A kind of nano alumina powder jointed manufacturing method and apparatus
Technical field
The present invention relates to technical field of nano material, particularly a kind of nano alumina powder jointed manufacturing method and apparatus.Said manufacturing method and apparatus is to be main raw material with pure aluminum, chlorine G&W, with the method and apparatus of CVD (Chemical Vapor Deposition, chemical vapour deposition) synthesizing nano alumina powder.
Background technology
Nano aluminium oxide is as a kind of novel high function fine inorganic material; Because it has high firmness, high characteristic such as heat-resisting and corrosion-resistant; Being widely used in fields such as catalysis, pottery, space flight and aviation, is that present usage quantity is maximum, most important nano-oxide, and market outlook are very wide.At present; Known nano alumina powder jointed method of manufacture is a lot, summarizes to get up mainly to be divided three classes: solid phase method, liquid phase method and vapor phase process, and wherein using many is liquid phase method; And make the nano alumina powder jointed raw materials used aluminum contained compound that is generally; The inventor does not also find about utilizing pure aluminum with the nano alumina powder jointed technology of the synthetic preparation of CVD (Chemical Vapor Deposition, chemical vapour deposition) through retrieval.
Summary of the invention
The present invention provides a kind of nano alumina powder jointed manufacturing method and apparatus; With pure aluminum, chlorine G&W is main raw material, with CVD (Chemical Vapor Deposition, chemical vapour deposition) synthesizing nano alumina powder; Technological process is simple, safety; Capacity usage ratio is high, and manufacturing cost is lower, and production nano alumina powder jointed has better dispersiveness.
Technical scheme of the present invention is:
A kind of nano alumina powder jointed method of manufacture is characterized in that, may further comprise the steps:
1) is the fusion pure aluminum at first, generates the gaseous state aluminum chloride with chlorine reaction then simple substance aluminium block heating and melting;
2) again gaseous state aluminum chloride and water vapor are reacted, generate aluminium sesquioxide solid particulate and hydrogen chloride gas;
3) the aluminium sesquioxide solid particulate that generates is carried out solid and gas with hydrogen chloride gas and separate, collect prepared solid and be nano alumina powder jointed, gas send the subsequent handling processing.
In the said step 1), through the adjustment chlorine flowrate, the production flow of the gaseous state aluminum chloride that the control reaction generates; Through importing a certain amount of nitrogen or argon gas of reacting of not participating in, the flow of control nitrogen or argon gas is with the concentration of adjustment gaseous state aluminum chloride.
Said step 2) in, import water vapor with certain flow, the reaction heat that before water vapor and gaseous state aluminum chloride react, discharges when absorption fusion pure aluminum and chlorine reaction, and make water vapor self reach the temperature requirement that reacts with the gaseous state aluminum chloride; When gaseous state aluminum chloride and water vapor react, import oxygen as catalyzer with certain flow.
Said step 2) in, through the temperature of reaction of control gaseous state aluminum chloride and water vapor, to generate the nano alumina powder jointed of different structure.
In the said step 3), before separating aluminium sesquioxide solid particulate and hydrogen chloride gas,, reduce the resultant temperature, make the active reduction of solid aluminium sesquioxide powder surface of generation through importing a certain amount of gas at normal temperature of reacting of not participating in.
A kind of nano alumina powder jointed manufacturing installation; It is characterized in that; Comprise molten bath, reactor drum and the separator of process furnace, double braid covering cartridge type, said process furnace places the bottom in molten bath, and the top in molten bath has the charging opening that adds the simple substance aluminium block to the inner core in molten bath; The bottom in molten bath has conduit from chlorine to the inner core in molten bath that carry, and the urceolus in molten bath connects the conduit of fluming water steam; The bottom of said reactor drum connects the gaseous state aluminum chloride pneumatic outlet that is positioned at the steam outlet at urceolus top, said molten bath and is positioned at inner core top, said molten bath; The top of reactor drum has the resultant transfer lime and is connected with said separator, has the collection mouth and the hydrogen chloride gas relief outlet of solid aluminium sesquioxide powder on the separator.
The top in said molten bath also has the gas duct of the adjustment aluminum chloride concentration that conveying do not participate in reacting, and said conduit is communicated with the aluminum chloride pneumatic outlet that is positioned at inner core top, said molten bath.
Has the conduit that imports catalytic gas on the urceolus in said molten bath.
Have air distribution outlet on the sidewall of said reactor head, said air distribution outlet is positioned at the top of the resultant transfer lime mouth of pipe of said reactor head.
The material of the inner core in said molten bath is stainless steel or tantalum alloy or nickelalloy or titanium alloy material; The material of the conduit of said conveying chlorine is a ceramic-like materials; The material of said reactor drum is titanium alloy or ceramic-like materials; Said reactor drum is 22.5mm for the end face radius, and length is the cylindrical shape of 450mm; Also has the liquidometer that shows fusion pure aluminum liquid liquid level on the said molten bath.
Technique effect of the present invention:
The meliority of nano alumina powder jointed method of manufacture provided by the invention is: 1) with generating the gaseous state aluminum chloride with chlorine reaction after the pure aluminum heating and melting; Expensive aluminum chloride than halogenide synthesis method is in the past used makes the manufacturing cost of nano-powder lower; When 2) chlorine is through molten aluminum liquid and pure aluminum reaction when generating the gaseous state aluminum chloride and emerging aluminium liquid liquid level; Discharge a large amount of reaction heat and pass to aluminium liquid; Make the water vapour that reacts with the gaseous state aluminum chloride sponge unnecessary a large amount of heat simultaneously, made full use of reaction heat, reduced cost on the one hand; Improve capacity usage ratio on the other hand, energy-saving and emission-reduction; 3) with in the past halogenide synthesis method relatively, saved complex structure, heating system that heat exchange efficiency is low, technological process is oversimplified; When 4) in the past halogenide was synthetic, when production system took place to leak, halt system as long as the present invention closes the chlorine passage, just can stop rapidly being harmful to leakage rapidly, has improved the security of production process; 5) compare with various liquid phase methods in the past, the product of manufacturing of the present invention has better dispersiveness.
Nano alumina powder jointed manufacturing installation provided by the invention, simple in structure, capacity usage ratio is high, and is safe and reliable.Comprise process furnace, double braid covering cartridge type molten bath, reactor drum and separator; The reaction that utilizes the inner core in double braid covering cartridge type molten bath to carry out fusion pure aluminum and chlorine generates the gaseous state aluminum chloride; The top in molten bath has the charging opening that adds the simple substance aluminium block to the molten bath inner core, and the bottom in molten bath has conduit from chlorine to the molten bath inner core that carry; The top of inner core also has the conduit of other gases of the adjustment aluminum chloride concentration that conveying do not participate in reacting, and can import a certain amount of other gases of not participating in reacting, the concentration of the gaseous state aluminum chloride that generates with adjustment; The urceolus in molten bath connects the conduit of fluming water steam, utilizes the annular urceolus fluming water steam that surrounds inner core, makes water vapour fully absorb react a large amount of reaction heat of release of fusion pure aluminum and chlorine simultaneously; Gaseous state aluminum chloride and water vapour react and generate nano-aluminium oxide and hydrogen chloride gas in reactor drum; The air distribution outlet that on the sidewall of the top of reactor drum, has other gases that importing do not participate in reacting; What can import appropriate amount does not participate in the gas at normal temperature of reacting; Reduce the resultant temperature, to reduce the surfactivity of the solid aluminium sesquioxide powder that generates, in order to avoid form reunion between powder or reduce agglomeration strength; Have the collection mouth and the gas discharge outlet of solid oxidation powder on the separator, solid is the nano-aluminium oxide powder, and hydrogen chloride gas send subsequent handling to carry out environmental protection treatment; Because fusion pure aluminum and chlorine through in the conduit input molten bath separately, if production system meets accident when leaking, as long as close the chlorine passage, just can stop rapidly being harmful to leakage respectively.
Description of drawings
Fig. 1 is the structural representation of apparatus of the present invention.
Reference numeral is listed as follows: 1-aluminium block charging opening, 2-valve, 3-valve, 4-molten bath inner core, 5-molten bath urceolus; 6-gaseous state aluminum chloride pneumatic outlet, 7-reactor drum, 8-air distribution outlet, 9-transfer lime, 10-separator; 11-water vapour conduit, 12-process furnace, 13-aluminium liquid liquidometer, 14-chlorine conduit, the gas duct of 15-adjustment aluminum chloride concentration; 16-catalytic gas conduit, the 17-steam outlet, the 18-powder is collected mouth, the outlet of 19-tail gas, 20-double braid covering cartridge type molten bath.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are described further.
A kind of nano alumina powder jointed method of manufacture may further comprise the steps: be the fusion pure aluminum with simple substance aluminium block heating and melting at first 1), generate the gaseous state aluminum chloride with chlorine reaction then; 2) again gaseous state aluminum chloride and water vapor are reacted, generate aluminium sesquioxide solid particulate and hydrogen chloride gas; 3) the aluminium sesquioxide solid particulate that generates is carried out solid and gas with hydrogen chloride gas and separate, collect prepared solid and be nano alumina powder jointed, gas send the subsequent handling processing.
Wherein, in the step 1), through the adjustment chlorine flowrate, the production flow of the gaseous state aluminum chloride that the control reaction generates; Through importing a certain amount of nitrogen or argon gas of reacting of not participating in, the flow of control nitrogen or argon gas is with the concentration of adjustment gaseous state aluminum chloride; Step 2) in, import water vapor with certain flow, the reaction heat that before water vapor and gaseous state aluminum chloride react, discharges when absorption fusion pure aluminum and chlorine reaction, and make water vapor self reach the temperature requirement that reacts with the gaseous state aluminum chloride; If fail to reach temperature of reaction, can reach temperature of reaction through improving water vapour initial temperature or heating means; When gaseous state aluminum chloride and water vapor react, import oxygen as catalyzer with certain flow; And, generate the nano alumina powder jointed of different structure through the temperature of reaction of gaseous state aluminum chloride in the controlling reactor and water vapor; For example, when the adjustment temperature of reaction is 900 ℃, can produce α phase nano aluminium oxide; When the adjustment temperature of reaction is 780 ℃, can produce γ phase nano aluminium oxide; When the adjustment temperature of reaction is 600 ℃, can produce amorphous nano aluminium oxide; In the step 3), before separating aluminium sesquioxide solid particulate and hydrogen chloride gas,, reduce the resultant temperature, make the active reduction of solid aluminium sesquioxide powder surface of generation through importing a certain amount of gas at normal temperature of reacting of not participating in.
As shown in Figure 1; A kind of nano alumina powder jointed manufacturing installation comprises process furnace 12, double braid covering cartridge type molten bath 20, reactor drum 7 and separator 10, and process furnace 12 places the bottom in molten bath 20; The top in molten bath 20 has the charging opening 1 that adds the simple substance aluminium block to molten bath inner core 4; Charging opening 1 below has valve 2 and valve 3, and the bottom in molten bath 20 has conduit 14 from chlorine to molten bath inner core 4 that carry, and the urceolus 5 in molten bath 20 connects the conduit 11 of fluming water steam; The bottom of reactor drum 7 connects the gaseous state aluminum chloride pneumatic outlet 6 that is positioned at the steam outlet 17 at molten bath urceolus 5 tops and is positioned at molten bath inner core 4 tops; The top of reactor drum 7 has resultant transfer lime 9 and is connected with separator 10, has the collection mouth 18 and the hydrogen chloride gas relief outlet 19 of solid aluminium sesquioxide powder on the separator 10; The top in molten bath 20 also has the gas duct 15 of the adjustment aluminum chloride concentration that conveying do not participate in reacting, and conduit 15 is communicated with the aluminum chloride pneumatic outlet 6 at molten bath inner core 4 tops; Also has the conduit 16 that imports catalytic gas on the urceolus 5 in molten bath 20; Has the liquidometer 13 that shows pure aluminum liquid liquid level in addition; The air distribution outlet 8 that has other gases that importing do not participate in reacting on the sidewall at reactor drum 8 tops; Air distribution outlet 8 is positioned at the top of the mouth of pipe of the resultant transfer lime 9 of reactor head; Make even air get into transfer lime 9 around, thereby resultant of reaction evenly is pressed into transfer lime 9; The material of molten bath inner core 4 is stainless steel or tantalum alloy or nickelalloy or titanium alloy material; Carry the selection of the conduit 14 of chlorine body to want and to corrode by resistance to chlorine, adopt the ceramic-like materials preparation; The material of reactor drum 7 is titanium alloy or ceramic-like materials, and selecting the end face radius for use is 22.5mm, and length is cylindrical shape or other shapes of 450mm.
The process that this device is made nano oxide powder is following: open valve 2 and 3; With simple substance aluminium block back valve-off 2 and 3 from the inner core 4 in charging opening 1 adding double braid covering cartridge type molten bath 20; Place the process furnace 12 of 20 bottoms, double braid covering cartridge type molten bath to begin heating,, stop heating to the complete fusion of aluminium block; Because subsequent reactions is thermopositive reaction, no longer need heating.Chlorine is passed through inner core 4 bottoms, conduit 14 importing molten bath; When chlorine is through molten aluminum in inner core 4 and reactive aluminum generate gaseous state aluminum chloride gas jet outlet 6 ejections at inner core 4 tops from the molten bath behind the aluminium liquid liquid level of emerging of gaseous state aluminum chloride; Get into reactor drum 7, and in the molten bath, discharge a large amount of reaction heat and pass to aluminium liquid.Can like nitrogen, argon gas etc., adjust the concentration of aluminum chloride through conduit 15 other gases that importing is not participated in reacting in inner core 4, the technical indicator of control product according to concrete needs.Water vapour is imported in the urceolus 5 of double layer sleeve barrel through conduit 11; In the circumferential weld between inner core and urceolus; Water vapour sponges the unnecessary heat that molten aluminum absorbs through barrel from reaction heat in uphill process, and after making the temperature that self reaches the reaction requirement, get into reactor drums 7 from exporting 6 ejections; If fail to reach temperature of reaction, it is temperature required to reach reaction through the method that improves the water vapour initial temperature or open the process furnace heating.Also can in the urceolus 5 of double layer sleeve barrel, import other subsequent reactions catalysis and use gas, as: oxygen, catalytic gas can import through conduit 16 or conduit 11 dual modes.After the reaction of gaseous state aluminum chloride and water vapour generates aluminium sesquioxide solid particulate and hydrogen chloride gas in reactor drum 7, enter in the separator 10 from the transfer lime 9 at reactor drum 7 tops; Aluminium sesquioxide wherein is exactly that the present invention is prepared nano alumina powder jointed; Do not participate in the gas that reacts through what near the air distribution outlet the interface of reactor drum 7 and separator 10 8 imported appropriate amounts; Make active reduction of powder surface of generation; Reunite or the reduction agglomeration strength in order to avoid form between powder; Air distribution outlet 8 is positioned at the top of transfer lime 9 mouths of pipe, make even air get into transfer lime 9 around, thereby resultant of reaction evenly is pressed into transfer lime 9.Gas and solid are separated in separator 10, and solid is the nano-powder that the present invention obtained, and gas send subsequent handling to carry out environmental protection treatment.When aluminium liquid liquidometer 13 shows the liquid level low level, open valve 2, put into an amount of aluminium block, valve-off 2 is opened valve 3 again and is let aluminium block fall into back valve-off 3 in the molten bath 4.
In concrete production process, when importing chlorine, through the adjustment chlorine flowrate, it is 0.02mol/s that the control aluminum chloride is produced flow; Be the concentration of adjustment gaseous state aluminum chloride, the nitrogen that reacts is not participated in general importing, and the flow of control nitrogen is 0.047mol/s; When the molten bath urceolus imports water vapour, the control steam rates is 0.2mol/s; When gaseous state aluminum chloride and water vapor react, import oxygen as catalyzer with certain flow, the flow of control oxygen is 0.067mol/s.Through the temperature of reaction of control gaseous state aluminum chloride and water vapor, generate the nano alumina powder jointed, concrete of different structure, when the adjustment temperature of reaction is 900 ℃, can produce α phase nano aluminium oxide; When the adjustment temperature of reaction is 780 ℃, can produce γ phase nano aluminium oxide; When the adjustment temperature of reaction is 600 ℃, can produce amorphous nano aluminium oxide.
Should be understood that; The above embodiment can make those skilled in the art more fully understand the invention; But do not limit the present invention in any way creation; All do not break away from the technical scheme and the improvement thereof of the spirit and the scope of the invention, and it all is encompassed in the middle of the protection domain of the invention patent.