CN110359064B - Preparation method of lanthanum-yttrium alloy - Google Patents
Preparation method of lanthanum-yttrium alloy Download PDFInfo
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Abstract
The invention discloses a preparation method of lanthanum yttrium alloy, which comprises the steps of electrolyzing an electrolysis raw material in a molten electrolyte; wherein, the electrolytic raw materials are lanthanum oxide and yttrium oxide; the electrolyte is a mixture containing alkali metal fluoride and rare earth fluoride and not containing magnesium fluoride. The lanthanum-yttrium alloy prepared by the method has high purity, low impurity content and low yttrium element extraction cost.
Description
Technical Field
The invention relates to a preparation method of a rare earth intermetallic alloy, in particular to a preparation method of a lanthanum-yttrium alloy.
Background
The yttrium element is a rare earth hydrogen storage material, can effectively prolong the cycle life of the rare earth hydrogen storage battery, reduce the weight of the battery and improve the unit weight energy storage. Because the melting point of the metal yttrium is high (1522 ℃), the metal yttrium is mostly prepared by a vacuum calcium thermal reduction method at present, the metal yttrium prepared by the method has high content of impurities such as calcium and the like, the metal yttrium has low purity and high production cost, and the application universality is seriously influenced. Lanthanum is the element with the highest hydrogen storage capacity in rare earth metals, has a lower melting point and a higher density, and is beneficial to low-temperature extraction and deposition separation by electrolysis. The lanthanum-yttrium alloy combines the characteristics of metal lanthanum and metal yttrium, is an excellent rare earth hydrogen storage material, can be prepared by adopting an electrolytic method, and has simple extraction process and low cost.
CN103849900A discloses a preparation method of rare earth alloy, which comprises the following steps: uniformly mixing a rare earth compound and metal powder in a molar ratio of 1: 2-6, pressing a test piece, compounding the test piece and a metal current collector to be used as a cathode, using graphite as an anode, and electrolyzing for 5-10 hours in a molten electrolyte containing chlorides or fluorides of alkali metals or alkaline earth metals at an electrolysis temperature of 500-900 ℃ and an electrolysis voltage of 1.8-3.2V in an inert atmosphere or an air atmosphere; and cooling the cathode product to normal temperature in an inert atmosphere, taking out, washing with water or an organic reagent, and drying in vacuum to obtain the rare earth alloy. The method only discloses a preparation method of rare earth elements and non-rare earth elements, and does not relate to a preparation method of lanthanum-yttrium alloy.
CN105624737A discloses a preparation method of rare earth yttrium neodymium magnesium alloy, which comprises the following steps: a graphite block is used as an anode, a molybdenum rod is used as an inert cathode, a molybdenum crucible tongs is used as an alloy collector, and a mixture of yttrium oxide, neodymium oxide and magnesium oxide is added into a fluoride molten salt electrolyte system consisting of yttrium fluoride, neodymium fluoride and lithium fluoride. The method does not relate to a preparation method of lanthanum yttrium alloy.
CN1147568A discloses a method for preparing mixed rare earth metal: performing oxide electrolysis on rare earth oxide in a fluoride system; the fluoride system comprises 10-30 wt% of lithium fluoride and 70-90 wt% of rare earth fluoride; the rare earth oxide comprises 50-70 wt% of lanthanum oxide, 1-3 wt% of cerium oxide, 3-6 wt% of praseodymium oxide and 22-37 wt% of neodymium oxide. The alloy of lanthanum, cerium, praseodymium and neodymium metal elements is prepared by the method, and the preparation of the lanthanum-yttrium alloy is not involved.
CN101240394A discloses a preparation process of a light rare earth-based heavy rare earth alloy, which comprises the following steps: the electrolyte consists of a matrix light rare earth metal fluoride, a matrix heavy rare earth metal fluoride, lithium fluoride and magnesium fluoride, and the oxide consists of a matrix light rare earth metal oxide and a matrix heavy rare earth metal oxide; the electrolysis temperature of the molten salt is between 1000 and 1200 ℃; the current density of the anode is 0.5-1.2A/cm2The cathode current density is 10-17A/cm2. The method only relates to the alloy consisting of lanthanum and bait elements, and does not relate to the preparation method of the lanthanum-yttrium alloy.
It can be seen that there is little description of the prior art disclosed to date on the preparation of lanthanum yttrium alloys.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing a lanthanum-yttrium alloy, wherein the lanthanum-yttrium alloy prepared by the method has high purity, low impurity content and low yttrium extraction cost. The invention adopts the following technical scheme to achieve the purpose.
A lanthanum yttrium alloy preparation method comprises the steps of electrolyzing an electrolysis raw material in a molten electrolyte;
wherein, the electrolytic raw materials are lanthanum oxide and yttrium oxide; the electrolyte is a mixture containing alkali metal fluoride and rare earth fluoride and not containing magnesium fluoride.
According to the preparation method of the invention, the electrolytic raw material preferably contains 85-96.5 wt% of lanthanum oxide and 3.5-15 wt% of yttrium oxide.
According to the preparation method of the invention, preferably, the electrolyte contains 75-95 wt% of rare earth fluoride and 5-15 wt% of alkali metal rare earth fluoride.
According to the production method of the present invention, preferably, the rare earth fluoride is a composition of lanthanum fluoride and yttrium fluoride.
According to the preparation method, the mass ratio of the lanthanum fluoride to the yttrium fluoride is preferably 1: 0.5-2.5.
According to the preparation method of the present invention, preferably, the alkali metal fluoride is selected from one or more of lithium fluoride, sodium fluoride or potassium fluoride.
According to the preparation method of the present invention, preferably, the electrolyte is a mixture of lithium fluoride, lanthanum fluoride and yttrium fluoride.
According to the preparation method of the invention, the electrolyte is preferably 25-60 wt% of lanthanum fluoride, 35-60 wt% of yttrium fluoride and 5-15 wt% of lithium fluoride.
According to the preparation method, preferably, the electrolysis current is 4500-8000A, the electrolysis voltage is 5-20V, the electrolysis temperature is 1000-1400 ℃, and the electrolysis time is 0.5-2 h.
According to the preparation method of the invention, the impurity content in the prepared lanthanum yttrium alloy is preferably less than 0.8 wt%.
The lanthanum-yttrium alloy obtained by electrolysis has high purity and less impurity content by taking lanthanum oxide and yttrium oxide as electrolysis raw materials, taking a mixture containing alkali metal fluoride and rare earth fluoride and not containing magnesium fluoride as an electrolyte. In the preferred technical scheme of the invention, the lanthanum-yttrium alloy prepared by taking the mixture of lithium fluoride, lanthanum fluoride and yttrium fluoride as the electrolyte has higher purity.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.
The preparation method of the lanthanum-yttrium alloy comprises the steps of electrolyzing an electrolysis raw material in an electrolyte; the electrolyte is a mixture containing alkali metal fluoride and rare earth fluoride and not containing magnesium fluoride. The specific steps can be that the electrolyte is uniformly mixed and added into an electrolytic cell, then the electrolyte is heated to a molten state, a cathode is inserted, then the power is switched on, and the uniformly mixed electrolytic raw material is added at a certain speed after the power is switched on, so that the lanthanum-yttrium alloy is obtained through electrolysis.
In the present invention, the electrolytic raw material may be 85 to 96.5 wt% of lanthanum oxide and 3.5 to 15wt% of yttrium oxide. Preferably, the electrolytic raw material contains 88-95 wt% of lanthanum oxide and 5-12 wt% of yttrium oxide. More preferably, the electrolytic raw material is 89-93 wt% of lanthanum oxide and 7-11 wt% of yttrium oxide. According to a specific embodiment of the present invention, the electrolytic raw material was 94.5 wt% of lanthanum oxide and 5.5 wt% of yttrium oxide. According to another specific embodiment of the present invention, the electrolytic raw material was 93wt% of lanthanum oxide and 7 wt% of yttrium oxide. According to still another embodiment of the present invention, the electrolytic raw material was 89.4 wt% of lanthanum oxide and 10.6 wt% of yttrium oxide. Thus, the purity of the lanthanum-yttrium alloy can be improved, and the impurity content can be reduced.
In the invention, the content of the rare earth fluoride in the electrolyte can be 75-95 wt%. Preferably, the content of the rare earth fluoride in the electrolyte is 80-95 wt%. More preferably, the content of the rare earth fluoride in the electrolyte is 85-95 wt%. The content of the alkali metal rare earth fluoride in the electrolyte is 3-15 wt%. Preferably, the content of the alkali metal rare earth fluoride in the electrolyte is 4-15 wt%. More preferably, the content of the alkali metal rare earth fluoride in the electrolyte is 5-15 wt%.
According to a specific embodiment of the present invention, the electrolyte may include 75 to 95 wt% of rare earth fluoride and 3 to 15wt% of alkali metal rare earth fluoride. According to another specific embodiment of the present invention, the electrolyte comprises 80 to 95 wt% of rare earth fluoride and 4 to 15wt% of alkali metal rare earth fluoride. According to still another embodiment of the present invention, the electrolyte comprises 85 to 95 wt% of rare earth fluoride and 5 to 15wt% of alkali metal rare earth fluoride. Thus, the purity of the lanthanum-yttrium alloy can be improved, and the impurity content can be reduced.
In the present invention, the rare earth fluoride is a combination of lanthanum fluoride and yttrium fluoride. The mass ratio of the lanthanum fluoride to the yttrium fluoride is 1: 0.5-2.5. Preferably, the mass ratio of the lanthanum fluoride to the yttrium fluoride is 1: 1.2-2.5. More preferably, the mass ratio of the lanthanum fluoride to the yttrium fluoride is 1: 2.1-2.5. Thus, the purity of the lanthanum-yttrium alloy can be improved, and the impurity content can be reduced.
In the present invention, the alkali metal fluoride is selected from one or more of lithium fluoride, sodium fluoride or potassium fluoride. Preferably, the alkali metal fluoride is selected from one or more of lithium fluoride or sodium fluoride. More preferably, the alkali metal fluoride is lithium fluoride. Thus, the purity of the lanthanum-yttrium alloy can be improved, and the impurity content can be reduced.
In the present invention, the electrolyte may be a mixture of lanthanum fluoride, yttrium fluoride and lithium fluoride. The lanthanum fluoride content in the electrolyte can be 25-60 wt%. Preferably, the content of lanthanum fluoride in the electrolyte is 25-40 wt%. More preferably, the content of lanthanum fluoride in the electrolyte is 25-30 wt%. The content of yttrium fluoride in the electrolyte can be 35-60 wt%. Preferably, the content of yttrium fluoride in the electrolyte is 45-60 wt%. More preferably, the content of yttrium oxide in the electrolyte is 50-60 wt%. The content of lithium fluoride in the electrolyte may be 5 to 15 wt%. Preferably, the content of the lithium fluoride in the electrolyte is 7-15 wt%. More preferably, the content of the lithium fluoride in the electrolyte is 12-15 wt%.
According to a specific embodiment of the present invention, the electrolyte comprises 25 to 60wt% of lanthanum fluoride, 35 to 60wt% of yttrium fluoride and 5 to 15wt% of lithium fluoride. According to another specific embodiment of the present invention, the electrolyte comprises 25 to 40 wt% of lanthanum fluoride, 45 to 60wt% of yttrium fluoride and 7 to 15wt% of lithium fluoride. According to still another embodiment of the present invention, the electrolyte is 25 to 30 wt% of lanthanum fluoride, 50 to 60wt% of yttrium fluoride and 12 to 15wt% of lithium fluoride.
According to a preferred embodiment of the invention, the electrolyte is 60wt% lanthanum fluoride, 35 wt% yttrium fluoride and 5wt% lithium fluoride. According to another preferred embodiment of the invention the electrolyte is 25 wt% lanthanum fluoride, 60wt% yttrium fluoride and 15wt% lithium fluoride. According to yet another embodiment of the invention, the electrolyte is 42 wt% lanthanum fluoride, 48 wt% yttrium fluoride and 10 wt% lithium fluoride. Thus, the purity of the lanthanum-yttrium alloy can be improved, and the impurity content can be reduced.
In the present invention, an alternating current arc machine may be used to heat the electrolyte to a molten state. The anode material for electrolysis of the invention can be graphite, and the cathode material can be tungsten or molybdenum. Preferably, the anode material of the present invention is graphite and the cathode material is tungsten.
In the present invention, the electrolysis time means a time from the completion of the electrolysis after the addition of all the electrolytic raw materials. The electrolysis current is 4500-8000A, the electrolysis voltage is 5-20V, the electrolysis temperature is 1000-1400 ℃, and the electrolysis time is 0.5-2 h. Preferably, the electrolytic current is 5000-7500A. More preferably, the electrolytic current is 5500 to 6500A. Preferably, the electrolytic voltage is 5-15V. More preferably, the electrolytic voltage is 8-12V. Preferably, the electrolysis temperature is 1000-1300 ℃. More preferably, the electrolysis temperature is 1000 to 1200 ℃. Preferably, the electrolysis time is 0.5-1.5 h. More preferably, the electrolysis time is 0.75-1 h. Therefore, the purity of the lanthanum-yttrium alloy can be improved, the impurity content can be reduced, and the distribution fluctuation of the lanthanum-yttrium element can be reduced.
In the invention, the speed of adding the electrolysis raw materials into the electrolytic bath can be 3-15 kg/h. Preferably, the feeding speed of the electrolytic raw materials into the electrolytic cell is 5-13 kg/h. More preferably, the feeding speed of the electrolysis raw materials into the electrolytic bath is 8-12 kg/h.
The content of impurities in the lanthanum-yttrium alloy prepared by the invention is less than 0.8 wt%. Preferably, the content of impurities in the lanthanum yttrium alloy is less than 0.5 wt%. More preferably, the content of impurities in the lanthanum yttrium alloy is less than 0.4 wt%.
In the following examples, the content of carbon was measured by a carbon sulfur analyzer, the content of iron was measured by an atomic absorption spectrophotometer, and the content of lanthanum and yttrium was measured by an inductively coupled plasma emission spectrometer (ICP).
Example 1
Uniformly mixing an electrolyte (lanthanum fluoride: yttrium fluoride: lithium fluoride in mass ratio: 54:36:10) and adding the electrolyte into an electrolytic cell (the anode is a graphite sheet and the cathode is a tungsten rod), heating the electrolyte to a molten state by using an alternating current arc striking machine, inserting the electrolyte into the cathode, electrifying, adding uniformly mixed electrolytic raw materials (6.615 kg of lanthanum oxide and 0.385kg of yttrium oxide) into the electrolytic cell at a speed of 10kg/h after electrifying, wherein the electrolytic current is 5800A, the electrolytic voltage is 10.3V, the electrolytic temperature is 1120 ℃, and the electrolytic time is 0.75 hour; and collecting the metal precipitated by the cathode to obtain the lanthanum-yttrium alloy. The obtained lanthanum-yttrium alloy was weighed and the contents of carbon, iron, lanthanum and yttrium contained in the lanthanum-yttrium alloy were measured, and the results are shown in table 1.
Example 2
Uniformly mixing an electrolyte (mass ratio of lanthanum fluoride to yttrium fluoride: lithium fluoride is 49:41:10) and adding the electrolyte into an electrolytic cell (an anode is a graphite sheet and a cathode is a tungsten rod), heating the electrolyte to a molten state by using an alternating current arc striking machine, inserting the electrolyte into the cathode, electrifying, adding uniformly mixed electrolytic raw materials (6.51 kg of lanthanum oxide and 0.49kg of yttrium oxide) into the electrolytic cell at a speed of 10kg/h after electrifying, wherein the electrolytic current is 5800A, the electrolytic voltage is 10.3V, the electrolytic temperature is 1120 ℃, and the electrolytic time is 0.75 hour; and collecting the metal precipitated by the cathode to obtain the lanthanum-yttrium alloy. The obtained lanthanum-yttrium alloy was weighed and the contents of carbon, iron, lanthanum and yttrium contained in the lanthanum-yttrium alloy were measured, and the results are shown in table 1.
Example 3
Uniformly mixing an electrolyte (lanthanum fluoride: yttrium fluoride: lithium fluoride in mass ratio: 42:48:10) and adding the electrolyte into an electrolytic cell (the anode is a graphite sheet and the cathode is a tungsten rod), heating the electrolyte to a molten state by using an alternating current arc striking machine, inserting the electrolyte into the cathode, electrifying, adding uniformly mixed electrolytic raw materials (6.258 kg of lanthanum oxide and 0.742kg of yttrium oxide) into the electrolytic cell at a speed of 10kg/h after electrifying, wherein the electrolytic current is 6200A, the electrolytic voltage is 10.3V, the electrolytic temperature is 1140 ℃, and the electrolytic time is 0.75 hour; and collecting the metal precipitated by the cathode to obtain the lanthanum-yttrium alloy. The obtained lanthanum-yttrium alloy was weighed and the contents of carbon, iron, lanthanum and yttrium contained in the lanthanum-yttrium alloy were measured, and the results are shown in table 1.
Example 4
Uniformly mixing an electrolyte (lanthanum fluoride: yttrium fluoride: lithium fluoride in mass ratio: 60:35:5) and adding the electrolyte into an electrolytic cell (the anode is a graphite sheet and the cathode is a tungsten rod), heating the electrolyte to a molten state by using an alternating current arc striking machine, inserting the electrolyte into the cathode, electrifying, adding uniformly mixed electrolytic raw materials (6.258 kg of lanthanum oxide and 0.742kg of yttrium oxide) into the electrolytic cell at a speed of 10kg/h after electrifying, wherein the electrolytic current is 6200A, the electrolytic voltage is 10.3V, the electrolytic temperature is 1140 ℃, and the electrolytic time is 0.75 hour; and collecting the metal precipitated by the cathode to obtain the lanthanum-yttrium alloy. The obtained lanthanum-yttrium alloy was weighed and the contents of carbon, iron, lanthanum and yttrium contained in the lanthanum-yttrium alloy were measured, and the results are shown in table 1.
Example 5
Uniformly mixing an electrolyte (lanthanum fluoride: yttrium fluoride: lithium fluoride in mass ratio: 25:60:15) and adding the electrolyte into an electrolytic cell (the anode is a graphite sheet and the cathode is a tungsten rod), heating the electrolyte to a molten state by using an alternating current arc striking machine, inserting the electrolyte into the cathode, electrifying, adding uniformly mixed electrolytic raw materials (6.258 kg of lanthanum oxide and 0.742kg of yttrium oxide) into the electrolytic cell at a speed of 10kg/h after electrifying, wherein the electrolytic current is 6200A, the electrolytic voltage is 10.3V, the electrolytic temperature is 1140 ℃, and the electrolytic time is 0.75 hour; and collecting the metal precipitated by the cathode to obtain the lanthanum-yttrium alloy. The obtained lanthanum-yttrium alloy was weighed and the contents of carbon, iron, lanthanum and yttrium contained in the lanthanum-yttrium alloy were measured, and the results are shown in table 1.
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Raw materials for electrolysis (kg) | 7 | 7 | 7 | 7 | 7 |
| Alloy output (kg) | 6.1 | 5.9 | 5.8 | 6.0 | 6.2 |
| Carbon content (wt%) | 0.029 | 0.036 | 0.015 | 0.018 | 0.021 |
| Iron content (wt%) | 0.173 | 0.258 | 0.132 | 0.125 | 0.173 |
| Lanthanum element content (wt%) | 94.15 | 92.8 | 89.5 | 90 | 89.4 |
| Content of Yttrium element (wt%) | 5.1 | 6.8 | 10.2 | 9.7 | 10.4 |
| Total impurity content (wt%) | 0.75 | 0.4 | 0.3 | 0.3 | 0.2 |
Comparative example
Uniformly mixing electrolyte (lanthanum fluoride: yttrium fluoride: lithium fluoride: magnesium fluoride: 70:18:9:3 in mass ratio) and adding the mixture into an electrolytic cell (the anode is a graphite sheet and the cathode is a tungsten rod), heating the electrolyte to a molten state by using an alternating current arc striking machine, inserting the electrolyte into the cathode, electrifying, adding the uniformly mixed electrolytic raw materials (5.6 kg of lanthanum oxide and 1.4kg of yttrium oxide) into the electrolytic cell at the speed of 10kg/h after electrifying, wherein the electrolytic temperature is 1020-1050 ℃, the current intensity is 6200A, and the current density of the cathode is 17A/cm3The current density of the anode is 1.1A/cm3Electrolyzing for 1 hour; collecting the metal precipitated by the cathode to obtain lanthanum-yttrium alloy. The obtained lanthanum-yttrium alloy was weighed and the contents of carbon, iron, lanthanum and yttrium contained in the lanthanum-yttrium alloy were measured, and the results are shown in table 2.
TABLE 2
| Comparative example | |
| Raw materials for electrolysis (kg) | 7 |
| Alloy output (kg) | 5.7 |
| Carbon content (wt%) | 0.058 |
| Iron content (wt%) | 0.37 |
| Content of magnesium element (wt%) | 1.47 |
| Lanthanum element content (wt%) | 79 |
| Content of Yttrium element (wt%) | 19 |
| Total impurity content (wt%) | 2 |
The present invention is not limited to the above-described embodiments, and any variations, modifications, and substitutions which may occur to those skilled in the art may be made without departing from the spirit of the invention.
Claims (3)
1. A method for preparing a lanthanum yttrium alloy, comprising the steps of electrolyzing an electrolysis raw material in a molten electrolyte; the anode material used for electrolysis is graphite, and the cathode material used for electrolysis is tungsten; the speed of adding the electrolysis raw materials into the electrolytic cell is 8-12 kg/h, the electrolysis current is 5000-7500A, the electrolysis voltage is 5-20V, the electrolysis temperature is 1000-1200 ℃, and the electrolysis time is 0.5-2 h;
the electrolytic material comprises lanthanum oxide and yttrium oxide, wherein the lanthanum oxide accounts for 89-93 wt%, and the yttrium oxide accounts for 7-11 wt%; the electrolyte contains 25-60 wt% of lanthanum fluoride, 35-60 wt% of yttrium fluoride and 5-15 wt% of lithium fluoride, and does not contain magnesium fluoride;
wherein the content of impurities in the lanthanum-yttrium alloy is less than 0.4 wt%.
2. The method of claim 1, wherein the electrolyte comprises 25 to 60wt% of lanthanum fluoride, 35 to 60wt% of yttrium fluoride, and 5 to 15wt% of lithium fluoride.
3. The method according to claim 1, wherein the electrolysis voltage is 5 to 15V and the electrolysis time is 0.5 to 1.5 hours.
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| CN112159993B (en) * | 2020-09-24 | 2022-03-29 | 江西江钨浩运科技有限公司 | Yttrium-containing mixed rare earth metal, rare earth hydrogen storage alloy and preparation method thereof |
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