CN113908955A - Treatment method of rare earth material for optical glass - Google Patents
Treatment method of rare earth material for optical glass Download PDFInfo
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- CN113908955A CN113908955A CN202111027838.6A CN202111027838A CN113908955A CN 113908955 A CN113908955 A CN 113908955A CN 202111027838 A CN202111027838 A CN 202111027838A CN 113908955 A CN113908955 A CN 113908955A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C19/00—Other disintegrating devices or methods
- B02C19/18—Use of auxiliary physical effects, e.g. ultrasonics, irradiation, for disintegrating
- B02C19/186—Use of cold or heat for disintegrating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D47/00—Separating dispersed particles from gases, air or vapours by liquid as separating agent
- B01D47/06—Spray cleaning
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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Abstract
The invention relates to the treatment of rare earth materials, in particular to a treatment method of rare earth materials for optical glass, which comprises the steps of crushing rare earth metal ores to ensure that the external surface temperature of the rare earth metal ores reaches 70-100 ℃, immediately spraying liquid nitrogen on the surfaces of rare earth metal ore particles, and standing for 3-5 min; and repeating the steps of crushing, heating, spraying liquid nitrogen and standing until 95-98 wt.% of the rare earth metal ore particles have a particle size of less than 45 microns; the invention realizes the high-efficiency dry crushing of the rare earth metal ore with lower cost and realizes the reduction of energy consumption; the increase of the amount of the rare earth metal ore caused by the crushing of the water mill is avoided, and the subsequent treatment requirement of high concentration by more alkali sources is avoided; the liquid nitrogen only reduces the temperature of rare earth metal ore particles without introducing new impurities and does not affect the quality of subsequent rare earth metal products.
Description
Technical Field
The invention relates to treatment of rare earth materials, in particular to a treatment method of a rare earth material for optical glass.
Background
At present, lanthanide optical glass is widely applied to cameras, and the components of the lanthanide optical glass contain more rare earth lanthanum oxide (La)2O3) The new material is a high-quality optical glass material necessary for manufacturing photoelectric products such as read-write lenses and imaging lenses, and can effectively enlarge the field of view of the lenses, improve the imaging quality of instruments, and miniaturize and lighten the lenses. Lanthanum added in the camera glass is a rare earth metal element, namely a rare earth element, and the occurrence state of the lanthanum in the earth crust is mainly three: (1) the rare earth elements participate in crystal lattices of minerals and form essential components of the minerals, and the minerals are generally called as rare earth minerals; monazite (REPO)4) Bastnaesite ([ La, Ce)]FCO3) All fall within this category. (2) The rare earth elements are dispersed in the mineral in the form of isomorphism replacing Ca, Sr, Ba, Mn, Zr and other elements in the mineral. The minerals are more in nature, but most of the minerals have lower rare earth content, and fluorite and apatite containing rare earth belong to the minerals. (3) The rare earth elements are in an ion adsorption state and are present on the surfaces or among particles of certain minerals, the minerals belong to weathering crust leaching type minerals, and the rare earth ions are adsorbed on the minerals related to the ore parent rock contained in the minerals before weathering.
Lanthanum, a rare earth element, is widely present in monazite and bastnaesite, and is conventionally treated mainly by crushing it by dry or water milling, followed by treatment of the crushed ore with concentrated aqueous sodium hydroxide at elevated temperature, such as described in US2811411A, where monazite sand is crushed to 100% pass through a sieve with a mesh size of 74 microns and 95 to 98% pass through a sieve with a mesh size of 44 microns, and it is also stated that if the monazite sand is crushed finer, the decomposition with sodium hydroxide is more satisfactory and the reaction time is shorter. The crushed monazite sand is treated with 30 to 70 wt% sodium hydroxide solution at 135 to 220 deg.c for 1 to 3 hr. The weight ratio of the sodium hydroxide to the monazite sand is between 2 and 3. However, the method has the direct defects that the monazite sand needs to be finely crushed, and a large amount of energy is consumed; in addition, in the case of dry crushing, fine dust is easily generated by fine crushing, causing environmental pollution, or requiring investment in dust treatment equipment resulting in excessively high treatment cost; in the case of water mill comminution, the ore slurry is diluted at the crusher outlet, so that the subsequent decomposition with sodium hydroxide is carried out in a concentrated medium. Therefore, it is necessary to let the ore slurry settle in order to extract as much water as possible after crushing. Therefore, a settling tank or a filter (higher investment) is necessary. The settled ore slurry often contains 25 to 40% water, which requires the use of large amounts of expensive flake caustic at a later stage to achieve the desired caustic concentration.
For another example, chinese patent publication No. CN1009115 discloses a method for treating rare earth metal ores, which comprises a first stage of crushing the ore and a second stage of decomposing the crushed ore at an elevated temperature with a concentrated aqueous alkali hydroxide solution, characterized in that the crushing is carried out in the presence of a concentrated aqueous alkali hydroxide solution at a temperature of less than or equal to 100 ℃. The method can avoid deep crushing of ore and realize pre-decomposition of ore in the crushing process. However, the above method still requires crushing treatment of ore from large to small particle sizes, and still consumes much energy.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for treating a rare earth material for optical glass, which realizes high-efficiency crushing of the rare earth material and realizes the aim of saving energy consumption.
In order to achieve the purpose, the invention adopts the following technical scheme:
a processing method of rare earth material for optical glass comprises crushing rare earth metal ore to make its external surface temperature reach 70-100 deg.C, immediately spraying liquid nitrogen onto the surface of rare earth metal ore particles, and standing for 3-5 min;
and repeating the steps of crushing, heating, spraying liquid nitrogen and standing until 95-98 wt.% of the rare earth metal ore particles have a particle size of less than 45 microns.
In a further technical scheme, the rare earth metal ore is subjected to rough crushing treatment in advance.
In a further technical scheme, the particle size of the rare earth metal ore is 10-30 meshes.
In a further technical scheme, the spraying amount of the liquid nitrogen is 100-600 mL/s.
In a further technical scheme, the method further comprises the steps of adding a strong alkaline solution into the crushed rare earth metal ore particles, uniformly stirring and mixing, heating to 120-150 ℃, and carrying out heat preservation treatment for at least 3 hours.
In a further technical scheme, the concentration of the strong alkaline solution is 30-65% by weight concentration.
In a further technical scheme, the strong alkaline solution is industrial sodium lye with the weight concentration of 48-58%.
Compared with the prior art, the invention has the following technical effects:
according to the processing method of the rare earth material for the optical glass, provided by the invention, the rare earth metal ore is crushed according to a traditional method, in the crushing process, the temperature of the rare earth metal ore is raised due to friction, more dust is generated, the surface temperature of the rare earth metal ore is suddenly reduced by spraying liquid nitrogen with extremely low temperature on the surface of the rare earth metal ore particles, and then the rare earth metal ore is cracked due to the internal and external temperature difference of the rare earth metal ore, so that the crushing efficiency of the rare earth metal ore is improved; in addition, the aim of dust fall is achieved by spraying liquid nitrogen, and environmental pollution generated in the crushing treatment process is avoided; and the crushing equipment is integrally cooled by spraying liquid nitrogen, so that the influence of long-term high-temperature work on the running stability and the service life of the crushing equipment is avoided.
By the treatment method provided by the invention, the high-efficiency dry crushing of the rare earth metal ore is realized at lower cost, and the reduction of energy consumption is directly realized; the increase of the amount of the rare earth metal ore caused by the crushing of the water mill is directly avoided, and the subsequent treatment requirement of high concentration by more alkali sources is avoided; and the invention avoids dust pollution produced in the process of crushing rare earth metal ore through the spraying treatment of liquid nitrogen, and the liquid nitrogen only can reduce the temperature of rare earth metal ore particles without introducing new impurities and can not affect the quality of subsequent rare earth metal products. Namely, the processing method provided by the invention has a better application prospect.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the invention is further clarified with the specific embodiments.
In the invention, the rare earth material for the optical glass specifically refers to lanthanide optical glass applied to a camera, and specifically refers to rare earth metal lanthanum (La-La) existing in monazite (REPO)4) And bastnaesite ([ La, Ce ]]FCO3) Among such rare earth minerals. The traditional method for realizing the enrichment and utilization of the rare earth elements has a plurality of disadvantages. The invention provides a method for processing rare earth materials for optical glass, which comprises the steps of crushing rare earth metal ores to enable the external surface temperature of the rare earth metal ores to reach 70-100 ℃, immediately spraying liquid nitrogen on the surfaces of rare earth metal ore particles, and standing for 3-5 min; and repeating the steps of crushing, heating, spraying liquid nitrogen and standing until 95-98 wt.% of the rare earth metal ore particles have a particle size of less than 45 microns.
The method comprises the following steps that liquid nitrogen is sprayed immediately after the temperature of the rare earth metal ore rises, the surface temperature of the rare earth metal ore is reduced through the liquid nitrogen with extremely low temperature, so that the difference between the internal temperature and the external temperature is large, further bursting occurs, the rare earth metal ore is promoted to reach the required granularity more efficiently, and the energy consumption for crushing is directly reduced; in addition, due to the spraying of the liquid nitrogen, the generation of dust is directly inhibited, and the pollution to the environment is avoided; furthermore, the use of the liquid nitrogen does not introduce new impurities into the rare earth metal ore, and does not influence the quality of subsequent rare earth metal products.
According to the method provided by the invention, in order to obtain better crushing effect, the rare earth metal ore is subjected to rough crushing treatment in advance. Further preferably, the rare earth metal ore has a particle size of 10 to 30 mesh.
According to the method provided by the invention, the spraying amount of the liquid nitrogen can directly influence the cracking effect of the rare earth metal ore, if the spraying amount is too small, a good cooling effect cannot be achieved, and if the spraying amount is too large, the cost is increased, and preferably, in the invention, the spraying amount of the liquid nitrogen is 100-600 mL/s.
According to the method provided by the invention, the method also comprises the steps of adding a strong alkaline solution into the crushed rare earth metal ore particles, uniformly stirring and mixing, heating to 120-150 ℃, and carrying out heat preservation treatment for at least 3 hours. According to the invention, the rare earth metal is enriched and utilized in the form of hydroxide by adding the concentrated alkaline solution into the rare earth metal ore particles with the granularity meeting the requirement.
Further, in the present invention, the alkaline solution may be selected from sodium hydroxide, potassium hydroxide or a mixture thereof commonly known to those skilled in the art.
According to the method provided by the invention, the concentration of the strong alkaline solution is 30-65% by weight. Further preferably, the strong alkaline solution is industrial sodium lye with the weight concentration of 48-58%.
The treatment method provided by the present invention is further described below by specific examples.
Example 1
Mixing monazite (REO: 54.23%, ThO)2：4.15％，CaO：1.98％，TiO2：1.68％，ZrO2：2.59％，SiO2：3.12％，Fe2O3：2.82％，U3O8: 1.12%) to 20 mesh;
further crushing the monazite to enable the surface temperature of the monazite to reach 80 ℃, spraying liquid nitrogen with the spraying amount of 500mL/s, and standing for 5 min;
then continuing to start the crushing, enabling the temperature to reach 70 ℃, continuing to spray liquid nitrogen, enabling the spraying amount of the liquid nitrogen to be 500mL/s, and standing for 5 min;
repeating the above operation 2 more times, it was found that 97.6 wt.% of the rare earth metal ore particles had a particle size below 45 microns;
adding sodium hydroxide solution (industrial sodium alkali solution with the concentration of 52 weight percent) into the rare earth metal ore particles, stirring and mixing uniformly, heating to 140 ℃, and carrying out heat preservation treatment for 3.5 hours to obtain the decomposition yield (the conversion rate of converting the phosphate of the rare earth metal and thorium into corresponding hydroxide) of 98.3 percent.
Through calculation, the weight ratio of the sodium hydroxide to the rare earth metal ore is 0.83 in terms of the total amount of the sodium hydroxide, which greatly reduces the usage amount of the sodium hydroxide compared with the traditional treatment method.
The foregoing shows and describes the general principles, essential features, and inventive features of this invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A processing method of rare earth material for optical glass is characterized in that the method comprises the steps of crushing rare earth metal ore to enable the external surface temperature of the rare earth metal ore to reach 70-100 ℃, immediately spraying liquid nitrogen on the surfaces of rare earth metal ore particles, and standing for 3-5 min;
and repeating the steps of crushing, heating, spraying liquid nitrogen and standing until 95-98 wt.% of the rare earth metal ore particles have a particle size of less than 45 microns.
2. The method according to claim 1, characterized in that said rare earth metal ore has been previously subjected to a rough crushing treatment.
3. The method of claim 2, wherein the rare earth metal ore has a particle size of 10-30 mesh.
4. The method as claimed in claim 1, wherein the spraying amount of the liquid nitrogen is 100-600 mL/s.
5. The method as claimed in claim 1, further comprising adding a strong alkaline solution to the crushed rare earth metal ore particles, stirring and mixing uniformly, raising the temperature to 120-150 ℃, and performing heat preservation treatment for at least 3 hours.
6. The method according to claim 5, wherein the strongly alkaline solution has a concentration of 30-65% by weight.
7. The method as claimed in claim 5, wherein the strongly alkaline solution is 48-58 wt% sodium industrial lye.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111027838.6A CN113908955B (en) | 2021-09-02 | 2021-09-02 | Treatment method of rare earth material for optical glass |
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| CN202111027838.6A CN113908955B (en) | 2021-09-02 | 2021-09-02 | Treatment method of rare earth material for optical glass |
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| CN113908955A true CN113908955A (en) | 2022-01-11 |
| CN113908955B CN113908955B (en) | 2023-09-08 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102004047977A1 (en) * | 2003-10-01 | 2005-04-21 | Iis Materials Corp Ltd | Process for crushing silicon blocks for recycling waste semiconductor silicon comprises heating a silicon block to be crushed, forcibly cooling the block, and using a force to crush the block |
| CN102343300A (en) * | 2011-08-17 | 2012-02-08 | 昆明理工大学 | Pretreatment method of magnetite |
| CN205518141U (en) * | 2016-01-11 | 2016-08-31 | 天津飞通机械制造有限公司 | Cooling breaker |
| CN107335518A (en) * | 2017-07-04 | 2017-11-10 | 青岛科锐思新材料科技有限公司 | A kind of microwave ore treatment method and device |
| CN112456839A (en) * | 2019-09-09 | 2021-03-09 | 罗定市宏泰建材有限公司 | Industrial waste residue crushing method |
| CN214021294U (en) * | 2020-09-25 | 2021-08-24 | 烟台瑞克工程机械有限公司 | Ore crushing device is used in mine |
-
2021
- 2021-09-02 CN CN202111027838.6A patent/CN113908955B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102004047977A1 (en) * | 2003-10-01 | 2005-04-21 | Iis Materials Corp Ltd | Process for crushing silicon blocks for recycling waste semiconductor silicon comprises heating a silicon block to be crushed, forcibly cooling the block, and using a force to crush the block |
| CN102343300A (en) * | 2011-08-17 | 2012-02-08 | 昆明理工大学 | Pretreatment method of magnetite |
| CN205518141U (en) * | 2016-01-11 | 2016-08-31 | 天津飞通机械制造有限公司 | Cooling breaker |
| CN107335518A (en) * | 2017-07-04 | 2017-11-10 | 青岛科锐思新材料科技有限公司 | A kind of microwave ore treatment method and device |
| CN112456839A (en) * | 2019-09-09 | 2021-03-09 | 罗定市宏泰建材有限公司 | Industrial waste residue crushing method |
| CN214021294U (en) * | 2020-09-25 | 2021-08-24 | 烟台瑞克工程机械有限公司 | Ore crushing device is used in mine |
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