CN1785803A - Continuous fluidized bed for gas phase preparing silicon dioxide and its industrial application - Google Patents
Continuous fluidized bed for gas phase preparing silicon dioxide and its industrial application Download PDFInfo
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Abstract
The present invention discloses a continuous fluidized bed for preparing silicon dioxide by using gas-phase process, and its industrial application. The described method adopts high-temperature mixed gas obtained by means of hydrogen gas combustion as fluidizing agent, in the fluidized bed reactor makes the nano SiO2 in the production process undergo the process of continuous deacidification treatment, and makes pH value of deacidified nano SiO2 be 3.7-4.2 and its water content be less than 2%.
Description
Technical Field
The invention relates to a fluidized bed reactor, in particular to nano silicon dioxide (SiO) for preparing by a gas phase method2) And industrial application thereof.
Background
Nano SiO prepared by gas phase method2The product is a high-tech inorganic fine chemical product, and can be widely applied to the fields of pre-rubber, coating, plastics, medicines, adhesives, printing ink, pesticides, catalysis, electronics, fine ceramics and the like besides the special properties of nano materials.
The white carbon black is prepared by using SiCl4Steam is prepared by high-temperature hydrolysis in oxyhydrogen flame, and the reaction equation is as follows:
or
As is clear from the above reaction formula, SiO accompanies2While a large amount of hydrogen chloride (HCl) gas is generated.
SiO2Is powder with small grain diameter (7-20nm) and large specific surface, so a large amount of HCl is absorbed in the preparation process. In the nano SiO2For most applications, for nano SiO2The amount of residual HCl adsorbed is critical, and the pH value is an important index for measuring the product quality. In addition, in the above reaction, the reactant water vapor is excessive, and the nano SiO2The product also absorbs a lot of water, and in order to meet the requirements of various application occasions, the contained water also needs to be removed together with HCl so as to meet the requirements of the specified product quality standard.
Gas phase method of nano SiO2In the production process, the nano SiO2Deacidification reactors are generally of two types. One is a fixed bed reactor, adding NH after preheating to a certain temperature3The dry air is introduced into the deacidification tower to be mixed with sodiumSiO rice2Powder contacts, and the deacidification effect is achieved through chemical reaction;
the other is to introduce air with high temperature into the fluidized bed, as disclosed in the patent of Sho 59-184710, and to achieve deacidification effect through long-term gas-solid two-phase mass transfer.
The first method artificially introduces impurities, which affect the product quality; the HCl generated by the reaction of the second method is secondarily adsorbed, the back mixing phenomenon is serious, the deacidification time is long, and the deacidified nano SiO has high purity2The water content of (A) is high, and the requirements of related aspects cannot be met.
Disclosure of Invention
One of the technical problems to be solved by the invention is to disclose a continuous fluidized bed of nano-silica prepared by a gas phase method, so as to overcome the defects in the prior art;
the second technical problem to be solved by the present invention is to disclose the application of the continuous fluidized bed in industry to meet the needs of the related aspects.
The continuous fluidized bed of the nano-silica prepared by the gas phase method comprises a cylindrical fluidized reaction section, a combustion device and an expansion collecting section:
the cylindrical fluidized reaction section is provided with a vertical fluidized reaction section clapboard, the upper part of the fluidized reaction section is positioned at the top end of the cylindrical fluidized reaction section, the lower part of the fluidized reaction section clapboard is spaced from the gas distributor, the two sides of the fluidized reaction section clapboard are connected with the inner wall of the cylindrical fluidized reaction section, and the fluidized reaction section clapboard can prevent solid-phase nascent state SiO2Back mixing;
the combustion device is arranged at the lower part of the fluidization reaction section, and a gas distributor is arranged between the combustion device and the fluidization reaction section and used for strengthening gas distribution and improving fluidization quality;
the expanded collection section is arranged at the upper part of the fluidized reaction section, the inner diameter of the expanded collection section is larger than that of the fluidized reaction section, an eccentric vertical collection section partition plate is arranged in the expanded collection section, the lower part of the expanded collection section is connected with the fluidized reaction section partition plate through an inclined plate, a gap is reserved between the upper part of the expanded collection section and the top end of the expanded collection section, and two sides of the collection section partition plate are connected with the inner wall of the expanded collection section to prevent gas-phase HCl back mixing and secondary adsorption;
SiO raw material2An inlet arranged at the top of the enlarged collecting section and connected with the fluidized reaction section through a connecting pipeCommunicating;
the product outlet is arranged at the middle upper part of the fluidized reaction section, and the tail gas outlet is arranged at the top of the enlarged collection section;
the continuous fluidized bed of the nano-silicon dioxide prepared by the gas phase method can be used for preparing the nano-silicon dioxide, and the application method comprises the following steps:
introducing hydrogen and air into a combustion device for combustion, introducinggas containing water vapor into a fluidized reaction section after passing through a body distributor, wherein the temperature of the gas containing water vapor is 300-650 ℃, the water vapor content is 5-25%, the gas velocity of the fluidized section is 2-15cm/s, the fluidization expansion rate is 3-7, the gas velocity of the expanded collection section is 0.5-1.5cm/s, and the average residence time is 15-30 min;
SiO raw material2Enters the fluidized reaction section through the inlet, and ensures the existence of SiO at the discharge port2The formed material seal is that the liquid level of the dense phase zone of the fluidized bed is kept 10-30cm above the discharge port.
Gas containing water vapor and SiO raw material entering into fluidized reaction zone2Deacidifying by gas-solid phase mass transfer to remove adsorbed SiO2HCl on the surface of the nano-SiO film reaches the aim of deacidification, so that the deacidified nano-SiO film is obtained2The pH of (A) is 3.7-4.2, and the water content is less than 2%.
The tail gas is discharged through a tail gas outlet, and the product is sent out through a product outlet.
Compared with the prior art, the lower part is directly heated by hydrogen combustion, so that the heat loss is reduced, and the energy consumption of industrial production is reduced; the baffle plate is adopted to prevent back mixing and secondary adsorption of gas-phase HCl and prevent nascent state SiO2Solid phase back mixing improves the deacidification quality in the continuous deacidification process; the back mixing of gas phase and solid phase is prevented, so that the time required by deacidification is greatly shortened; the deacidification quality is improved.
Drawings
FIG. 1 is a schematic view of a structure of a continuous fluidized bed.
Detailed Description
Referring to fig. 1, the continuous fluidized bed of nano-silica prepared by a vapor phase process of the present invention comprises a cylindrical fluidized reaction section 2, a combustion apparatus 1, and an enlarged collection section 3:
the cylindrical fluidized reaction section 2 is provided with a vertical fluidized reaction section clapboard 12, the upper part of the cylindrical fluidized reaction section 2 is positioned at the top end of the cylindrical fluidized reaction section 2, and a gap H is reserved between the lower part of the cylindrical fluidized reaction section 2 and a gas distributor, wherein the gap H is 5-40% of the height of the fluidized reaction section according to the invention, and the two sides of the fluidized reaction section clapboard 12 are connected with the inner wall of the cylindrical fluidized reaction section 2;
the combustion device 2 provided with a hydrogen and air inlet 8 is arranged at the lower part of the fluidized reaction section 2, and a gas distributor 7 is arranged between the combustion device 2 and the fluidized reaction section; the combustion device 2 and the gas distributor 7 are conventional devices and have no particular requirement;
the expansion collecting section 3 is disposed at the upper portion of the fluidized reaction section 2, the inner diameter of the expansion collecting section 2 is larger than that of the fluidized reaction section 2, and the inner diameter of the expansion collecting section 2 is that of the fluidized reaction section 2? Do? In the expanded collection section, an eccentric vertical collection section partition plate 11 isarranged, the lower part of the expanded collection section is connected with a fluidized reaction section partition plate 12 through an inclined plate 111, a gap H2 is reserved between the upper part of the expanded collection section and the top end of the expanded collection section 3, the gap H2 is 1-10% of the height of the expanded collection section 3, and two sides of the collection section partition plate are connected with the inner wall of the expanded collection section;
SiO raw material2The inlet 9 is arranged at the top of the expanded collecting section 3 and is communicated with the fluidized reaction section 2 through a connecting pipe 301;
the product outlet 6 is arranged at the middle upper part of the fluidized reaction section 2, and the tail gas outlet 10 is arranged at the top of the enlarged collection section.
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1
The interval H is 10% of the height of the fluidized reaction zone, the interval H2 is 3% of the height of the enlarged collecting section 3, and the inner diameter of the enlarged collecting section 2 is 5 times the inner diameter of the fluidized reaction zone 2.
Introducing hydrogen and air into a combustion device for combustion, wherein the gas containing water vapor enters a fluidized reaction section after passing through a body distributor, the temperature of the gas containing water vapor is 300 ℃, the water vapor content is 5%, the gas velocity of the fluidized section is 2cm/s, the fluidization expansion rate is 3, the gas velocity of the expanded collection section is 0.5cm/s, and the average residence time is 15 min;
SiO raw material2Enters the fluidized reaction section through the inlet, and ensures the existence of SiO at the discharge port2The formed material seal is that the liquid level of the dense phase zone of the fluidized bed is kept 10cm above the discharge hole.
Gas containing water vapor and SiO raw material entering into fluidized reaction zone2Deacidifying by gas-solid phase mass transfer to remove adsorbed SiO2HCl on the surface of the substrate reaches the purpose of deacidification. The tail gas is discharged through a tail gas outlet (10), and the product is sent out through a product outlet (6).
And (3) product analysis results:
before deacidification: nano SiO2pH of (2): 2.40 of containing H2O: 4.0% and a specific surface area of 135m2/g；
After deacidification: nano SiO2pH of (2): 3.8, containing H2O: 2.5%, specific surface area 128m2/g。
Example 2
The interval H is 15% of the height of the fluidized reaction zone, the interval H2 is 1% of the height of the enlarged collecting section 3, and the inner diameter of the enlarged collecting section 2 is 3 times the inner diameter of the fluidized reaction zone 2.
Introducing hydrogen and air into a combustion device for combustion, wherein the gas containing water vapor enters a fluidized reaction section after passing through a body distributor, the temperature of the gas containing water vapor is 650 ℃, the water vapor content is 25%, the gas velocity of the fluidized section is 15cm/s, the fluidization expansion rate is 7, the gas velocity of the expanded collection section is 1.5cm/s, and the average residence time is 30 min;
SiO raw material2Enters the fluidized reaction section through the inlet, and ensures the existence of SiO at the discharge port2The formed material seal is to keep the liquid level of the dense phase zone of the fluidized bed 30cm above the discharge port. The tail gas is discharged through a tail gas outlet (10), and the product is sent out through a product outlet (6).
Gas containing water vapor and SiO raw material entering into fluidized reaction zone2Deacidifying by gas-solid phase mass transfer to remove adsorbed SiO2HCl on the surface of the substrate reaches the purpose of deacidification.
And (3) product analysis results:
before deacidification: nano SiO2pH of (2): 2.40 of containing H2O: 5% of specific surface area 290m2/g；
After deacidification: nano SiO2pH of (2): 3.8, containing H2O: 1.7% and a specific surface area of 282m2/g。
Claims (6)
1. A continuous fluidized bed of nano-silica prepared by a gas phase method is characterized by comprising a cylindrical fluidized reaction section (2), a combustion device (1) and an expansion collection section (3):
a vertical fluidization reaction section partition plate (12) is arranged in the cylindrical fluidization reaction section (2), the upper part of the vertical fluidization reaction section partition plate is positioned at the top end of the cylindrical fluidization reaction section (2), a gap H is reserved between the lower part of the vertical fluidization reaction section partition plate and a gas distributor, and two sides of the fluidization reaction section partition plate (12) are connected with the inner wall of the cylindrical fluidization reaction section (2);
a combustion device (2) provided with a hydrogen and air inlet (8) is arranged at the lower part of the fluidized reaction section (2), and a gas distributor (7) is arranged between the combustion device (2) and the fluidized reaction section;
the expanded collection section (3) is arranged at the upper part of the fluidized reaction section (2), the inner diameter of the expanded collection section (2) is larger than that of the fluidized reaction section (2), an eccentric vertical collection section partition plate (11) is arranged in the expanded collection section, the lower part of the expanded collection section is connected with a fluidized reaction section partition plate (12) through an inclined plate (111), a gap H2 is reserved between the upper part of the expanded collection section and the top end of the expanded collection section (3), and two sides of the collection section partition plate are connected with the inner wall of the expanded collection section;
SiO raw material2The inlet (9) is arranged at the top of the expanded collecting section (3) and is communicated with the fluidized reaction section (2) through a connecting pipe (301);
the product outlet (6) is arranged at the middle upper part of the fluidized reaction section (2), and the tail gas outlet (10) is arranged at the top of the expanding and collecting section.
2. The continuous fluidized bed of nano-silica prepared by a vapor phase method according to claim 1, wherein a gap is left between the lower part and the gas distributor, and the gap H is 5-40% of the height of the fluidized reaction section.
3. The continuous fluidized bed of nanosilica prepared by gas phase process according to claim 1, characterized in that the interval H2 is 1-10% of the height of the enlarged collection section (3).
4. The continuous fluidized bed of nano-silica produced by the gas phase process according to claim 1, wherein the inner diameter of the expanded collection section (2) is 2 to 6 times the inner diameter of the fluidized reaction section (2).
5. Industrial application of the continuous fluidized bed of nano-silica prepared by the gas phase method according to any one of claims 1 to 4, which is used for preparing nano-silica.
6. Use according to claim 5, characterized in that it comprises the following steps: introducing hydrogen and air into a combustion device for combustion, introducing gas containing water vapor into a fluidized reaction section after passing through a body distributor, wherein the temperature of the gas containing water vapor is 300-650 ℃, the water vapor content is 5-25%, the gas velocity of the fluidized section is 2-15cm/s, the fluidization expansion rate is 3-7, the gas velocity of the expanded collection section is 0.5-1.5cm/s, and the average residence time is 15-30 min;
SiO raw material2Enters the fluidized reaction section through the inlet, and ensures the existence of SiO at the discharge port2The formed material seal is that the liquid level of the dense phase zone of the fluidized bed is kept 10-30cm above the discharge hole;
the tail gas is discharged through a tail gas outlet (10), and the product is sent out through a product outlet (6).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100431955C (en) * | 2006-09-04 | 2008-11-12 | 上海氯碱化工股份有限公司 | Apparatus and method of synthesizing acidic material on SiO2 surface by eliminating gas phase method |
| CN102992330A (en) * | 2011-09-13 | 2013-03-27 | 赤峰盛森硅业科技发展有限公司 | Fluidized bed deacidification purification device and process |
| CN112090215A (en) * | 2020-09-17 | 2020-12-18 | 郑州格矽科技发展有限公司 | Device and method for treating adsorbate on surface of ultrafine powder |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3981690A (en) * | 1975-01-15 | 1976-09-21 | The United States Of America As Represented By The United States Energy Research And Development Administration | Agglomerating combustor-gasifier method and apparatus for coal gasification |
| US4419965A (en) * | 1981-11-16 | 1983-12-13 | Foster Wheeler Energy Corporation | Fluidized reinjection of carryover in a fluidized bed combustor |
| CN1023382C (en) * | 1987-03-14 | 1994-01-05 | 中国石油化工总公司 | Fluidized-bed reactor |
| US5243770A (en) * | 1991-07-12 | 1993-09-14 | The Babcock & Wilcox Company | Fluid bed material transfer apparatus |
| JPH0831253A (en) * | 1994-05-11 | 1996-02-02 | Tanaka Kikinzoku Kogyo Kk | Electric contact material |
| CN1188532A (en) * | 1996-02-08 | 1998-07-22 | Abb.专利有限公司 | Device for separating solids particles from gas flow of fluid bed |
| JPH10122509A (en) * | 1996-10-22 | 1998-05-15 | Mitsubishi Heavy Ind Ltd | Fluidized bed combustion device |
| CN2512997Y (en) * | 2001-11-15 | 2002-09-25 | 沈阳环境科学研究所 | Dry vortex bed fume purifier |
-
2005
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100431955C (en) * | 2006-09-04 | 2008-11-12 | 上海氯碱化工股份有限公司 | Apparatus and method of synthesizing acidic material on SiO2 surface by eliminating gas phase method |
| CN102992330A (en) * | 2011-09-13 | 2013-03-27 | 赤峰盛森硅业科技发展有限公司 | Fluidized bed deacidification purification device and process |
| CN102992330B (en) * | 2011-09-13 | 2015-04-08 | 赤峰盛森硅业科技发展有限公司 | Fluidized bed deacidification purification device and process |
| CN112090215A (en) * | 2020-09-17 | 2020-12-18 | 郑州格矽科技发展有限公司 | Device and method for treating adsorbate on surface of ultrafine powder |
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