CN1648052A - Method for preparing rare-earth oxide - Google Patents
Method for preparing rare-earth oxide Download PDFInfo
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- CN1648052A CN1648052A CN 200410036484 CN200410036484A CN1648052A CN 1648052 A CN1648052 A CN 1648052A CN 200410036484 CN200410036484 CN 200410036484 CN 200410036484 A CN200410036484 A CN 200410036484A CN 1648052 A CN1648052 A CN 1648052A
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Abstract
The present invention relates to a method of preparing RE oxide. The apparatus for preparing RE oxide is rotary kiln for burning RE carbonate or oxalate to prepare RE oxide. The rotary kiln includes heating furnace and two horizontal rotating kiln bodies through the heating furnace, and each of the rotating kiln bodies has material inlet in the front end, material outlet in the back end, kiln rotating unit and support unit. The main technological conditions include burning decomposition temperature 750-900 deg.c, and burning decomposition time 30-60 min. The present invention has raised production efficiency, low cost and high product quality.
Description
Technical field:
The invention belongs to the rare earth element production method, relate in particular to equipment and preparation technology's method of preparation rare earth oxide.
Background technology:
Rare earth element is the special element of a class, because it has special atomic structure and performance, is widely used in multiple fields such as metallurgy, electronics, chemistry, nuclear power.The production method of rare earth element generally is that the natural rare earth associated minerals that will crush carry out floating and enriching and become concentrate, is convenient to the carbonate or the solid chloride that separate and transport through decomposing, being converted into after the removal of impurities again.Carbonate or solid chloride are dissolved as liquid chloride, carrying out extracting and separating with extraction agent again is single or partially mixed muriate, be carbonate or oxalate with bicarbonate of ammonia or oxalic acid with its precipitation separation then, be decomposed into rare earth oxide through high temperature sintering again.This oxide compound promptly can be used as commodity selling, also can further be processed as rare earth element or other rare-earth products.China scientific research department achievement aspect rare-earth extraction separating process is remarkable a few years ago, developed sophisticated, advanced separating technology, but, because total consumption of rare-earth products is very low after all, manufacturing enterprise's quantity is few, scale is also little, and except that separating technology, other operation is all used for reference the common method of traditional industries, produce basic for many years not improvement on the basis of the existing conditions no matter how simple and crude.The production method for preparing rare earth oxide by rare earth carbonate or oxalate calcination that adopts at present is generally two kinds, a kind of is principle, facility and the technology of using for reference traditional Wingdale lime calcining, rare earth carbonate or oxalate are put into ceramic alms bowl body, be emitted in the kiln body in similar limestone kiln, with coal naked light high temperature sintering, form rare earth oxide.This method belongs to batch production, and labour intensity is big, and equipment loss is big, and particularly traditional production method heavy contamination, decomposition reaction is unbalanced, consistence is poor, influences the quality of product.Another kind is flat rotary kiln, adopts electrically heated or the calcination of coal naked light.Though this method belongs to continuous production, with the former common ground be static calcination.Energy consumption height when adopting electrically heated, equipment loss is big, and homogeneity of product is poor, adopts coal to heat, and quality product is influenced, and consistence is poor.Because rare earth resources concentrates on China more than 80%, external generally is that the rare earth oxide of using China's outlet is reprocessed, relevant document is less, have not yet to see abroad about the rare earth carbonate calcination is decomposed into the rare earth oxide novel process, particularly about using the bibliographical information that rotary kiln carries out the calcination decomposition.
Summary of the invention:
In order to save energy consumption, reduce labor intensity, enhance productivity, improve the quality of products, the inventor provides a kind of and can implement calcination continuously and decompose the technical scheme that rare earth carbonate or oxalate prepare rare earth oxide.
Technical scheme under the present invention is a kind of preparation method of rare earth oxide, and this method comprises that employing can be implemented calcination decomposition rare earth carbonate continuously or oxalate prepares the equipment-rotary kiln of rare earth oxide and adopts this rotary kiln to prepare the processing condition and the working method of rare earth oxide.
The rotary kiln that adopts among the preparation method of rare earth oxide of the present invention is to aim at that calcination decomposes that rare earth carbonate or oxalate prepare rare earth oxide and the rotary kiln that designs, what it comprised process furnace and passed that the horizontal installation of two corresponding side walls of process furnace is provided with can be along the tubular kiln body of axis rotation, high back is low before the kiln body, the front end of kiln body is provided with opening for feed, the rear end is provided with discharge port, is positioned at the outer kiln body of body of heater and is provided with power set and the rolling support device that drives the rotation of kiln body.
Rotary kiln described in the preparation method of the present invention, the length-to-diameter ratio of its kiln body (ratio of the total length of kiln body and kiln body internal diameter) is (10～20): 1; Its axis is horizontal by the inclination angle of 5～15 degree.
Rotary kiln described in the preparation method of the present invention, its process furnace is provided with some fire doors, in stove near the position of kiln body, segmentation is provided with some points for measuring temperature, the discharge port of kiln body is provided with material collecting device, and opening for feed is provided with loading hopper, is provided with device for recovering powder above loading hopper.
Rotary kiln described in the preparation method of the present invention, the below of said loading hopper is equipped with vibrator, and this structure can make the unimpeded downslide of raw material, prevents that raw material from stopping up.
Rotary kiln described in the preparation method of the present invention, the inwall of said kiln body is provided with turn-down rig, and its effect is that upset is heated evenly it by the material of calcination when the kiln body rotates.This device can adopt the scraper plate that is fixed on the kiln body inwall, and scraper plate can be arranged in parallel with axis or oblique or eccentric pattern, and the easiest scraper plate is the reinforcing bar that is welded on the kiln body inwall.
Rotary kiln described in the preparation method of the present invention, said kiln body one end is installed rotational power plant, power set comprises the follower gear that is fixedly installed on the kiln body, and what be meshed with follower gear is fixed in driving toothed gear and corresponding speed-regulating actuator on the power output shaft; The other end corresponding with it is provided with rolling support device, and described bracing or strutting arrangement comprises the traffic cycle that is fixedly installed on the kiln body, mini-roundabout and the base for supporting on the rack shaft of being installed in that rolls and contact with the cylindrical of traffic cycle.This structure can make the kiln body be in equilibrium state preferably in rotation, prevents that the kiln body from rocking in rotation process and tilt.
The concrete structure of the rotary kiln described in the preparation method of the present invention comprises process furnace 7 and is arranged on fire door 4 on the process furnace 7, the kiln bodies 6 that low inclination angle, high back was 5～15 degree before two corresponding side walls of passing process furnace 7 were provided with; The front end of kiln body 6 is provided with opening for feed, opening for feed is provided with loading hopper 2, opening for feed can be installed vibrator 14 or adopt spiral charging or other known technologies, is provided with retrieving arrangement 1 above opening for feed, and retrieving arrangement 1 can adopt fiber bag precipitator or other known technology; Kiln body 6 rear ends are provided with discharge port, and discharge port is provided with material collecting device 9, can adopt funnel-form or other common structure; Front and back kiln body region outside being positioned at body of heater, be respectively arranged with and drive power set and the bracing or strutting arrangement that the kiln body rotates, the concrete structure of power set adopts the follower gear 3 that is fixedly installed on the kiln body 6, what be meshed with follower gear 3 is fixed in driving toothed gear 13 on the power output shaft 12, bracing or strutting arrangement specifically can adopt and be fixedly installed in traffic cycle 8 on the kiln body 6, the cylindrical of traffic cycle 8 contacts with the cylindrical of mini-roundabout 10 on being installed in support 11 rotating shafts, and mini-roundabout is generally two; The inwall of kiln body 6 is provided with turn-down rig, specifically can adopt the scraper plate 5 that is fixed on the kiln body inwall, also can adopt projection of being positioned at the column on the kiln body inwall etc. similarly can reach other known structures of stirring effect; Be close to kiln outer wall position point for measuring temperature 15 is set respectively at process furnace 7 inner kiln tube outer wall leading portions, stage casing, back segment, be used to be connected and installed occasionally other temperature measuring equipment of thermoelectricity, detect each section of control kiln body temperature, its testing method and mounting means can adopt known technology.
The material of making the kiln body can adopt the common metal material, and is ideal with stainless material.
The type of heating of process furnace can adopt the heating of directly burning of coal or other fuel, also can adopt electrically heated, and the heating operation that directly burns is convenient, but temperature control has fluctuation among a small circle, and the electrically heated temperature control is accurate, but it is higher to consume energy.
It is as follows to adopt the rotary kiln described in the preparation method of the present invention to prepare the technical process of rare earth oxide:
Open the rotational power plant power supply, start speed-regulating actuator, driven rotary kiln kiln body rotates; At kiln body leading portion, stage casing, back segment difference heat temperature raising, make it reach preset temperature; Raw material rare earth carbonate or oxalate are added from opening for feed, because the kiln body has certain obliquity, raw material is stirred down and kiln wall uniform contact at drive and scraper plate that the kiln body rotates, and move slowly, at kiln body leading portion drying and dehydrating, after being subjected to high temperature sintering, kiln body stage casing is decomposed into rare earth oxide, after the cooling of kiln body back segment, from discharge hole for discharge, cooling, packing.Carbonic acid gas that generates in the production process and water vapour discharge after the retrieving arrangement of opening for feed top reclaims dust.
It is as follows to adopt the rotary kiln described in the preparation method of the present invention to prepare the processing condition of rare earth oxide:
The main technique controlling index that adopts the rotary kiln described in the preparation method of the present invention to prepare rare earth oxide is two, and one is the calcination decomposition temperature, and one is the calcination resolving time.
In the production process, generally the kiln body is divided into leading portion, stage casing, three zones of back segment and carries out temperature control, kiln body stage casing is the calcination decomposition region, kiln body leading portion is dry, dehydration zone, back segment is cooling and follow-up decomposition region, its length is respectively 3～6 times of kiln body internal diameter, kiln body stage casing is the principal reaction zone, the calcination decomposition course is mainly finished in the stage casing, said herein calcination decomposition temperature promptly is meant the shown temperature of thermocouple temperature measurement device of installing at the point for measuring temperature in kiln body stage casing, and the said calcination resolving time promptly is meant the time of material through kiln body stage casing.
The inventor tests definite after deliberation, and in rare earth oxide preparation method of the present invention, calcination decomposition temperature scope is 750～900 ℃; Calcination resolving time scope is: 30～60min.Temperature cross low or too short decomposition of time incomplete, the too high or overlong time of temperature easily causes local sintering.
Through comprehensive screening and assessment, the inventor confirms that preferred calcination decomposition temperature scope is 800～850 ℃, and calcination resolving time scope is 40～45min, and prepared with this understanding rare-earth oxidation amount is very good.
Among the rare earth oxide preparation method of the present invention, other processing condition comprise:
450～650 ℃ of kiln body leading portion and back segment temperature controlling range;
Kiln body rotating speed 5～10 commentaries on classics/min;
Material accounts for 1/8～1/10 of kiln body capacity in the kiln.
The quality index of raw material rare earth carbonate or oxalate is among the rare earth oxide preparation method of the present invention: carbonate: TREO 〉=38% Fe
2O
3≤ 0.01% CaO≤0.05% SO
2≤ 0.05%
Oxalate: TREO 〉=30% Fe
2O
3≤ 0.01% CaO≤0.02% SO
2≤ 0.01%
The quality index of the prepared product rare earth oxide of rare earth oxide preparation method of the present invention is:
REO (burning till) TREO 〉=99%Fe by carbonate
2O
3≤ 0.01%CaO≤0.05%SO
2≤ 0.05%
REO (burning till) TREO 〉=99%Fe by oxalate
2O
3≤ 0.01%CaO≤0.02%SO
2≤ 0.01%
TREO represents the total rare earth (TRE) oxide compound in the These parameters, and REO represents rare earth oxide, is the versatility code in the industry standard.
Because the preparation method of rare earth oxide of the present invention has used the rotary kiln that can be continuously produced, the flow operations and the preferred processing condition of continous-stable, thereby, at aspects such as enhancing productivity, reduce cost, improve the quality of products, all obtained significant benefit.Its superiority mainly show following some:
1. compared with prior art, the preparation method of rare earth oxide of the present invention can raise labour productivity 60～100%.
2. compared with prior art, preparation method's ton product cost of rare earth oxide of the present invention can reduce by 800～1200 yuan.
3. compared with prior art, rare earth oxide preparation method's of the present invention product percent of pass can improve 5%.
4. compared with prior art, quality of the present invention significantly improves.Good product consistency, sampling analysis TREO differs and is no more than 0.2% every half an hour; Epigranular, large granular impurity reduces to 0.5% by 10%; The impurity content of sulfur dioxide reduces to 0.05% by 0.3%.
Description of drawings:
Fig. 1 is rotary kiln concrete structure figure of the present invention;
Wherein, 1. retrieving arrangement, 2. loading hopper, 3. follower gear, 4. fire door, 5. scraper plate, 6. kiln body, 7. process furnace, 8. traffic cycle, 9. material collecting device, 10. mini-roundabout, 11. supports, 12. power output shaft, 13. driving toothed gears, 14. vibrators, 15. points for measuring temperature.
Embodiment:
Now illustrate the specific embodiment of the present invention
The long 8m of kiln body, diameter 55cm, the kiln body stage casing long 3m in calcination decomposition region,
The kiln body axis is horizontal by 8 degree inclination angles, and kiln body rotating speed is 8 commentaries on classics/min,
820 ℃-850 ℃ of calcination decomposition temperatures, 550 ℃～600 ℃ of kiln body front and rear sections temperature,
Calcination resolving time 40min,
Hourly output 75Kg.
Making the cerium oxide yield is 〉=98.5%, and purity is 〉=99.9%,
Foreign matter content≤0.1%, sulphur content≤0.01%,
| ????TREO | ????CeO 2/REO | ????Fe 2O 3 | ????CaO | ????SO 2 | |
| Customer requirement: | ????≥99％ | ????≥99.9％ | ??≤0.01％ | ??≤0.02％ | ??≤0.02％ |
| Raw material is formed: | ????40.28％ | ????≥99.9％ | ??≤0.01％ | ??0.012％ | ??≤0.01％ |
| Product analysis: | ????99.62％ | ????≥99.9％ | ??≤0.01％ | ??0.013％ | ??≤0.01％ |
The long 13m of kiln body, diameter 65cm, the kiln body stage casing long 4m in calcination decomposition region,
The kiln body axis is horizontal by 15 degree inclination angles, and kiln body rotating speed is 5 commentaries on classics/min,
770 ℃-800 ℃ of calcination decomposition temperatures, 450 ℃～500 ℃ of kiln body front and rear sections temperature,
Calcination resolving time 45min,
Hourly output 125Kg.
Making the oxide compound yield is 〉=98.7%, and purity is 〉=99%,
Foreign matter content≤1%, sulphur content≤0.10%,
| ????TREO | ????CeO 2/REO | ????Fe 2O 3 | ????CaO | ????SO 2 | |
| Customer requirement: | ????≥95％ | ????≥58％ | ???≤0.05％ | ??≤0.20％ | ??≤0.20％ |
| Raw material is formed: | ????43.65％ | ????59.22％ | ???0.03％ | ??0.16％ | ??0.05％ |
| Product analysis: | ????95.52％ | ????59.23％ | ???0.04％ | ??0.15％ | ??0.10％ |
The long 4.2m of kiln body, diameter 40cm, the kiln body stage casing long 2m in calcination decomposition region,
The kiln body axis is horizontal by 15 degree inclination angles, and kiln body rotating speed is the 7 commentaries on classics/people,
850 ℃-870 ℃ of calcination decomposition temperatures, 600 ℃～650 ℃ of kiln body front and rear sections temperature,
Calcination resolving time 35min,
Hourly output 30Kg,
Making the Neodymium trioxide yield is 〉=99.5%, and purity is 〉=99.5%,
Foreign matter content≤0.3%, sulphur content≤0.01%.
| ????TREO | ??Nd 2O 3/REO | ??Fe 2O 3 | ??CaO | ??SO 2 | |
| Customer requirement: | ????≥99％ | ????≥99.5％ | ??≤0.01％ | ??≤0.02％ | ??≤0.02％ |
| Raw material is formed: | ????42.12％ | ????99.7％ | ??≤0.01％ | ??0.012％ | ??≤0.01％ |
| Product analysis: | ????99.62％ | ????99.6％ | ??≤0.01％ | ??0.013％ | ??≤0.01％ |
The long 4.8m of kiln body, diameter 45cm, the kiln body stage casing long 2m in calcination decomposition region,
The kiln body axis is horizontal by 10 degree inclination angles, and kiln body rotating speed is 5 commentaries on classics/min,
870 ℃-900 ℃ of calcination decomposition temperatures, 600 ℃～650 ℃ of kiln body front and rear sections temperature
Calcination resolving time 60min,
Hourly output 20Kg,
Making the yttrium oxide yield is 〉=99.5%, and purity is 〉=99.9%,
Foreign matter content≤0.1%, sulphur content≤0.05%.
| ????TREO | ????Y 2O 3/REO | ????Fe 2O 3 | ????CaO | ???SO 2 | |
| Customer requirement: | ????≥99％ | ????≥99.9％ | ??≤0.01％ | ??≤0.03％ | ??≤0.05％ |
| Raw material is formed: | ????32.10％ | ????99.93％ | ??0.01％ | ??0.018％ | ??0.02％ |
| Product analysis: | ????99.62％ | ????≥99.9％ | ??≤0.01％ | ??0.02％ | ??0.03％ |
The long 12m of kiln body, diameter 60cm, the kiln body stage casing long 4m in calcination decomposition region,
The kiln body axis is horizontal by 5 degree inclination angles, and kiln body rotating speed is 10 commentaries on classics/min,
800 ℃-830 ℃ of calcination decomposition temperatures, 550 ℃～600 ℃ of kiln body front and rear sections temperature,
Calcination resolving time 30min,
Kiln body rotating speed is 8 rev/mins, hourly output 100Kg,
Making Praseodymium trioxide neodymium yield is 〉=98.5%, and purity is 〉=99%,
Matter content≤0.5%, sulphur content≤0.01%.
| ????TREO | ??Nd 2O 3/REO | ??Fe 2O 3 | ??CaO | ??SO 2 | |
| Customer requirement: | ????≥99％ | ????75％ | ??≤0.01％ | ??≤0.05％ | ??≤0.02％ |
| Raw material is formed: | ????42.05％ | ????75.3％ | ??≤0.01％ | ??0.03％ | ??≤0.01％ |
| Product analysis: | ????99.62％ | ????75.5％ | ??≤0.01％ | ??0.04％ | ??≤0.01％ |
Claims (7)
1. the preparation method of a rare earth oxide, it comprises that rare earth carbonate is decomposed in the enforcement calcination or oxalate prepares the equipment of rare earth oxide and the processing condition that this equipment of employing prepares rare earth oxide, it is characterized in that the equipment that is adopted is to aim at that calcination decomposes that rare earth carbonate or oxalate prepare rare earth oxide and the rotary kiln that designs, what it comprised process furnace and passed that the horizontal installation of two corresponding side walls of process furnace is provided with can be along the tubular kiln body of axis rotation, high back is low before the kiln body, the front end of kiln body is provided with opening for feed, the rear end is provided with discharge port, and the kiln body two ends outside being positioned at body of heater are respectively arranged with and drive power set and the rolling support device that the kiln body rotates; The main technique condition that adopts described rotary kiln to prepare rare earth oxide is: calcination decomposition temperature scope is 750～900 ℃, and calcination resolving time scope is: 30～60min.
2. the preparation method of rare earth oxide as claimed in claim 1 is characterized in that the length-to-diameter ratio of said rotary kiln kiln body is (10～20): 1; Its axis is horizontal by the inclination angle of 5～15 degree.
3. the preparation method of rare earth oxide as claimed in claim 1, the structure that it is characterized in that said rotary kiln comprise process furnace (7) and be arranged on fire door (4) on the process furnace (7), passes the kiln body (6) that two corresponding side walls of process furnace (7) are provided with; The front end of kiln body (6) is provided with opening for feed, and opening for feed is provided with loading hopper (2), and opening for feed is installed vibrator 14 or adopted spiral charging, is provided with retrieving arrangement (1) above opening for feed; Kiln body (6) rear end is provided with discharge port, and discharge port is provided with material collecting device 9; Front and back kiln body region outside being positioned at body of heater, be respectively arranged with and drive power set and the bracing or strutting arrangement that the kiln body rotates, power set adopts the follower gear 3 that is fixedly installed on the kiln body 6, what be meshed with follower gear 3 is fixed in driving toothed gear 13 on the power output shaft 12, bracing or strutting arrangement adopts and to be fixedly installed in traffic cycle 8 on the kiln body 6, and the cylindrical of traffic cycle 8 contacts with the cylindrical of mini-roundabout 10 on being installed in support 11 rotating shafts; The inwall of kiln body 6 is provided with turn-down rig, and turn-down rig adopts the scraper plate 5 that is fixed on the kiln body inwall; Be close to kiln outer wall position at leading portion, stage casing, the back segment of process furnace 7 inner kiln tubes 6 point for measuring temperature 15 is set respectively.
4. the preparation method of rare earth oxide as claimed in claim 1, it is characterized in that the processing condition that the described rotary kiln of said employing prepares rare earth oxide are: calcination decomposition temperature span of control is 800～850 ℃; The calcination resolving time is 40～45min.
5. the preparation method of rare earth oxide as claimed in claim 1, it is characterized in that the processing condition that the described rotary kiln of said employing prepares rare earth oxide are: kiln body leading portion and back segment temperature controlling range are 450～650 ℃.
6. the preparation method of rare earth oxide as claimed in claim 1 is characterized in that the processing condition that the described rotary kiln of said employing prepares rare earth oxide are: kiln body rotating speed 5～10 commentaries on classics/min.
7. the preparation method of rare earth oxide as claimed in claim 1, it is characterized in that the processing condition that the described rotary kiln of said employing prepares rare earth oxide are: material accounts for 1/8～1/10 of kiln body capacity in the kiln.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410036484 CN1648052A (en) | 2004-12-13 | 2004-12-13 | Method for preparing rare-earth oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410036484 CN1648052A (en) | 2004-12-13 | 2004-12-13 | Method for preparing rare-earth oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1648052A true CN1648052A (en) | 2005-08-03 |
Family
ID=34868526
Family Applications (1)
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|---|---|---|---|
| CN 200410036484 Pending CN1648052A (en) | 2004-12-13 | 2004-12-13 | Method for preparing rare-earth oxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113860348A (en) * | 2021-09-17 | 2021-12-31 | 聂磊 | Rare earth oxidation roasting furnace capable of reducing air pollution |
| CN115010163A (en) * | 2022-05-20 | 2022-09-06 | 全南县新资源稀土有限责任公司 | Rare earth oxide with low apparent density and preparation method thereof |
-
2004
- 2004-12-13 CN CN 200410036484 patent/CN1648052A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113860348A (en) * | 2021-09-17 | 2021-12-31 | 聂磊 | Rare earth oxidation roasting furnace capable of reducing air pollution |
| CN113860348B (en) * | 2021-09-17 | 2024-01-05 | 聂磊 | Rare earth oxidizing roasting furnace capable of reducing air pollution |
| CN115010163A (en) * | 2022-05-20 | 2022-09-06 | 全南县新资源稀土有限责任公司 | Rare earth oxide with low apparent density and preparation method thereof |
| CN115010163B (en) * | 2022-05-20 | 2024-04-09 | 全南县新资源稀土有限责任公司 | Rare earth oxide with low apparent density and preparation method thereof |
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