and the compatibility are very poor.Typically ultrafine quartz powder is surface-treated by silane coupler, improves its mobility and divide
Scattered property, while the compatibility of ultrafine quartz powder and Organic substance can be improved, enhancing is bonded with epoxy resin etc..
Surface treatment is generally divided into two kinds of dry and wet, carries out frequently with reactor, retort wet under laboratory condition
Method is modified.Wet-process modified is a little that powder body is well dispersed in the slurry, is conducive to modifying agent to be evenly coated at powder granule surface,
Suitable for the powder-modified of various granularity level.Have the disadvantage that technique is more complicated, it is modified finish rear powder body need to carry out filtering, dry,
The operation such as break up.
Dry modification process is simple, and general industry metaplasia is produced.But dry process is for superfine powder
There is poor dispersion, the shortcoming of modifying agent covering property difference.Therefore the difficult point of dry method modification is to be completely dispersed how granule, modifying agent
Each particle surface is evenly coated at, and cost is also considered as when being modified on a large scale in addition, is completed the addition of coupling agent
It is modified and as excessive too many.
The method of modifying such as Chinese invention patent CN201410407421.6 and CN201410486281.6 are using at wet method
Reason, is carried out in water, and modified silica flour slurry must be through the operations such as centrifugation, filtration, drying, grinding, screening, ability
The powder body of former particle size distribution is reduced to, complex technical process is not suitable for large-scale production；Chinese invention patent
CN201510307525.4, using dry method, but its material do not carry out it is pre-dispersed, modifying agent addition it is uneven, this outer grinding with change
Property simultaneously carry out, modification process time is long.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of ultrafine quartz powder of median≤2 μm
Scale surface treatment method.
In order to realize the purpose, technical scheme is as follows：The rule of the superfine quartz powder of median≤2 μm
Modelling surface treatment method, it is characterised in that comprise the following steps：1）By silane coupler, ethanol, water in mass ratio (20～
30):(60～75):(5～10) mixing, acetic acid being added as hydrolyst, it is 3.5～5 to adjust pH value, hydrolysis time 10～
30min, it is standby in addition hold-up tank after the completion of hydrolysis；
2）Pending superfine quartz powder is added in feed bin, starts discharge valve, discharge valve discharge quantity is adjusted by converter,
By mixing chamber subsequently into V-Mixer, dispersion after the ultrasonic disperse sieve on the blended room top of superfine quartz powder is pre-dispersed
Mesh size is 40～100 mesh；
3）Silane coupler after hydrolyzing in hold-up tank enters steam jet ejector, Jing steam jet ejector atomized sprays by regulating valve
Into mixing chamber, contact with superfine quartz powder in mixing chamber, and be attached on superfine quartz powder in V-Mixer, V
Using being flexible coupling between type mixer and mixing chamber, connect during charging, charging is disconnected after finishing, and closes charge door；
4）Stirring paddle is set in V-Mixer, and superfine quartz powder and silane coupler are abundant under the stirring action of stirring paddle
Mixing, silane coupler is evenly coated at superfine quartz powder surface, in coupling agent-X group can hydrolyze generation silanol base,
Silanol base and SiO2Surface hydroxyl reacts to form alcoxyl structure and slough water, and powder granule is changed into hydrophobicity from hydrophilic；
5）After the completion of mixing, V-Mixer discharging butterfly valve is opened, superfine powder loads 24～48h of closed preservation in hermetic bag, table
Face modification is completed.
The silane coupler is γ-aminopropyltrimethoxysilane, γ-glycidoxypropyl trimethoxy silicon
Alkane, γ-methacryloxypropyl trimethoxy silane or tetramethyl-disilazane.
Beneficial effects of the present invention：1）The present invention adopts dry modification process, process is simple to break up without the need for filtering drying
Operation, treating capacity are big, and production efficiency is high, and different according to V-Mixer volume, treating capacity is up to 1～10 ton per hour.2）Pass through
Superfine quartz powder is pre-dispersed, and steam jet ejector is uniformly sprayed on powder granule after modifying agent is atomized, and is significantly improved and is changed
Property efficiency, reduce amount of modifier.
Specific embodiment
Embodiment 1
A kind of scale surface treatment method of the superfine quartz powder of median≤2 μm, comprises the following steps：
1）Coupling agent γ-methacryloxypropyl trimethoxy silane is carried out into prehydrolysis, coupling agent, ethanol, water press matter
Amount compares 30:60:10 mixing, while adding acetic acid as hydrolyst, adjust pH value 3.5-5, hydrolysis time 30min.Hydrolysis
After the completion of add hold-up tank in；
2）D50=1.50 μm of pending superfine quartz powder, D90=3.66 μm, specific surface area is 10.35m2/ g, will be pending
During superfine quartz powder adds feed bin, start discharge valve, it is 100kg/min discharge valve discharge quantity to be adjusted by converter, is fed
Time 15min, it is mixed subsequently into V-type by mixing chamber after the ultrasonic disperse sieve on the blended room top of superfine quartz powder is pre-dispersed
Conjunction machine, dispersion mesh size are 40 mesh；
3）Silane coupler after hydrolyzing in hold-up tank enters steam jet ejector, Jing steam jet ejector atomized sprays by regulating valve
Into mixing chamber, contact with superfine quartz powder in mixing chamber, and be attached on superfine quartz powder in V-Mixer, V
Using being flexible coupling between type mixer and mixing chamber, connect during charging, charging is disconnected after finishing, and closes charge door；It is logical
Cross feeding quantity and silica flour specific surface area is calculated and is coupled agent flux, be coupled agent flux=quartzy powder body feeding quantity * 0.15%* per minute
Specific surface area=1.55kg/min；
4）Stirring paddle is set in V-Mixer, and superfine quartz powder and silane coupler are abundant under the stirring action of stirring paddle
Mixing, silane coupler is evenly coated at superfine quartz powder surface, in coupling agent-X group can hydrolyze generation silanol base,
Silanol base and SiO2Surface hydroxyl reacts to form alcoxyl structure and slough water, and powder granule is changed into hydrophobicity from hydrophilic；
5）After the completion of mixing, V-Mixer discharge valve is opened, superfine powder loads closed preservation 48h in hermetic bag, and surface is modified
Process is completed.Modified powder fluidity, favorable dispersibility, are provided simultaneously with good hydrophobicity, and 72h is immiscible with water.
Embodiment 2
A kind of scale surface treatment method of the superfine quartz powder of median≤2 μm, comprises the following steps：
1）Coupling agent γ-glycidoxypropyltrimewasxysilane is carried out into prehydrolysis, coupling agent, ethanol, water press quality
Than 20:75:5 mixing, while adding acetic acid as hydrolyst, adjust pH value 3.5-5, hydrolysis time 30min.Hydrolysis is completed
In adding hold-up tank afterwards；
2）D50=1.20 μm of pending superfine quartz powder, D90=3.12 μm, specific surface area is 11.60m2/ g, will be pending
During superfine quartz powder adds feed bin, start discharge valve, it is 150kg/min discharge valve discharge quantity to be adjusted by converter, is fed
Time 10min, it is mixed subsequently into V-type by mixing chamber after the ultrasonic disperse sieve on the blended room top of superfine quartz powder is pre-dispersed
Conjunction machine, dispersion mesh size are 100 mesh；
3）Silane coupler after hydrolyzing in hold-up tank enters steam jet ejector, Jing steam jet ejector atomized sprays by regulating valve
Into mixing chamber, contact with superfine quartz powder in mixing chamber, and be attached on superfine quartz powder in V-Mixer, V
Using being flexible coupling between type mixer and mixing chamber, connect during charging, charging is disconnected after finishing, and closes charge door；It is logical
Cross feeding quantity and silica flour specific surface area is calculated and is coupled agent flux, be coupled agent flux=quartzy powder body feeding quantity * 0.15%* per minute
Specific surface area=2.61kg/min；
4）Stirring paddle is set in V-Mixer, and superfine quartz powder and silane coupler are abundant under the stirring action of stirring paddle
Mixing, silane coupler is evenly coated at superfine quartz powder surface, in coupling agent-X group can hydrolyze generation silanol base,
Silanol base and SiO2Surface hydroxyl reacts to form alcoxyl structure and slough water, and powder granule is changed into hydrophobicity from hydrophilic；
5）After the completion of mixing, V-Mixer discharge valve is opened, superfine powder loads closed preservation 24h in hermetic bag, and surface is modified
Process is completed.Modified powder fluidity, favorable dispersibility, are provided simultaneously with good hydrophobicity, and 24h is immiscible with water.
Embodiment 3
A kind of median is comprised the following steps less than the scale surface treatment method of≤2 μm of superfine quartz powder：
1）Coupling agent γ-aminopropyltrimethoxysilane is carried out into prehydrolysis, coupling agent, ethanol, water in mass ratio 25:70:8 mix
Close, while adding acetic acid as hydrolyst, adjust pH value 3.5-5, hydrolysis time 30min.Storage is added after the completion of hydrolysis
In tank；
2）D50=1.90 μm of pending superfine quartz powder, D90=4.85 μm, specific surface area is 8.26m2/ g, pending is surpassed
During fine quartz powder body adds feed bin, start discharge valve, it is 200kg/min discharge valve discharge quantity to be adjusted by converter, during charging
Between 7.5min, it is mixed subsequently into V-type by mixing chamber after the ultrasonic disperse sieve on the blended room top of superfine quartz powder is pre-dispersed
Conjunction machine, dispersion mesh size are 70 mesh；
3）Silane coupler after hydrolyzing in hold-up tank enters steam jet ejector, Jing steam jet ejector atomized sprays by regulating valve
Into mixing chamber, contact with superfine quartz powder in mixing chamber, and be attached on superfine quartz powder in V-Mixer, V
Using being flexible coupling between type mixer and mixing chamber, connect during charging, charging is disconnected after finishing, and closes charge door；It is logical
Cross feeding quantity and silica flour specific surface area is calculated and is coupled agent flux, be coupled agent flux=quartzy powder body feeding quantity * 0.15%* per minute
Specific surface area=2.47kg/min；
4）Stirring paddle is set in V-Mixer, and superfine quartz powder and silane coupler are abundant under the stirring action of stirring paddle
Mixing, silane coupler is evenly coated at superfine quartz powder surface, in coupling agent-X group can hydrolyze generation silanol base,
Silanol base and SiO2Surface hydroxyl reacts to form alcoxyl structure and slough water, and powder granule is changed into hydrophobicity from hydrophilic；
5）After the completion of mixing, V-Mixer discharge valve is opened, superfine powder loads closed preservation 36h in hermetic bag, and surface is modified
Process is completed.Modified powder fluidity, favorable dispersibility, are provided simultaneously with good hydrophobicity, and 48h is immiscible with water.
The above, is only presently preferred embodiments of the present invention, not makees any pro forma restriction to the present invention；Appoint
What those of ordinary skill in the art, under without departing from technical solution of the present invention ambit, all using the side of the disclosure above
Method and technology contents make many possible variations and modification, or the equivalent reality for being revised as equivalent variations to technical solution of the present invention
Apply example.Therefore, every content without departing from technical solution of the present invention, is done to above example according to the technical spirit of the present invention
Any simple modification, equivalent, equivalence changes and modification, still fall within the range of technical solution of the present invention protection.
Claims (2)
1. the scale surface treatment method of the superfine quartz powder of median≤2 μm, it is characterised in that including following step
Suddenly：1）By silane coupler, ethanol, water (20～30) in mass ratio:(60～75):(5～10) mix, acetic acid is added as water
Solution catalyst, it is 3.5～5,10～30min of hydrolysis time to adjust pH value, standby in addition hold-up tank after the completion of hydrolysis；
2）Pending superfine quartz powder is added in feed bin, starts discharge valve, discharge valve discharge quantity is adjusted by converter,
By mixing chamber subsequently into V-Mixer, dispersion after the ultrasonic disperse sieve on the blended room top of superfine quartz powder is pre-dispersed
Mesh size is 40～100 mesh；
3）Silane coupler after hydrolyzing in hold-up tank enters steam jet ejector, Jing steam jet ejector atomized sprays by regulating valve
Into mixing chamber, contact with superfine quartz powder in mixing chamber, and be attached on superfine quartz powder in V-Mixer, V
Using being flexible coupling between type mixer and mixing chamber, connect during charging, charging is disconnected after finishing, and closes charge door；
4）Stirring paddle is set in V-Mixer, and superfine quartz powder and silane coupler are abundant under the stirring action of stirring paddle
Mixing, silane coupler are evenly coated at superfine quartz powder surface；
5）After the completion of mixing, V-Mixer discharging butterfly valve is opened, superfine powder loads 24～48h of closed preservation in hermetic bag, table
Face modification is completed.
2. the scale surface treatment method of the superfine quartz powder of median≤2 μm according to claim 1, which is special
Levy and be, the silane coupler be γ-aminopropyltrimethoxysilane, γ-glycidoxypropyltrimewasxysilane,
γ-methacryloxypropyl trimethoxy silane or tetramethyl-disilazane.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108929572A (en) * | 2018-08-06 | 2018-12-04 | 宁波普莱斯帝金属制品有限公司 | A kind of preparation method being alkylated superfine talcum powder |
| CN113150387A (en) * | 2021-04-21 | 2021-07-23 | 江苏联瑞新材料股份有限公司 | Preparation method of hydrophobic silicon micro powder |
| CN113354960A (en) * | 2021-05-24 | 2021-09-07 | 广东海浦倍尔新材料有限公司 | Modified inorganic nano particle and preparation method thereof |
| CN113750914A (en) * | 2021-08-05 | 2021-12-07 | 华东理工大学 | Silicon dioxide aerogel modification method |
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| CN113150387A (en) * | 2021-04-21 | 2021-07-23 | 江苏联瑞新材料股份有限公司 | Preparation method of hydrophobic silicon micro powder |
| CN113354960A (en) * | 2021-05-24 | 2021-09-07 | 广东海浦倍尔新材料有限公司 | Modified inorganic nano particle and preparation method thereof |
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Address after: 751 No. 233010 Anhui province Bengbu Longzihu East Avenue Applicant after: BENGBU SILICON-BASED MATERIALS INDUSTRIAL TECHNOLOGY RESEARCH INSTITUTE CO., LTD. Address before: Tu Shan Lu Yuhui District 233010 Anhui city of Bengbu Province, No. 1047 Applicant before: BENGBU SILICON-BASED MATERIALS INDUSTRIAL TECHNOLOGY RESEARCH INSTITUTE CO., LTD. |
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| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170329 |