CN117923435A - Tellurium purification method - Google Patents
Tellurium purification method Download PDFInfo
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- CN117923435A CN117923435A CN202410054658.4A CN202410054658A CN117923435A CN 117923435 A CN117923435 A CN 117923435A CN 202410054658 A CN202410054658 A CN 202410054658A CN 117923435 A CN117923435 A CN 117923435A
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- tellurium
- liquid
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- time
- purifying
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- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 96
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000000746 purification Methods 0.000 title abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 238000001816 cooling Methods 0.000 claims abstract description 16
- 239000002893 slag Substances 0.000 claims abstract description 16
- 239000000047 product Substances 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- 239000006227 byproduct Substances 0.000 claims abstract description 10
- 238000005266 casting Methods 0.000 claims abstract description 9
- 239000012263 liquid product Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000005868 electrolysis reaction Methods 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 239000000654 additive Substances 0.000 abstract description 5
- 230000000996 additive effect Effects 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 description 23
- 239000011734 sodium Substances 0.000 description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 description 3
- 239000008399 tap water Substances 0.000 description 3
- 235000020679 tap water Nutrition 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to the technical field of metal metallurgy, and discloses a tellurium purification method. The method comprises the following steps: (1) Completely melting tellurium slices at the temperature of 650-700 ℃, preserving heat for a period of time, then cooling to 440-460 ℃, and carrying out first slag removal to obtain molten tellurium liquid and byproducts; (2) Heating the molten tellurium liquid to 650-700 ℃ again, preserving heat for a period of time, then cooling to 440-460 ℃, and carrying out slag dragging for the second time to obtain molten tellurium liquid and byproducts; and (3) casting the molten tellurium liquid into ingots to obtain tellurium products. The method has simple process and convenient operation, and only controls the temperature of the melting furnace to melt tellurium simple substances, and utilizes the inconsistent melting points of the simple substances to carry out slag-fishing solid-liquid separation so as to achieve high-efficiency purification. The invention does not need to add any additive or dangerous chemical reaction, and has safe operation and high feasibility.
Description
Technical Field
The invention belongs to the technical field of metal metallurgy, and relates to a tellurium purification method.
Background
Tellurium is in VI A group in periodic table, and tellurium simple substance is a nonmetallic material with metallic luster, and is an important industrial raw material in the technical field of chemical environmental protection. The tellurium slices can be separated out from the cathode plate by an electrolysis method to extract simple substance tellurium, and the main components of the tellurium slices obtained by the electrolysis method are Te, na and S, and contain a small amount of Na and S impurities. This is because the separated tellurium simple substance is gradually electrodeposited in the sodium hydroxide solution environment, and other impurities such as Na salt are intercalated in the tellurium sheet.
At present, na and other impurities in the electrolytic tellurium flakes can be effectively separated through a casting process, and the tellurium flakes are purified. Such as: patent CN115465842 a discloses a 4N tellurium casting method, in which when tellurium is heated to 500-550 ℃, additive calcium chloride and sodium hydroxide in precipitated tellurium flakes react chemically to generate sodium chloride with high melting point, so that the sodium chloride is separated from high-temperature molten tellurium liquid, then the sodium chloride floats upwards through standing, floats on the surface of the molten tellurium liquid, and finally is fished out to realize sodium removal. However, the method needs to add additives to perform chemical reaction to separate out sodium chloride, and the separation is performed in a molten state, and the process involves chemical reaction, and has high requirements on reaction time and reaction environment.
Disclosure of Invention
In view of the foregoing problems in the prior art, an object of the present invention is to provide a method for purifying tellurium. The method is simple to operate, low in cost and capable of effectively separating Na and other impurities.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for purifying tellurium, comprising the steps of:
(1) Completely melting tellurium slices at the temperature of 650-700 ℃, preserving heat for a period of time, then cooling to 440-460 ℃, and carrying out first slag removal to obtain molten tellurium liquid and byproducts;
(2) Heating the molten tellurium liquid to 650-700 ℃ again, preserving heat for a period of time, then cooling to 440-460 ℃, and carrying out slag dragging for the second time to obtain molten tellurium liquid and byproducts;
(3) Casting the molten tellurium liquid into ingots to obtain tellurium products.
Further, the tellurium flakes are tellurium flakes obtained by electrolysis.
Further, before the tellurium sheet in the step (1) is melted, clean water is used for cleaning the tellurium sheet until the pH value of the cleaned water is 7-8.
Further preferably, the method further comprises drying the cleaned tellurium flakes.
Further preferably, the drying temperature is 150-200 ℃ and the drying time is 7-10 h.
Further, in the step (1), heat preservation is carried out for 2-3 hours.
Further, in the step (2), heat preservation is carried out for 2-3 hours.
Further, the step (3) specifically comprises: pouring the molten tellurium liquid obtained in the step (2) into a mould, and air-cooling and forming.
Further, the method also comprises the step of sampling and analyzing the tellurium product obtained in the step (3), for example, the Na content is more than 30ppm, and the steps (1) and (3) are repeated until the Na content is less than 30 ppm.
Compared with the prior art, the invention has the beneficial effects that:
The method has simple process and convenient operation, only dissolves tellurium simple substances by controlling the temperature of the melting furnace, and performs slag-fishing solid-liquid separation by utilizing inconsistent melting points of the simple substances, thereby achieving high-efficiency purification.
The invention does not need to add any additive or dangerous chemical reaction, and has safe operation and high feasibility.
The method has simple operation and low cost, and can effectively separate Na and other impurities.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
fig. 1 is a process flow diagram of the tellurium purification method of the present invention.
Detailed Description
The tellurium purification method provided by the embodiment comprises the following steps:
(1) Completely melting tellurium slices at the temperature of 650-700 ℃, preserving heat for a period of time, then cooling to 440-460 ℃, and carrying out first slag removal to obtain molten tellurium liquid and byproducts;
(2) Heating the molten tellurium liquid to 650-700 ℃ again, preserving heat for a period of time, then cooling to 440-460 ℃, and carrying out slag dragging for the second time to obtain molten tellurium liquid and byproducts;
(3) Casting the molten tellurium liquid into ingots to obtain tellurium products.
As one of the preferable schemes of the embodiment, the tellurium flakes are put into a graphite crucible furnace, preferably about 750kg of tellurium flakes are put into each furnace, the temperature of the furnace is raised at 650-700 ℃, the temperature is kept for a period of time after the tellurium flakes are completely dissolved in the furnace, most of impurities in the tellurium flakes float on the surface of the solution in a solid state, the temperature is reduced to 440-460 ℃, and then slag is fished for removing impurities and Na salt and other impurities are produced. And (3) when the impurities are not removed completely, opening the graphite crucible furnace to perform secondary heating to completely dissolve tellurium in the furnace, preserving heat for a period of time, performing secondary cooling to 440-460 ℃, performing secondary slag dragging and impurity removal on the furnace, and secondarily producing Na-containing salt and other impurities. Finally casting into ingot to obtain tellurium product.
As one preferable mode of the present embodiment, the tellurium pieces are those obtained by electrolysis.
As one of the preferable schemes of the embodiment, before the tellurium sheet in the step (1) is melted, clean water is used for cleaning the tellurium sheet until the pH value of the cleaned washing water is 7-8. The electrically resolved tellurium flakes are soaked in tap water, and are generally washed for 2-3 times for about 20min each time in order to control the pH value to 7-8. Preferably, the method further comprises the step of drying the cleaned tellurium slices. Further preferably, the drying temperature is 150-200 ℃ and the drying time is 7-10 h.
As one of the preferable schemes of the embodiment, in the step (1), the heat is preserved for 2-3 hours.
In the step (2), the heat is preserved for 2-3 hours as one of the preferable schemes of the embodiment.
As one of the preferable schemes of the present embodiment, the step (3) specifically includes: pouring the molten tellurium liquid obtained in the step (2) into a mould, and air-cooling and forming.
As one of the preferable schemes of the embodiment, the method further comprises sampling and analyzing the tellurium product obtained in the step (3), for example, na content is more than 30ppm, and repeating the steps (1) and (3) until Na content is less than 30 ppm.
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments are shown, for the purpose of illustrating the invention, but the scope of the invention is not limited to the specific embodiments shown.
Unless defined otherwise, all technical and scientific terms used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the scope of the present invention.
Example 1
And taking the tellurium slices which are subjected to electrolytic precipitation, wherein the output batch number of the tellurium slices is 001. Repeatedly soaking and cleaning for 3 times by using tap water until the pH value of the cleaned clean water is 8; then the mixture is put into an oven for baking for 6 hours at 200 ℃, and then the mixture is directly sampled and detected for each impurity content. As apparent from Table 1, the contents of Na and S impurities were high and were found to be 4800mg/kg or more.
Feeding materials at the temperature of 450 ℃ under the control of the furnace temperature, wherein the total feeding materials are 749.5kg; heating to 700 ℃ after the feeding is finished, preserving heat for 2 hours after tellurium flakes in the furnace are completely melted, then cooling to 450 ℃, and carrying out one-time slag dragging until tellurium liquid in the furnace has uniform color and no obvious suspended particles;
Controlling the furnace to raise the temperature to 700 ℃ for the second time, keeping the temperature for 2 hours after thoroughly melting, then carrying out the cooling to 450 ℃ for the second time, and carrying out the slag skimming and impurity removal for the second time;
and then casting to obtain the finished product.
And finally, sampling analysis is carried out, and the detected result accords with a 4N tellurium product. And the produced byproducts are uniformly stored, so that the recycling rate is increased.
Example 2
And taking the tellurium slices which are separated out through electrolysis, wherein the output batch number of the tellurium slices is 002 batches. Repeatedly soaking and cleaning for 3 times by using tap water until the pH value of the cleaned clean water is 8; and then baking for 6 hours at 200 ℃ in an oven, sampling and detecting the content of each impurity. As apparent from Table 1, the contents of Na, S, as and Al impurities were high.
Feeding materials at the temperature of 450 ℃ under the control of the furnace temperature, wherein the total feeding materials are 749.8kg; heating to 700 ℃ after the feeding is finished, preserving heat for 2 hours after tellurium flakes in the furnace are completely melted, then cooling to 450 ℃, and carrying out one-time slag dragging until tellurium liquid in the furnace has uniform color and no obvious suspended particles;
Controlling the furnace to raise the temperature to 700 ℃ for the second time, preserving heat for 2 hours after the furnace is thoroughly melted, then carrying out the second cooling to 450 ℃ for the second time, and carrying out slag skimming and impurity removal for the second time;
and then casting to obtain the finished product.
And finally, sampling analysis is carried out, and the detected result accords with a 4N tellurium product. And the produced byproducts are uniformly stored, so that the recycling rate is increased.
The tellurium chips and products of examples 1 and 2 were subjected to impurity detection, and the results are shown in Table 1 below:
TABLE 1
As can be seen from table 1: according to the invention, the temperature of the melting furnace can be controlled, the temperature is increased and decreased twice, slag is fished twice, impurities are removed, na salt and other impurities can be effectively removed, and the purity of the tellurium simple substance is purified to a great extent. Through the technical scheme, the tellurium simple substance can be purified without adding any additive and dangerous chemical reaction, and the method has obvious effect and high feasibility.
Meanwhile, the results of comparative examples 1 and 2 show that the impurities in different batches of raw materials have larger difference, but the impurities can be effectively removed after the two-time slag removal and impurity removal of the tellurium by the method, which proves that the tellurium purification method has strong applicability.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. A method for purifying tellurium, comprising the steps of:
(1) Completely melting tellurium slices at the temperature of 650-700 ℃, preserving heat for a period of time, then cooling to 440-460 ℃, and carrying out first slag removal to obtain molten tellurium liquid and byproducts;
(2) Heating the molten tellurium liquid to 650-700 ℃ again, preserving heat for a period of time, then cooling to 440-460 ℃, and carrying out slag dragging for the second time to obtain molten tellurium liquid and byproducts;
(3) Casting the molten tellurium liquid into ingots to obtain tellurium products.
2. The method for purifying tellurium according to claim 1, wherein the tellurium pieces are those obtained by electrolysis.
3. The method for purifying tellurium according to claim 1, wherein the tellurium sheet in step (1) is washed with clean water before melting until the pH of the washed water is 7 to 8.
4. A method for purifying tellurium as recited in claim 3, further comprising drying the cleaned tellurium sheet.
5. The method for purifying tellurium according to claim 4, wherein the drying temperature is 150 to 200℃and the drying time is 7 to 10 hours.
6. The method for purifying tellurium according to claim 1, wherein in the step (1), the temperature is kept for 2 to 3 hours.
7. The method for purifying tellurium according to claim 1, wherein in the step (2), the temperature is kept for 2 to 3 hours.
8. The method for purifying tellurium according to claim 1, wherein the step (3) is specifically: pouring the molten tellurium liquid obtained in the step (2) into a mould, and air-cooling and forming.
9. A method for purifying tellurium as claimed in claim 1, further comprising subjecting the tellurium product obtained in the step (3) to a sampling analysis, for example, a Na content of more than 30ppm, repeating the steps (1) and (3) until the Na content is less than 30 ppm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410054658.4A CN117923435A (en) | 2024-01-15 | 2024-01-15 | Tellurium purification method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410054658.4A CN117923435A (en) | 2024-01-15 | 2024-01-15 | Tellurium purification method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117923435A true CN117923435A (en) | 2024-04-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202410054658.4A Pending CN117923435A (en) | 2024-01-15 | 2024-01-15 | Tellurium purification method |
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| Country | Link |
|---|---|
| CN (1) | CN117923435A (en) |
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- 2024-01-15 CN CN202410054658.4A patent/CN117923435A/en active Pending
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