CN206590908U - A kind of oxidizing process continuously prepares Nano-meter SiO_22Device - Google Patents

Abstract

The utility model is related to a kind of nano material preparation facilities, and particularly a kind of oxidizing process continuously prepares Nano-meter SiO_2₂Device, including charging smelting system, it is characterised in that：It is connected successively with waste gas spreading system and classification collection system by exhaust gases passes above charging smelting system, diffusion valve is provided between discarded diffusion system and classification collection system.The utility model can continuously, produce in enormous quantities Nano-meter SiO_2₂Micro mist.

Description

A kind of oxidizing process continuously prepares Nano-meter SiO_22Device

Technical field

The utility model is related to nano material preparation facilities and its method, and particularly a kind of oxidizing process connects continuously preparing nano SiO₂The device of micro mist.

Background technology

Inorganic non-metallic material silica is nontoxic, tasteless, pollution-free, because it is a kind of in unformed white powder, therefore And can be by particle size control in smaller range（Particle diameter is usually 20~200nm）, and it is high, dispersed with chemical purity The characteristic such as good, specific surface area is big, wear-resisting, corrosion-resistant, is important a member in nano material.Because nano-silica surface is deposited It is such as small with the property not available for conventional powders material in undersaturated double bond and the hydroxyl of different bond styles The features such as dimensional effect, surface-interface effect, quantum tunneling effect, macro quanta tunnel effect and special optical, thus table Reveal special mechanics, optics, electricity, both thermally and chemically magnetics, characteristic, add and prepare skill recently as nano silicon The development of art and going deep into for study on the modification, nano silicon is in rubber, plastics, coating, functional material, communication, electronics, biology The numerous areas such as and medical science is widely used.

At present, preparing the main method of nano silicon has chemical precipitation method, vapor phase method, sol-gel process, microemulsion Method, gravity Method, mechanical crushing method etc., but the above method takes that human resources are larger, and production cost is higher, and is not suitable for large quantities of Amount, consecutive production.

The content of the invention

The utility model proposes that a kind of oxidizing process continuously prepares pure nanoscale SiO aiming above mentioned problem₂Micro mist Device.

Oxidizing process of the present utility model continuously prepares Nano-meter SiO_2₂The device of micro mist, including charging smelting system, its feature It is：It is connected successively with waste gas spreading system and classification collection system by exhaust gases passes above charging smelting system, it is discarded to put Diffusion valve is provided between the system of dissipating and classification collection system.

Nano-meter SiO_2 is continuously prepared as the utility model oxidizing process₂A kind of preferred scheme of the device of micro mist, the charging Smelting system includes intermediate frequency furnace, be provided with intermediate frequency furnace above crucible, crucible be provided with seal closure, seal closure and Crucible bottom is provided with the snorkel being connected with oxygen station；The side of crucible is provided with charging deck；The waste gas is put The system of dissipating includes water-cooled flue, air intake device and the exhaust stack being connected with exhaust gases passes；The classification collection system includes multiple Back-blowing dust removing device with air exhauster is set outside the cloth bag collection device being connected with air exhauster, cloth bag collection device；Cloth bag is received Classification screen cloth is provided with exhaust gases passes between acquisition means, the bottom of cloth bag collection device sets the encryption with sprayer unit Room.

Further, described charging smelting system and waste gas spreading system are additionally provided with temperature measurer, described oxygen station It is additionally provided with pressure measurement instrument.

Further, the snorkel includes upper snorkel and the crucible bottom being connected above seal closure with hoisting mechanism Double gas blow pipes.

Further, it is additionally provided with air draught cooling valve on the exhaust gases passes.

It is preferred that, the crucible includes the graphite crucible being connected with jacking system, and graphite crucible bottom is provided with small opening, stone BN or ZrB matter crucibles are provided with outside black crucible bottom.

The utility model similar prepares Nano-meter SiO_2 with existing₂Micro mist method is compared, and it significantly has the beneficial effect that： 1st, because the utility model is applied to continuously prepare Nano-meter SiO_2₂Micro mist, therefore, with existing Nano-meter SiO_2₂Micro mist preparation method phase Than, using this method can continuously, produce in enormous quantities Nano-meter SiO_2₂Micro mist.

2nd, due to the utility model can using the raw material of high-purity, reaction container used material can manual control, so The controllable prepared SiO for obtaining high-purity₂Micro mist.

3rd, therefore, can indirect control because the utility model can control extent of reaction speed by adjusting oxygen supply intensity Yield.

4th, because the utility model can be by adjusting oxygen supply intensity or classification collection system, therefore, SiO₂The grain of micro mist Degree can be with manual control, to adapt to different use requirements.

5th, the utility model and existing Nano-meter SiO_2₂Micro mist preparation method is compared, and this method belongs to oxidizing process and continuously prepared Nano-meter SiO_2₂Micro mist category, therefore, Nano-meter SiO_2 can be prepared at low cost using this method₂Micro mist.

7th, the utility model automaticity is higher, small investment, is adapted to existing manufacturing enterprise or other smelting enterprises enter Row technology upgrading is improved.

Brief description of the drawings

Fig. 1 is that the utility model oxidizing process continuously prepares Nano-meter SiO_2₂The structural representation of device.

Embodiment

Embodiment 1：As shown in figure 1, continuously preparing Nano-meter SiO_2 using a kind of oxidizing process₂The device and process of micro mist, Once prepare Nano-meter SiO_2₂Micro mist, this method content is as follows：Debugging each equipment ensures after can normally producing, into graphite crucible 2 Install the selected silico briquettes of 2kg additional, purity ensures more than 99.9999%, Task-size Controlling is in 20~100mm, and moisture is controlled 0.5% Hereinafter, with 50kW power to electricity, the electrified regulation graphite crucible 2 of intermediate frequency furnace 1 can make its temperature rise very rapidly up to industrial silicon fusing point it On（1410℃）, industrial silicon can be all melted in 15min.To prevent the oxidation in startup stage graphite, silicon liquid is polluted in efflorescence, The valve 3 on exhaust stack can be opened, by the flue gas produced in start-up course by seal closure 4 and exhaust gases passes 5 individually by putting Separate tube 6 is discharged.Now, seal closure 4 is removed, is lifted graphite crucible using lowering or hoisting gear 7, the silicon liquid of melting is leaked by bottom Hole leaks into resistance to silicon corrosion and not in BN the or ZrB matter crucibles of contaminated industry silicon, then cover seal closure, continues to be powered but reduction power To 20~35kW, sensing silicon liquid is set to heat up.When temperature measurer 13, which determines furnace temperature, to be reached in the range of 1450~1550 DEG C, according in stove Level change, cold burden is added constantly melted in stove using charging deck 8.Now blown by being arranged on the double of Medium frequency induction furnace bottom Tracheae 9 is blown into silicon liquid in the gaseous mixture of oxygen and air, 0.8~1.6MPa of air pressure, refining furnace, refining process into stove and can gone The impurity such as Ca, Al in desilication slag, it is ensured that SiO₂Purity.The hoisting mechanism 10 set by electric furnace top, by upper snorkel Oxygen rifle 11 be down in stove inside silicon liquid, by blowing O₂Exothermic reaction is produced there is provided chemical heat with silicon liquid, both reduces electric energy, Ensure Si+O again₂→SiO₂The generation of reaction, now pours into clinker in slag cylinder 12, remaining purer silicon liquid in stove.With above-mentioned top The multiple oxygen blast gas method refining silicon liquid in bottom can also make silicon liquid in stove produce stirring action, constantly update liquid level, SiO₂Flue dust is not Stopping pregnancy is given birth to and escaped.Now, diffusion valve 14 is opened, the valve 17,18,19 closed at the top of cloth bag collection device makes flue gas first lead to Classification screen cloth 15,16 is crossed, the larger particle of granularity in flue gas is removed, the temperature of moment observation temperature measurer 20 becomes in reset procedure Change, air draught cooling valve 21 is opened when temperature is too high by flue gas cool-down.After 5min, the valve at the top of cloth bag collection device is opened 17th, 18,19 and air exhauster 22, flue gas is guided to cloth bag collection device 23,24,25, cloth bag collection device bottom is simultaneously closed off Portion's valve 26,27,28, SiO is collected by cloth bag graded collecting device or according to flue resistance difference₂Micro mist, is next opened Back-blowing dust removing device 29,30,31, it is ensured that most SiO₂Micro mist can be purified and collect.Treat SiO₂Micro mist collects dress in cloth bag classification Add up in putting to after a certain amount of, cloth bag collection device bottom valve 26,27,28 is opened, by SiO₂Micro mist importing encryption room 32, 33rd, 34 while spray, be collected into containing SiO₂The slurry of micro mist.Hereafter encryption room bottom valve 35,36,37 is opened, and is utilized Conveyer belt 38 is transmitted, and obtains containing SiO₂The slurry of micro mist, precipitates through sedimentation basin, dries, packs, you can obtain Nano-meter SiO_2₂Micro mist Finished product.After testing, the Nano-meter SiO_2 produced using this technology₂Particulate average grain diameter is in the range of 44~79nm, and purity reaches More than 99.3%.Experimental study shows：This process production efficiency is up to 97~99.5%；If using a 25kg intermediate frequency sense Answer stove, 0.5 kg/hr of nano silicon yield.If analogizing the nano silicon year using a 500kg intermediate frequency furnace Yield is up to 75 tons/year.

Embodiment 2：As shown in figure 1, continuously preparing Nano-meter SiO_2 using a kind of oxidizing process₂The device and process of micro mist, Continuously prepare Nano-meter SiO_2₂Micro mist, this method content is as follows：Debugging each equipment ensures after can normally producing, into graphite crucible 2 Install selected silico briquette additional, purity ensures more than 99.9999%, Task-size Controlling in 20~100mm, moisture control 0.5% with Under, with 50kW power to electricity, the electrified regulation graphite crucible 2 of intermediate frequency furnace 1 can be such that its temperature rises very rapidly up on industrial silicon fusing point （1410℃）, industrial silicon can be all melted in 15min.To prevent the oxidation in startup stage graphite, efflorescence pollution silicon liquid can To open the valve 3 on exhaust stack, by the flue gas produced in start-up course by seal closure 4 and exhaust gases passes 5 individually by diffusing Pipe 6 is discharged.Now, seal closure 4 is removed, is lifted graphite crucible using lowering or hoisting gear 7, the silicon liquid of fusing is passed through bottom small opening Leak into resistance to silicon corrosion and not in BN the or ZrB matter crucibles of contaminated industry silicon, then cover seal closure, continue to be powered but reduce power extremely 20~35kW, makes sensing silicon liquid heat up.Now by be arranged on double gas blow pipes 9 of Medium frequency induction furnace bottom into stove oxygen blast gas and The gaseous mixture of air（0.8~1.6MPa of air pressure）, silicon liquid in refining furnace can remove Ca, Al in white residue etc. in refining process miscellaneous Matter, it is ensured that SiO₂Purity.The hoisting mechanism 10 set by electric furnace top, silicon liquid in stove is down to by the oxygen rifle 11 of upper snorkel Inside, by blowing O₂Exothermic reaction is produced there is provided chemical heat with silicon liquid, that is, is reduced electric energy, ensured Si+O again₂→SiO₂Reaction Generation, now clinker is poured into slag cylinder 12, remaining purer silicon liquid in stove.With above-mentioned top and bottom complex blowing oxygen method refined silicon Liquid can also make silicon liquid in stove produce stirring action, constantly update liquid level, SiO₂Flue dust is constantly produced and escaped.Now, beat Diffusion valve 14 is opened, the valve 17,18,19 closed at the top of cloth bag collection device makes flue gas first pass through classification screen cloth 15,16, removed The larger particle of granularity in flue gas, the moment observes the temperature change of temperature measurer 20 in reset procedure, is opened when temperature is too high Air draught cooling valve 21 is by flue gas cool-down.After 5min, the valve 17,18,19 and air exhauster 22 at the top of cloth bag collection device are opened, will Flue gas is guided to cloth bag collection device 23,24,25, is simultaneously closed off cloth bag collection device bottom valve 26,27,28, is passed through cloth Bag graded collecting device collects SiO according to flue resistance difference₂Micro mist, next opens back-blowing dust removing device 29,30,31, Ensure majority SiO₂Micro mist can be purified and collect.Treat SiO₂Micro mist adds up in impingement dust collector to after a certain amount of, opens cloth Bag collection device bottom valve 26,27,28, by SiO₂Micro mist is sprayed while importing encryption room 32,33,34, is collected into containing SiO₂ The slurry of micro mist.Hereafter encryption room bottom valve 35,36,37 is opened, obtains containing SiO₂The slurry of micro mist, precipitated through sedimentation basin, Dry, pack, you can obtain Nano-meter SiO_2₂Micro mist finished product.Collecting SiO₂During micro mist, refining furnace is not powered off, and utilizes thermometric The chronometry furnace temperature of instrument 13, keeps it in the range of 1450~1550 DEG C, when silicon liquid level declines in stove, passes through charging deck 8 Cold burden is continuously added in stove and melted, in the case where maintaining furnace temperature, the silicon liquid amount of melting in holding furnace, and repeat the above steps, Nano-meter SiO_2 can continuously be prepared₂Micro mist.Experimental study shows：This process production efficiency is up to 97~99.5%；If adopted With a 25kg intermediate frequency furnace, 0.5 kg/hr of nano silicon yield.If analogized using a 500kg intermediate frequency furnace Nano silicon annual production up to 75 tons/year.

It is understood that specifically described above with respect to of the present utility model, be merely to illustrate the utility model and not The technical scheme described by the utility model embodiment is limited to, it will be understood by those within the art that, still can be with The utility model is modified or equivalent substitution, to reach identical technique effect；As long as satisfaction uses needs, all in this reality Within new protection domain.

Claims (6)

1. a kind of oxidizing process continuously prepares Nano-meter SiO_2₂Device, including charging smelting system, it is characterised in that：Feed melting system System top is connected with waste gas spreading system and classification collection system successively by exhaust gases passes, discards diffusion system and classification is collected Diffusion valve is provided between system.

2. a kind of oxidizing process continuously prepares Nano-meter SiO_2 according to claim 1₂Device, it is characterised in that：The charging is molten Refining system, which includes being provided with intermediate frequency furnace, intermediate frequency furnace above crucible, crucible, to be provided with seal closure, seal closure and earthenware Crucible bottom is provided with the snorkel being connected with oxygen station；The side of crucible is provided with charging deck；The waste gas spreading System includes water-cooled flue, air intake device and the exhaust stack being connected with exhaust gases passes；It is described classification collection system include it is multiple with The back-blowing dust removing device with air exhauster is set outside the connected cloth bag collection device of air exhauster, cloth bag collection device；Cloth bag is collected Classification screen cloth is provided with exhaust gases passes between device, the bottom of cloth bag collection device sets the encryption with sprayer unit Room.

3. a kind of oxidizing process continuously prepares Nano-meter SiO_2 according to claim 2₂Device, it is characterised in that：Described charging Smelting system and waste gas spreading system are additionally provided with temperature measurer, and described oxygen station is additionally provided with pressure measurement instrument.

4. a kind of oxidizing process continuously prepares Nano-meter SiO_2 according to claim 2₂Device, it is characterised in that：The snorkel Including the upper snorkel being connected above seal closure with hoisting mechanism and double gas blow pipes of crucible bottom.

5. a kind of oxidizing process continuously prepares Nano-meter SiO_2 according to claim 2₂Device, it is characterised in that：The flue gas leads to Air draught cooling valve is additionally provided with road.

6. a kind of oxidizing process continuously prepares Nano-meter SiO_2 according to claim 2₂Device, it is characterised in that：The crucible bag The graphite crucible being connected with jacking system is included, graphite crucible bottom is provided with outside small opening, graphite crucible bottom and is provided with BN or ZrB Matter crucible.