CN102923678A - Method for preparing anhydrous tellurium tetrachloride by using tellurium dioxide as raw material - Google Patents
Method for preparing anhydrous tellurium tetrachloride by using tellurium dioxide as raw material Download PDFInfo
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- CN102923678A CN102923678A CN2012104775185A CN201210477518A CN102923678A CN 102923678 A CN102923678 A CN 102923678A CN 2012104775185 A CN2012104775185 A CN 2012104775185A CN 201210477518 A CN201210477518 A CN 201210477518A CN 102923678 A CN102923678 A CN 102923678A
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Abstract
The invention relates to a method for preparing anhydrous tellurium tetrachloride by using tellurium dioxide as a raw material. The preparation process is as follows: easily-available tellurium dioxide in the industry with purity of 99.9% is used as the raw material; the tellurium dioxide is reduced into metal tellurium powder with the purity more than 99.9% by a hydrogen reduction method; the metal tellurium powder is chloridized by dried chlorine to obtain the anhydrous tellurium tetrachloride; the tellurium tetrachloride is distilled to separate out about 10% of first runnings; then about 90% of distillate is obtained subsequently; the distillate is the anhydrous tellurium tetrachloride with the purity more than 99.99%; obtained anhydrous tellurium tetrachloride with the purity more than 99.99% is hydrolyzed to obtain high-purity tellurium dioxide with the purity of 99.9999%; the tellurium dioxide with the purity of 99.99999% is reduced by hydrogen to obtain high-purity tellurium with the purity more than 99.99999%. The method for preparing the anhydrous tellurium tetrachloride by using the tellurium dioxide as the raw material is provided for related industries, and the method is simple in production method, high in product purity and low in preparation cost.
Description
Technical field
The present invention relates to a kind of method for preparing anhydrous tellurium tetrachloride take tellurium dioxide as raw material, the dissipated metal compound prepares category in the genus non-ferrous metal metallurgy.
Background technology
High-purity material is the foundation stone of material technology progress, high purity tellurium is widely used in semiconductor material, is the main raw material(s) of preparation infrared detecting materials, solar cell, electrooptic modulator, X-ray detection X material and material of cooling etc. such as CdTe, HgCdTe, CdZnTe, PbTe, BiTe; Even because very micro-impurity also can cause material electrical property variation, the purity of tellurium is the important factor that directly affects material property; Traditional metallic tellurium production technique, first the various tellurium raw materials that contain to be refined into the higher tellurium dioxide of purity, then it is dissolved in the sodium hydroxide solution, and behind removing heavy-metal impurity, be mixed with electrolytic solution, through electrolysis output electrolysis tellurium, the purity of electrolysis tellurium is generally 99.99%, in order to prepare the higher metallic tellurium of purity, the normal process combination that adopts Dian Xie – vacuum distilling obtains the tellurium of 99.999% purity, or the electrolysis tellurium to obtain purity through the empty Zheng Liu of Zhen – zone melting be 99.9999% tellurium; But, obtaining in the process of high purity metal tellurium the separation difficult of selenium with the empty Zheng Liu of Zhen – zone melting, also have simultaneously the residual of the impurity such as sodium, calcium and iron, the purity of metallic tellurium is brought up to more than 99.9999% very difficult, the apparatus expensive of using simultaneously, cost is high; By preparation and the rectifying of tellurium tetrachloride, and the hydrolysis of high-pure anhydrous tellurium tetrachloride, can obtain 99.9999% high-purity tellurium dioxide, the latter can make grade and surpass 99.99999% high purity tellurium through hydrogen reduction; Therefore, take the tellurium dioxide of low-purity as raw material, prepare anhydrous tellurium tetrachloride and have realistic meaning.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing anhydrous tellurium tetrachloride take tellurium dioxide as raw material, for relevant industries provide a kind of method for preparing anhydrous tellurium tetrachloride take tellurium dioxide as raw material.
Technical scheme of the present invention is: a kind of method for preparing anhydrous tellurium tetrachloride take tellurium dioxide as raw material, it is characterized in that: preparation flow is as raw material take the tellurium dioxide of the industrial purity that very easily obtains as 99.9%, at first it is reduced into purity with hydrogen reduction method and is higher than 99.9% metallic tellurium powder, then the metallic tellurium powder is carried out chlorination with dry chlorine gas, obtain anhydrous tellurium tetrachloride; Tellurium tetrachloride is isolated first approximately 10% singlings through distillation, and approximately 90% the overhead product that obtains subsequently is purity greater than 99.99% anhydrous tellurium tetrachloride;
Preparation process is: be that 99.9% tellurium dioxide is placed on graphite and burns in the boat with purity, be placed in the tubular electric furnace that is provided with the stainless steel boiler tube; Flow velocity with 3L-30 L/min in tubular electric furnace passes into hydrogen, and at 500-550 ℃ of lower reduction 7-9h, it is 99.9% metallic tellurium powder that reaction finishes to obtain purity; The metallic tellurium powder that hydrogen reduction the is obtained volume of packing into is in the thermal glass there-necked flask of 1-5L, from there-necked flask one side mouth one thermal glass tubule is inserted into the bottle bottom; With the nitrogen of drying the air in the there-necked flask is caught up with first, with the electrical heat tracing cover there-necked flask is heated to 250 ℃, flow velocity with 2-200ml/min passes into dry chlorine gas by the thermal glass tubule, the metallic tellurium powder begins chlorination, change gradually the tellurous chloride liquid of black into, continue to pass into chlorine, tellurous chloride changes liquid tellurium tetrachloride gradually into, still contains some tellurous chloride in the product tellurium tetrachloride; With electric mantle the there-necked flask vial of splendid attire tellurium tetrachloride is heated to 420 ℃, with the chlorine air-flow material in the there-necked flask is distilled, in another receiving flask, obtain purity and be 99.99% tellurium tetrachloride, tellurium tetrachloride in the receiving flask is moved to distillation tower, the inner nitrogen replacement of using of distillation tower, be heated to 420 ℃ with electric mantle, condenser is heated to 270 ℃, and this moment, tellurium tetrachloride began to distillate; About 10% singlings are separated, and approximately 90% the overhead product that obtains subsequently is purity greater than 99.99% anhydrous tellurium tetrachloride.
Be that raw material prepares purity that the method for anhydrous tellurium tetrachloride obtains and is hydrolyzed greater than 99.99% anhydrous tellurium tetrachloride with tellurium dioxide, can obtain 99.9999% high-purity tellurium dioxide, after hydrogen reduction, can make grade and surpass 99.99999% high purity tellurium.
Advantage of the present invention has provided a kind of method for preparing anhydrous tellurium tetrachloride take tellurium dioxide as raw material, and production method is simple and easy, product purity is high, preparation cost is low.
Description of drawings
Fig. 1 is preparation flow figure of the present invention.
Embodiment
With reference to Fig. 1 embodiment of the present invention is illustrated with the following examples: the present invention at first is that 99.9% tellurium dioxide is placed on graphite and burns in the boat with purity, graphite is burnt in the tubular electric furnace of stainless steel boiler tube that boat is placed on diameter 110mm, long 2.5m, flow velocity with 3L/min in tubular electric furnace passes into hydrogen, at 500-550 ℃ of lower reduction 7-9h, it is 99.9% metallic tellurium powder 350g that reaction finishes to obtain purity.In general, hydrogen reduction can improve the grade of metallic tellurium powder to a certain extent, removes some volatile impurity.
Be in the thermal glass there-necked flask of 1L with the 350g metallic tellurium powder volume of packing into, from there-necked flask one side mouth one thermal glass tubule be inserted into the bottle bottom.With the nitrogen of drying the air in the there-necked flask is caught up with first, with the electrical heat tracing cover there-necked flask is heated to 250 ℃, pass into dry chlorine gas with the flow velocity of 20ml/min by the thermal glass tubule.The metallic tellurium powder begins chlorination, changes gradually the tellurous chloride liquid of black into, continues to pass into chlorine, and tellurous chloride changes liquid tellurium tetrachloride gradually into.
Still contain some tellurous chloride in the product tellurium tetrachloride, with electric mantle the there-necked flask vial of splendid attire tellurium tetrachloride is heated to 420 ℃, with the chlorine air-flow material in the there-necked flask is distilled, in another receiving flask, obtain purity and be 99.99% tellurium tetrachloride.
Obtaining weight is the tellurium tetrachloride of 737 grams, and tellurium tetrachloride is moved to distillation tower, and distillation tower is inner uses nitrogen replacement, is heated to 420 ℃ with electric mantle, and condenser is heated to 270 ℃, and this moment, tellurium tetrachloride began to distillate.About 10% singlings are separated, and approximately 90% the overhead product that obtains subsequently is purity greater than 99.99% anhydrous tellurium tetrachloride.
Approximately 10% singlings are the relatively poor tellurium tetrachloride of purity that contains the impurity such as selenium, phosphorus, sulphur, arsenic, tin, gallium, with approximately 74 the gram the tellurium tetrachloride singlings be dissolved in the 90ml pure water, obtain the aqueous solution of tellurium tetrachloride.It is slowly splashed in the 1.5L pure water it under agitation is hydrolyzed, namely generate the white precipitate of tellurium dioxide.The latter after filtration with the eccysis chlorion, obtain being reused as the tellurium dioxide of initial feed.
Claims (1)
1. a method for preparing anhydrous tellurium tetrachloride take tellurium dioxide as raw material is characterized in that, comprises the following steps: with purity to be that 99.9% tellurium dioxide is placed on graphite and burns in the boat, is placed in the tubular electric furnace that is provided with the stainless steel boiler tube; Flow velocity with 3L-30 L/min in tubular electric furnace passes into hydrogen, and at 500-550 ℃ of lower reduction 7-9h, it is 99.9% metallic tellurium powder that reaction finishes to obtain purity; The metallic tellurium powder that hydrogen reduction the is obtained volume of packing into is in the thermal glass there-necked flask of 1-5L, from there-necked flask one side mouth one thermal glass tubule is inserted into the bottle bottom; With the nitrogen of drying the air in the there-necked flask is caught up with first, with the electrical heat tracing cover there-necked flask is heated to 250 ℃, flow velocity with 2-200ml/min passes into dry chlorine gas by the thermal glass tubule, the metallic tellurium powder begins chlorination, change gradually the tellurous chloride liquid of black into, continue to pass into chlorine, tellurous chloride changes liquid tellurium tetrachloride gradually into, still contains some tellurous chloride in the product tellurium tetrachloride; With electric mantle the there-necked flask vial of splendid attire tellurium tetrachloride is heated to 420 ℃, with the chlorine air-flow material in the there-necked flask is distilled, in another receiving flask, obtain purity and be 99.99% tellurium tetrachloride, tellurium tetrachloride in the receiving flask is moved to distillation tower, the inner nitrogen replacement of using of distillation tower, be heated to 420 ℃ with electric mantle, condenser is heated to 270 ℃, and this moment, tellurium tetrachloride began to distillate; About 10% singlings are separated, and approximately 90% the overhead product that obtains subsequently is purity greater than 99.99% anhydrous tellurium tetrachloride.
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| CN2012104775185A CN102923678A (en) | 2012-11-22 | 2012-11-22 | Method for preparing anhydrous tellurium tetrachloride by using tellurium dioxide as raw material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110775948A (en) * | 2019-12-05 | 2020-02-11 | 成都理工大学 | Method for improving reduction efficiency of tellurium oxide |
| CN114195105A (en) * | 2021-12-15 | 2022-03-18 | 株洲科能新材料股份有限公司 | Preparation method of high-purity tellurium dioxide |
| CN114229806A (en) * | 2021-12-01 | 2022-03-25 | 广东先导稀贵金属材料有限公司 | Method for preparing crystal-grade tellurium dioxide by hydrolysis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63285106A (en) * | 1987-05-15 | 1988-11-22 | Sumitomo Metal Mining Co Ltd | Production of high-purity tellurium dioxide |
| JPS63286531A (en) * | 1987-05-18 | 1988-11-24 | Sumitomo Metal Mining Co Ltd | Manufacture of high purity tellurium |
| CN102153054A (en) * | 2011-05-03 | 2011-08-17 | 嘉兴市达泽光电技术有限公司 | Preparation method of high purity tellurium |
-
2012
- 2012-11-22 CN CN2012104775185A patent/CN102923678A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63285106A (en) * | 1987-05-15 | 1988-11-22 | Sumitomo Metal Mining Co Ltd | Production of high-purity tellurium dioxide |
| JPS63286531A (en) * | 1987-05-18 | 1988-11-24 | Sumitomo Metal Mining Co Ltd | Manufacture of high purity tellurium |
| CN102153054A (en) * | 2011-05-03 | 2011-08-17 | 嘉兴市达泽光电技术有限公司 | Preparation method of high purity tellurium |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110775948A (en) * | 2019-12-05 | 2020-02-11 | 成都理工大学 | Method for improving reduction efficiency of tellurium oxide |
| CN114229806A (en) * | 2021-12-01 | 2022-03-25 | 广东先导稀贵金属材料有限公司 | Method for preparing crystal-grade tellurium dioxide by hydrolysis |
| CN114229806B (en) * | 2021-12-01 | 2024-01-09 | 广东先导稀贵金属材料有限公司 | Method for preparing crystal-grade tellurium dioxide by hydrolysis |
| CN114195105A (en) * | 2021-12-15 | 2022-03-18 | 株洲科能新材料股份有限公司 | Preparation method of high-purity tellurium dioxide |
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Application publication date: 20130213 |