CN116161688A - Preparation method of nano spherical alumina - Google Patents

Preparation method of nano spherical alumina Download PDF

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Publication number
CN116161688A
CN116161688A CN202211587879.5A CN202211587879A CN116161688A CN 116161688 A CN116161688 A CN 116161688A CN 202211587879 A CN202211587879 A CN 202211587879A CN 116161688 A CN116161688 A CN 116161688A
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alumina
gas
spherical alumina
suspension
distributor
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杨强
张奋航
魏测武
石海龙
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Yaan Bestry Performance Materials Corp
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Yaan Bestry Performance Materials Corp
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/30—Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
    • 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
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
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  • Thermal Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention belongs to the technical field of alumina processing, and discloses a method for preparing nano spherical alumina, which comprises the following steps: s1, heating and gasifying low-boiling-point organic aluminum; s2, mixing and burning gasification gas, natural gas and oxygen; s3, dispersing combustion products into water through a distributor to form alumina suspension; and S4, spray drying the alumina suspension to obtain the nano spherical alumina. The method takes low-boiling-point organic aluminum as a raw material, and the raw material is heated and gasified and then mixed with natural gas and oxygen for combustion to generate combustion products, the combustion products are quickly cooled in water, gas-solid separation is realized, alumina suspension is formed, and nano spherical alumina is obtained through spray drying. The process flow is simple, no pollutant is produced in the preparation process, the requirement on equipment is low, and the obtained nano spherical alumina has good dispersibility, regular particle shape, uniform size and good sphericity.

Description

Preparation method of nano spherical alumina
Technical Field
The invention belongs to the technical field of alumina processing, and particularly relates to a preparation method of nano spherical alumina.
Background
The nanometer spherical alumina has the advantages of high strength, high hardness, good stability, large specific surface area, good fluidity, low shrinkage, good wear resistance, strong insulating property, high resistivity and the like, has wide application prospect in the fields of precision ceramics, polishing, grinding and the like, and increases the market demand year by year.
At present, various methods for preparing nano spherical alumina are available, for example, a continuous preparation process of high-purity nano alumina is disclosed in patent CN1810646a, aluminum trichloride is gasified at high temperature and then mixed with hydrogen and oxygen for combustion, the aluminum trichloride undergoes hydrolysis condensation reaction by utilizing moisture and high temperature generated by the combustion of hydrogen and oxygen to generate nano alumina and hydrogen chloride, and the nano alumina is obtained through gas-solid separation. However, the aluminum trichloride is used as a raw material, contains chlorine element, has strong corrosiveness and has high requirements on production equipment; the subsequent dechlorination treatment is needed, and the working procedure is complex; adopts hydrogen as fuel, has higher cost,
for example, patent CN108483474a discloses a method for preparing nano-sized spherical alumina using a soluble aluminum salt (e.g., al (NO) 3 ) 3 ·9H 2 O) is sequentially dissolved in deionized water, ammonium citrate solution and absolute ethyl alcohol, and then is led into a hydrothermal reaction kettle to carry out hydrothermal reaction to obtain a precipitate, and the precipitate is washed, dried and ground to obtain the nano-scale spherical alumina particles. In the preparation process, a large amount of reagents such as ammonium citrate solution, absolute ethyl alcohol and the like are used, so that the production cost and the subsequent wastewater treatment cost are high; the final nano-scale spherical alumina product is obtained through grinding, and the problems of difficult control of sphericity of the product, irregular particle shape, poor size uniformity and the like exist, so that the application performance of the product is affected.
Disclosure of Invention
The invention aims to solve the problems in the prior art, and provides a preparation method of nano spherical alumina. The method has the advantages of simple process flow, no generation of pollutants in the preparation process, low equipment requirement, good dispersibility, regular and uniform shape and good sphericity of the obtained nano spherical alumina.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the nano spherical alumina comprises the following steps:
s1, heating and gasifying low-boiling-point organic aluminum;
s2, mixing and burning gasification gas, natural gas and oxygen;
s3, dispersing combustion products into water through a distributor to form alumina suspension;
and S4, spray drying the alumina suspension to obtain the nano spherical alumina.
Preferably, the low boiling point organoaluminum comprises one or more of aluminum isopropoxide, aluminum n-butoxide, aluminum t-butoxide, aluminum sec-butoxide and triethylaluminum.
Preferably, the low boiling point organoaluminum comprises organoaluminum a and organoaluminum B, the boiling point of organoaluminum B is higher than that of organoaluminum a, and the molar ratio of organoaluminum a to organoaluminum B is 1:0.05 to 0.8.
Preferably, in step S1, the organoaluminum is heated and gasified in a gasifier at a temperature of 150-250 ℃.
Preferably, the gasification gas is introduced into a combustion chamber through an induced draft fan to be mixed and combusted with natural gas and oxygen, and the molar ratio of the organic aluminum to the oxygen to the natural gas is 1: 14-18: 0.5-2.
Preferably, the gasification gas is introduced into a combustion chamber through an induced draft fan, the introduction flow of the gasification gas is 0.5-2.5L/min, the gasification gas is completely combusted in the combustion chamber, and the temperature in the combustion chamber is 1100-1500 ℃.
Preferably, the combustion products are introduced into the suspension tank by the distributor, and the outlet of the distributor is positioned at a liquid level depth of the suspension tank of 0.5m or less.
Preferably, the temperature of the combustion products discharged from the outlet of the distributor is 300-500 ℃, and the water temperature in the suspension tank is controlled to be 90 ℃ or below.
Preferably, the distributor comprises a spiral pipe arranged vertically and a gas distribution head positioned at the bottom of the spiral pipe;
the outer wall of the spiral pipe is provided with spiral blades which extend to the outer side and the inner side of the spiral respectively;
the gas distribution head is downward in opening and comprises a gas distribution cover and a flow guide piece arranged on the inner side of the gas distribution cover, and an annular outlet with a downward opening is formed between the gas distribution cover and the flow guide piece.
Preferably, in the step S4, the concentration of the alumina suspension subjected to spray drying is 35-55%, the air inlet temperature of spray drying is 220-280 ℃, and the air outlet temperature is not lower than 150 ℃.
Compared with the prior art, the invention has the beneficial effects that:
the invention takes low boiling point (boiling point is 250 ℃ and below) organic aluminum as raw material, and then the organic aluminum is heated and gasified, mixed with natural gas and oxygen to generate combustion products, the combustion products are introduced into water to quickly cool, gas-solid separation is realized at the same time, alumina suspension is formed, and spray drying is carried out after the alumina suspension reaches a certain concentration, thus obtaining the nano spherical alumina.
Taking aluminum isopropoxide as an example, the reaction principle of the invention is as follows:
CH 4 +2O 2 →CO 2 +2H 2 o+delta (the main component of natural gas is CH 4 ）
C 9 H 21 AlO 3 +3H 2 O +Δ→3C 3 H 7 OH+Al(OH) 3
2Al(OH) 3 +Δ→Al 2 O 3 +3H 2 O
2C 3 H 7 OH+9O 2 →6CO 2 +8H 2 O+Δ
The preparation method has the advantages of simple process flow, production of alumina, water and carbon dioxide after mixed combustion, no generation of pollutant, low treatment cost of waste and sewage, low requirement on equipment and low equipment investment; the combustion products are generated by mixing and burning in a dispersed airflow mode in a combustion chamber, the combustion products are directly led into water to form suspension with good dispersion, and then spray drying is carried out to obtain the product, wherein the formed product is nano-scale spherical alumina, has regular shape, good sphericity and uniform size, has good application performance, and particularly has good polishing effect.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a process for preparing nano-spherical alumina.
FIG. 2 is a schematic view of the structure of the combustion chamber and the suspension tank.
Fig. 3 is a schematic elevational view of the burner.
Reference numerals:
1. a combustion chamber; 11. a combustion chamber; 111. a first through hole; 112. a second through hole; 12. a first charging chamber; 13. a second charging chamber; 14. a burner;
2. a suspension tank;
3. a distributor; 31. a spiral tube; 311. a helical blade; 32. a gas distribution head; 321. a gas distribution cover; 322. and a flow guiding piece.
Detailed Description
Hereinafter, only certain exemplary embodiments are briefly described. As will be recognized by those of skill in the pertinent art, the described embodiments may be modified in numerous different ways without departing from the spirit or scope of the embodiments of the present invention. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive.
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
As shown in fig. 1, the method for preparing nano spherical alumina provided by the embodiment of the invention comprises the following steps:
s1, placing analytically pure aluminum isopropoxide into a gasification furnace, heating to control the temperature in the gasification furnace within a range of 150-170 ℃ and gasifying the aluminum isopropoxide to obtain gasified gas.
S2, introducing generated gasified gas into a combustion chamber through a draught fan, and mixing and burning the gasified gas with natural gas and oxygen which are introduced into the combustion chamber, wherein the molar ratio of aluminum isopropoxide to oxygen to natural gas is controlled to be 1:15: and 0.8, controlling the flow rate of gasification gas introduced into the combustion chamber through the induced draft fan to be about 2.0L/min, and simultaneously controlling the temperature in the combustion chamber to be in the range of 1100-1500 ℃ in the combustion process, so as to ensure that the gasification gas is fully combusted, and ensure that aluminum hydroxide generated by gasification of aluminum isopropoxide is completely reacted to generate aluminum oxide after high temperature. The combustion products comprise alumina particles, water vapor, carbon dioxide and other high-temperature flue gases.
S3, after the combustion products enter the distributor through the pipeline, the combustion products are dispersed into water in the suspension tank, the distributor extends to below the water surface of the suspension tank, the outlet of the distributor is controlled to be positioned at the depth of 0.5m or below the liquid surface of the suspension tank, alumina particles in high-temperature flue gas are ensured to be completely trapped in the water body to form alumina suspension, and the alumina particles are prevented from being carried out of the suspension tank by the flue gas, so that the yield of alumina is prevented from being influenced. Meanwhile, the temperature of the combustion products discharged from the outlet of the distributor is controlled within the range of 300-500 ℃, so that the phenomenon that water in a suspension tank directly boils due to overhigh temperature or the combustion products adhere to a pipeline and the distributor due to overhigh temperature is avoided; the temperature of the water body in the suspension tank is controlled to be 90 ℃ or below, and the cooling and interception effects of the water body are ensured.
S4, discharging the alumina suspension in the suspension tank after the alumina suspension reaches a certain concentration for spray drying, controlling the concentration of the alumina in the alumina suspension to be within 50-52% during spray drying, controlling the air inlet temperature of the spray drying to be 220-250 ℃, controlling the air outlet temperature to be not lower than 150 ℃, and obtaining the nano spherical alumina particles after spray drying.
Example 2
The embodiment of the invention provides a preparation method of nano spherical alumina, which comprises the following steps:
s1, placing analytically pure aluminum tert-butoxide into a gasification furnace, heating to control the temperature in the gasification furnace within 160-180 ℃ and gasifying the aluminum tert-butoxide to obtain gasified gas.
S2, introducing generated gasified gas into a combustion chamber through a draught fan, and mixing and burning the gasified gas with natural gas and oxygen which are introduced into the combustion chamber, wherein the molar ratio of the aluminum tert-butoxide to the oxygen to the natural gas is controlled to be 1:18: and 0.5, controlling the flow rate of gasification gas introduced into the combustion chamber through the induced draft fan to be about 1.5L/min, and controlling the temperature in the combustion chamber to be within the range of 1100-1500 ℃ in the combustion process. The combustion products comprise alumina particles, water vapor, carbon dioxide and other high-temperature flue gases.
S3, after the combustion products enter the distributor through the pipeline, the combustion products are dispersed into water in the suspension tank, the distributor extends to below the water surface of the suspension tank, the outlet of the distributor is controlled to be positioned at the liquid level depth of the suspension tank by 0.5m or less, and meanwhile, the temperature of the combustion products discharged from the outlet of the distributor is controlled to be within the range of 300-500 ℃; the temperature of the water body in the suspension tank is controlled to be 85 ℃ or below, and the cooling and interception effects of the water body are ensured.
S4, discharging the alumina suspension in the suspension tank after the alumina suspension reaches a certain concentration for spray drying, controlling the concentration of alumina in the alumina suspension to be within a range of 40-50% during spray drying, controlling the air inlet temperature of spray drying to be 220-250 ℃, controlling the air outlet temperature to be not lower than 150 ℃, and obtaining the nano spherical alumina particles after spray drying.
Example 3
The embodiment of the invention provides a preparation method of nano spherical alumina, which comprises the following steps:
s1, putting analytically pure aluminum sec-butoxide into a gasification furnace, heating to control the temperature in the gasification furnace within the range of 210-250 ℃ and gasifying the aluminum sec-butoxide to obtain gasified gas.
S2, introducing generated gasified gas into a combustion chamber through a draught fan, and mixing and burning the gasified gas with natural gas and oxygen which are introduced into the combustion chamber, wherein the molar ratio of the aluminum sec-butoxide to the oxygen to the natural gas is controlled to be 1:15:2, controlling the flow rate of gasification gas introduced into the combustion chamber by the induced draft fan to be about 2.5L/min, and controlling the temperature in the combustion chamber to be in the range of 1100-1500 ℃ in the combustion process. The combustion products comprise alumina particles, water vapor, carbon dioxide and other high-temperature flue gases.
S3, after the combustion products enter the distributor through the pipeline, the combustion products are dispersed into water in the suspension tank, the distributor extends to below the water surface of the suspension tank, the outlet of the distributor is controlled to be positioned at the liquid level depth of the suspension tank by 0.5m or less, and meanwhile, the temperature of the combustion products discharged from the outlet of the distributor is controlled to be within the range of 300-500 ℃; the temperature of the water body in the suspension tank is controlled to be 85 ℃ or below, and the cooling and interception effects of the water body are ensured.
S4, discharging the alumina suspension in the suspension tank after the alumina suspension reaches a certain concentration for spray drying, controlling the concentration of alumina in the alumina suspension to be in a range of 35-45% during spray drying, controlling the air inlet temperature of the spray drying to be 240-280 ℃, controlling the air outlet temperature to be not lower than 150 ℃, and obtaining the nano spherical alumina particles after spray drying.
Example 4
The embodiment of the invention provides a preparation method of nano spherical alumina, which comprises the following steps:
s1, preparing analytically pure aluminum isopropoxide (organic aluminum A) and aluminum sec-butoxide (organic aluminum B) according to a molar ratio of 1: and 0.1, adding the aluminum isopropoxide and the aluminum sec-butoxide into a gasification furnace, heating the mixture to control the temperature in the gasification furnace within the range of 210-250 ℃, and gasifying the aluminum isopropoxide and the aluminum sec-butoxide to obtain gasified gas.
S2, introducing generated gasified gas into a combustion chamber through a draught fan, mixing and burning the gasified gas with natural gas and oxygen which are introduced into the combustion chamber, and specifically controlling the molar ratio of aluminum isopropoxide to aluminum sec-butoxide to the oxygen and the natural gas to be 1:18:1.2, controlling the flow rate of gasification gas introduced into the combustion chamber by the induced draft fan to be about 2.25L/min, and controlling the temperature in the combustion chamber to be within the range of 1100-1500 ℃ in the combustion process. The combustion products comprise alumina particles, water vapor, carbon dioxide and other high-temperature flue gases.
S3, after the combustion products enter the distributor through the pipeline, the combustion products are dispersed into water in the suspension tank, the distributor extends to below the water surface of the suspension tank, the outlet of the distributor is controlled to be positioned at the liquid level depth of the suspension tank by 0.5m or less, and meanwhile, the temperature of the combustion products discharged from the outlet of the distributor is controlled to be within the range of 300-500 ℃; the temperature of the water body in the suspension tank is controlled to be 90 ℃ or below, and the cooling and interception effects of the water body are ensured.
S4, discharging the alumina suspension in the suspension tank after the alumina suspension reaches a certain concentration for spray drying, controlling the concentration of alumina in the alumina suspension to be within 50-55% during spray drying, controlling the air inlet temperature of spray drying to be 240-280 ℃, controlling the air outlet temperature to be not lower than 150 ℃, and obtaining the nano spherical alumina particles after spray drying.
Example 5
The embodiment of the invention provides a preparation method of nano spherical alumina, which comprises the following steps:
s1, preparing analytically pure aluminum isopropoxide (organic aluminum A) and aluminum tert-butoxide (organic aluminum B) according to a molar ratio of 1: and 0.5, adding the mixture into a gasification furnace, heating the mixture to control the temperature in the gasification furnace within 160-180 ℃ and gasifying aluminum isopropoxide and aluminum tert-butoxide to obtain gasified gas.
S2, introducing generated gasified gas into a combustion chamber through a draught fan, mixing and burning the gasified gas with natural gas and oxygen which are introduced into the combustion chamber, and specifically controlling the molar ratio of aluminum isopropoxide to tertiary aluminum butoxide to the oxygen to the natural gas to be 1:18:1.5, controlling the flow rate of gasification gas introduced into the combustion chamber by the induced draft fan to be about 2.25L/min, and controlling the temperature in the combustion chamber to be within the range of 1100-1500 ℃ in the combustion process. The combustion products comprise alumina particles, water vapor, carbon dioxide and other high-temperature flue gases.
S3, after the combustion products enter the distributor through the pipeline, the combustion products are dispersed into water in the suspension tank, the distributor extends to below the water surface of the suspension tank, the outlet of the distributor is controlled to be positioned at the liquid level depth of the suspension tank by 0.5m or less, and meanwhile, the temperature of the combustion products discharged from the outlet of the distributor is controlled to be within the range of 300-500 ℃; the temperature of the water body in the suspension tank is controlled to be 90 ℃ or below, and the cooling and interception effects of the water body are ensured.
S4, discharging the alumina suspension in the suspension tank after the alumina suspension reaches a certain concentration for spray drying, controlling the concentration of alumina in the alumina suspension to be within 50-55% during spray drying, controlling the air inlet temperature of spray drying to be 240-280 ℃, controlling the air outlet temperature to be not lower than 150 ℃, and obtaining the nano spherical alumina particles after spray drying.
The method has the advantages that two organic aluminum raw materials with different boiling points are used for production, the content of the organic aluminum raw materials with higher boiling points is controlled at a lower level, the heating gasification process can be carried out at a relatively higher heating gasification temperature, the heating gasification time is shortened, and the condition that the gasification furnace runs in a no-load mode due to complete gasification of the raw materials in the production process is avoided.
TABLE 1 detection results of nanosphere-shaped alumina produced by the experiments of examples 1-5
Project Example 1 Example 2 EXAMPLE 3 Example 4 Example 5
Average particle diameter (nm) 37±0.08 53±1.02 49±0.76 86±2.22 62±3.15
Sphericity (%) ≥80 ≥80 ≥80 ≥80 ≥80
In summary, the invention takes low boiling point (boiling point is 250 ℃ and below) organic aluminum as raw material, and then the organic aluminum is heated and gasified, mixed with natural gas and oxygen to generate combustion products, the combustion products are introduced into water to quickly cool, gas-solid separation is realized at the same time, alumina suspension is formed, and spray drying is carried out after the alumina suspension reaches a certain concentration, thus obtaining the nano spherical alumina. The process flow is simple, alumina, water and carbon dioxide are generated after mixed combustion, no pollutant is generated, the sewage and waste treatment cost is low, the equipment requirement is low, and the equipment investment is low; the combustion products are generated by mixing and burning in a dispersed airflow mode in a combustion chamber, the combustion products are directly led into water to form a suspension with good dispersion, and then spray drying is carried out to obtain the product, wherein the formed product is nano-scale (10 nm-100 nm) spherical alumina, has regular shape and good sphericity (more than or equal to 80%), has uniform size, has good application performance, and particularly has good polishing effect.
Example 6
The embodiment of the invention provides a production system suitable for the preparation method of nano spherical alumina in embodiments 1 to 5, which comprises a gasification furnace, a combustion chamber 1, a suspension tank 2, a spray drying device and the like which are sequentially connected.
The gasification gas outlet of the gasification furnace is connected with the combustion chamber 1 through a pipeline, and an induced draft fan is arranged on the connecting pipeline and used for introducing gasification gas into the combustion chamber 1. The gasification furnace is also provided with an inert gas inlet, when the content of gasification gas in the gasification furnace is small, part of inert gas (such as nitrogen) can be added as a carrier, so that the gasification gas is smoothly introduced into the combustion chamber 1 by the induced draft fan.
As shown in fig. 2 and 3, the combustion chamber 1 has a combustion chamber 11, a first charging chamber 12 and a second charging chamber 13 provided outside the front end of the combustion chamber 11. The front end of the combustion chamber 11 is provided with a burner 14, and the burner 14 is connected with a natural gas pipeline and can uniformly distribute and send natural gas; and the burner 14 has a swirl passage communicating the first charging chamber 12 and the combustion chamber 11; the first charging chamber 12 is connected to a line for delivering oxygen. It will be appreciated that ignition means are provided on the inside or side of the burner 14 for ignition combustion of the burner 14.
A plurality of first through holes 111 and second through holes 112 are formed in the side wall of the front end of the combustion chamber 11, wherein the first through holes 111 are communicated with the first feeding chamber 12 and the combustion chamber 11, and the second through holes 112 are communicated with the second feeding chamber 13 and the combustion chamber 11. I.e. oxygen is dispersed into the combustion chamber 11 by the swirl channel of the burner 14 and the first plurality of through holes 111. The second charging cavity 13 is an annular cavity surrounding the outer side of the combustion cavity 11, an inlet is arranged on the annular cavity and is communicated with the outlet end of the induced draft fan through a pipeline, namely gasification gas enters the second charging cavity 13 from the inlet and is dispersed into the combustion cavity 11 through a plurality of second through holes 112. The combustion chamber 1 can effectively ensure that gasification gas, natural gas and oxygen are fully mixed and combusted, and the three gases cannot interfere with each other before mixed combustion.
The side wall of the combustion chamber 11 is a curved surface chamber, a smoke outlet is arranged at the lower side of the rear end of the combustion chamber, the smoke outlet and the combustion chamber 11 are of a curved surface transitional closing-in structure, smoke dust in combustion products is ensured to be collected and discharged, and the smoke dust is not easy to accumulate in the combustion chamber 11.
The suspension tank 2 is arranged below the combustion chamber 1, the distributor 3 is arranged in the suspension tank 2, the distributor 3 is connected with a smoke outlet of the combustion chamber 1 through a section of vertical pipeline, and combustion products directly travel into the distributor 3 and then enter into a water body of the suspension tank 2.
As shown in fig. 2, the distributor 3 is installed in the suspension tank 2 in a vertical arrangement, and the distributor 3 includes a spiral pipe 31 in a vertical arrangement and a gas distribution head 32 at the bottom of the spiral pipe 31. Spiral blades 311 extending spirally are respectively arranged on the inner side and the outer side of the spiral outside of the spiral pipe 31, and the spiral blades 311 extend outwards or inwards in the radial direction of the projection area of the spiral pipe 31, so that the spiral pipe 31 and the spiral blades 311 thereon are matched with the suspension tank 2, and a spiral-like flow channel is formed from the bottom to the upper part of the suspension tank 2.
The gas distribution head 32 is installed at the bottom of the spiral tube 31 and is an outlet part of combustion products (flue gas), and an opening of the gas distribution head is arranged downward. The air distribution head 32 comprises an air distribution cover 321 and a flow guide piece 322 arranged below the inner side of the air distribution cover 321. Wherein the air distribution cover 321 is a flaring cover body with a small upper part and a big lower part; the guide piece 322 is a conical shell and is connected to the right lower part of the gas distribution cover 321 through a connecting rod; an annular outlet with a downward opening is formed between the air distribution cover 321 and the flow guide piece 322. The air distribution head 32 is located in the middle of the right lower part of the spiral tube 31, and is coaxially arranged with the spiral tube 31, and the flaring size of the air distribution cover 321 is smaller than the projection size of the spiral blade 311 extending outwards.
In operation, the distributor 3 is submerged below the liquid level of the suspension tank 2, i.e. the spiral pipe 31 is located completely below the liquid level. The combustion products (flue gas) enter the spiral tube 31 of the distributor 3 and exchange heat with the water body in the suspension tank 2 in the descending process, so that the high-temperature flue gas is rapidly cooled. The length of the spiral tube 31 section is not less than 0.5m, so that the temperature of the flue gas can be reduced to below 500 ℃ when the flue gas reaches the gas distribution head 32. The spiral blades 311 enable the suspension tank 21 to form a spiral flow channel which runs up and down, so that the distance from the outlet of the gas distribution head 32 to the water surface is prolonged, the baffle effect is achieved on alumina suspended in the water body, and the alumina is prevented from being taken away along with the overflow of the flue gas to the water surface; inhibiting water rolling phenomenon generated when flue gas enters a water body; simultaneously, the spiral blades 311 also play a role in heat conduction, accelerate heat exchange between flue gas and water, and shorten the length of the distributor 3 and the depth of the water in the suspension tank 2.
The suspension tank 2 is provided with a liquid level monitor, a water supplementing port, an automatic water inlet valve associated with the liquid level monitor and the like. The side wall of the suspension tank 2 is provided with a transparent observation hole, the bottom is provided with a liquid outlet, and the upper part is provided with a smoke outlet. The drain port is used for draining the alumina suspension.
In summary, the production system is provided with the specific combustion chamber 1, the suspension tank 2 and the distributor 3, is suitable for the process operation of the nano spherical alumina preparation method, and ensures the efficient implementation of the nano spherical alumina preparation method.

Claims (10)

1. The preparation method of the nano spherical alumina is characterized by comprising the following steps of:
s1, heating and gasifying low-boiling-point organic aluminum;
s2, mixing and burning gasification gas, natural gas and oxygen;
s3, dispersing combustion products into water through a distributor to form alumina suspension;
and S4, spray drying the alumina suspension to obtain the nano spherical alumina.
2. The method of claim 1, wherein the low boiling point organoaluminum comprises one or more of aluminum isopropoxide, aluminum n-butoxide, aluminum t-butoxide, aluminum sec-butoxide, and triethylaluminum.
3. The method for preparing nano-spherical alumina according to claim 2, wherein the low boiling point organoaluminum comprises organoaluminum a and organoaluminum B, the boiling point of organoaluminum B is higher than that of organoaluminum a, and the molar ratio of organoaluminum a to organoaluminum B is 1:0.05 to 0.8.
4. The method for preparing nano-spherical alumina according to claim 1 or 3, wherein in step S1, the organic aluminum is heated and gasified in a gasifier at a temperature of 150-250 ℃.
5. The method for preparing nano-spherical alumina according to claim 1, wherein the gasification gas is introduced into the combustion chamber through a draught fan to be mixed and combusted with natural gas and oxygen, and the molar ratio of the organic aluminum to the oxygen to the natural gas is 1: 14-18: 0.5-2.
6. The method for preparing nano-spherical alumina according to claim 5, wherein the gasification gas is introduced into the combustion chamber through the induced draft fan, the introduction flow rate of the gasification gas is 0.5-2.5 l/min, the gasification gas is completely combusted in the combustion chamber, and the temperature in the combustion chamber is 1100-1500 ℃.
7. The method for producing nano-spherical alumina according to claim 1, wherein the combustion products are introduced into a suspension tank from the distributor, and the outlet of the distributor is located at a liquid level depth of 0.5m or less in the suspension tank.
8. The method for producing nano-spherical alumina according to claim 1 or 7, wherein the temperature of the combustion product discharged from the outlet of the distributor is 300 to 500 ℃, and the water temperature in the suspension tank is controlled to 90 ℃ or lower.
9. The method for preparing nano-spherical alumina according to claim 7, wherein the distributor comprises a spiral pipe arranged vertically and a gas distribution head positioned at the bottom of the spiral pipe;
the outer wall of the spiral pipe is provided with spiral blades which extend to the outer side and the inner side of the spiral respectively;
the gas distribution head is downward in opening and comprises a gas distribution cover and a flow guide piece arranged on the inner side of the gas distribution cover, and an annular outlet with a downward opening is formed between the gas distribution cover and the flow guide piece.
10. The method according to claim 1, wherein in the step S4, the concentration of the alumina suspension subjected to spray drying is 35-55%, the air inlet temperature of spray drying is 220-280 ℃, and the air outlet temperature is not lower than 150 ℃.
CN202211587879.5A 2022-12-12 2022-12-12 Preparation method of nano spherical alumina Pending CN116161688A (en)

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JPH11147711A (en) * 1997-11-11 1999-06-02 Asahi Glass Co Ltd Alumina fine sphere and its production
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CN101066773A (en) * 2007-06-11 2007-11-07 华东理工大学 Gas phase process of preparing nanometer alumina particle
CN101513394A (en) * 2009-03-30 2009-08-26 浙江新和成股份有限公司 Continuous preparation method for nanometer dispersed vitamin A microcapsule
CN106348306A (en) * 2016-10-21 2017-01-25 浙江华飞电子基材有限公司 Preparation method for spherical nano-silicon dioxide
CN106698509A (en) * 2015-11-17 2017-05-24 林莉 Composite nano zirconium oxide with uniform particle size distribution, and continuous preparation method and equipment thereof
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* Cited by examiner, † Cited by third party
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US3130008A (en) * 1949-11-23 1964-04-21 Cabot Corp Method of preparing metallic oxides by hydrolysis of metallic halides
JPH11147711A (en) * 1997-11-11 1999-06-02 Asahi Glass Co Ltd Alumina fine sphere and its production
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