CN103183352B - A kind of production method of Superfine Silica Dioxide - Google Patents

A kind of production method of Superfine Silica Dioxide Download PDF

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Publication number
CN103183352B
CN103183352B CN201310113429.7A CN201310113429A CN103183352B CN 103183352 B CN103183352 B CN 103183352B CN 201310113429 A CN201310113429 A CN 201310113429A CN 103183352 B CN103183352 B CN 103183352B
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micron
granularity
carbon black
white carbon
silica dioxide
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CN103183352A (en
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袁波
袁建东
袁涛
任启军
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Weifang Jiejia New Material Co., Ltd
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WEIFANG JIEJIA CHEMICAL CO Ltd
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Abstract

The present invention relates to a kind of production method of Superfine Silica Dioxide, comprise the following steps: (1), according to weight percent, is got the white carbon black auxiliary material 10 ~ 20% that the white carbon black major ingredient 80 ~ 90% of granularity 300-400 micron and granularity are 150-200 micron, fully mixed; (2) by mixed material at 120-140 DEG C, constant temperature 3 ~ 6 hours, then Temperature fall is to room temperature; (3) supersonic jet mill is utilized to be ground into the product of granularity for 1-5 micron the material after cooling.Production method production technique of the present invention is simple, not high to ingredient requirement, can reduce production cost greatly.

Description

A kind of production method of Superfine Silica Dioxide
Technical field
The present invention relates to a kind of production method of Superfine Silica Dioxide, belong to new chemical materials field.
Background technology
Background technology silicon-dioxide 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 2the high-technology fields such as thin-film material then need the silicon-dioxide by high purity, ultra-fine, high whiteness.
Superfine Silica Dioxide is a kind of inorganic fine chemicals, because its tool educates uncommon particle characteristics, and namely minimum particle diameter (particle diameter of primary structure is 7 ~ 16nm), huge specific surface area (100-400m 2/ g), high purity (> 99.8) and its chaining tendency etc., show remarkable reinforcing, thickening property, thixotropy, extinction, dispersiveness, insulativity, non-stick property etc.Thus the fields such as rubber chamber, coating, tackiness agent, makeup, ink, plastics, medicine, agricultural chemicals, sealing agent are widely used in.
Domestic Superfine Silica Dioxide powder body material preparation is confined to gas phase synthesis method preparation, the Superfine Silica Dioxide powder body material prepared has the advantage of narrow particle size distribution (5-40nm), high purity and high whiteness, but mountain is in production capacity low (domestic current maximum production capacity 50 tons/year), energy consumption is high, price high (more than 70,000 yuan/ton), constrains its applying at industrial circles such as rubber, coating, paint.Along with high speed development and the industrial upgrading of China's manufacturing industry, rising fast to Superfine Silica Dioxide powder body material demand in domestic market, can only rely on import at present.Therefore country is own lists the technology of preparing of Superfine Silica Dioxide powder body material in emphasis program for tackling key problems in science and technology.
The preparation of Supermicro-composite material generally adopts Ball-stirring mill, vibration mill, sand milling, machine for cutting charge into pieces, ball mill, airflow milling, high-pressure water jet and mechanical shock pulverizer to carry out superfine grinding processing.Patent as publication number CN101074099A: adopt high-temperature calcination kaolin (not containing organic composition) to be raw material, through heating acidolysis mineral substance, washing, dehydration and drying process, prepare cellular silica powder body material, then be prepared into Superfine Silica Dioxide powder body material through hypersonic air flow pulverizing.The patent of number Authorization Notice No. CN100368291C: 97% will be more than or equal to containing silicon-dioxide, granularity is that 80 ~ 100 object silica powder raw ores wash desliming on agitating ball mill, silicon-dioxide after washing desliming is made into the ore pulp aqueous solution that concentration is 40% ~ 60%, add the tensio-active agent of 0.1-0.3wt%, with ZrO 2ball is ball-milling medium, and ratio of grinding media to material is 3:1 ~ 5:1, at agitating ball mill grinding 2 ~ 6h, add the concentrated hydrochloric acid of 1-3wt% and the hydrofluoric acid ball milling 0.5 ~ 2h again of 1-3wt% again, then add sodium hydroxide adjusted to ph between 2 ~ 3, add amine salt, grinding 5 ~ 10min, removing surfactant foam, leave standstill, remove upper strata clear water, then wash suction filtration, dry, obtain Superfine Silica Dioxide.The complex process of these two kinds of preparation methods, production cost is higher.What particularly utilize supersonic speed pulverizer to pulverize is higher to the requirement of raw material, needs now raw material to be prepared into cellular silica powder body material, could pulverize.
Summary of the invention
The invention provides a kind of production method of Superfine Silica Dioxide, it solve the complex process of the production method of existing Superfine Silica Dioxide, the problems such as production cost is high.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A preparation method for Superfine Silica Dioxide, comprises the following steps:
(1) according to weight percent, get the white carbon black auxiliary material 10 ~ 20% that the white carbon black major ingredient 80 ~ 90% of granularity 300-400 micron and granularity are 150-200 micron, fully mix;
(2) by mixed material at 120-140 DEG C, constant temperature 3 ~ 6 hours, then Temperature fall is to room temperature;
(3) supersonic jet mill is utilized to be ground into the product of granularity for 1-5 micron the material after cooling.
Further, a preferred embodiment of the present invention: according to weight percent, white carbon black major ingredient be 85% and white carbon black auxiliary material be 15%.
Further, a preferred embodiment of the present invention: described thermostat temperature is 135 DEG C, constant temperature time is 4 hours.
Further, a preferred embodiment of the present invention: the granularity of described white carbon black major ingredient to be the granularity of 330-380 micron and white carbon black auxiliary material be 180-200 micron.
Beneficial effect of the present invention:
The present invention is with the white carbon black of granularity 300-400 micron for major ingredient, and the white carbon black of 150-200 micron is auxiliary material, dewaters through high temperature, then utilizes supersonic jet mill to pulverize, the silicon dioxide powder of 1 ~ 5 micron.Production technique is simple, not high to ingredient requirement, can reduce production cost greatly.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is production technological process of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
As shown in Figure 1, a kind of preparation method of Superfine Silica Dioxide, comprises the following steps:
(1) according to weight percent, get the white carbon black auxiliary material 10 ~ 20% that the white carbon black major ingredient 80 ~ 90% of granularity 300-400 micron and granularity are 150-200 micron, fully mix;
(2) by mixed material at 120-140 DEG C, constant temperature 3 ~ 6 hours, then Temperature fall is to room temperature;
(3) supersonic jet mill is utilized to be ground into the product of granularity for 1-5 micron the material after cooling.
Embodiment 1
A preparation method for Superfine Silica Dioxide, comprises the following steps:
(1) according to weight percent, get the white carbon black auxiliary material 20% that the white carbon black major ingredient 80% of granularity 300-400 micron and granularity are 150-200 micron, fully mix;
(2) by mixed material at 140 DEG C, constant temperature 3 hours, then Temperature fall is to room temperature;
(3) material after Drying and cooling is transported to feeding apparatus mouth by transit wagon for subsequent use;
Open large-scale air and be compressed into complete equipment, before noting large-scale compressor start, first cooling-water pump is opened cooling apparatus;
Open air compressing gas sweetening drying installation, rise to 8.5 kilograms of pressure through power-assisted (after Hydrothermal Synthesis) with the high pressure dry gas after refining plant dry decontamination for subsequent use;
By the dry high pressure gas that purified through Cemented filling in supersonic speed pulverizer, open main frame valve, form negative pressure through high-pressure rotary speed in main body and suck material drying by feed-pipe from feed bin, material sprays convection current material 2 through porous and doubly forms the pulverizing of ultra-fine microstage to velocity of sound collision, comminuting matter rises in classification trapping storehouse automatically after reaching required control criterion, material is introduced discharging bin by air inducing equipment by main frame and trapping storehouse blue wind pipeline gently.Then lay the material inspection by sampling of having produced through extra pulse, carry out after the assay was approved filling, cross claim, sealing, hit-gain trust, then finished product.The granularity of the finished product of gained is at 1-5 micron.
Embodiment 2
A preparation method for Superfine Silica Dioxide, comprises the following steps:
(1) according to weight percent, get the white carbon black auxiliary material 15% that the white carbon black major ingredient 85% of granularity 300-400 micron and granularity are 150-200 micron, fully mix;
(2) by mixed material at 135 DEG C, constant temperature 4 hours, then Temperature fall is to room temperature;
(3) material after Drying and cooling is transported to feeding apparatus mouth by transit wagon for subsequent use;
Open large-scale air and be compressed into complete equipment, before noting large-scale compressor start, first cooling-water pump is opened cooling apparatus;
Open air compressing gas sweetening drying installation, rise to 8.5 kilograms of pressure through power-assisted (after Hydrothermal Synthesis) with the high pressure dry gas after refining plant dry decontamination for subsequent use;
By the dry high pressure gas that purified through Cemented filling in supersonic speed pulverizer, open main frame valve, form negative pressure through high-pressure rotary speed in main body and suck material drying by feed-pipe from feed bin, material sprays convection current material 2 through porous and doubly forms the pulverizing of ultra-fine microstage to velocity of sound collision, comminuting matter rises in classification trapping storehouse automatically after reaching required control criterion, material is introduced discharging bin by air inducing equipment by main frame and trapping storehouse blue wind pipeline gently.Then lay the material inspection by sampling of having produced through extra pulse, carry out after the assay was approved filling, cross claim, sealing, hit-gain trust, then finished product.The granularity of the finished product of gained is between 1-3 micron.
Embodiment 3
A preparation method for Superfine Silica Dioxide, comprises the following steps:
(1) according to weight percent, get the white carbon black auxiliary material 10% that the white carbon black major ingredient 90% of granularity 330-380 micron and granularity are 180-200 micron, fully mix;
(2) by mixed material at 120 DEG C, constant temperature 6 hours, then Temperature fall is to room temperature;
(3) material after Drying and cooling is transported to feeding apparatus mouth by transit wagon for subsequent use;
Open large-scale air and be compressed into complete equipment, before noting large-scale compressor start, first cooling-water pump is opened cooling apparatus;
Open air compressing gas sweetening drying installation, rise to 8.5 kilograms of pressure through power-assisted (after Hydrothermal Synthesis) with the high pressure dry gas after refining plant dry decontamination for subsequent use;
By the dry high pressure gas that purified through Cemented filling in supersonic speed pulverizer, open main frame valve, form negative pressure through high-pressure rotary speed in main body and suck material drying by feed-pipe from feed bin, material sprays convection current material 2 through porous and doubly forms the pulverizing of ultra-fine microstage to velocity of sound collision, comminuting matter rises in classification trapping storehouse automatically after reaching required control criterion, material is introduced discharging bin by air inducing equipment by main frame and trapping storehouse blue wind pipeline gently.Then lay the material inspection by sampling of having produced through extra pulse, carry out after the assay was approved filling, cross claim, sealing, hit-gain trust, then finished product.The granularity of the finished product of gained is at 1-3 micron.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (4)

1. a preparation method for Superfine Silica Dioxide, is characterized in that, comprises the following steps:
(1) according to weight percent, get the white carbon black auxiliary material 10 ~ 20% that the white carbon black major ingredient 80 ~ 90% of granularity 300-400 micron and granularity are 150-200 micron, fully mix;
(2) by mixed material at 120-140 DEG C, constant temperature 3 ~ 6 hours, then Temperature fall is to room temperature;
(3) supersonic jet mill is utilized to be ground into the product of granularity for 1-5 micron the material after cooling.
2. the preparation method of a kind of Superfine Silica Dioxide according to claim 1, is characterized in that: according to weight percent, and 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 Superfine Silica Dioxide according to claim 1, is characterized in that: described thermostat temperature is 135 DEG C, and constant temperature time is 4 hours.
4. the preparation method of a kind of Superfine Silica Dioxide according to any one of claims 1 to 3, is characterized in that: the granularity of described white carbon black major ingredient is the granularity of 330-380 micron and white carbon black auxiliary material is 180-200 micron.
CN201310113429.7A 2013-04-03 2013-04-03 A kind of production method of Superfine Silica Dioxide Active CN103183352B (en)

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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 (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7695705B2 (en) * 2005-08-26 2010-04-13 Ppg Industries Ohio, Inc. Method and apparatus for the production of ultrafine silica particles from solid silica powder and related coating compositions

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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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.

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