CN108423702A - The production equipment and preparation method of rare earth oxide - Google Patents
The production equipment and preparation method of rare earth oxide Download PDFInfo
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- CN108423702A CN108423702A CN201810634893.3A CN201810634893A CN108423702A CN 108423702 A CN108423702 A CN 108423702A CN 201810634893 A CN201810634893 A CN 201810634893A CN 108423702 A CN108423702 A CN 108423702A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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Abstract
The present invention relates to the technical fields of material, and more particularly, to the production equipment and preparation method of a kind of rare earth oxide, the production equipment of the rare earth oxide includes：Reactor, microwave heating equipment, carrier gas tank and fluid reservoir；Microwave heating equipment is sleeved on the outside of reactor；Reactor includes the air inlet section being sequentially connected, contraction section, trunnion section and air outlet section；The gas of carrier gas tank includes oxygen, and carrier gas tank is connected to air inlet section, so that gas can enter reactor, and is flowed along the length direction of reactor；Fluid reservoir is connected to trunnion section, so that re chloride enters in reactor, is flowed to air outlet section, and reacted with oxygen and generate rare earth oxide and hydrogen chloride.It is even that the production equipment solves existing Preparation equipment uneven heating, easily occurs that local temperature is excessively high, and outer layer heat affected zone molecular motion is active, easily forms the aggregation of product ecto-entad；So that agglomeration easily occurs for product, the technical problem that grain size is uneven, pattern is different is caused.
Description
Technical field
The present invention relates to the technical field of material, the production equipment more particularly, to a kind of rare earth oxide and preparation side
Method.
Background technology
Rare earth oxide has very extensive purposes, for example, lanthana is widely used in manufacture special alloy precision optics glass
Glass, high refractive optics fiberboard are suitble to do video camera, camera, micro- lens head and high optics instrument prism, ceramic condenser
Device and catalysts etc..Cerium oxide is widely used in oxidant, the catalyst of organic reaction, photo chromic glass and enamel glass
Deng.Praseodymium oxide is used in architectural pottery and domestic ceramics, is mixed and made into color glaze with ceramic glaze, also can individually be made under-glaze pigment,
Manufactured pigment is pure color, simple and elegant in faint yellow.Neodymia is mainly used as the colorant of glass, ceramics, manufactures neodymium metal
1.5%-2.5% Nanometer-sized Neodymium Oxides are added in the raw material of raw material and ferromagnetism neodymium iron boron, magnesium alloy or aluminium alloy, and alloy can be improved
High-temperature behavior, air-tightness and corrosion resistance, be widely used as aerospace material.Samarium oxide can be made to absorb the luminous glass of infrared ray
Glass additive, the coating in photosensitive material, and samarium processed bore permanent-magnet material and production samarium metal etc..
CN103833064A discloses a kind of method that the pyrolysis of rare-earth chloride solution jet stream prepares rare earth oxide, skill
Art route is pumped directly into jet reactor as shown in Figure 1, by combustion gas or kerosene and oxygen combustion formation high temperature mixed tail gas
In, heat source and working fluid as pyrolytic reaction；Rare-earth chloride solution is by jet reactor by conveying liquid inlet
Into ejector；And heating and gasifying in the case of a high temperature, the micro-bubble of Dispersed precipitate is formed, concurrent heat solution is obtained by the reaction dilute
Native oxide powder and high temperature pyrolysis tail gas containing hydrogen chloride gas.But such preparation method, the heat transfer type of generation
For by outer and interior, it is excessively high easily to there is local temperature；Outer layer heat affected zone molecular motion is active, and it is poly- easily to form product ecto-entad
Collection；So that agglomeration easily occurs for product, cause grain size unevenness, pattern different.
Invention content
The purpose of the present invention is to provide the production equipments of rare earth oxide, to alleviate existing Preparation equipment uneven heating
Even, it is excessively high local temperature easily occur, and outer layer heat affected zone molecular motion is active, easily forms the aggregation of product ecto-entad；So that production
Agglomeration easily occurs for object, causes grain size unevenness, the different technical problem of pattern.
The production equipment of rare earth oxide provided by the invention, including：Reactor, microwave heating equipment, for accommodating gas
The carrier gas tank of body and the fluid reservoir for holding re chloride；
The microwave heating equipment is sleeved on the outside of the reactor, for adding to the reaction of the rare earth chloride, water and oxygen
Heat；
The reactor includes the air inlet section being sequentially connected, contraction section, trunnion section and air outlet section；
The gas of the carrier gas tank includes oxygen, and the carrier gas tank is connected to the air inlet section, so that the gas can
It is flowed into the reactor, and along the length direction of the reactor；
The fluid reservoir is connected to the trunnion section, so that the re chloride enters in the reactor, to institute
Air outlet section flowing is stated, and is reacted with the oxygen and generates rare earth oxide and hydrogen chloride.
Further, the reactor is venturi jet reactor；
The venturi jet reactor further includes diffuser, diffuser setting the trunnion section and air outlet section it
Between.
Further, the microwave heating equipment is set in the trunnion section to the air outlet section.
Further, the fluid reservoir is connected to by connecting tube with the trunnion section.
Further, the reactor is tilted or is vertically arranged, and the air inlet section is higher than the air outlet section.
Further, the production equipment of the rare earth oxide further includes cyclone separator, the cyclone separator with
The outlet of the air outlet section, so that the rare earth oxide and hydrogen chloride realize gas solid separation.
Further, the solution of the fluid reservoir further includes dispersant.
Further, a concentration of 50-300g/L of the re chloride, the re chloride enter the larynx
The flow of pipeline section is 100-10000L/h；
The gas flow is 5-3000Nm3/h, and is provided between the carrier gas tank and the approach section for controlling
The flowmeter of gas flow processed.
The preparation method of rare earth oxide provided by the invention, step include：
Oxygen is injected from the air inlet section of reactor, and flows to air outlet section；
Microwave heating equipment is opened, is heated；
When microwave heating equipment is heated to assigned temperature, re chloride enters from the trunnion section of the reactor, penetrates
The oxygen entered collides with re chloride, and re chloride is made to be atomized, and makes re chloride with oxygen in height
It reacts under tender feeling condition, generates rare earth oxide and tail gas HCl；
Separating treatment is carried out to rare earth oxide and tail gas HCl.
Further, the rare earth chloride includes LaCl3、CeCl3、PrCl3、NdCl3、SmCl3、EuCl3、GdCl3、
DyCl3、HoCl3、ErCl3、TmCl3、YbCl3、LuCl3、ScCl3And YCl3；
The rare earth chloride corresponds to the rare earth oxide generated：La2O3、CeO2、Pr2O3、Nd2O3、Sm2O3、
Eu2O3、Gd2O3、Dy2O3、Ho2O3、Er2O3、Tm2O3、Yb2O3、Lu2O3、Sc2O3And Y2O3。
Compared with prior art, the device have the advantages that：
The production equipment of rare earth oxide provided by the invention, by by the gas input reactor in carrier gas tank,
In, gas includes oxygen, and reactor includes the air inlet section being sequentially connected, contraction section, trunnion section and air outlet section, and gas is from air inlet
Section enters, and by contraction section, the cross-sectional area of flowing is gradually reduced, and accelerates the flow velocity of gas；Re chloride is from fluid reservoir
Into the trunnion section of reactor, collide with the swiftly flowing gas of entrance, meanwhile, microwave heating equipment adds reactor
Heat makes to be in hot environment in reactor, to make re chloride generate atomizing effect, can preferably in gas
Oxygen is reversed to answer, and generates rare earth oxide and tail gas hydrogen chloride.
In addition, in the present invention, being heated to reactor by microwave heating equipment, the rare earth chloride in reactor can be made
Solution and oxygen are by uniform heat, and heating speed is very fast, so as to reduce the case where product grain reunion is lumpd, carry
High granulation uniformity, enables grain size to reach micro/nano level, is more in line with industrial requirements.
Wherein, the method for preparing rare earth oxide is：First, gas is injected from the air inlet section of reactor, and flows to outlet
Section；Next, opening microwave heating equipment, heated, gas is made to carry out preheating and subsequent heating；When microwave heating fills
Set and be heated to assigned temperature, make re chloride from the trunnion section of the reactor enter, by with high temperature and flow at high speed
The collision that occurs of gas, so that re chloride is atomized, meanwhile, it is anti-that chemistry occurs for oxygen in rare earth chloride, water and gas
It answers, generates rare earth oxide and tail gas HCl；Solid and gas separation finally is carried out to the rare earth oxide of generation and tail gas HCl, is obtained dilute
Native oxide.
Description of the drawings
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, in being described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, other drawings may also be obtained based on these drawings.
Fig. 1 is the flow chart of prior art preparation rare earth oxide；
Fig. 2 is the structural schematic diagram of the production equipment of rare earth oxide provided in an embodiment of the present invention；
Fig. 3 is the another form of schematic diagram of the production equipment of rare earth oxide provided in an embodiment of the present invention；
Fig. 4 is rare earth oxide preparation flow figure provided in an embodiment of the present invention.
Icon：10- venturi jet reactors；20- microwave heating equipments；30- carrier gas tanks；40- fluid reservoirs；11-
Air inlet section；12- contraction sections；13- trunnion sections；14- diffusers；15- air outlet sections；41- connecting tubes.
Specific implementation mode
Technical scheme of the present invention is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
The every other embodiment that personnel are obtained without making creative work, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that term "center", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" be based on the orientation or positional relationship shown in the drawings, merely to
Convenient for the description present invention and simplify description, do not indicate or imply the indicated device or element must have a particular orientation,
With specific azimuth configuration and operation, therefore it is not considered as limiting the invention.In addition, term " first ", " second ",
" third " is used for description purposes only, and is not understood to indicate or imply relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
Can also be electrical connection to be mechanical connection；It can be directly connected, can also indirectly connected through an intermediary, Ke Yishi
Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood at this with concrete condition
Concrete meaning in invention.
As shown in Figure 1, the production equipment of rare earth oxide provided in this embodiment, including：Reactor, microwave heating equipment
20, the carrier gas tank 30 for accommodating gas and the fluid reservoir 40 of re chloride is held；Microwave heating equipment 20 is sleeved on instead
It answers on the outside of device, is heated for reacting rare earth chloride, water and oxygen；Reactor includes the air inlet section 11 being sequentially connected, contraction section
12, trunnion section 13 and air outlet section 15；The gas of carrier gas tank 30 includes oxygen, and carrier gas tank 30 is connected to air inlet section 11, so that gas
Reactor can be entered, and flowed along the length direction of reactor；Fluid reservoir 40 is connected to trunnion section 13, so that rare earth chloride is molten
Liquid enters in reactor, is flowed to air outlet section 15, and is reacted with oxygen and generate rare earth oxide and hydrogen chloride.
The production equipment of rare earth oxide provided in this embodiment, by by the gas input reactor in carrier gas tank 30
It is interior, wherein gas includes oxygen, and reactor includes the air inlet section 11 being sequentially connected, contraction section 12, trunnion section 13 and air outlet section
15, gas enters from air inlet section 11, and by contraction section 12, the cross-sectional area of the flowing of gas is gradually reduced, and can accelerate gas
Flow velocity；Re chloride enters the trunnion section 13 of reactor from fluid reservoir 40, is sent out with the swiftly flowing gas of entrance
Raw collision, meanwhile, microwave heating equipment 20 heats reactor, makes to be in hot environment in reactor, to make rare earth chloride
Solution generates atomizing effect, can preferably with the oxygen in gas is reversed answers, generate rare earth oxide and tail gas hydrogen chloride.
In addition, in the present embodiment, being heated to reactor by microwave heating equipment 20, the chlorination in reactor can be made
Earth solution and oxygen are by uniform heat, and heating speed is very fast, so as to reduce the feelings of product grain reunion caking
Condition improves granulation uniformity, so that grain size is reached micro/nano level, be more in line with industrial requirements.
Wherein, it please continue to refer to Fig. 1, and combines shown in Fig. 4, the method for preparing rare earth oxide is：First, gas is from anti-
It answers the air inlet section 11 of device to inject, and flows to air outlet section 15；Next, open microwave heating equipment 20, heated, make gas into
Row preheating and subsequent heating；When microwave heating equipment 20 is heated to assigned temperature, make re chloride from reactor
Trunnion section 13 enters, and by the collision with high temperature and the generation of swiftly flowing gas, re chloride is made to be atomized, meanwhile, chlorine
The oxygen changed in rare earth, water and gas chemically reacts, and generates rare earth oxide and tail gas HCl；Finally to the rare earth of generation
Oxide and tail gas HCl carry out solid and gas separation, obtain rare earth oxide.
It should be noted that reactor is venturi jet reactor 10；Venturi jet reactor 10 further includes diffusion
Section 14, diffuser 14 are arranged between trunnion section 13 and air outlet section 15.
By the way that diffuser 14 is arranged between trunnion section 13 and air outlet section 15, the cross-sectional area of diffuser 14 gradually increases,
The re chloride of atomization and the flow velocity of gas can be slowed down, the expansion of venturi jet reactor 10 is rested on both to make
The time for dissipating section 14 and air outlet section 15 is longer, and then so that rare earth chloride, oxygen and water is reacted, and generates rare earth oxygen
Compound and tail gas HCl.
It should be noted that gas in carrier gas tank 30 can be a variety of, for example, can be air or purity oxygen, as long as
Include oxygen in gas, and other gases are difficult to react with other substances and nontoxic.
In addition, it is necessary to explanation, there are many types of rare earth chloride, for example, LaCl3、CeCl3、PrCl3、NdCl3、
SmCl3、EuCl3、GdCl3、DyCl3、HoCl3、ErCl3、TmCl3、YbCl3、LuCl3、ScCl3And YCl3。
Correspondingly, the rare earth oxide and hydrogen chloride that rare earth chloride, water and oxygen generate, wherein the rare earth of generation
Oxide can be La2O3、CeO2、Pr2O3、Nd2O3、Sm2O3、Eu2O3、Gd2O3、Dy2O3、Ho2O3、Er2O3、Tm2O3、Yb2O3、
Lu2O3、Sc2O3And Y2O3。
Wherein, by taking the chemical equation of Ce and Re as an example.
2CeCl3(s)+3H2O(g)+1/2O2(g)→2CeO2(s)+6HCl(g)；
2ReCl3(s)+3H2O(g)→2Re2O3(s)+6HCl(g)。
It should be noted that re chloride can spray into either to inject by connecting tube 41 by nozzle,
The present embodiment, fluid reservoir 40 are connected to trunnion section 13 by connecting tube 41, are connected to by connecting tube 41, and rare earth chloride can be increased
The flow of solution, and the case where while reducing using nozzle blocks, needs replacing nozzle, increase cost.
Please continue to refer to Fig. 1, in the present embodiment, microwave heating equipment 20 is set in trunnion section 13 to air outlet section 15.It is logical
It crosses and microwave heating equipment 20 is set in trunnion section 13 to air outlet section 15, the heating of re chloride and oxygen can be extended
Time is at hot environment, and then can fully be reacted to extend the reaction time.
It should be noted that the product generated includes rare earth oxide and tail gas hydrogen chloride, wherein rare earth oxide is solid
Body substance, hydrogen chloride are gaseous matter, prepare rare earth oxide and need to carry out gas solid separation.
Wherein, there are many modes for rare earth oxide and tail gas HCl separation, are specifically illustrated below.
For example, as shown in figure 3, reactor is tilted or is vertically arranged, and air inlet section 11 is higher than air outlet section 15.It is,
Since venturi jet reactor 10 tilts or is vertically arranged, under gravity, the tail gas hydrogen chloride quality of generation compared with
Gently, it can flow up, HCL can be made to be discharged from upper end, and the rare earth oxide generated can be discharged from lower end, and then realize
The gas solid separation for generating product, obtains rare earth oxide.
Alternatively, for example, the production equipment of rare earth oxide further includes cyclone separator, cyclone separator and air outlet section 15
Outlet, so that rare earth oxide and hydrogen chloride realize gas solid separation.It is, gas-solid point can be made by cyclone separator
From to realize the separation of rare earth oxide and hydrogen chloride, finally obtaining rare earth oxide.
In addition, in order to keep product rare earth oxide particles more uniform, the solution of fluid reservoir 40 further includes dispersant,
It includes re chloride and dispersant in fluid reservoir 40, dispersant can enter text simultaneously with re chloride to be exactly
In mound in jet reactor 10, the rare earth oxide particles of preparation can be made more uniform by dispersant.
It should be noted that there are many types of dispersant, for example, dispersant is ethylene glycol or citric acid.
It should be noted that oxygen and re chloride contact and reaction, need matched preferably concentration ratio, at this
In embodiment, a concentration of 50-300g/L of re chloride, the flow that re chloride enters trunnion section 13 is 100-
10000L/h；Gas flow is 5-3000Nm3/ h, and be provided between carrier gas tank 30 and approach section for controlling gas stream
The flowmeter of amount.The flow velocity that gas can be controlled by flowmeter enables oxygen and rare earth chloride to be easy fully collision and instead
It answers.
Furthermore, it is necessary to explanation, microwave heating equipment 20 work one section when after, make venturi jet reactor 10
After interior temperature reaches oxygen gas and water and the specific temperature of rare earth chloride reaction, re chloride is set to enter venturi jet stream anti-
It answers in device 10.Wherein, after 20 heating time of microwave heating equipment is 3-15s, re chloride is from venturi jet reactor
10 trunnion section 13 enters.
Wherein, 20 heating temperature of microwave heating equipment can reach 500-1600 DEG C, and the dilute reaction of different chlorinations needs
Heating temperature is different.Wherein, for cerium chloride, microwave heating temperature is preferably 1100K, microwave heating time 5s.For
Other rare earth oxide heating temperatures are preferably 1400K, heating time 5s.
Finally it should be noted that：The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, it will be understood by those of ordinary skill in the art that：Its according to
So can with technical scheme described in the above embodiments is modified, either to which part or all technical features into
Row equivalent replacement；And these modifications or replacements, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of production equipment of rare earth oxide, which is characterized in that including：Reactor, microwave heating equipment, for accommodating gas
The carrier gas tank of body and the fluid reservoir for holding re chloride；
The microwave heating equipment is sleeved on the outside of the reactor, is heated for reacting the rare earth chloride, water and oxygen；
The reactor includes the air inlet section being sequentially connected, contraction section, trunnion section and air outlet section；
The gas of the carrier gas tank includes oxygen, and the carrier gas tank is connected to the air inlet section, so that the gas can enter
The reactor, and flowed along the length direction of the reactor；
The fluid reservoir is connected to the trunnion section so that the re chloride enter the reactor in, to it is described go out
Gas section flows, and is reacted with the oxygen and generate rare earth oxide and hydrogen chloride.
2. the production equipment of rare earth oxide according to claim 1, which is characterized in that the reactor is penetrated for venturi
Flow reactor；
The venturi jet reactor further includes diffuser, and the diffuser is arranged between the trunnion section and air outlet section.
3. the production equipment of the rare earth oxide according to claim 2, which is characterized in that the microwave heating equipment is arranged
In the trunnion section to the air outlet section.
4. the production equipment of rare earth oxide according to claim 1, which is characterized in that the fluid reservoir passes through connecting tube
It is connected to the trunnion section.
5. the production equipment of rare earth oxide according to claim 1, which is characterized in that the reactor is tilted or erected
Straight setting, and the air inlet section is higher than the air outlet section.
6. according to the production equipment of claim 1-5 any one of them rare earth oxides, which is characterized in that further include whirlwind
Separator, the outlet of the cyclone separator and the air outlet section, so that the rare earth oxide and hydrogen chloride realize gas
Gu separation.
7. according to the production equipment of claim 1-5 any one of them rare earth oxides, which is characterized in that the fluid reservoir
Solution further include dispersant.
8. according to the production equipment of claim 1-5 any one of them rare earth oxides, which is characterized in that the chlorination is dilute
Native solution concentration is 50-300g/L, and the flow that the re chloride enters the trunnion section is 100-10000L/h；
The gas flow is 5-3000Nm3/h, and is provided between the carrier gas tank and the approach section for controlling gas
The flowmeter of body flow.
9. a kind of preparation method of rare earth oxide, which is characterized in that its step includes：
Oxygen is injected from the air inlet section of reactor, and flows to air outlet section；
Microwave heating equipment is opened, is heated；
When microwave heating equipment is heated to assigned temperature, re chloride enters from the trunnion section of the reactor, injection
Oxygen collides with re chloride, and re chloride is made to be atomized, and makes re chloride with oxygen in high tender feeling
It reacts under condition, generates rare earth oxide and tail gas HCl；
Separating treatment is carried out to rare earth oxide and tail gas HCl.
10. the preparation method of rare earth oxide according to claim 9, which is characterized in that the rare earth chloride includes
LaCl3、CeCl3、PrCl3、NdCl3、SmCl3、EuCl3、GdCl3、DyCl3、HoCl3、ErCl3、TmCl3、YbCl3、LuCl3、
ScCl3And YCl3；
The rare earth chloride corresponds to the rare earth oxide generated：La2O3、CeO2、Pr2O3、Nd2O3、Sm2O3、Eu2O3、
Gd2O3、Dy2O3、Ho2O3、Er2O3、Tm2O3、Yb2O3、Lu2O3、Sc2O3And Y2O3。
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| CN201810634893.3A CN108423702A (en) | 2018-06-22 | 2018-06-22 | The production equipment and preparation method of rare earth oxide |
Applications Claiming Priority (1)
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| CN201810634893.3A CN108423702A (en) | 2018-06-22 | 2018-06-22 | The production equipment and preparation method of rare earth oxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110498439A (en) * | 2019-09-27 | 2019-11-26 | 中国恩菲工程技术有限公司 | Prepare the method with the scandium oxide powder of porous structure |
| CN111826173A (en) * | 2019-10-24 | 2020-10-27 | 中国船舶重工集团公司第七一一研究所 | Reaction device, production system and production method for preparing low-carbon olefin |
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| CN103833064A (en) * | 2014-01-03 | 2014-06-04 | 东北大学 | Preparation method for rare earth oxide through jet pyrolysis of rare earth chloride solution |
| CN105271351A (en) * | 2015-10-27 | 2016-01-27 | 昆明理工大学 | Method for preparing cerium oxide with rare earth cerium chloride |
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| CN103833064A (en) * | 2014-01-03 | 2014-06-04 | 东北大学 | Preparation method for rare earth oxide through jet pyrolysis of rare earth chloride solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110498439A (en) * | 2019-09-27 | 2019-11-26 | 中国恩菲工程技术有限公司 | Prepare the method with the scandium oxide powder of porous structure |
| CN110498439B (en) * | 2019-09-27 | 2022-12-23 | 中国恩菲工程技术有限公司 | Method for preparing scandium oxide powder with porous structure |
| CN111826173A (en) * | 2019-10-24 | 2020-10-27 | 中国船舶重工集团公司第七一一研究所 | Reaction device, production system and production method for preparing low-carbon olefin |
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Application publication date: 20180821 |
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