CN102502745B - Manufacture method and device of nanometer alumina powder - Google Patents
Manufacture method and device of nanometer alumina powder Download PDFInfo
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- CN102502745B CN102502745B CN201110380691.9A CN201110380691A CN102502745B CN 102502745 B CN102502745 B CN 102502745B CN 201110380691 A CN201110380691 A CN 201110380691A CN 102502745 B CN102502745 B CN 102502745B
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Abstract
The invention provides a manufacture method and device of nanometer alumina powder. Elemental aluminum, chlorine gas and water are used as main raw materials, a chemical vapor method is used for synthesizing the nanometer alumina powder, the technological process is simple and safe, the energy utilization rate is high, the manufacture cost is lower, and the produced nanometer alumina powder has better dispersibility. The method comprises the following steps that: 1) firstly, an elemental aluminum block is heated and melt into melt elemental aluminum, and then, the elemental aluminum is in the reaction with the chlorine gas to generate gaseous aluminum trichloride; 2) the gaseous aluminum trichloride and water steam are subjected to reaction for generating aluminum oxide solid particles and hydrogen chloride gas; and 3) the generated aluminum oxide solid particles and the hydrogen chloride gas are subjected to solid and gas separation, the collected prepared solid is the nanometer alumina powder, and the gas is sent to a subsequent work procedure to be treated.
Description
Technical field
The present invention relates to technical field of nano material, particularly a kind of nano alumina powder jointed manufacturing method and apparatus.Described manufacturing method and apparatus is take pure aluminum, chlorine G&W as main raw material, 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 rigidity, the high characteristic such as heat-resisting and corrosion-resistant, being widely used in the fields such as catalysis, pottery, space flight and aviation, is current usage quantity maximum, most important nano-oxide, and market outlook are very wide.At present, known nano alumina powder jointed manufacture method is a lot, sum up mainly and be divided three classes: solid phase method, liquid phase method and vapor phase process, wherein applying many is liquid phase method, and manufacture the nano alumina powder jointed raw materials used aluminum contained compound that is generally, the inventor, through retrieval, does not also find about utilizing the nano alumina powder jointed technology of the synthetic preparation of CVD for pure aluminum (Chemical Vapor Deposition, chemical vapour deposition).
Summary of the invention
The invention provides a kind of nano alumina powder jointed manufacturing method and apparatus, take pure aluminum, chlorine G&W as 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 nano alumina powder jointed manufacture method, is characterized in that, comprises the following steps:
1) be first melting pure aluminum by simple substance aluminium block heating and melting, then generate gaseous state aluminum chloride with chlorine reaction;
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 of generation and hydrogen chloride gas are carried out to solid and gas and separate, collect prepared solid and be nano alumina powder jointed, gas send subsequent handling processing.
Described step 1) in, by adjusting chlorine flowrate, control the production flow of the gaseous state aluminum chloride of reaction generation; By importing a certain amount of nitrogen or argon gas that does not participate in reaction, control the flow of nitrogen or argon gas, to adjust the concentration of gaseous state aluminum chloride.
Described step 2) in, import water vapor with certain flow, the reaction heat discharging absorb melting pure aluminum and chlorine reaction before water vapor and gaseous state aluminum chloride react time, and make water vapor self reach the temperature requirement reacting with gaseous state aluminum chloride; In the time that gaseous state aluminum chloride and water vapor react, import oxygen as catalyzer using certain flow.
Described step 2) in, by controlling the temperature of reaction of gaseous state aluminum chloride and water vapor, to generate the nano alumina powder jointed of different structure.
Described step 3) in, separating before aluminium sesquioxide solid particulate and hydrogen chloride gas, by importing a certain amount of gas at normal temperature that does not participate in reaction, reduce resultant temperature, make the solid aluminium sesquioxide powder surface activity decreased generating.
A kind of nano alumina powder jointed manufacturing installation, it is characterized in that, comprise molten bath, reactor and the separator of process furnace, double braid covering cartridge type, described process furnace is placed in the bottom in molten bath, the top in molten bath has the charging opening that adds 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 carrying water vapor; The bottom connection of described reactor is positioned at the steam outlet at urceolus top, described molten bath and is positioned at the gaseous state aluminum chloride pneumatic outlet at inner core top, described molten bath; The top of reactor has resultant transfer lime and is connected with described separator, has collection mouth and the hydrogen chloride gas relief outlet of solid aluminium sesquioxide powder on separator.
The top in described molten bath also has conveying and does not participate in the gas duct of adjustment aluminum chloride concentration of reaction, and described conduit is communicated with the aluminum chloride pneumatic outlet that is positioned at inner core top, described molten bath.
On the urceolus in described molten bath, there is the conduit that imports catalytic gas.
On the sidewall of described reactor head, have air distribution outlet, described air distribution outlet is positioned at the top of the resultant transfer lime mouth of pipe of described reactor head.
The material of the inner core in described molten bath is stainless steel or tantalum alloy or nickelalloy or titanium alloy material; The material of the conduit of described conveying chlorine is ceramic-like materials; The material of described reactor is titanium alloy or ceramic-like materials; Described reactor is that end face radius is 22.5mm, the cylindrical shape that length is 450mm; On described molten bath, also there is the liquidometer that shows melting pure aluminum liquid liquid level.
Technique effect of the present invention:
The superiority of nano alumina powder jointed manufacture method provided by the invention is: 1) will after pure aluminum heating and melting, generate gaseous state aluminum chloride with chlorine reaction, the expensive aluminum chloride using than halogenide synthesis method in the past, makes the manufacturing cost of nano-powder lower; 2) when chlorine is by molten aluminum liquid, react with pure aluminum when generating 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 reacting with gaseous state aluminum chloride sponge unnecessary amount of heat simultaneously, take full advantage of reaction heat, reduce on the one hand cost, improve on the other hand capacity usage ratio, energy-saving and emission-reduction; 3) with halogenide synthesis method comparison in the past, save complex structure, heating system that heat exchange efficiency is low, technological process is simplified; 4), when halogenide is in the past synthetic, when production system occurs to leak, halt system rapidly, as long as the present invention closes chlorine passage, just can stop being rapidly harmful to leakage, has improved the security of production process; 5) compare with various liquid phase methods in the past, the product of manufacture 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, safe and reliable.Comprise process furnace, double braid covering cartridge type molten bath, reactor and separator, utilize the inner core in double braid covering cartridge type molten bath to carry out melting pure aluminum and generate gaseous state aluminum chloride with reacting of chlorine, the top in molten bath has the charging opening that adds simple substance aluminium block to molten bath inner core, and the bottom in molten bath has conduit from chlorine to molten bath inner core that carry; The top of inner core also has conveying and does not participate in the conduit of other gases of the adjustment aluminum chloride concentration of reaction, can import a certain amount of other gases that do not participate in reaction, to adjust the concentration of gaseous state aluminum chloride of generation; The urceolus in molten bath connects the conduit of carrying water vapor, utilizes the annular urceolus that surrounds inner core to carry water vapour, makes water vapour fully absorb react a large amount of reaction heat of release of melting pure aluminum and chlorine simultaneously; In reactor, gaseous state aluminum chloride and water vapour react and generate nano-aluminium oxide and hydrogen chloride gas, on the sidewall of the top of reactor, there is the air distribution outlet that importing does not participate in other gases of reaction, can import the gas at normal temperature that does not participate in reaction of appropriate amount, reduce resultant temperature, to reduce the surfactivity of the solid aluminium sesquioxide powder generating, reunite or reduce agglomeration strength in order to avoid form between powder; Collection mouth and the gas discharge outlet on separator with solid oxidation powder, solid is nano-aluminium oxide powder, and hydrogen chloride gas send subsequent handling to carry out environmental protection treatment; Because melting pure aluminum and chlorine are respectively by conduit input molten bath separately, if production system meets accident while leakage, as long as close chlorine passage, just can stop being rapidly harmful to leakage.
Accompanying drawing explanation
Fig. 1 is the structural representation of apparatus of the present invention.
Reference numeral lists 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, 8-air distribution outlet, 9-transfer lime, 10-separator, 11-water vapour conduit, 12-process furnace, 13-aluminium liquid liquidometer, 14-chlorine conduit, 15-adjusts the gas duct of aluminum chloride concentration, 16-catalytic gas conduit, 17-steam outlet, 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 nano alumina powder jointed manufacture method, comprises the following steps: be first 1) melting pure aluminum by simple substance aluminium block heating and melting, then generate gaseous state aluminum chloride with chlorine reaction; 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 of generation and hydrogen chloride gas are carried out to solid and gas and separate, collect prepared solid and be nano alumina powder jointed, gas send subsequent handling processing.
Wherein, step 1) in, by adjusting chlorine flowrate, control the production flow of the gaseous state aluminum chloride of reaction generation; By importing a certain amount of nitrogen or argon gas that does not participate in reaction, control the flow of nitrogen or argon gas, to adjust the concentration of gaseous state aluminum chloride; Step 2) in, import water vapor with certain flow, the reaction heat discharging absorb melting pure aluminum and chlorine reaction before water vapor and gaseous state aluminum chloride react time, and make water vapor self reach the temperature requirement reacting with gaseous state aluminum chloride; If fail to reach temperature of reaction, can reach temperature of reaction by improving water vapour initial temperature or heating means; In the time that gaseous state aluminum chloride and water vapor react, import oxygen as catalyzer using certain flow; And by the temperature of reaction of gaseous state aluminum chloride and water vapor in control reactor, generate the nano alumina powder jointed of different structure; For example, when adjustment temperature of reaction is 900 ℃, can produce α phase nano aluminium oxide; When adjustment temperature of reaction is 780 ℃, can produce γ phase nano aluminium oxide; When adjustment temperature of reaction is 600 ℃, can produce amorphous nano aluminium oxide; Step 3) in, separating before aluminium sesquioxide solid particulate and hydrogen chloride gas, by importing a certain amount of gas at normal temperature that does not participate in reaction, reduce resultant temperature, make the solid aluminium sesquioxide powder surface activity decreased generating.
As shown in Figure 1, a kind of nano alumina powder jointed manufacturing installation, comprise process furnace 12, double braid covering cartridge type molten bath 20, reactor 7 and separator 10, process furnace 12 is placed in the bottom in molten bath 20, the top in molten bath 20 has the charging opening 1 that adds 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 carrying water vapor; The bottom connection of reactor 7 is positioned at the steam outlet 17 at molten bath urceolus 5 tops and is positioned at the gaseous state aluminum chloride pneumatic outlet 6 at molten bath inner core 4 tops; The top of reactor 7 has resultant transfer lime 9 and is connected with separator 10, has collection mouth 18 and the hydrogen chloride gas relief outlet 19 of solid aluminium sesquioxide powder on separator 10; The top in molten bath 20 also has conveying and does not participate in the gas duct 15 of adjustment aluminum chloride concentration of reaction, and conduit 15 is communicated with the aluminum chloride pneumatic outlet 6 at molten bath inner core 4 tops; On the urceolus 5 in molten bath 20, also there is the conduit 16 that imports catalytic gas; There is in addition the liquidometer 13 that shows pure aluminum liquid liquid level; On the sidewall at reactor 8 tops, there is the air distribution outlet 8 that importing does not participate in other gases of reaction, 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 enter transfer lime 9 around, thereby resultant of reaction is evenly 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 to corrode by resistance to chlorine, adopt ceramic-like materials preparation; The material of reactor 7 is titanium alloy or ceramic-like materials, and selecting end face radius is 22.5mm, the cylindrical shape that length is 450mm or other shapes.
The process that this device is manufactured nano oxide powder is as follows: open valve 2 and 3, by simple substance aluminium block valve-off 2 and 3 after charging opening 1 adds the inner core 4 in double braid covering cartridge type molten bath 20, the process furnace 12 that is placed in 20 bottoms, double braid covering cartridge type molten bath starts heating, to the complete melting of aluminium block, stop heating, because subsequent reactions is thermopositive reaction, no longer need heating.Chlorine is imported to molten bath inner core 4 bottoms by conduit 14; At the interior chlorine of inner core 4 during by molten aluminum and reactive aluminum generate gaseous state aluminum chloride and emerge after aluminium liquid liquid level from gaseous state aluminum chloride gas jet outlet 6 ejections at molten bath inner core 4 tops, enter reactor 7, and in molten bath, discharge a large amount of reaction heat and pass to aluminium liquid.Can not participate in by conduit 15 according to specific needs other gases of reaction to the interior importing of inner core 4, as nitrogen, argon gas etc., adjust the concentration of aluminum chloride, control the technical indicator of product.Water vapour is imported by conduit 11 in the urceolus 5 of double layer sleeve barrel, in circumferential weld between inner core and urceolus, water vapour sponges by barrel the waste heat that molten aluminum absorbs from reaction heat in uphill process, and make self to reach after the temperature of reaction requirement, enter reactor 7 from exporting 6 ejections, if fail to reach temperature of reaction, can reach reaction by the method for raising water vapour initial temperature or the heating of unlatching process furnace temperature required.Also can be to other subsequent reactions catalysis gases of the interior importing of the urceolus of double layer sleeve barrel 5, as: oxygen, catalytic gas can import by conduit 16 or 11 two kinds of modes of conduit.React with water vapour and generate after aluminium sesquioxide solid particulate and hydrogen chloride gas at the interior gaseous state aluminum chloride of reactor 7, enter in separator 10 from the transfer lime 9 at reactor 7 tops; Aluminium sesquioxide is wherein exactly that the present invention is prepared nano alumina powder jointed; What import appropriate amount by near the air distribution outlet 8 interface of reactor 7 and separator 10 does not participate in the gas that reacts, make the powder surface activity decreased generating, reunite or reduce 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 enter transfer lime 9 around, thereby resultant of reaction is evenly pressed into transfer lime 9.Separated at the interior gas of separator 10 and solid, the nano-powder that solid obtains for the present invention, gas send subsequent handling to carry out environmental protection treatment.In the time that aluminium liquid liquidometer 13 shows liquid level low level, open valve 2, put into appropriate aluminium block, valve-off 2, then open valve 3 and allow aluminium block fall into the interior rear valve-off 3 in molten bath 4.
In concrete production process, in the time importing chlorine, by adjusting chlorine flowrate, controlling aluminum chloride production flow is 0.02mol/s; For adjusting the concentration of gaseous state aluminum chloride, general importing does not participate in the nitrogen of reaction, and the flow of controlling nitrogen is 0.047mol/s; In the time importing water vapour to molten bath urceolus, control steam rates is 0.2mol/s; In the time that gaseous state aluminum chloride and water vapor react, import oxygen as catalyzer using certain flow, the flow of controlling oxygen is 0.067mol/s.By controlling the temperature of reaction of gaseous state aluminum chloride and water vapor, generate the nano alumina powder jointed, concrete of different structure, when adjustment temperature of reaction is 900 ℃, can produce α phase nano aluminium oxide; When adjustment temperature of reaction is 780 ℃, can produce γ phase nano aluminium oxide; When adjustment temperature of reaction is 600 ℃, can produce amorphous nano aluminium oxide.
Should be understood that; the above embodiment can make the invention of those skilled in the art's comprehend; but do not limit the present invention in any way creation; all do not depart from technical scheme and the improvement thereof of the spirit and scope of the invention, and it is all encompassed in the middle of the protection domain of the invention patent.
Claims (9)
1. a nano alumina powder jointed manufacturing installation, it is characterized in that, comprise molten bath, reactor and the separator of process furnace, double braid covering cartridge type, described process furnace is placed in the bottom in molten bath, the top in molten bath has the charging opening that adds 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 carrying water vapor; The bottom connection of described reactor is positioned at the steam outlet at urceolus top, described molten bath and is positioned at the gaseous state aluminum chloride pneumatic outlet at inner core top, described molten bath; The top of reactor has resultant transfer lime and is connected with described separator, has collection mouth and the hydrogen chloride gas relief outlet of solid aluminium sesquioxide powder on separator.
2. nano alumina powder jointed manufacturing installation according to claim 1, it is characterized in that, the top in described molten bath also has conveying and does not participate in the gas duct of adjustment aluminum chloride concentration of reaction, and described conduit is communicated with the aluminum chloride pneumatic outlet that is positioned at inner core top, described molten bath.
3. nano alumina powder jointed manufacturing installation according to claim 1, is characterized in that, has the conduit that imports catalytic gas on the urceolus in described molten bath.
4. nano alumina powder jointed manufacturing installation according to claim 1, is characterized in that, on the sidewall of described reactor head, has air distribution outlet, and described air distribution outlet is positioned at the top of the resultant transfer lime mouth of pipe of described reactor head.
5. nano alumina powder jointed manufacturing installation according to claim 1, is characterized in that, the material of the inner core in described molten bath is stainless steel or tantalum alloy or nickelalloy or titanium alloy material.
6. nano alumina powder jointed manufacturing installation according to claim 1, is characterized in that, the material of the conduit of described conveying chlorine is ceramic-like materials.
7. nano alumina powder jointed manufacturing installation according to claim 1, is characterized in that, the material of described reactor is titanium alloy or ceramic-like materials.
8. nano alumina powder jointed manufacturing installation according to claim 1, is characterized in that, described reactor is that end face radius is 22.5mm, the cylindrical shape that length is 450mm.
9. nano alumina powder jointed manufacturing installation according to claim 1, is characterized in that, also has the liquidometer that shows melting pure aluminum liquid liquid level on described molten bath.
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| CN104609375A (en) * | 2014-12-03 | 2015-05-13 | 胡晞 | Nano oxide composite powder and preparation method |
| CN105084400A (en) * | 2015-09-18 | 2015-11-25 | 东北大学 | Device and method for preparing activated aluminum oxide |
| CN106241845B (en) * | 2016-08-29 | 2017-12-22 | 何顺爱 | A kind of ultrapure ball-aluminium oxide powder preparation method |
| CN111874930A (en) * | 2020-08-10 | 2020-11-03 | 南通江山农药化工股份有限公司 | Method for preparing low-iron ion nano alumina by gas phase method and product thereof |
| CN112047712A (en) * | 2020-08-19 | 2020-12-08 | 南通江山农药化工股份有限公司 | Nano heat insulation plate and preparation method thereof |
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Effective date of registration: 20160616 Address after: North building, No. 218 building A1 Xinghu Street Industrial Park of Suzhou city in Jiangsu province 215125 3 floor G36 Patentee after: Suzhou Huaweite Powder Technology Co.,Ltd. Address before: Xinghu Street Industrial Park of Suzhou city in Jiangsu province 215000 No. 218 building C9 Room 101 Patentee before: Suzhou Huaweite Powder Technology Co.,Ltd. Patentee before: Hu Xi |
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