CN103183352A - Production method of ultra-fine silicon dioxide - Google Patents
Production method of ultra-fine silicon dioxide Download PDFInfo
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- CN103183352A CN103183352A CN2013101134297A CN201310113429A CN103183352A CN 103183352 A CN103183352 A CN 103183352A CN 2013101134297 A CN2013101134297 A CN 2013101134297A CN 201310113429 A CN201310113429 A CN 201310113429A CN 103183352 A CN103183352 A CN 103183352A
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Abstract
The invention relates to a production method of ultra-fine silicon dioxide, which comprises the following steps: (1) taking 80 to 90 percent of white carbon black main material with a granularity of 300 to 400 microns, taking 10 to 20 percent of white carbon black auxiliary material with a granularity of 150 to 200 microns according to weight percent , and mixing the white carbon black main material and the white carbon black auxiliary material fully,(2) keeping the mixed material for 3 to 6 hours at a constant temperature of 120-140 DEG C, and then cooling down to the room temperature naturally, and (3) pulverizing the cooled down material into product with a granularity of 1 to 5 microns by using a supersonic airflow pulverizer. The production method, provided by the invention, has the advantages that the production technology is simple; the requirement on the raw material is not high; and the production cost can be greatly reduced.
Description
Technical field
The present invention relates to a kind of production method of ultra tiny silicon-dioxide, belong to the new chemical materials field.
Background technology
Background technology silicon-dioxide is as a kind of important industrial raw material, in field extensive application such as building materials, chemical industry, medical treatment, things.As glass, plastics, rubber, paint, water-proof and anti-corrosive material etc.Special cermacis, high-grade paint paint, Electronic Packaging, optical-fibre communications, unicircuit, opticinstrument, Si0
2High-technology fields such as thin-film material then need be used the silicon-dioxide of high purity, ultra-fine, high whiteness.
Ultra tiny silicon-dioxide is a kind of inorganic fine chemicals, because its tool is educated uncommon particle characteristics, (particle diameter of primary structure is 7～16nm) to namely minimum particle diameter, huge specific surface area (100-400m
2/ g), high purity (＞99.8) and its chaining tendency etc. show remarkable reinforcement, thickening property, thixotropy, extinction, dispersiveness, insulativity, non-stick property etc.Thereby be widely used in fields such as rubber chamber, coating, tackiness agent, makeup, printing ink, plastics, medicine, agricultural chemicals, sealing agent.
Domestic ultra tiny silicon-dioxide powdery material preparation is confined to the gas phase synthesis method preparation, the ultra tiny silicon-dioxide powdery material of preparing has the advantage of narrow particle size distribution (5-40nm), high purity and high whiteness, but the mountain is in production capacity low (50 tons/year of domestic present maximum production capacities), the energy consumption height, price height (more than 70,000 yuan/ton) has restricted its applying at industrial circles such as rubber, coating, paint.Along with the manufacturing high speed development of China and industrial upgrading, the domestic market can only rely on import at present to ultra tiny silicon-dioxide powdery materials demand amount fast rise.Therefore country is own lists the technology of preparing of ultra tiny silicon-dioxide powdery material in the emphasis program for tackling key problems in science and technology.
The preparation of ultra tiny material generally adopts stirring mill, vibration mill, sand milling, the machine of delaminating, ball mill, airflow milling, high-pressure water jet and mechanical shock pulverizer to carry out superfine grinding processing.Patent as publication number CN101074099A: adopting high-temperature calcination kaolin (not containing organic composition) is raw material, through heating acidolysis mineral substance, washing, dehydration and drying process, prepare the cellular silica powder body material, pulverize through hypersonic air flow again and be prepared into ultra tiny silicon-dioxide powdery material.The patent of number Granted publication CN100368291C: will contain silicon-dioxide more than or equal to 97%, granularity is that 80～100 purpose silica powder raw ores are washed desliming at agitating ball mill, it is 40%～60% the ore pulp aqueous solution that the silicon-dioxide of washing after the desliming is made into concentration, the tensio-active agent that adds 0.1-0.3wt% is with ZrO
2Ball is ball-milling medium, and ratio of grinding media to material is 3:1～5:1, grinds 2～6h at agitating ball mill, the hydrofluoric acid that adds the concentrated hydrochloric acid of 1-3wt% and 1-3wt% again is ball milling 0.5～2h again, add sodium hydroxide then and adjust the pH value between 2～3, add amine salt, grind 5～10min, remove surfactant foam, leave standstill, remove the upper strata clear water, wash suction filtration again, oven dry namely gets ultra tiny silicon-dioxide.These two kinds of preparation methods' complex process, production cost is higher.Utilize particularly that the supersonic speed pulverizer pulverizes to the requirement of raw material than higher, need existing feedstock production is become the cellular silica powder body material, could pulverize.
Summary of the invention
The invention provides a kind of production method of ultra tiny silicon-dioxide, it has solved the complex process of the production method of existing ultra tiny silicon-dioxide, problems such as production cost height.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of preparation method of ultra tiny silicon-dioxide may further comprise the steps:
(1) according to weight percent, get the white carbon black major ingredient 80～90% of granularity 300-400 micron and the white carbon black auxiliary material 10～20% that granularity is the 150-200 micron, fully mix;
(2) with mixed material at 120-140 ℃, constant temperature 3～6 hours cools to room temperature then naturally;
(3) material after will lowering the temperature utilizes supersonic jet mill to be ground into granularity to be the product of 1-5 micron.
Further, a preferred embodiment of the present invention: according to weight percent, the white carbon black major ingredient be 85% and the white carbon black auxiliary material be 15%.
Further, a preferred embodiment of the present invention: described thermostat temperature is 135 ℃, and constant temperature time is 4 hours.
Further, a preferred embodiment of the present invention: the granularity of described white carbon black major ingredient is that the granularity of 330-380 micron and white carbon black auxiliary material is the 180-200 micron.
Beneficial effect of the present invention:
The present invention is major ingredient with the white carbon black of granularity 300-400 micron, and the white carbon black of 150-200 micron is auxiliary material, dewaters through high temperature, utilizes supersonic jet mill to pulverize then, get final product 1～5 micron silicon dioxide powder.Production technique is simple, and is not high to ingredient requirement, can reduce production costs greatly.
Description of drawings
In order to be illustrated more clearly in the embodiment of the invention or technical scheme of the prior art, to do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art below, apparently, accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is technological process of production figure of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the invention, the technical scheme in the embodiment of the invention is clearly and completely described, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that obtains under the creative work prerequisite.
As shown in Figure 1, a kind of preparation method of ultra tiny silicon-dioxide may further comprise the steps:
(1) according to weight percent, get the white carbon black major ingredient 80～90% of granularity 300-400 micron and the white carbon black auxiliary material 10～20% that granularity is the 150-200 micron, fully mix;
(2) with mixed material at 120-140 ℃, constant temperature 3～6 hours cools to room temperature then naturally;
(3) material after will lowering the temperature utilizes supersonic jet mill to be ground into granularity to be the product of 1-5 micron.
Embodiment 1
A kind of preparation method of ultra tiny silicon-dioxide may further comprise the steps:
(1) according to weight percent, get the white carbon black major ingredient 80% of granularity 300-400 micron and the white carbon black auxiliary material 20% that granularity is the 150-200 micron, fully mix;
(2) with mixed material at 140 ℃, constant temperature 3 hours cools to room temperature then naturally;
(3) will drying cooled material, to be transported to the equipment mouth that feeds intake by transit wagon standby;
Open large-scale air and be compressed into complete equipment, note earlier cooling-water pump being opened cooling apparatus before the large-scale compressor start;
Open air pressurized gas purge drying device, it is standby to rise to 8.5 kilograms of pressure through power-assisted (after hydro-thermal is synthetic) with the high pressure dry gas behind the refining plant dry decontamination;
With purify good dry high pressure gas through pipe-line transportation to the supersonic speed pulverizer, open the main frame valve, form negative pressure through high-pressure rotary speed in the main body and suck the oven dry material by feed-pipe from feed bin, material forms ultra-fine microstage to the velocity of sound collision for 2 times through porous injection convection current material and pulverizes, comminuting matter rises in the classification capture storehouse after reaching required control criterion automatically, and feed bin is introduced out with material gently by air inducing equipment in main frame and blue airduct road, capture storehouse.Lay through extra pulse then and produce good material inspection by sampling, carry out can after the assay was approved, cross claim, seal, hit-gain trust, finished product then.The granularity of the finished product of gained is at the 1-5 micron.
Embodiment 2
A kind of preparation method of ultra tiny silicon-dioxide may further comprise the steps:
(1) according to weight percent, get the white carbon black major ingredient 85% of granularity 300-400 micron and the white carbon black auxiliary material 15% that granularity is the 150-200 micron, fully mix;
(2) with mixed material at 135 ℃, constant temperature 4 hours cools to room temperature then naturally;
(3) will drying cooled material, to be transported to the equipment mouth that feeds intake by transit wagon standby;
Open large-scale air and be compressed into complete equipment, note earlier cooling-water pump being opened cooling apparatus before the large-scale compressor start;
Open air pressurized gas purge drying device, it is standby to rise to 8.5 kilograms of pressure through power-assisted (after hydro-thermal is synthetic) with the high pressure dry gas behind the refining plant dry decontamination;
With purify good dry high pressure gas through pipe-line transportation to the supersonic speed pulverizer, open the main frame valve, form negative pressure through high-pressure rotary speed in the main body and suck the oven dry material by feed-pipe from feed bin, material forms ultra-fine microstage to the velocity of sound collision for 2 times through porous injection convection current material and pulverizes, comminuting matter rises in the classification capture storehouse after reaching required control criterion automatically, and feed bin is introduced out with material gently by air inducing equipment in main frame and blue airduct road, capture storehouse.Lay through extra pulse then and produce good material inspection by sampling, carry out can after the assay was approved, cross claim, seal, hit-gain trust, finished product then.The granularity of the finished product of gained is between the 1-3 micron.
Embodiment 3
A kind of preparation method of ultra tiny silicon-dioxide may further comprise the steps:
(1) according to weight percent, get the white carbon black major ingredient 90% of granularity 330-380 micron and the white carbon black auxiliary material 10% that granularity is the 180-200 micron, fully mix;
(2) with mixed material at 120 ℃, constant temperature 6 hours cools to room temperature then naturally;
(3) will drying cooled material, to be transported to the equipment mouth that feeds intake by transit wagon standby;
Open large-scale air and be compressed into complete equipment, note earlier cooling-water pump being opened cooling apparatus before the large-scale compressor start;
Open air pressurized gas purge drying device, it is standby to rise to 8.5 kilograms of pressure through power-assisted (after hydro-thermal is synthetic) with the high pressure dry gas behind the refining plant dry decontamination;
With purify good dry high pressure gas through pipe-line transportation to the supersonic speed pulverizer, open the main frame valve, form negative pressure through high-pressure rotary speed in the main body and suck the oven dry material by feed-pipe from feed bin, material forms ultra-fine microstage to the velocity of sound collision for 2 times through porous injection convection current material and pulverizes, comminuting matter rises in the classification capture storehouse after reaching required control criterion automatically, and feed bin is introduced out with material gently by air inducing equipment in main frame and blue airduct road, capture storehouse.Lay through extra pulse then and produce good material inspection by sampling, carry out can after the assay was approved, cross claim, seal, hit-gain trust, finished product then.The granularity of the finished product of gained is at the 1-3 micron.
The above only is preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. the preparation method of a ultra tiny silicon-dioxide is characterized in that, may further comprise the steps:
(1) according to weight percent, get the white carbon black major ingredient 80～90% of granularity 300-400 micron and the white carbon black auxiliary material 10～20% that granularity is the 150-200 micron, fully mix;
(2) with mixed material at 120-140 ℃, constant temperature 3～6 hours cools to room temperature then naturally;
(3) material after will lowering the temperature utilizes supersonic jet mill to be ground into granularity to be the product of 1-5 micron.
2. the preparation method of a kind of ultra tiny silicon-dioxide according to claim 1, it is characterized in that: according to weight percent, described white carbon black major ingredient is 85%, and described white carbon black auxiliary material is 15%.
3. the preparation method of a kind of ultra tiny silicon-dioxide according to claim 1, it is characterized in that: described thermostat temperature is 135 ℃, constant temperature time is 4 hours.
4. according to the preparation method of each described a kind of ultra tiny silicon-dioxide of claim 1～3, it is characterized in that: the granularity of described white carbon black major ingredient is that the granularity of 330-380 micron and white carbon black auxiliary material is the 180-200 micron.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310113429.7A CN103183352B (en) | 2013-04-03 | 2013-04-03 | A kind of production method of Superfine Silica Dioxide |
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| CN201310113429.7A CN103183352B (en) | 2013-04-03 | 2013-04-03 | A kind of production method of Superfine Silica Dioxide |
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| CN103183352B CN103183352B (en) | 2015-08-19 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111204769A (en) * | 2020-01-14 | 2020-05-29 | 中南大学 | Method for preparing spherical white carbon black by supersonic carbon dioxide fluid carbonization method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070048206A1 (en) * | 2005-08-26 | 2007-03-01 | Ppg Industries Ohio, Inc. | Method and apparatus for the production of ultrafine silica particles from solid silica powder and related coating compositions |
| CN1958446A (en) * | 2006-11-17 | 2007-05-09 | 四川大学 | Method for preparing high purity super fine silicon miropowder by using powder of natural quartz |
| CN102145898A (en) * | 2011-05-05 | 2011-08-10 | 张冬玲 | Production method of silicon dioxide ultrafine powder |
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2013
- 2013-04-03 CN CN201310113429.7A patent/CN103183352B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070048206A1 (en) * | 2005-08-26 | 2007-03-01 | Ppg Industries Ohio, Inc. | Method and apparatus for the production of ultrafine silica particles from solid silica powder and related coating compositions |
| CN1958446A (en) * | 2006-11-17 | 2007-05-09 | 四川大学 | Method for preparing high purity super fine silicon miropowder by using powder of natural quartz |
| CN102145898A (en) * | 2011-05-05 | 2011-08-10 | 张冬玲 | Production method of silicon dioxide ultrafine powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111204769A (en) * | 2020-01-14 | 2020-05-29 | 中南大学 | Method for preparing spherical white carbon black by supersonic carbon dioxide fluid carbonization method |
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Address after: Hao Cheng Cun Cun Xi, Binhai District, Weifang City, Shandong Province Patentee after: Weifang Jiejia New Material Co., Ltd Address before: Hao Cheng Cun Cun Xi, Binhai District, Weifang City, Shandong Province Patentee before: WEIFANG JIEJIA CHEMICAL Co.,Ltd. |