CN108217610A - A kind of tellurobismuthite extracts tellurium dioxide method - Google Patents

A kind of tellurobismuthite extracts tellurium dioxide method Download PDF

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Publication number
CN108217610A
CN108217610A CN201711447396.4A CN201711447396A CN108217610A CN 108217610 A CN108217610 A CN 108217610A CN 201711447396 A CN201711447396 A CN 201711447396A CN 108217610 A CN108217610 A CN 108217610A
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China
Prior art keywords
tellurium
roasting
tellurobismuthite
immersion liquid
miberal powder
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CN201711447396.4A
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Chinese (zh)
Inventor
周堃
曾英
龙剑平
王珂
王云燕
谢刚
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Chengdu Univeristy of Technology
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Chengdu Univeristy of Technology
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Priority to CN201711447396.4A priority Critical patent/CN108217610A/en
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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
    • C01B19/004Oxides; Hydroxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00Selenium; Tellurium; Compounds thereof
    • C01B19/001Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

The invention discloses a kind of tellurobismuthites to extract tellurium dioxide method, and tellurium bismuth raw ore is crushed to more than 90% to 200 mesh;Miberal powder 450 DEG C of 5~6h of roasting in roaster after crushing;Miberal powder continues to be crushed to 90% up to more than 200 mesh after roasting;Pretreatment miberal powder is added in into prepared hydrochloric acid solution slowly, external force stirs 3~4h;Immersion liquid is filtered to take, adjusts immersion liquid acidity to 0~1mol/L;Above-mentioned immersion liquid is extracted with P507, extraction takes raffinate later except iron;Extract above-mentioned raffinate with TBP, take extraction oil phase, be stripped with water, dry, obtain more than 99% tellurium dioxide.Compared with prior art, the present invention extracts tellurium dioxide by raw material of tellurobismuthite, and process route is relatively easy, and raw material availability is high, and single to solve current tellurium raw material sources, tellurium production capacity deficiency problem provides new path.It has the value of popularization and application.

Description

A kind of tellurobismuthite extracts tellurium dioxide method
Technical field
The present invention relates to metallurgical technology field more particularly to a kind of tellurobismuthite extraction tellurium dioxide methods.
Background technology
In modern society, with the appearance of various functions material, people are increasing to various rare earth element demands.Tellurium As a kind of dissipated metal for possessing special nature, there are many excellent performances, be to make semiconductor, cooling module, photo elements The material of main part of part is widely used in the high-tech areas such as Aeronautics and Astronautics, electronics.With space flight and aviation, military affairs, electronics and system The rapid development of cold, glass, organic synthesis industry new and high technology, demand and purity requirement to tellurium and its compound are increasingly Height is referred to as " vitamin " of industry.
In field of metallurgy, the application of tellurium has accounted for 78% using total amount;Limitation is compared in the tellurium application of early stage.In secondary generation During boundary's Great War, tellurium is that just have as vulcanizing agent for natural rubber production until later stage the 1950s as one kind The element of industrial utility value is in traditional industry field.Tellurium can enhance the machining property of steel, improve stainless steel, mild steel Machining yield.Tellurium can enhance the thermal shock resistance of iron, mechanical resistant vibration performance, improve its Sprouting resistance and anti-fatigue performance.It is this Mine, automation, railway and miscellaneous equipment are had been used to by the processed steel of tellurium.Tellurium is added in lead, tin to be carried respectively The corrosion resistance and anti-fatigue performance of high lead, the tensile strength for improving tin alloy and reduction processing hardening effect.It is added to tellurium Copper can also improve its machining property, improve corrosion resistance.The tellurium of addition 0.05% can produce a kind of tin and close in tin Gold, in the case where progress cold rolling and decrement are 50%, the tensile strength of this tin alloy is twice of common tin.
In petrochemical industry field, tellurium has accounted for 12% in the application of oil and chemical field;Tellurium is as catalyst and vulcanization Agent synthesizes for rubber, can improve the efficiency of rubber production;Tellurium can play important work in the electrolysis of nickel, used in electrolyte Middle addition NaTeO 3 (75ml/L) can ultimately form anticorrosive very strong electrolytic nickel with regard to that can generate one layer of excessive nickel layer, the latter Layer.Tellurium catalyst is applied in cracking of oil, hydrogenation of coal etc..Tellurium is added to be also prevented from the oxygen of methyl polysilicone alkane Change.It is used as toner and kollag etc. in photography, press, tellurium also presents good application effect.
In electronic enterprises, dosage of the tellurium on electronics and electrical industry has been more than 8%.It is mainly used for photoreceptor. Since sensitive volume of the SeTe and SeAs alloys within the unit interval is higher, tellurium chromium mercury compound is red for military and space system The main light-sensitive material of external detector, telluride chromium are then applied to electro-optical system with its good extinction characteristic, and the U.S. is in army The high-purity tellurium used in thing is up to 99.99999%.Using the light sensitive characteristic of the function admirable containing tellurium compound, in resource investigation, defend Star aerial survey, laser guidance etc. show prominent advantage, and obtain in modern American is to the war in Iraq dripping most The performance of cause.In solar cell, diode, detector, thin film field-effect device, thermo-electric generation etc., tellurium also has extensively Application.In the photosensitive element of photomechanical production and laser printing and duplicating, tellurium is an important photoresist element.Exactly tellurium exists Above-mentioned performance in terms of photoelectron just plays an important role in 21 century most glamour industry.
Since tellurium is hardly formed the mineral deposit with extraction value in nature, the raw material for extracting tellurium in the world is main It is to be obtained from the dirt mud and body refuse in copper, nickel or lead electrolysis anode sludge and its smelting byproducts, production sulfuric acid or pulping process, Production cost is high, and the rate of recovery is low.1991, in Sichuan Province Shimian County, Dashuigou Independent Tellurium was found that global the first independent tellurium ore deposit, fills up A blank in theory of mineral deposit geology, and will change to rare element into the understanding of ore deposit ability, this will change the world of tellurium resource Distribution Pattern, and there is a possibility that China becomes a Ge Di resources big country.
It is an object of the invention to extract tellurium dioxide by raw material of Sichuan Province of China somewhere tellurobismuthite, process route is opposite Simply, raw material availability is high, and single to solve current tellurium raw material sources, tellurium production capacity deficiency problem provides new path.At present, Completely seldom come the technique developed as raw material using tellurobismuthite, therefore, the technique is relatively new, is completely suitable for industrializing.
Invention content
The purpose of the present invention is that solve the above-mentioned problems and provides a kind of tellurobismuthite extraction tellurium dioxide method.
The present invention is achieved through the following technical solutions above-mentioned purpose:
Step of the present invention is as follows:
(1) tellurium bismuth raw ore is crushed to more than 90% to 200 mesh;
(2) miberal powder 450 DEG C of 5~6h of roasting in roaster after crushing;
(3) miberal powder continues to be crushed to 90% up to more than 200 mesh after roasting;
(4) pretreatment miberal powder is added in into prepared hydrochloric acid solution slowly, external force stirs 3~4h;
(5) immersion liquid is filtered to take, immersion liquid acidity is adjusted to 0~1mol/L using miberal powder after roasting;
(6) above-mentioned immersion liquid is extracted with P507, extraction takes raffinate later except iron;
(7) extract above-mentioned raffinate with TBP, take extraction oil phase, be stripped with water, be dehydrated, dry, obtain more than 99% titanium dioxide Tellurium.
Further, 450 DEG C of 5~6h of roasting of miberal powder in the step (2), its object is to roast to solve a large amount of sulphur packets in ore deposit Tellurium problem is wrapped up in, and tellurium is become into oxide, convenient follow-up leaching.
Further, miberal powder continues to be crushed to 90% up to more than 200 mesh after roasting in the step (3), and its object is to solve Sintering mineral powder problem after certainly roasting.
Further, the step (in 5) adjusts immersion liquid acidity to 0~1mol/L, and its object is to improve follow-up P507 extractions Take efficiency.
The beneficial effects of the present invention are:
The present invention is a kind of tellurobismuthite extraction tellurium dioxide method, and compared with prior art, the present invention is using tellurobismuthite as original Material extraction tellurium dioxide, process route is relatively easy, and raw material availability is high, single for the current tellurium raw material sources of solution, tellurium production capacity Insufficient problem provides new path.It has the value of popularization and application.
Specific embodiment
The invention will be further described below:
Step of the present invention is as follows:
(1) tellurium bismuth raw ore is crushed to more than 90% to 200 mesh;
(2) miberal powder 450 DEG C of 5~6h of roasting in roaster after crushing;
(3) miberal powder continues to be crushed to 90% up to more than 200 mesh after roasting;
(4) pretreatment miberal powder is added in into prepared hydrochloric acid solution slowly, external force stirs 3~4h;
(5) immersion liquid is filtered to take, immersion liquid acidity is adjusted to 0~1mol/L using the tellurobismuthite powder after roasting;
(6) above-mentioned immersion liquid is extracted with P507, extraction takes raffinate later except iron;
(7) extract above-mentioned raffinate with TBP, take extraction oil phase, be stripped with water, dry, obtain more than 99% tellurium dioxide.
Further, 450 DEG C of 5~6h of roasting of miberal powder in the step (2), its object is to roast to solve a large amount of sulphur packets in ore deposit Tellurium problem is wrapped up in, and tellurium is become into oxide, convenient follow-up leaching.
Further, miberal powder continues to be crushed to 90% up to more than 200 mesh after roasting in the step (3), and its object is to solve Sintering mineral powder problem after certainly roasting.
Further, the step (in 5) adjusts immersion liquid acidity to 0~1mol/L, and its object is to improve follow-up P507 extractions Take efficiency.
Example 1
The miberal powder 50g pre-processed is taken, 3.5h is sufficiently stirred in prepared hydrochloric acid solution, immersion liquid is taken to adjust acidity and is arrived 0.5mol/L extracts the immersion liquid with the P507 that volume fraction is 60%, and iron extracts extracting rate up to more than 99.9%, by raffinate volume Score 40%TBP is extracted, and extraction oil phase is stripped with water, and precipitation filtering is dehydrated, and drying, weighing obtains tellurium dioxide purity and reaches 99.31%.
Example 2
The miberal powder 50g pre-processed is taken, 4h is sufficiently stirred in prepared hydrochloric acid solution, immersion liquid is taken to adjust acidity and is arrived 0.7mol/L extracts the immersion liquid with the P507 that volume fraction is 60%, and iron extracts extracting rate up to more than 99.8%, by raffinate volume Score 40%TBP is extracted, and extraction oil phase is stripped with water, precipitation filtering, drying, and weighing obtains tellurium dioxide purity and reaches 99.22%.
Example 3
The miberal powder 50g pre-processed is taken, 3h is sufficiently stirred in prepared hydrochloric acid solution, immersion liquid is taken to adjust acidity and is arrived 0.2mol/L extracts the immersion liquid with the P507 that volume fraction is 60%, and iron extracts extracting rate up to more than 99.92%, by raffinate body Fraction 40%TBP is extracted, and extraction oil phase is stripped with water, precipitation filtering, drying, and weighing obtains tellurium dioxide purity and reaches 99.19%.
Example 4
The miberal powder 50g pre-processed is taken, 3.5h is sufficiently stirred in prepared hydrochloric acid solution, immersion liquid is taken to adjust acidity and is arrived 0.15mol/L extracts the immersion liquid with the P507 that volume fraction is 60%, and iron extracts extracting rate up to more than 99.99%, by raffinate body Fraction 40%TBP is extracted, and extraction oil phase is stripped with water, precipitation filtering, drying, and weighing obtains tellurium dioxide purity and reaches 99.38%.
Basic principle of the invention and main feature and advantages of the present invention has been shown and described above.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its Equivalent thereof.

Claims (4)

1. a kind of tellurobismuthite extracts tellurium dioxide method, it is characterised in that:Step is as follows:
(1) tellurium bismuth raw ore is crushed to more than 90% to 200 mesh;
(2) miberal powder 450 DEG C of 5~6h of roasting in roaster after crushing;
(3) miberal powder continues to be crushed to 90% up to more than 200 mesh after roasting;
(4) pretreatment miberal powder is added in into prepared hydrochloric acid solution slowly, external force stirs 3~4h;
(5) immersion liquid is filtered to take, immersion liquid acidity is adjusted to 0~1mol/L using the tellurobismuthite powder after roasting;
(6) above-mentioned immersion liquid is extracted with P507, extraction takes raffinate later except iron;
(7) extract above-mentioned raffinate with TBP, take extraction oil phase, be stripped with water, dry, obtain more than 99% tellurium dioxide.
2. a kind of tellurobismuthite extraction tellurium dioxide method according to claim 1, it is characterised in that:In the step (2) Tellurium its object is to roast to solve the problems, such as a large amount of sulphur package telluriums in ore deposit, and is become oxide, side by 450 DEG C of 5~6h of roasting of miberal powder Continue leaching after an action of the bowels.
3. a kind of tellurobismuthite extraction tellurium dioxide method according to claim 1, it is characterised in that:In the step (3) Miberal powder continues to be crushed to 90% up to more than 200 mesh after roasting, its object is to solve the problems, such as roasting after sintering mineral powder.
4. a kind of tellurobismuthite extraction tellurium dioxide method according to claim 1, it is characterised in that:The step (in 5) Immersion liquid acidity is adjusted to 0~1mol/L using the tellurobismuthite powder after roasting, its object is to improve follow-up P507 extraction efficiencies.
CN201711447396.4A 2017-12-27 2017-12-27 A kind of tellurobismuthite extracts tellurium dioxide method Pending CN108217610A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4875417A (en) * 1972-01-17 1973-10-11
CN101880763A (en) * 2010-06-30 2010-11-10 四川鑫炬矿业资源开发股份有限公司 Method for gathering tellurium by roasting kawazulite and catalyst
CN103264997A (en) * 2013-05-28 2013-08-28 河北工业大学 Method for extracting tellurium from low-concentration tellurium solution
CN104627970A (en) * 2013-11-07 2015-05-20 孔龙 Method used for segmented recycling and separating of selenium and tellurium
CN106542508A (en) * 2016-11-09 2017-03-29 四川鑫炬新兴新光源材料有限公司 A kind of ultra-fine 4N tellurium dioxide raw powder's production technology and application
CN106987706A (en) * 2017-04-13 2017-07-28 成都理工大学 A kind of leaching method of tellurobismuthite

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS4875417A (en) * 1972-01-17 1973-10-11
CN101880763A (en) * 2010-06-30 2010-11-10 四川鑫炬矿业资源开发股份有限公司 Method for gathering tellurium by roasting kawazulite and catalyst
CN103264997A (en) * 2013-05-28 2013-08-28 河北工业大学 Method for extracting tellurium from low-concentration tellurium solution
CN104627970A (en) * 2013-11-07 2015-05-20 孔龙 Method used for segmented recycling and separating of selenium and tellurium
CN106542508A (en) * 2016-11-09 2017-03-29 四川鑫炬新兴新光源材料有限公司 A kind of ultra-fine 4N tellurium dioxide raw powder's production technology and application
CN106987706A (en) * 2017-04-13 2017-07-28 成都理工大学 A kind of leaching method of tellurobismuthite

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