CN101693551A - Method for removing arsenic in the process of extracting germanium by distillation - Google Patents
Method for removing arsenic in the process of extracting germanium by distillation Download PDFInfo
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- CN101693551A CN101693551A CN200910233353A CN200910233353A CN101693551A CN 101693551 A CN101693551 A CN 101693551A CN 200910233353 A CN200910233353 A CN 200910233353A CN 200910233353 A CN200910233353 A CN 200910233353A CN 101693551 A CN101693551 A CN 101693551A
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- germanium
- arsenic
- distillation
- dioxide
- chlorine
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Abstract
The invention discloses an arsenic removable method used during a distillation and germanium extract production process. A process flow thereof includes adding raw materials containing arsenic and germanium and proportional germanium dioxide into a distillation still, adding hydrochloric acid and introducing chlorine for 15-30min, stirring and introducing steam to heat, and then distilling germanium tetrachloride. Addition (weight ratio) of manganese dioxide is set as that: arsenic: manganese dioxide=1: 5-50, and chlorine aerated flow takes 0.5-50 litre/min. The arsenic removal method can smoothly remove arsenic trichloride during a germanium tetrachloride distillation process, simultaneously, severally controls usage of C12, and reduces influence on environment to the utmost extent.
Description
Technical field
The present invention relates to the dearsenicating method in a kind of process of extracting germanium by distillation.
Background technology
In the still-process of germanium concentrate, usually run into arsenic, arsenic is very big to the extension product influence of germanium, therefore must remove.Because process is a chlorinated distillation, therefore, it is mainly to generate arsenic trichloride (AsCl
3) formal adjoint in germanium tetrachloride (GeCl
4) generative process in.For purifying germanium tetrachloride (GeCl
4) anatomized arsenic trichloride (AsCl
3) correlation properties.Arsenic trichloride (AsCl
3), outward appearance and proterties: the colourless or faint yellow oily liquids of being fuming, molecular weight 181.28, vapour pressure 1.33kPa (normal temperature), boiling point: 130.2 ℃.As can be seen, arsenic trichloride (AsCl
3) boiling point and germanium tetrachloride (GeCl
4) 84 ℃ of boiling points close.Because macroscopic view goes up the control for reaction, can not reach the required perfect condition of arsenic removal, so will suitably handle trivalent arsenic.
Summary of the invention
At problems of the prior art, this patent utilization adds oxygenant in still-process, and tervalent arsenic is oxidized into the arsenic acid of pentavalent, and its temperature can not be distilled when 100 ℃～130 ℃ left and right sides.The present invention adopts following technical scheme:
Dearsenicating method in a kind of process of extracting germanium by distillation is characterized in that:
To contain arsenic germanium raw material and the certain proportion germanium dioxide joins still kettle, and add hydrochloric acid and logical chlorine 15～30min, and stir, logical steam heating distills out germanium tetrachloride.
Condition: 1) the add-on arsenic of Manganse Dioxide: Manganse Dioxide=1: 5～50 (weight ratio);
2) flow of logical chlorine is 0.5～50 liter/minute.
The beneficial effect of the invention:
Can remove the arsenic trichloride in the germanium tetrachloride still-process smoothly.Simultaneously, also Cl has been controlled in strictness
2Consumption, reduced influence to greatest extent to environment.
Description of drawings
Fig. 1 is the dearsenicating method FB(flow block) of the embodiment of the invention.
Embodiment
Below by specific embodiment technical solution of the present invention is described further.
Corresponding following chemical reaction takes place in usually, different oxygenants:
The oxygenant chemical reaction
Cl
2 Cl
2+AsCl
3+4H
2O＝H
3AsO
4+5HCl
MnO
2 MnO
2+4HCl＝Cl
2↑+MnCl
2+2H
2O?Cl
2+AsCl
3+4H
2O＝H
3AsO
4+5HCl
In addition, when the content of arsenic was micro-, we used FeCl
3It is carried out oxidation and carries out suitable absorption, can not distill thereby make micro-arsenic enter liquid phase.
Usually, can carry out the analysis of each constituent content at the raw material that enters distillation process, analytical results comprises arsenical amount.The grade of supposing arsenic among certain a collection of raw material M is X, then can calculate needed Cl in the chlorinated distillation process
2Amount, its weight is calculated as follows:
{[74.61g/mol/(35.45g/mol*3+74.61g/mol)]/(M*X)/(35.45g/mol*3+74.61g/mol)}*(35.45g/mol*2)
After the simplification be: MA=0.1614/ (M*X)
Be converted into required MnO
2Amount as follows:
{[74.61g/mol/(35.45g/mol*3+74.61g/mol)]/(M*X)/(35.45g/mol*3+74.61g/mol)}*(54.94g/mol+16.00g/mol*2)
After the simplification be: MB=0.918/ (M*X)
As shown in Figure 1, present method adopts the method that adds Manganse Dioxide and logical chlorine in process of production, with AsCl
3Be oxidized to AsCl
5, AsCl
5275.6 ℃ of boiling points are because AsCl
5Boiling point height, so AsCl
5Be difficult for along with GeCl
4Distill, thereby stay in the mother liquor.So, can remove arsenic trichloride in the germanium tetrachloride still-process smoothly.Simultaneously, also Cl has been controlled in strictness
2Consumption, reduced influence to greatest extent to environment.
Condition: 1) the add-on arsenic of Manganse Dioxide: Manganse Dioxide=1: 5～50 (weight ratio);
2) flow of logical chlorine is 0.5～50 liter/minute.
Though the present invention with preferred embodiment openly as above; but they are not to be used for limiting the present invention; anyly be familiar with this skill person; without departing from the spirit and scope of the invention; from when can doing various variations or retouching, so being as the criterion of should being defined with the application's claim protection domain of protection scope of the present invention.
Claims (3)
1. the dearsenicating method in the process of extracting germanium by distillation is characterized in that:
To contain arsenic germanium raw material and the certain proportion germanium dioxide joins still kettle, and add hydrochloric acid and logical chlorine 15～30min, and stir, logical steam heating distills out germanium tetrachloride.
2. the dearsenicating method in the process of extracting germanium by distillation according to claim 1 is characterized in that:
The add-on of Manganse Dioxide (weight ratio), arsenic: Manganse Dioxide=1: 5～50.
3. the dearsenicating method in the process of extracting germanium by distillation according to claim 1 is characterized in that:
0.5～50 liter/minute of the flow of logical chlorine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910233353A CN101693551A (en) | 2009-10-20 | 2009-10-20 | Method for removing arsenic in the process of extracting germanium by distillation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910233353A CN101693551A (en) | 2009-10-20 | 2009-10-20 | Method for removing arsenic in the process of extracting germanium by distillation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101693551A true CN101693551A (en) | 2010-04-14 |
Family
ID=42092567
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910233353A Pending CN101693551A (en) | 2009-10-20 | 2009-10-20 | Method for removing arsenic in the process of extracting germanium by distillation |
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|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967007A (en) * | 2010-11-23 | 2011-02-09 | 云南临沧鑫圆锗业股份有限公司 | Process method for improving chlorination distillation recovery rate of coarse germanium dioxide |
| CN102531043A (en) * | 2010-12-24 | 2012-07-04 | 北京有色金属研究总院 | Method for removing impurity arsenic from germanium tetrachloride |
| CN103183375A (en) * | 2011-12-29 | 2013-07-03 | 北京有色金属研究总院 | Preparation purification method of germanium tetrachloride for optical fiber |
| CN114105195A (en) * | 2021-12-31 | 2022-03-01 | 红河砷业有限责任公司 | Method for reducing tin content in arsenic trichloride |
-
2009
- 2009-10-20 CN CN200910233353A patent/CN101693551A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101967007A (en) * | 2010-11-23 | 2011-02-09 | 云南临沧鑫圆锗业股份有限公司 | Process method for improving chlorination distillation recovery rate of coarse germanium dioxide |
| CN101967007B (en) * | 2010-11-23 | 2012-01-04 | 云南临沧鑫圆锗业股份有限公司 | Process method for improving chlorination distillation recovery rate of coarse germanium dioxide |
| CN102531043A (en) * | 2010-12-24 | 2012-07-04 | 北京有色金属研究总院 | Method for removing impurity arsenic from germanium tetrachloride |
| CN103183375A (en) * | 2011-12-29 | 2013-07-03 | 北京有色金属研究总院 | Preparation purification method of germanium tetrachloride for optical fiber |
| CN114105195A (en) * | 2021-12-31 | 2022-03-01 | 红河砷业有限责任公司 | Method for reducing tin content in arsenic trichloride |
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Application publication date: 20100414 |