CN105399103A - Fumed silica flatting powder and preparation method thereof - Google Patents
Fumed silica flatting powder and preparation method thereof Download PDFInfo
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- CN105399103A CN105399103A CN201510978703.6A CN201510978703A CN105399103A CN 105399103 A CN105399103 A CN 105399103A CN 201510978703 A CN201510978703 A CN 201510978703A CN 105399103 A CN105399103 A CN 105399103A
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- silicon
- flatting silica
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- aerosil flatting
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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
- C01B33/126—Preparation of silica of undetermined type
-
- 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
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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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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- 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
- C01P2006/12—Surface area
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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
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses fumed silica flatting powder and its preparation method. Base stock of the flatting powder is uniform fumed silica with its particle size being 3-8 micrometers. The base stock undergoes surface amination treatment. The preparation method comprises the following steps: hydrolyzing chlorosilane in high-temperature oxyhydrogen flame to prepare the nanometer fumed silica; during aggregation process, surface amination treatment is finished; a product with by-products removed is ground to specific particle size, and then grading treatment is carried out to prepare the fumed silica flatting powder. The product can be widely used in multiple complex systems to achieve an excellent flatting effect.
Description
Technical field
The present invention relates to a kind of flatting silica, particularly relate to a kind of aerosil flatting silica and preparation method thereof.
Background technology
In recent years, the coating of China and leather market were through development, and ultimate production leaps to the first in the world.The once advantages such as once the light coating of high gloss had been bright in colour with it, bright, deeply like by human consumer, but along with the raising of people's living standard, human consumer feels that hard-gloss paint film forming rear surface is reflective more serious, the eyes of people are harmful to, on the other hand the aesthetic standards of human consumer are more and more inclined to leisure, fashion and personalization, and China's automobile and household electric appliances is flourish in addition.Result in people sharply to increase the low-luster coating and leather products demand with soft outward appearance, the demand of various flatting silica also constantly increases.
Tradition flatting silica mainly contains following five classes: paraffin, talcum powder, polyacrylamide, precipitated silica, undressed fumed silica.Mainly there is following shortcoming in this five classes flatting silica: the transparency is bad, affects the color and luster of coating itself; Adding proportion is excessive, high cost; Anti scuffing performance is bad; Dispersing property is bad; Comparatively large on dope viscosity impact, be unfavorable for construction.
Summary of the invention
The object of the present invention is to provide a kind of aerosil flatting silica and preparation method thereof, solve the existing flatting silica transparency bad, affect the color and luster of coating itself; Adding proportion is excessive, high cost; Anti scuffing performance is bad; Dispersing property is bad; Comparatively large on dope viscosity impact, be unfavorable for the problem of constructing.
The present invention is achieved by the following technical solutions:
A kind of aerosil flatting silica, the content >99% of its silicon-dioxide quality mark, its specific surface area is 100-400m2/g; Its primary partical diameter is 8-15 nanometer, and after grinding stage treatment, median size is 3-8 micron.
The nano-silica surface of above-mentioned aerosil flatting silica is through amido process in hydrophobic performance, and its hydrophobic rate is 25%-65%, and hydrophobic rate calculates with nano-silica surface hydroxyl ratio.
The metal ion content of above-mentioned aerosil flatting silica is not more than 60ppm.
A preparation method for aerosil flatting silica, is realized by following steps:
Step one, chlorosilane gas after vaporizer high-temperature evaporation are under the bringing into adding warm air, continuous input silicon dioxde reaction device, add hot hydrogen and input silicon dioxde reaction device continuously by hydrogen inlet, there is pyrohydrolysis in the thermal-flame of the hydrogen of chlorosilane in silicon dioxde reaction device, oxygen combustion and generate nano silicon, control the reaction ratio of chlorosilane, hydrogen, oxygen, make chlorosilane: hydrogen: oxygen proportion is 1:0.05-0.4:0.75-1.05, in aforementioned proportion, the unit of chlorosilane is kg, the unit of hydrogen is NM
3, oxygen unit be NM
3;
The nano silicon that step 2, reaction generate enters collector to be assembled, surface treatment agent after high-temperature evaporation inputs collector leading portion continuously by treatment agent entrance, control the mass ratio of nano silicon, treatment agent, make nano silicon: treatment agent is 1:0.01-0.15;
Step 3, reaction suppressor after high-temperature evaporation input collector end continuously by inhibitor entrance, the nano silicon reaching processing requirements is undertaken by inhibitor stopped reaction, and silica aggregate is completed in collector, control the mass ratio of nano silicon, inhibitor, make nano silicon: inhibitor is 1:0-0.35;
Step 4, the silicon-dioxide assembled input finishing apparatus continuously and remove its by product, make its 4% methanol solution pH value reach 6-8;
Step 5, remove by product after silicon-dioxide utilize rotatory feeder valve continus convergence to harmonious material device, evenly micronizer mill is delivered to again by harmonious material device, in pulverizer, silicon-dioxide is pulverized, controlling the median size after pulverizing is D50, make its D50 be 3-8 micron, and make its plastisied dispersion D90-D10/D50<1.0;
Step 6, through pulverizing after silicon-dioxide be fed continuously to surge tank, evenly stage equipment is delivered to again by rotatory feeder valve, sizing screening is carried out to the silicon-dioxide of specified particle diameter and plastisied dispersion, silicon-dioxide after sizing screening is delivered to feed bin through discharge port, gets product after packaging.
In step one, selected chlorosilane can be the mixture of silicon tetrachloride, trichlorosilane, monomethyl trichlorosilane, monomethyl hydrogen dichlorosilane and above chlorosilane.
In step 2 and step 3, treatment agent entrance and inhibitor entrance all arrange multiple entrance, by different in-let dimple surface-treateds reaction initial time and intermission.
In step 5, harmonious material device, except getting rid of gas unnecessary in material, also has a function to be cool, after temperature of charge reaches room temperature, is delivered to micronizer mill again.
Described treatment agent can be methylamine, dimethylamine, Trimethylamine 99 or above any two kinds or three kinds of mixtures.
Described inhibitor can be methyl alcohol, ethanol, ethylene glycol, propyl alcohol, nitrogen or above any two kinds or three kinds or four kinds or five kinds of mixtures.
Technique effect of the present invention is: the present invention has high transparent, does not affect the color and luster of coating itself; High extinction, general adding proportion can meet the requirements of extinction effect at 0.5%-2%; Polymolecularity, can reach good distribution in polarity or non-polar system, not produce precipitation; The anti scuffing performance that coating surface is stronger can be given; The viscosity of coating itself is not had an impact.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of preparation method of the present invention.
In the drawings, 1, silicon dioxde reaction device 2, collector 3, finishing apparatus 4, harmonious material device 5, micronizer mill 6, surge tank 7, stage equipment 8, feed bin.
Embodiment
Describe below in conjunction with accompanying drawing 1 beneficial effect that the present invention has in detail, be intended to help reader to understand essence of the present invention better, but any restriction can not be formed to enforcement of the present invention and protection domain.
A kind of aerosil flatting silica, the content >99% of its silicon-dioxide quality mark, its specific surface area is 100-400m2/g; Its primary partical diameter is 8-15 nanometer, and after grinding stage treatment, median size is 3-8 micron.
The nano-silica surface of above-mentioned aerosil flatting silica is through amido process in hydrophobic performance, and its hydrophobic rate is 25%-65%, and hydrophobic rate calculates with nano-silica surface hydroxyl ratio.
The metal ion content of above-mentioned aerosil flatting silica is not more than 60ppm.
A kind of aerosil flatting silica and preparation scheme thereof, concrete steps are as follows:
1, the silicon tetrachloride gas after vaporizer high-temperature evaporation is under the intervention adding warm air, continuous input silicon dioxde reaction device (1), add hot hydrogen and input silicon dioxde reaction device (1) continuously by hydrogen inlet, there is pyrohydrolysis in the thermal-flame of the hydrogen of chlorosilane in silicon dioxde reaction device (1), oxygen combustion and generate nano silicon, control the reaction ratio of chlorosilane, hydrogen, oxygen, make chlorosilane (kg): hydrogen (NM
3): oxygen (NM
3) be 1:0.32:0.95;
2, the nano silicon that reaction generates enters collector (2) to be assembled, treatment agent Trimethylamine 99 after high-temperature evaporation inputs collector (2) leading portion continuously by treatment agent entrance, control the mass ratio of nano silicon, treatment agent, make nano silicon: treatment agent is 1:0.07;
3, the reaction suppressor ethylene glycol after high-temperature evaporation and nitrogen mixture input collector (2) end continuously by inhibitor entrance, nano silicon place being reached processing requirements is undertaken by inhibitor stopped reaction, and silica aggregate is completed in collector (2), control the mass ratio of nano silicon, inhibitor, make nano silicon: inhibitor is 1:0.24;
4, the silicon-dioxide assembled inputs finishing apparatus (3) continuously and removes its by product, makes its 4% methanol solution pH value reach 6-8;
5, the silicon-dioxide removed after by product utilizes rotatory feeder valve continus convergence to harmonious material device (4), when in harmonious material device (4), temperature of charge is reduced to room temperature, micronizer mill (5) is evenly delivered to by rotary feeding valve, in micronizer mill (5), silicon-dioxide is pulverized, control the median size D50 after pulverizing, setting pulverizing requires that D50 is 5 microns, and recording its plastisied dispersion is 0.75;
6, the silicon-dioxide after pulverizing is fed continuously to surge tank (6), stage equipment (7) is evenly delivered to again by rotatory feeder valve, classification removal is carried out to the particle that particle diameter is less than 3.8 microns and more than 6.2 microns, silicon-dioxide after sizing screening is delivered to feed bin (8) through discharge port, gets product after packaging.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (9)
1. an aerosil flatting silica, is characterized in that, the content >99% of its silicon-dioxide quality mark, and its specific surface area is 100-400m2/g; Its primary partical diameter is 8-15 nanometer, and after grinding stage treatment, median size is 3-8 micron.
2. a kind of aerosil flatting silica according to claim 1, it is characterized in that, the nano-silica surface of described aerosil flatting silica is hydrophobic performance through amido process, its hydrophobic rate is 25%-65%, and hydrophobic rate calculates with nano-silica surface hydroxyl ratio.
3. a kind of aerosil flatting silica according to claim 1, is characterized in that, the metal ion content of described aerosil flatting silica is not more than 60ppm.
4. a preparation method for aerosil flatting silica, is characterized in that,
(1) the silicon tetrachloride gas after vaporizer high-temperature evaporation is under the intervention adding warm air, continuous input silicon dioxde reaction device (1), add hot hydrogen and input silicon dioxde reaction device (1) continuously by hydrogen inlet, there is pyrohydrolysis in the thermal-flame of the hydrogen of chlorosilane in silicon dioxde reaction device (1), oxygen combustion and generate nano silicon, control the reaction ratio of chlorosilane, hydrogen, oxygen, make chlorosilane (kg): hydrogen (NM
3): oxygen (NM
3) be 1:0.32:0.95;
(2) nano silicon that reaction generates enters collector (2) to be assembled, treatment agent Trimethylamine 99 after high-temperature evaporation inputs collector (2) leading portion continuously by treatment agent entrance, control the mass ratio of nano silicon, treatment agent, make nano silicon: treatment agent is 1:0.07;
(3) the reaction suppressor ethylene glycol after high-temperature evaporation and nitrogen mixture input collector (2) end continuously by inhibitor entrance, nano silicon place being reached processing requirements is undertaken by inhibitor stopped reaction, and silica aggregate is completed in collector (2), control the mass ratio of nano silicon, inhibitor, make nano silicon: inhibitor is 1:0.24;
(4) silicon-dioxide assembled inputs finishing apparatus (3) continuously and removes its by product, makes its 4% methanol solution pH value reach 6-8;
(5) silicon-dioxide removed after by product utilizes rotatory feeder valve continus convergence to harmonious material device (4), when in harmonious material device (4), temperature of charge is reduced to room temperature, micronizer mill (5) is evenly delivered to by rotary feeding valve, in micronizer mill (5), silicon-dioxide is pulverized, control the median size D50 after pulverizing, setting pulverizing requires that D50 is 5 microns, and recording its plastisied dispersion is 0.75;
(6) silicon-dioxide after pulverizing is fed continuously to surge tank (6), stage equipment (7) is evenly delivered to again by rotatory feeder valve, classification removal is carried out to the particle that particle diameter is less than 3.8 microns and more than 6.2 microns, silicon-dioxide after sizing screening is delivered to feed bin (8) through discharge port, gets product after packaging.
5. the preparation method of a kind of aerosil flatting silica according to claim 4, it is characterized in that, in step one, selected chlorosilane can be the mixture of silicon tetrachloride, trichlorosilane, monomethyl trichlorosilane, monomethyl hydrogen dichlorosilane and above chlorosilane.
6. the preparation method of a kind of aerosil flatting silica according to claim 4, it is characterized in that, in step 2 and step 3, treatment agent entrance and inhibitor entrance all arrange multiple entrance, by different in-let dimple surface-treateds reaction initial time and intermission.
7. the preparation method of a kind of aerosil flatting silica according to claim 4, it is characterized in that, in step 5, harmonious material device is except getting rid of gas unnecessary in material, also have a function to be cool, after temperature of charge reaches room temperature, be delivered to micronizer mill again.
8. the preparation method of a kind of aerosil flatting silica according to claim 4, is characterized in that, described treatment agent can be methylamine, dimethylamine, Trimethylamine 99 or above any two kinds or three kinds of mixtures.
9. the preparation method of a kind of aerosil flatting silica according to claim 4, it is characterized in that, described inhibitor can be methyl alcohol, ethanol, ethylene glycol, propyl alcohol, nitrogen or above any two kinds or three kinds or four kinds or five kinds of mixtures.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106634149A (en) * | 2016-11-15 | 2017-05-10 | 浙江富士特硅材料有限公司 | Preparation method of gas-phase silicon dioxide for delustering coating |
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US5458916A (en) * | 1992-07-02 | 1995-10-17 | Wacker-Chemie Gmbh | Hydrophobicization of pyrogenic silica |
CN1422805A (en) * | 2002-12-30 | 2003-06-11 | 广州吉必时科技实业有限公司 | High-dispersion nano silicon dioxide preparation method |
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CN101723317B (en) * | 2009-12-09 | 2013-02-27 | 广州吉必盛科技实业有限公司 | Method and device for on-line continuous surface treatment of hydrophilic nano-silicon dioxide |
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2015
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Patent Citations (4)
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US5458916A (en) * | 1992-07-02 | 1995-10-17 | Wacker-Chemie Gmbh | Hydrophobicization of pyrogenic silica |
CN1422805A (en) * | 2002-12-30 | 2003-06-11 | 广州吉必时科技实业有限公司 | High-dispersion nano silicon dioxide preparation method |
CN1687246A (en) * | 2005-03-28 | 2005-10-26 | 广州吉必时科技实业有限公司 | Method for preparing hydrophobic type nano silicon dioxide thruogh continuous surface treatment |
CN101723317B (en) * | 2009-12-09 | 2013-02-27 | 广州吉必盛科技实业有限公司 | Method and device for on-line continuous surface treatment of hydrophilic nano-silicon dioxide |
Non-Patent Citations (3)
Title |
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中国国家标准化管理委员会 等: ""气相二氧化硅"", 《中国标准化》 * |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106634149A (en) * | 2016-11-15 | 2017-05-10 | 浙江富士特硅材料有限公司 | Preparation method of gas-phase silicon dioxide for delustering coating |
CN106634149B (en) * | 2016-11-15 | 2019-09-20 | 浙江富士特硅材料有限公司 | A kind of preparation method of antiglossing pigment fumed silica |
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Denomination of invention: Fumed silica flatting powder and preparation method thereof Effective date of registration: 20181105 Granted publication date: 20171205 Pledgee: China Co truction Bank Corp Jingdezhen branch Pledgor: JIANGXI BLACKCAT CARBON BLACK CO., LTD. Registration number: 2018360000029 |
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