CN116253296A - Method for extracting tellurium from matte - Google Patents

Method for extracting tellurium from matte Download PDF

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Publication number
CN116253296A
CN116253296A CN202310016297.XA CN202310016297A CN116253296A CN 116253296 A CN116253296 A CN 116253296A CN 202310016297 A CN202310016297 A CN 202310016297A CN 116253296 A CN116253296 A CN 116253296A
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stirring
tellurium
matte
copper matte
copper
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CN116253296B (en
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曹文标
王洪波
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Yongxing County Hongfu Metal Co ltd
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Yongxing County Hongfu Metal Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00Selenium; Tellurium; Compounds thereof
    • C01B19/02Elemental selenium or tellurium
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention provides a method for extracting tellurium from copper matte, which takes copper matte as a raw material and adopts a pyrogenic process or/and a wet process to prepare a target product; the pyrogenic process comprises the following specific steps: crushing raw material copper matte, adding crude lead and crushed copper matte into a smelting pot, completely melting the materials, adding alkali, and stirring for reaction to obtain a target product; the wet process comprises the following specific steps: drying raw material copper matte, crushing by a crusher, ball milling, screening to obtain copper matte powder, transferring into a reaction kettle, adding hot water for soaking, adding sulfuric acid, stirring for reaction, stopping stirring and naturally settling, putting bottom slurry into a slurry tank, obtaining filter cakes and filtrate by a filter press, transferring the filtrate into the reaction kettle, adding alkali for stirring and neutralizing for reaction, stopping stirring and naturally settling, and performing filter pressing by the bottom slurry filter press to obtain slag, thereby obtaining the target product. The tellurium white product with the tellurium content of more than or equal to 20 percent is prepared by adopting the process of the invention, the tellurium recovery rate is high, and the low matte utilization value is effectively improved.

Description

Method for extracting tellurium from matte
Technical Field
The invention relates to the field of metal processing, in particular to a method for extracting tellurium from copper matte.
Background
Copper concentrate is smelted in a closed blast furnace, reverberatory furnace, electric furnace or flash furnace to produce matte. Copper matte is a compound of copper and sulfur, and is copper matte (Cu 2 S about 80% copper), about 60% copper, about low copper (40% copper or less). At present, the effective utilization of the low-copper matte is limited, and further research on the deep processing technology of the low-copper matte is very needed, so that the utilization value of the low-copper matte is further improved.
The main products of tellurium include: metal tellurium, tellurium dioxide, tellurium powder and high purity tellurium. Tellurium is mainly used in metallurgical, chemical industries and catalysts, photovoltaic solar panels, electronics and others. The application of tellurium in the metallurgical industry accounts for about 42% of the total application. Tellurium is mainly used as an alloying element for nonferrous metals and steels in the metallurgical industry.
Disclosure of Invention
In view of the above, the invention provides a method for extracting tellurium from copper matte, which aims to effectively extract tellurium from low copper matte and prepare tellurium products.
The technical scheme of the invention is realized as follows:
a method for extracting tellurium from copper matte is to prepare a target product by taking copper matte as a raw material and adopting a pyrogenic process or/and a wet process.
Further, the copper-containing raw material contains 20-40% of copper and 5-15% of tellurium.
Further, the pyrogenic process comprises the following specific steps: crushing raw material copper matte, adding crude lead and crushed copper matte into a smelting pot, completely melting the materials, adding alkali, and stirring for reaction to obtain a target product.
Further, the pyrogenic process comprises the following specific steps: crushing raw material copper matte, adding crude lead and crushed copper matte into a smelting pot, heating to 390-410 ℃, stirring, continuously heating to 700-750 ℃, completely melting the materials, adding alkali, and stirring for reacting for 2.5-3.5 h to obtain a target product; the mass ratio of the crude lead to the crushed matte is 3.5-4.5: 1, a step of; the addition amount of the alkali is 19-21 times of the tellurium mass in the copper matte; the alkali is sodium hydroxide or potassium hydroxide.
Further, the wet process specifically comprises the following steps: drying raw material copper matte, crushing by a crusher, ball milling, screening to obtain copper matte powder, transferring into a reaction kettle, adding hot water for soaking, adding sulfuric acid, stirring for reaction, stopping stirring and naturally settling, putting bottom slurry into a slurry tank, obtaining filter cakes and filtrate by a filter press, transferring the filtrate into the reaction kettle, adding alkali for stirring and neutralizing for reaction, stopping stirring and naturally settling, and performing filter pressing by the bottom slurry filter press to obtain slag, thereby obtaining the target product.
Further, the wet process specifically comprises the following steps: drying raw material matte, crushing by a crusher, ball milling and screening to obtain the matte powder with the particle size less than or equal to 60 meshes, transferring into a reaction kettle, adding hot water for soaking, adding sulfuric acid until the acid content is 25% -35% w/w, stirring and reacting for 2.5-3.5 hours, stopping stirring and naturally settling for 1.5-2.5 hours for solid-liquid layering, placing bottom slurry into a slurry tank, obtaining a filter cake and filtrate by a filter press, transferring the filtrate into the reaction kettle, adding alkali for stirring and neutralizing for 1.5-2.5 hours, stopping stirring and naturally settling for 1.5-2.5 hours, and performing filter pressing on the bottom slurry by the filter press to obtain slag, thereby obtaining a target product; the hot water soaking time is 20-40min.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention takes low copper matte as raw material, adopts a pyrogenic process or/and a wet process to prepare the tellurium white product with the tellurium content of more than or equal to 20 percent, has high tellurium recovery rate and effectively improves the utilization value of the low copper matte.
(2) The invention provides a plurality of processes, which can be selected according to own equipment, can help to reduce the actual production cost and improve the feasibility and adaptability of the tellurium white product made of low copper matte.
(3) The invention has short process flow and simple operation, and can be produced in large scale.
Drawings
FIG. 1 is a schematic illustration of the pyrogenic process flow of example 1
Fig. 2 is a schematic of the wet process flow of example 5.
Detailed Description
In order to better understand the technical content of the present invention, the following provides specific examples to further illustrate the present invention.
The experimental methods used in the embodiment of the invention are conventional methods unless otherwise specified.
Materials, reagents, and the like used in the examples of the present invention are commercially available unless otherwise specified.
Example 1A method of extracting tellurium from copper matte
The fire process comprises the following steps: crushing raw material copper matte (about 30% of copper and 10% of tellurium) for standby, adding 16t of crude lead and 4t of crushed copper matte into a 20t smelting pot with stirring, heating to 400 ℃ at a speed of 9.0 ℃/min, starting stirring at a stirring speed of 60rpm, continuously heating to 700 ℃ at a speed of 4.0 ℃/min, fully melting the materials, adding alkali according to a ratio of 1:20 (tellurium: alkali, w/w), continuously stirring and reacting for 3.0h, keeping the stirring speed of 60rpm, and reacting to obtain a tellurium white product, wherein the tellurium content is more than 25%.
Experiments show that the alkali is sodium hydroxide or potassium hydroxide, the stirring speed is 50-70 rpm, and the tellurium white product can be obtained under the conditions.
Example 2A method of extracting tellurium from copper matte
The fire process comprises the following steps: crushing raw material copper matte (about 30% containing copper and 10% containing tellurium) for standby, adding 14t of crude lead and 4t of crushed copper matte into a 20t smelting pot with stirring, heating to 390 ℃ at a speed of 8.5 ℃/min, starting stirring at a stirring speed of 60rpm, continuously heating to 700 ℃ at a speed of 3.8 ℃/min, and completely melting the materials according to a ratio of 1:21 And (tellurium: sodium hydroxide, w/w) adding sodium hydroxide, continuously stirring and reacting for 2.5h, keeping the stirring rotation speed at 60rpm, and reacting to obtain a tellurium white product, wherein the tellurium content is more than 25%, and the tellurium recovery rate is more than 95%.
Example 3A method of extracting tellurium from copper matte
The fire process comprises the following steps: crushing raw material copper matte (about 30% containing copper and 10% containing tellurium) for standby, adding 18t of crude lead and 4t of crushed copper matte into a 20t smelting pot with stirring, heating to 410 ℃ at a speed of 9.5 ℃/min, starting stirring at a stirring speed of 60rpm, continuously heating to 750 ℃ at a speed of 4.2 ℃/min, and completely melting the materials according to a ratio of 1:19 And (tellurium: sodium hydroxide, w/w) adding sodium hydroxide, continuously stirring and reacting for 3.5h, keeping the stirring rotation speed at 60rpm, and reacting to obtain a tellurium white product, wherein the tellurium content is more than 25%, and the tellurium recovery rate is more than 95%.
Example 4A method of extracting tellurium from copper matte
Based on example 1, the first temperature rise rate was controlled: heating to 400 ℃ at the speed of 4.5 ℃/min, and controlling the second heating speed: the temperature was raised to 700℃at a rate of 5.5℃per minute. As a result, the tellurium content of the tellurium white product was reduced to about 22%. The tellurium content of the product obtained in example 1 is higher than that in example 4, and it is possible that the temperature raising procedure in example 1 is more favorable for the reaction to be sufficient.
Example 5A method of extracting tellurium from copper matte
Wet process: stoving copper matte (30% copper and 10% tellurium), crushing with crusher, ball milling at 400rpm for 2.0 hr, sieving to obtain copper matte powder with particle size below 60 mesh, soaking in hot water for 30min, adding sulfuric acid to acid content of 30%, stirring at 10rpm for 3.0 hr, stopping stirring for natural settling for 2.0 hr to separate solid from liquid, adding bottom slurry into slurry tank, filtering to obtain filter cake and filtrate, stirring at 40rpm for neutralizing for 2.0 hr, stopping stirring for 2.0 hr, and filtering with filter press to obtain residue with tellurium content of 50% (dry weight) to obtain tellurium white product with tellurium content over 30% and tellurium recovery rate over 98%.
Experiments show that the alkali is sodium hydroxide or potassium hydroxide, and the tellurium white product can be obtained; in addition, the filter cake can be sold, and the filter cake contains valuable metals such as copper, gold, silver and the like.
Example 6A method of extracting tellurium from copper matte
Wet process: stoving copper matte (30% copper and 10% tellurium), crushing with crusher, ball milling at 380rpm for 4.0 hr, sieving to obtain copper matte powder with particle size below 60 mesh, soaking in hot water for 30min, adding sulfuric acid to acid content of 30%, stirring at 12rpm for 2.5 hr, stopping stirring for natural settling for 2.5 hr to separate solid from liquid, adding bottom slurry into slurry tank, filtering to obtain filter cake and filtrate, stirring at 35rpm for 2.5 hr, adding sodium hydroxide, stopping stirring for natural settling for 2.5 hr, and filtering with bottom slurry filter to obtain slag with tellurium content of 50% (dry weight) to obtain tellurium white product with tellurium content of 30% or above and tellurium recovering rate of 98%.
Example 7A method of extracting tellurium from copper matte
Wet process: stoving copper matte (30% copper and 10% tellurium), crushing with crusher, ball milling at 420rpm for 2.0 hr, sieving to obtain copper matte powder with particle size below 60 mesh, soaking in hot water for 30min, adding sulfuric acid to acid content of 30%, stirring at 8rpm for 3.5 hr, stopping stirring for natural settling for 2.5 hr to separate solid from liquid, adding bottom slurry into slurry tank, filtering to obtain filter cake and filtrate, stirring at 45rpm for 2.5 hr, adding sodium hydroxide, stopping stirring for natural settling for 2.5 hr, and filter pressing with bottom slurry filter to obtain slag with tellurium content of 50% (dry weight) to obtain tellurium white product with tellurium content of 30% or above and tellurium recovering rate of 98%.
Example 8A method of extracting tellurium from copper matte
Wet process: stoving copper matte (30% copper and 10% tellurium), crushing with crusher, ball milling at 400rpm for 2.0 hr, sieving to obtain copper matte powder with particle size below 60 mesh, soaking in hot water for 30min, adding sulfuric acid to acid content of 30%, stirring at 20rpm for 3.0 hr, stopping stirring, naturally settling for 2.0 hr to separate solid from liquid, adding bottom slurry into slurry tank, filtering to obtain filter cake and filtrate, stirring the filtrate in the reactor at 20rpm to neutralize for 2.0 hr, stopping stirring, naturally settling for 2.0 hr, and press filtering with bottom slurry filter to obtain slag containing 50% (dry weight) to obtain tellurium white product.
It was found that after adjusting the stirring conditions for the two reactions, the tellurium content of the tellurium white product obtained in example 8 was reduced to about 27%. Example 8 the tellurium content of the tellurium white product produced in example 5 is higher than in example 5, probably because the stirring conditions of example 5 are relatively more fully reacted.
Example 9A method of extracting tellurium from copper matte
Wet process: stoving copper matte (30% copper and 10% tellurium), crushing with crusher, ball milling at 300rpm for 1.0 hr, sieving to obtain copper matte powder with particle size below 40 mesh, soaking in hot water for 30min, adding sulfuric acid to acid content of 30%, stirring at 10rpm for 3.0 hr, stopping stirring, naturally settling for 2.0 hr to separate solid from liquid, adding bottom slurry into slurry tank, filtering to obtain filter cake and filtrate, stirring the filtrate in the reactor at 40rpm to neutralize for 2.0 hr, stopping stirring, naturally settling for 2.0 hr, and press filtering with bottom slurry filter to obtain slag containing 50% (dry weight) to obtain tellurium white product.
It was found that after adjusting the ball milling conditions, the tellurium content of the tellurium white product prepared in example 9 was reduced to about 28%. The tellurium content of the tellurium white product obtained in example 9 is reduced compared with that in example 5, and it is possible that the ball milling condition of example 5 is relatively more favorable for subsequent full reaction to obtain the copper matte powder.
The results of the tellurium white products prepared in examples 1-9 are summarized as follows:
process for producing a solid-state image sensor Tellurium content (%) Tellurium recovery (%)
Example 1 Fire method 25.91 95.81
Example 2 Fire method 25.10 95.48
Example 3 Fire method 25.25 95.53
Example 4 Fire method 22.07 93.66
Example 5 Wet process 30.87 98.34
Example 6 Wet process 30.56 98.51
Example 7 Wet process 30.38 98.38
Example 8 Wet process 27.01 96.87
Example 9 Wet process 28.23 97.54
In summary, the invention takes low copper matte as raw material, adopts a pyrogenic process or/and a wet process to prepare the tellurium white product with the tellurium content of more than or equal to 20 percent, has high tellurium recovery rate and effectively improves the utilization value of the low copper matte.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.

Claims (10)

1. A method for extracting tellurium from copper matte is characterized in that the copper matte is used as a raw material, and a target product is prepared by adopting a pyrogenic process or/and a wet process.
2. The method of extracting tellurium from copper matte of claim 1, wherein the pyrometallurgical process comprises the steps of: crushing raw material copper matte, adding crude lead and crushed copper matte into a smelting pot, completely melting the materials, adding alkali, and stirring for reaction to obtain a target product.
3. The method of extracting tellurium from matte of claim 2, wherein the pyrogenic process comprises the specific steps of: crushing raw material copper matte, adding crude lead and crushed copper matte into a smelting pot, heating to 390-410 ℃, stirring, continuously heating to 700-750 ℃, completely melting the materials, adding alkali, and stirring for reacting for 3-4 hours to obtain the target product.
4. A method for extracting tellurium from copper matte according to claim 3, wherein the mass ratio of the lead bullion to the crushed copper matte is 3.5-4.5: 1, a step of; the addition amount of the alkali is 19-21 times of the tellurium mass in the copper matte.
5. A method for extracting tellurium from matte according to claim 3, wherein the first heating rate: heating to 390-410 ℃ at a speed of 8.5-9.5 ℃/min, and heating for the second time: raising the temperature to 700-750 ℃ at the speed of 3.8-4.2 ℃/min; the stirring rotation speed is 50-70 rpm.
6. The method of extracting tellurium from matte of claim 1, wherein the wet process comprises the steps of: drying raw material copper matte, crushing by a crusher, ball milling, screening to obtain copper matte powder, transferring into a reaction kettle, adding hot water for soaking, adding sulfuric acid, stirring for reaction, stopping stirring and naturally settling, putting bottom slurry into a slurry tank, obtaining filter cakes and filtrate by a filter press, transferring the filtrate into the reaction kettle, adding alkali for stirring and neutralizing for reaction, stopping stirring and naturally settling, and performing filter pressing by the bottom slurry filter press to obtain slag, thereby obtaining the target product.
7. The method for extracting tellurium from matte of claim 6, wherein the wet process comprises the specific steps of: drying raw material matte, crushing by a crusher, ball milling, screening to obtain the matte powder with the particle size less than or equal to 60 meshes, transferring into a reaction kettle, adding hot water for soaking, adding sulfuric acid until the acid content is 25% -35% w/w, stirring and reacting for 2.5-3.5 h, stopping stirring and naturally settling for 1.5-2.5h for solid-liquid layering, placing bottom slurry into a slurry tank, obtaining a filter cake and filtrate by a filter press, transferring the filtrate into the reaction kettle, adding alkali for stirring and neutralizing for 1.5-2.5h, stopping stirring and naturally settling for 1.5-2.5h, and performing filter pressing on the bottom slurry by the filter press to obtain a slag, thereby obtaining the target product.
8. The method of extracting tellurium from copper matte of claim 7, wherein the hot water soak time is 20-40 minutes.
9. The method for extracting tellurium from matte according to claim 7, wherein the rotation speed of the ball milling is 380-420 rpm, and the ball milling time is 2-4 hours; the rotation speed of the stirring reaction is 8-12 rpm; the rotation speed of the stirring neutralization reaction is 35-45 rpm.
10. The method for extracting tellurium from matte according to claim 1, wherein the matte material contains 20% -40% copper and 5% -15% tellurium.
CN202310016297.XA 2023-01-06 2023-01-06 Method for extracting tellurium from matte Active CN116253296B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004218001A (en) * 2003-01-14 2004-08-05 Mitsubishi Materials Corp Treatment method for selenium and tellurium
CN102586600A (en) * 2011-01-18 2012-07-18 郴州市金贵银业股份有限公司 Process for recycling valuable metal from lead copper matte
CN105967153A (en) * 2016-05-06 2016-09-28 郴州市金贵银业股份有限公司 Technology for recovering tellurium from high-tellurium slag
CN110004298A (en) * 2019-04-04 2019-07-12 福建铭祥金属材料有限公司 A kind of industry dangerous waste Resource comprehensive utilization method
CN112063854A (en) * 2020-09-02 2020-12-11 河南豫光金铅股份有限公司 Method for comprehensively recovering bismuth, silver and copper metals by taking precious lead as raw material
CN112695199A (en) * 2020-12-15 2021-04-23 广东先导稀贵金属材料有限公司 Method for extracting tellurium and copper from tellurium-copper slag

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004218001A (en) * 2003-01-14 2004-08-05 Mitsubishi Materials Corp Treatment method for selenium and tellurium
CN102586600A (en) * 2011-01-18 2012-07-18 郴州市金贵银业股份有限公司 Process for recycling valuable metal from lead copper matte
CN105967153A (en) * 2016-05-06 2016-09-28 郴州市金贵银业股份有限公司 Technology for recovering tellurium from high-tellurium slag
CN110004298A (en) * 2019-04-04 2019-07-12 福建铭祥金属材料有限公司 A kind of industry dangerous waste Resource comprehensive utilization method
CN112063854A (en) * 2020-09-02 2020-12-11 河南豫光金铅股份有限公司 Method for comprehensively recovering bismuth, silver and copper metals by taking precious lead as raw material
CN112695199A (en) * 2020-12-15 2021-04-23 广东先导稀贵金属材料有限公司 Method for extracting tellurium and copper from tellurium-copper slag

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