CN108101001A - Powder body material preparation facilities - Google Patents
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- CN108101001A CN108101001A CN201810098097.2A CN201810098097A CN108101001A CN 108101001 A CN108101001 A CN 108101001A CN 201810098097 A CN201810098097 A CN 201810098097A CN 108101001 A CN108101001 A CN 108101001A
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- C01—INORGANIC CHEMISTRY
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- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/20—Methods for preparing oxides or hydroxides in general by oxidation of elements in the gaseous state; by oxidation or hydrolysis of compounds in the gaseous state
- C01B13/22—Methods for preparing oxides or hydroxides in general by oxidation of elements in the gaseous state; by oxidation or hydrolysis of compounds in the gaseous state of halides or oxyhalides
- C01B13/24—Methods for preparing oxides or hydroxides in general by oxidation of elements in the gaseous state; by oxidation or hydrolysis of compounds in the gaseous state of halides or oxyhalides in the presence of hot combustion gases
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Abstract
The invention discloses a kind of powder body material preparation facilities, it is with vaporizer, mixed gas supply mechanism, air mixing machine structure, intersect gas supply mechanism and reative cell, wherein, mixed gas supply mechanism has mixing gas outlet, intersecting gas supply mechanism has cricoid intersection gas outlet, intersect gas outlet to be located between mixing gas outlet and the entrance of reative cell, and it is adjustable with mixing the distance between gas outlet to intersect gas outlet, the flame lighted at intersection gas outlet carries out the hydridization reaction of powder body material into reative cell jointly after can crossing with mixing the flame lighted at gas outlet, by adjusting intersection gas outlet with mixing the distance between gas outlet, it can obtain the hydridization powder body material with different structure.The powder body material preparation facilities structure design is exquisite, can be used for the production that vapor phase method realizes hydridization powder body material, has the advantages that applied widely, strong applicability.
Description
Technical field
The present invention relates to powder body material field, more particularly, to a kind of powder body material preparation facilities.
Background technology
Gas-phase process is one of main technique methods for preparing high pure and ultra-fine powder material.The technical method is used at present
Realizing the product of industrialized production has fumed silica, vapor phase method aluminium oxide, vapor phase method titanium oxide etc., and main technique is
Using progress pyrohydrolysis contracting after presoma (such as silicon tetrachloride, the aluminium chloride, titanium tetrachloride) vaporization of oxide powder material
It closes and obtains oxide powder, reaction principle is as follows：
MClx+H2+O2→M2Ox+HCl
Wherein M is Si, Al, Ti, Zr etc., and X is natural number, corresponding with the chemical valence of corresponding metallic element.
Vapor phase method powder body material production typical process flow it is all similar (such as US3954945, US4048290 and
Technological process disclosed in the patents such as ZL02149782.6), substantially comprising following technological process：(1) feed vaporization：Forerunner
The vaporization of body；(2) raw material mixes：Predecessor is mixed with hydrogen and oxygen (air)；(3) react：Predecessor carries out pyrohydrolysis
Reaction；(4) particle buildup：The oxide particle aggregation of reaction production, convenient for collecting；(5) gas solid separation：Oxide particle with it is anti-
Byproduct gas and the gas of excess is answered to be separated；(6) depickling：By-product and absorption during elimination reaction is in oxygen
The by-product of compound powder surface.
However, current gas-phase process is all to prepare simple oxide powder material, for many oxide powder
Compound (hydridization) technology of preparing do not have substantially.And vapor phase method oxide hybrid material is prepared using existing technology, by
In device structure designs the problem of, it is difficult to the structure of hybrid material is controlled, product stability there is also very big problem,
It is difficult to realize industrialization.Also have at present and such product is developed using sol-gel method, but sol-gel method is for product
It controls extremely difficult, it is difficult to metal oxide hybrid material uniformly, stable is obtained, and prepared using sol-gel method
The product that metal oxide hybrid material, product structure and performance are obtained with gas-phase process is very different.
The content of the invention
Based on this, it is necessary to provide a kind of powder body material for being used for vapor phase method and can be used in preparing hybrid material and prepare
Device.
A kind of powder body material preparation facilities, including vaporizer, mixed gas supply mechanism, air mixing machine structure, intersect gas supply mechanism and
Reative cell；For the vaporizer for being vaporized processing to raw material, the vaporizer has multiple, vapour described in wherein at least one
Change device with the mixed gas supply mechanism connection to provide the first vaporization raw material to the mixed gas supply mechanism, and wherein at least have one
A vaporizer connects to provide the second vaporization raw material, the mixed gas supply machine to the air mixing machine structure with the air mixing machine structure
Structure is used to the described first vaporization raw material being uniformly mixed with reaction gas, and the mixed gas supply mechanism has mixing gas outlet, institute
Air mixing machine structure is stated for the described second vaporization raw material to be uniformly mixed with reaction gas, the air mixing machine structure intersects supply with described
Mechanism connection, the intersection gas supply mechanism have cricoid intersection gas outlet, and the intersection gas outlet is located at the mixing outlet
Between mouth and the entrance of the reative cell, and the intersection gas outlet and described the distance between the gas outlet that mixes are adjustable, described
The reaction can be entered jointly with described mix by intersecting the flame lighted at gas outlet after the flame lighted at gas outlet crosses
Room.
In one of the embodiments, the mixed gas supply mechanism has main part and chuck portion, and the main part has
Mixed gas chamber and the multiple air inlets connected with the mixed gas chamber, the chuck portion be set on the main part and with institute
Stating has gap between main part, and the chuck portion has what is connect with the gap to be used for for vaporizing raw material and/or reaction gas
The air inlet that body enters, the main part is open to be formed with the chuck portion at one end described mixes gas outlet.
In one of the embodiments, the main part is in hollow tubular, is divided in the mixed gas chamber equipped with multi-layer gas
It falls apart, the mixed indoor gas flow of air cavity is divided into multiply by every layer of gas dispersion plate.
In one of the embodiments, the internal diameter of the main part is blended from one end equipped with the air inlet to described
One end of gas port is gradually reduced, and close to it is described mixing gas outlet one end, between the chuck portion and the main part
Gap is gradually reduced.
In one of the embodiments, detector unit is equipped in the mixed gas supply mechanism.
In one of the embodiments, the intersection gas supply mechanism is hollow cylinder-like structure, and inside is equipped with annular shape
The intersection gas outlet, and be equipped on the outside and the air inlet for intersecting gas outlet and connecting, the intersection gas supply mechanism
Housing, which is equipped with, connects the cushion chamber for intersecting gas outlet and the air inlet.
In one of the embodiments, the opening direction for intersecting gas outlet is tilted towards the reative cell；And/or
There are two the air inlets for intersecting gas supply mechanism, and two air inlets are oppositely arranged.
In one of the embodiments, the gas outlet that intersects is set close to one end of the intersection gas supply mechanism, described
Intersect the other end of gas supply mechanism to dock with one end fixation of the entrance of the reative cell.
In one of the embodiments, the vaporizer includes feeding mechanism, heating arrangements, heat exchange mechanisms, discharging mechanism
And control mechanism, the heat exchange mechanisms have vaporization chamber and heating chamber, the vaporization chamber is equipped with pressure detecting element, the charging
Mechanism and the discharging mechanism connect respectively with the vaporization chamber, and the heating arrangements are connected with the heating chamber, the charging
Mechanism, the discharging mechanism and heating arrangements be equipped with detector unit, the control mechanism for control the feeding mechanism,
The discharging mechanism and the heating arrangements.
In one of the embodiments, the feeding mechanism includes feed pipe and the feed rate being located on the feed pipe
Meter and inlet control valve, the feed pipe are equipped with the detector unit, and the heating arrangements include circulation pipe and are located at
Temperature control valve on the circulation pipe, one end that the circulation pipe is connected with the heating chamber are equipped with temperature detection member
Part, the heat exchange mechanisms coat the heat exchange kettle of the vaporization chamber for the heating chamber, and the discharging mechanism includes discharge nozzle and sets
Reactor effluent stream gauge on the discharge nozzle, the discharge nozzle are equipped with the detector unit, the control mechanism and institute
State feed flow meter, the inlet control valve, the temperature control valve and reactor effluent stream gauge connection.
Above-mentioned powder body material preparation facilities has vaporizer, mixed gas supply mechanism, air mixing machine structure, intersects gas supply mechanism and anti-
Room is answered, wherein, mixed gas supply mechanism has mixing gas outlet, and intersecting gas supply mechanism has cricoid intersection gas outlet, intersects
Gas port is located between mixing gas outlet and the entrance of reative cell, and intersection gas outlet is adjustable with mixing the distance between gas outlet,
The flame lighted at intersection gas outlet carries out powder into reative cell jointly after can crossing with mixing the flame lighted at gas outlet
The hydridization reaction of body material, obtains hybrid material.The first vaporization raw material can such as be lighted via mixing gas outlet, the second vaporization
Raw material is lighted via gas outlet is intersected, and by adjusting intersecting gas outlet and mixing the distance between gas outlet, can obtain by second
Vaporize cladded type hydridization powder of the raw material powder particle cladding obtained by the reaction by the first vaporization raw material powder particle obtained by the reaction
Body material or the hydridization powder body material for obtaining two kinds of particle interpenetrating networks.The powder body material preparation facilities structure design
Exquisiteness can be used for the production that vapor phase method realizes hydridization powder body material, have the advantages that applied widely, strong applicability.
Description of the drawings
Fig. 1 is the structure diagram of the powder body material preparation facilities of an embodiment；
Fig. 2 is the structure diagram of vaporizer in Fig. 1；
Fig. 3 is the structure diagram of Tu1Zhong mixed gas supplies mechanism；
Fig. 4 is the structure diagram for intersecting gas supply mechanism in Fig. 1；
Fig. 5 is mixed gas supply mechanism, the cooperation schematic diagram for intersecting gas supply mechanism and reative cell；
Fig. 6 is infrared spectrogram.
Specific embodiment
For the ease of understanding the present invention, the present invention is described more fully below with reference to relevant drawings.In attached drawing
Give presently preferred embodiments of the present invention.But the present invention can realize in many different forms, however it is not limited to this paper institutes
The embodiment of description.On the contrary, the purpose for providing these embodiments is to make the understanding to the disclosure more thorough
Comprehensively.
It should be noted that when element is referred to as " being fixed on " another element, it can be directly on another element
Or there may also be elements placed in the middle.When an element is considered as " connection " another element, it can be directly connected to
To another element or it may be simultaneously present centering elements.
Unless otherwise defined, all of technologies and scientific terms used here by the article is with belonging to technical field of the invention
The normally understood meaning of technical staff is identical.Term used in the description of the invention herein is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
The arbitrary and all combination of the Listed Items of pass.
The principle that gas-phase process prepares oxide powder material is as follows：
By the study found that when preparing the hybrid material of two or more oxides, crucial governing factor is to ensure that
Presoma (the MCl of different oxidesx) stablize supply.Because the entire production process of gas-phase process is continuous dynamic, if
Ensure the stability of the different element ratios of hybrid material, it is necessary to assure the ratio that various presomas enter reaction system is kept
Stablize.In addition it is also necessary to ensure that various raw material reactions are uniform, so as to fulfill the control to hybrid material structure.
The present invention provides a kind of powder body materials that metal oxide hybrid material is prepared using gas-phase process to prepare dress
It puts, mentality of designing is that two or more metal oxide precursors are respectively adopted vaporizer to be vaporized, each by setting
The control parameter of a vaporizer controls various predecessor vaporizations into the amount of reactor.In addition, by controlling various predecessor gas
Body enters the order of reative cell, can obtain the oxide hybridized material of different structure.
Specifically, as shown in Figure 1, the powder body material preparation facilities 10 of an embodiment of the present invention, including vaporizer 100,
Mixed gas supply mechanism 200, air mixing machine structure 300 intersect gas supply mechanism 400 and reative cell 500.Vaporizer 100 be used for raw material into
Row vaporization process.In the present embodiment, vaporizer 100 has multiple, wherein at least one vaporizer 100 and mixed gas supply machine
Structure 200 connects to provide the first vaporization raw material, and wherein at least one vaporizer 100 and mixed gas to mixed gas supply mechanism 200
Mechanism 300 connects to provide the second vaporization raw material to air mixing machine structure 300.Mixed gas supply mechanism 200 is used to vaporize raw material by first
It is uniformly mixed with reaction gas.Air mixing machine structure 300 is used to the second vaporization raw material being uniformly mixed with reaction gas.The reaction gas
Body refers to the mixed gas that hydrogen mixes according to a certain percentage with oxygen.
As shown in Fig. 3, Fig. 4 and Fig. 5, in the present embodiment, mixed gas supply mechanism 200 has mixing gas outlet 201.It is mixed
Mechanism of qi structure 300 is connected with intersecting gas supply mechanism 400, and intersecting gas supply mechanism 400 has cricoid intersection gas outlet 402.Intersect
Gas port 402 is located between mixing gas outlet 201 and the entrance of reative cell 500, and intersects gas outlet 402 with mixing gas outlet 201
The distance between it is adjustable, intersecting the flame 21 lighted at gas outlet 402 can hand over mixing the flame 22 lighted at gas outlet 201
Enter reative cell 500 after remittance jointly.Flame 21 can carry out the miscellaneous of powder body material into reative cell 500 jointly after crossing with flame 22
Change reaction, obtain hybrid material, it such as can be by the mixed gas of the first vaporization raw material and reaction gas via mixing gas outlet 201
It lights, the mixed gas of the second vaporization raw material and reaction gas is lighted via gas outlet 402 is intersected, by adjusting gas outlet is intersected
402, with mixing the distance between gas outlet 201, can obtain by the second vaporization raw material powder particle cladding obtained by the reaction by first
It vaporizes the cladded type hydridization powder body material of raw material powder particle obtained by the reaction or obtains two kinds of particle interpenetrating networks
Hydridization powder body material.10 structure design of powder body material preparation facilities is exquisite, can be used for vapor phase method and realizes hydridization powder body material
Production, there is applied widely, strong applicability.
It please join Fig. 2, in the present embodiment, vaporizer 100 includes feeding mechanism 110, heating arrangements 120, heat exchange mechanisms
130th, discharging mechanism 140 and control mechanism (not shown).Heat exchange mechanisms 130 have vaporization chamber 131 and heating chamber 132.Vaporization chamber
131 are equipped with pressure detecting element (P in figure).Feeding mechanism 110 and discharging mechanism 140 connect respectively with vaporization chamber 131.Heater
Structure 120 is connected with heating chamber 132.Feeding mechanism 110, discharging mechanism 140 and heating arrangements 120 are equipped with detector unit (figure
Middle T).Control mechanism is used to control feeding mechanism 110, discharging mechanism 140 and heating arrangements 120.
Further, the feeding mechanism 110 of present embodiment includes feed pipe 111 and the feeding flow being located on feed pipe 111
Gauge 112 and inlet control valve 113, feed pipe 111 are equipped with detector unit；Heating arrangements 120 include circulation pipe 121 and
The temperature control valve 122 being located on circulation pipe 121, one end that circulation pipe 121 is connected with heating chamber 132 are equipped with temperature detection member
Part, by the way of circulation pipe 121 goes out liquid with the mode that heating chamber 132 connects using bottom liquid inlet top, to be heating chamber 132 and vapour
The substance changed in device 131 carries out sufficient heat exchange；Heat exchange mechanisms 130 coat the heat exchange kettle of vaporization chamber 131 for heating chamber 132；
Discharging mechanism 140 includes discharge nozzle 141 and the reactor effluent stream gauge 142 being located on discharge nozzle 141, and discharge nozzle is equipped with temperature detection
Element；Control mechanism is connected with feed flow meter 112, inlet control valve 113, temperature control valve 122 and reactor effluent stream gauge 142,
Complex control system is formed, to control corresponding valve by the coherent signal gathered in time (such as temperature, pressure and flow signal)
Door opening degree.
Vaporizer 100 with said structure can realize uniform, the stable vaporization and raw material supply of raw material, after guarantee
The stability of continuous hydridization reaction.
Please join Fig. 3 again, in the present embodiment, mixed gas supply mechanism 200 has main part 210 and chuck portion 220.Main body
The air inlet for being used to enter for vaporization raw material and reaction gas that portion 210 has mixed gas chamber 211 and connected with mixed gas chamber 211
Mouth 212 and 213, vaporization raw material can enter via air inlet 212, and reaction gas can enter via air inlet 213；Or portion
Reaction gas is divided to enter together with vaporization raw material via air inlet 212, remaining reaction gas enters via air inlet 213.Chuck
Portion 220 is set on main part 210 and has gap 221 between main part 210.Chuck portion 220 has to be connected with gap 221
Be used for for vaporization raw material and/or reaction gas enter air inlet 222.Main part 210 and chuck portion 220 opening shape at one end
Into mixing gas outlet 201.The mixed gas supply mechanism 200 of present embodiment has main part 210 and chuck portion 220, from main part
The gas burning that 210 mixed gas chamber 211 sprays can form flame 223, and the gas burning sprayed from gap 221 can form fire
Flame 224, flame 224, which is coated on around flame 223, can be used as protection flame.
The main part 210 of present embodiment is in hollow tubular, mixes and multi-layer gas dispersion plate 230 is equipped in gas chamber 211.Gas
Body dispersion plate 230 can be in cellular or divergent shape.Every layer of gas dispersion plate 230 is by the gas in mixed gas chamber 211
Body runner is divided into multiply.By setting gas dispersion plate 230, the first vaporization raw material can be caused to be sufficiently mixed with reaction gas
It is even, gas dispersion plate 230 is particularly layered setting, the mixing that can further improve the first vaporization raw material and reaction gas is imitated
Fruit.
Further, the internal diameter of the main part 210 of present embodiment is from one end equipped with air inlet 212 and 213 to blending
One end of gas port 201 is gradually reduced.In diagrammatically shown specific embodiment, this, which is gradually reduced, refers to distributed gradual contracting
It is small, multistage can be such as formed, each section of internal diameter is basically identical, from one end equipped with air inlet 212 and 213 to mixing gas outlet
201 one end, latter section of internal diameter reduce compared with the last period.It, can be further by the way that the internal diameter of mixed gas chamber 211 is gradually reduced
The mixed effect of the first vaporization raw material and reaction gas is improved, and the mixed gas at mixing gas outlet 210 can be improved
Pressure, sprayed convenient for flame 223.Further, close to one end of mixing gas outlet 201, chuck portion 220 and main part
Gap between 210 is also gradually reduced, and can also so improve the pressure that the gas at mixing gas outlet 210 sprays, be convenient for
Flame 224 sprays.
In the present embodiment, detector unit 240 is equipped in mixed gas supply mechanism 200.Detector unit 240 can
With the gas temperature in the real-time mixed gas chamber 211 of detection, convenient for grasping the temperature conditions in mixed gas chamber 211 in real time, ensure the
One raw material is in vapor state always.
It please join Fig. 4, the gas supply mechanism 400 that intersects of present embodiment is hollow cylinder-like structure.Intersect gas supply mechanism 400
Inside be equipped with circular intersection gas outlet 402, and be equipped with the air inlet 401 connected with intersecting gas outlet 402 on the outside.It hands over
The housing for pitching gas supply mechanism 400 is equipped with connection intersection gas outlet 402 and the cushion chamber 403 of the air inlet 401.
Further, in the present embodiment, there are two the air inlets 401 for intersecting gas supply mechanism 400, and two air inlets
401 are oppositely arranged；Intersect gas outlet 402 to set close to the one end for intersecting gas supply mechanism 400, intersect the another of gas supply mechanism 400
It holds to fix with one end of the entrance of reative cell 500 and dock, be fixedly connected such as by flange arrangement.Intersect gas outlet 402
Opening direction orientating reaction room 500 tilts, so that the mixed gas of the second vaporization raw material and reaction gas is with fixed angle tilt
Into reative cell 500.
Above-mentioned powder body material preparation facilities 10 has vaporizer 100, mixed gas supply mechanism 200, air mixing machine structure 300, intersection
Gas supply mechanism 400 and reative cell 500.As shown in figure 5, mixed gas supply mechanism 200 has mixing gas outlet 201, intersect air feeder
Structure 400 has cricoid intersection gas outlet 402, intersects gas outlet 402 and is located at mixing gas outlet 201 and the entrance of reative cell 500
Between, and intersection gas outlet 402 is adjustable with mixing the distance between gas outlet 201, so as to intersect the fire lighted at gas outlet 402
Flame carries out powder body material into reative cell 500 jointly hydridization after can crossing with mixing the flame lighted at gas outlet 201 is anti-
Should, obtain hybrid material.
The powder body material preparation facilities of the present invention is described in further detail below in conjunction with specific embodiment.
Principles and methods
Prepare SiO2/Al2O3、SiO2/TiO2Or Al2O3/TiO2Hybrid material
Wherein prepare SiO2Presoma (raw material) selection SiCl4, Al2O3Predecessor selection AlCl3, prepare TiO2Before
Drive object is SiCl4, their own reaction principle is as follows：
As can be seen that the raw material proportioning in reaction equation is different from reaction equation (1)~(3), and at normal temperatures,
SiCl4It is liquid, its boiling point is 57.6 DEG C；And AlCl3It is then solid (powder) at normal temperatures, it starts to rise at 178 DEG C
China；TiCl4It is liquid under room temperature, boiling point is 136.4 DEG C.
Since the state of various predecessors is different, also difference is larger for vapourizing temperature, so preparing SiO2/Al2O3Hydridization material
During material, it is necessary to respectively with different material carburetors, while the feed vaporization rate of vaporizer is strictly controlled, just can guarantee two
The ratio of a precursor gas is stablized.In addition, if using traditional vapor phase method oxide technique, two kinds of precursor gas with
H2And O2Mixing, then carries out combustion reaction, then due to the reaction gas (H of each autoreaction needs of two kinds of predecessors2And O2) no
Together, easily cause local reaction gas deficiency or excessive, it is unstable to ultimately result in hybrid material surface texture.And this method
The hybrid material of acquisition is also SiO2And Al2O3Unordered hydridization.
Preparing SiO2/TiO2During hybrid material, although the predecessor of the two is liquid, react required theoretical anti-
Answer gas also identical, but this is that molar ratio is identical, since the molecular weight difference of the two is larger, so mass ratio is also deposited
In bigger difference.Further, since nearly 80 DEG C of the vapourizing temperature gap of the two, if so using same material carburetor, from
Direct boiling after liquid charging stock mixing, then due to the difference of two kinds of feed vaporization rates, it is impossible to ensure that the two mixed gas is uniform.
And use powder body material preparation facilities 10 of the present invention, then above-mentioned problem can be solved, is distinguished using two vaporizers 100
Raw material is vaporized, and by the way that temperature, the signals such as pressure and flow are linked, it can be achieved that raw material stablizes supply.
To prepare SiO2/Al2O3Exemplified by hybrid material, SiCl4It can enter after vaporization from air inlet 212, reaction gas is from air inlet 213
Into they are in mixed gas chamber 211, it can be achieved that uniformly mixing after the effect of gas dispersion plate 230；AlCl3It is and anti-after vaporization
Gas is answered to enter after being mixed in air mixing machine structure 300 through air inlet 401 and intersects gas supply mechanism 400.In addition, in air inlet 222,
H can be passed through2, O2Or protective gas of the mixed gas of the two as flame.It is supplied by mixed gas supply mechanism 200 with intersecting
The distance between mechanism of qi structure 400 makes to be spaced a distance between them, can so allow SiCl4It first burns, forms SiO2Particle,
Then again with AlCl3Flame converges so that Al2O3Particle can be in SiO2Particle surface is grown, and realizes Al2O3Coated Si O2Structure
SiO2/Al2O3Hybrid material.In addition, SiCl4And AlCl3The feed entrance point of gas exchanges, then SiO can be achieved2Cladding
Al2O3The SiO of structure2/Al2O3Hybrid material.And if the mixed gas supply mechanism 200 of upper end and lower end are intersected gas supply mechanism
400 connect together, then SiO can be achieved2And Al2O3The SiO of particle inierpeneirating network structure2/Al2O3The preparation of hybrid material.
Embodiment 1
SiCl is controlled in first vaporizer4Boil-off rate be 6.0kg/h, the SiCl of vaporization4Into mixed gas supply
Controlled at 130 ± 5 DEG C before the air inlet of mechanism.Hydrogen and amount of oxygen press SiCl4：H2：O2=1:2.55:1.5 ratio
(molar ratio), hydrogen elder generation and SiCl4Gas mixing, an air inlet of main body enters mixed gas supply mechanism, into mixing
Temperature is controlled before gas supply mechanism at 150 ± 5 DEG C.Oxygen (calculates) another of main body with the oxygen content in air 21%
Air inlet enters mixed gas supply mechanism, and temperature is controlled at 150 ± 5 DEG C.In addition SiCl is pressed4：O2=1:The oxygen of 0.8 ratio is (with sky
Oxygen content 21% in gas calculates) enter the gap between chuck portion and main part from the air inlet in chuck portion, temperature control exists
150±5℃。
AlCl3Raw material vaporizes in second vaporizer, and it is 1.3kg/h, the AlCl after vaporization to control boil-off rate3Gas
With H2And O2By AlCl3：H2：O2=1:1.65:1.05 ratio (molar ratio) mixing after Self-crossover gas supply mechanism air inlet into
Enter and intersect gas supply mechanism, it is 220 ± 5 DEG C that mixed gas is kept, which to enter preceding temperature,.
The distance between gas supply mechanism is intersected for 30cm with lower end in the mixed gas supply mechanism of holding upper end, by this technique system
Standby is Al2O3Coated Si O2The SiO of structure2/Al2O3Hybrid material is denoted as 1# samples.
Embodiment 2
In the technique and ratio of embodiment 1, various raw materials are supplied, the mixed gas supply mechanism of upper end and lower end are intersected confession
Mechanism of qi structure connects together, and distance therebetween is 0cm, is SiO by the preparation of this technique2With Al2O3Inierpeneirating network structure
SiO2/Al2O3Hybrid material is denoted as 2# samples.
Embodiment 3
By embodiment 1 material exchange, AlCl is controlled in first vaporizer3Boil-off rate for 2.0kg/h, vaporization
AlCl3Controlled at 220 ± 5 DEG C before the air inlet into mixed gas supply mechanism.Hydrogen and amount of oxygen press AlCl3：
H2：O2=1:2.05:1.25 ratios (molar ratio), hydrogen elder generation and AlCl3Gas mixing, an air inlet of main body enter
Mixed gas supply mechanism controls temperature into mixed gas supply mechanism at 220 ± 5 DEG C before.Oxygen is (with the oxygen content 21% in air
Calculating) another air inlet of main body enters mixed gas supply mechanism, and temperature is controlled at 220 ± 5 DEG C.In addition AlCl is pressed3：O2
=1:The oxygen of 0.85 ratio (is calculated) air inlet from chuck portion with the oxygen content in air 21% and enters chuck portion and main body
Gap between portion, temperature are controlled at 220 ± 5 DEG C.
SiCl4Raw material is vaporized from second vaporizer, and it is 3kg/h, the SiCl after vaporization to control boil-off rate4Gas with
H2And O2By SiCl4：H2：O2=1:2.45:The air inlet of Self-crossover gas supply mechanism enters after 1.45 ratio (molar ratio) mixing
Intersect gas supply mechanism, it is 150 ± 5 DEG C that mixed gas is kept, which to enter preceding temperature,.
The distance between gas supply mechanism is intersected for 30cm with lower end in the mixed gas supply mechanism of holding upper end, by this technique system
Standby is SiO2Coat Al2O3The SiO of structure2/Al2O3Hybrid material is denoted as 3# samples.
By above-mentioned similar technique, type of feed and combination are converted, TiO can be prepared respectively2/SiO2, TiO2/Al2O3,
TiO2/ZrO2, SiO2/ZrO2, Al2O3/ZrO2Wait hybrid materials.
The method that above-mentioned sample is dissolved by using HF tests the content of SiO2, test result such as table 1.In addition also to sample
Examination of infrared spectrum is carried out respectively, and the results are shown in Figure 6.
Table 1
| Sample ID | Theoretical SiO2Content | Survey content |
| 1# | 68.17% | 45.17% |
| 2# | 68.17% | 57.66% |
| 3# | 40.93% | 38.85% |
In terms of 1 test result of table, 1# samples are Al2O3Coated Si O2The SiO of structure2/Al2O3Hybrid material, theoretical two
Silica content is 68.17%, but actually measure the result is that 45.17%, and theoretical value deviation is larger, has been primarily due to
A part of SiO2It is by Al2O3Cladding, HF are poorly soluble the SiO being wrapped by completely2, so actual measurement content will contain less than theory
Amount.But since silica occupies the majority, so thering is a big chunk silica to be simply partly wrapped by, so still
It can be dissolved by HF.2# sample designs are SiO2With Al2O3The SiO of inierpeneirating network structure2/Al2O3Hybrid material, because also there is part
SiO2By Al2O3Cladding, so silica actual measurement content is more slightly lower than theoretical content, this is more conform with the knot of inierpeneirating network structure
Fruit.3# samples are SiO2Coat Al2O3The SiO of structure2/Al2O3Hybrid material, dioxide-containing silica measured result and theoretical content
It is close, SiO2Almost all is in outside.
Although from the spectrogram 6 of infrared spectrum as can be seen that due to synergistic effect, Partial Feature summit is blanked, right
Than 1# samples spectrogram and pure SiO2With pure Al2O3Spectrogram can be seen that in 1# sample spectrograms, in 570cm-1And 670cm-1Near
Or the obvious characteristic peak there are aluminium oxide, illustrates that still there are aluminium oxide for 1# sample surfaces；Compare 3# samples spectrogram with
Pure SiO2With pure Al2O3Spectrogram can be seen that.The characteristic peak of silica is substantially, the characteristic peak of aluminium oxide is blanked substantially,
It is substantially SiO to illustrate 3# samples2Coat Al2O3Structure.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and description is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that come for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of powder body material preparation facilities, which is characterized in that supplied including vaporizer, mixed gas supply mechanism, air mixing machine structure, intersection
Mechanism of qi structure and reative cell；For being vaporized processing to raw material, the vaporizer has multiple the vaporizer, wherein at least there is one
A vaporizer vaporizes raw material with the mixed gas supply mechanism connection to provide first to the mixed gas supply mechanism, and wherein
At least one described vaporizer is connected with the air mixing machine structure to provide the second vaporization raw material to the air mixing machine structure, described mixed
It closes gas supply mechanism to be used to the described first vaporization raw material being uniformly mixed with reaction gas, the mixed gas supply mechanism, which has, to be blended
Gas port, the air mixing machine structure be used for by described second vaporization raw material be uniformly mixed with reaction gas, the air mixing machine structure with it is described
Intersect gas supply mechanism connection, the intersection gas supply mechanism has cricoid intersection gas outlet, and the intersection gas outlet is located at described
It mixes between gas outlet and the entrance of the reative cell, and the intersection gas outlet can with described the distance between the gas outlet that mixes
It adjusts, the flame lighted at gas outlet that intersects can enter institute jointly with described mix after the flame lighted at gas outlet crosses
State reative cell.
2. powder body material preparation facilities as described in claim 1, which is characterized in that the mixed gas supply mechanism has main part
With chuck portion, the main part has mixed gas chamber and the multiple air inlets connected with the mixed gas chamber, the chuck portion
It is set on the main part and there is gap between the main part, the chuck portion has connects air inlet with the gap
Mouthful, the main part is open to be formed with the chuck portion at one end described mixes gas outlet.
3. powder body material preparation facilities as claimed in claim 2, which is characterized in that the main part is in hollow tubular, described
Equipped with multi-layer gas dispersion plate in mixed gas chamber, the mixed indoor gas flow of air cavity is divided into more by every layer of gas dispersion plate
Stock.
4. powder body material preparation facilities as claimed in claim 3, which is characterized in that the internal diameter of the main part is from equipped with described
One end of air inlet to it is described mixing gas outlet one end be gradually reduced, and close to it is described mixing gas outlet one end, it is described
Gap between chuck portion and the main part is gradually reduced.
5. powder body material preparation facilities as described in claim 1, which is characterized in that temperature is equipped in the mixed gas supply mechanism
Detecting element.
6. such as powder body material preparation facilities according to any one of claims 1 to 5, which is characterized in that the intersection air feeder
Structure is hollow cylinder-like structure, and inside is equipped with the circular intersection gas outlet, and is equipped with intersects with described on the outside
The air inlet of gas port connection, the housing for intersecting gas supply mechanism, which is equipped with, connects the intersection gas outlet and the buffering of the air inlet
Chamber.
7. powder body material preparation facilities as claimed in claim 6, which is characterized in that the opening direction court for intersecting gas outlet
It is tilted to the reative cell；And/or
There are two the air inlets for intersecting gas supply mechanism, and two air inlets are oppositely arranged.
8. powder body material preparation facilities as described in claim 1, which is characterized in that the intersection gas outlet is close to the intersection
One end of gas supply mechanism is set, and the other end for intersecting gas supply mechanism is fixed with one end of the entrance of the reative cell to be docked.
9. such as powder body material preparation facilities according to any one of claims 1 to 5, which is characterized in that the vaporizer includes
Feeding mechanism, heating arrangements, heat exchange mechanisms, discharging mechanism and control mechanism, the heat exchange mechanisms have vaporization chamber and heating chamber,
The vaporization chamber is equipped with pressure detecting element, and the feeding mechanism and the discharging mechanism connect respectively with the vaporization chamber, institute
It states heating arrangements to connect with the heating chamber, the feeding mechanism, the discharging mechanism and heating arrangements are equipped with temperature detection member
Part, the control mechanism are used to control the feeding mechanism, the discharging mechanism and the heating arrangements.
10. powder body material preparation facilities as claimed in claim 9, which is characterized in that the feeding mechanism include feed pipe and
The feed flow meter and inlet control valve being located on the feed pipe, the feed pipe are equipped with the detector unit, institute
Heating arrangements are stated to be connected with the heating chamber including circulation pipe and the temperature control valve being located on the circulation pipe, the circulation pipe
One end be equipped with the detector unit, the heat exchange mechanisms coat the heat exchange kettle of the vaporization chamber, institute for the heating chamber
Stating discharging mechanism includes discharge nozzle and the reactor effluent stream gauge being located on the discharge nozzle, and the discharge nozzle is examined equipped with the temperature
Survey element, the control mechanism and the feed flow meter, the inlet control valve, the temperature control valve and the reactor effluent stream
Gauge connects.
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| CN201810098097.2A CN108101001B (en) | 2018-01-31 | 2018-01-31 | Powder material preparation device |
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| CN201810098097.2A CN108101001B (en) | 2018-01-31 | 2018-01-31 | Powder material preparation device |
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Cited By (1)
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| EP3900822A4 (en) * | 2019-05-31 | 2022-03-02 | Guangzhou Huifu Research Institute Co., Ltd. | Gas nozzle, gas reaction device and gas hydrolysis reaction method |
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