CN107935028A - A kind of catalyst type high pu-rity germanium production method - Google Patents
A kind of catalyst type high pu-rity germanium production method Download PDFInfo
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- CN107935028A CN107935028A CN201711389191.5A CN201711389191A CN107935028A CN 107935028 A CN107935028 A CN 107935028A CN 201711389191 A CN201711389191 A CN 201711389191A CN 107935028 A CN107935028 A CN 107935028A
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- germanium
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- tetrachloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G17/00—Compounds of germanium
- C01G17/02—Germanium dioxide
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of catalyst type high pu-rity germanium production method, it is characterised in that including：Concentrated hydrochloric acid is added to germanium concentrate and prepares germanium tetrachloride, distilation is carried out to germanium tetrachloride using rectifying column by the use of hydrogen chloride as protection gas, second distillation purification is carried out to the germanium tetrachloride after purification, further improve the concentration of germanium tetrachloride, germanium tetrachloride in the totally-enclosed hydrolysis kettle with agitating device under cryogenic by being hydrolyzed, hydrolysate is washed, clarification is stood after the completion of washing, using vacuum filter, secondary washing is carried out to the germanium dioxide after vacuum filter, clarification, filtering, germanium dioxide after filtering is dried in vacuo, crushing packing is carried out after drying, obtain catalyst type high-purity germanium dioxide, by germanium tetrachloride being hydrolyzed at low ambient temperatures reaction, the germanium dioxide generated after reaction has certain dissolubility, it can be dissolved in water.
Description
Technical field
The present invention relates to chemistry, metallurgical technology field, espespecially a kind of catalyst type high pu-rity germanium production method.
Background technology
Germanium dioxide is white powder or colourless crystallization, is tetragonal crystal system, hexagonal crystal system or amorphous body, six sides crystallization with
β-quartz isomorphism, germanium are four-coordination;Four directions crystallization has stipoverite type structure, and similar to rutile, wherein germanium is hexa-coordinate, high
Pressure, amorphous germanium dioxide is changed into hexa-coordinate structure, and as pressure reduces, germanium dioxide also gradually becomes the knot of four-coordination
Structure, the germanium dioxide of class Rutile structure can be changed into another rhombic system chloride-calcium type structure, titanium dioxide under high pressure
Germanium is not soluble in water and hydrochloric acid, is dissolved in lye generation germanate.The germanium dioxide of class Rutile structure is than six side's germanium dioxides more
Soluble easily in water, it can produce germanic acid when being acted on water, and germanium dioxide, in 1000 °C of heat altogether, can obtain germanium monoxide with germanium powder,
It is not soluble in water, do not reacted with water.
The content of the invention
To solve the above problems, the present invention provides a kind of catalyst type high pu-rity germanium production method, by low temperature ring
Germanium tetrachloride is hydrolyzed under border reaction, the germanium dioxide generated after reaction has certain dissolubility, can be dissolved in water.
To reach above-mentioned purpose, the present invention is realized using following technology, a kind of catalyst type high pu-rity germanium production method, its
It is characterized in that, including：
1）, to germanium concentrate add concentrated hydrochloric acid prepare germanium tetrachloride, by the use of hydrogen chloride as protection gas use rectifying column to germanium tetrachloride
Distilation is carried out, second distillation purification is carried out to the germanium tetrachloride after purification, further improves the concentration of germanium tetrachloride；
2）, germanium tetrachloride under cryogenic by being hydrolyzed in the totally-enclosed hydrolysis kettle with agitating device, to hydrolysate
Washing, stands clarification, using vacuum filter after the completion of washing；
3）, secondary washing, clarification, filtering are carried out to the germanium dioxide after vacuum filter, the germanium dioxide after filtering is carried out true
Sky is dry, carries out crushing packing after dry, obtains catalyst type high-purity germanium dioxide.
As a further improvement on the present invention, the hydrolysising reacting temperature control is at 1-10 DEG C.
As a further improvement on the present invention, 84-86 DEG C of the germanium tetrachloride rectification and purification temperature.
As a further improvement on the present invention, when the settling time is 24 small.
As a further improvement on the present invention, the hydrolysis pure water is using adding twice, and second of addition is the
Twice of addition.
The present invention has the advantages that compared with prior art:
1st, Design Conception of the invention in industry belongs to proposes first, and temperature when being hydrolyzed by controlling germanium tetrachloride, generation is touched
Matchmaker's type germanium dioxide, makes germanium dioxide have certain water solubility, can be dissolved in water.
Embodiment
Embodiment 1
A kind of catalyst type high pu-rity germanium production method, it is characterised in that including：
1）, to germanium concentrate add concentrated hydrochloric acid prepare germanium tetrachloride, by the use of hydrogen chloride as protection gas use rectifying column to germanium tetrachloride
Distilation is carried out, second distillation purification is carried out to the germanium tetrachloride after purification, further improves the concentration of germanium tetrachloride；
2）, germanium tetrachloride under cryogenic by being hydrolyzed in the totally-enclosed hydrolysis kettle with agitating device, to hydrolysate
Washing, stands clarification, using vacuum filter after the completion of washing；
3）, secondary washing, clarification, filtering are carried out to the germanium dioxide after vacuum filter, the germanium dioxide after filtering is carried out true
Sky is dry, carries out crushing packing after dry, obtains catalyst type high-purity germanium dioxide.
As a further improvement on the present invention, the hydrolysising reacting temperature control is at 1-10 DEG C.
As a further improvement on the present invention, 84-86 DEG C of the germanium tetrachloride rectification and purification temperature.
As a further improvement on the present invention, when the settling time is 24 small.
As a further improvement on the present invention, the hydrolysis pure water is using adding twice, and second of addition is the
Twice of addition.
The Design Conception of the present invention in industry belongs to be proposed first, temperature when being hydrolyzed by controlling germanium tetrachloride, generation
Catalyst type germanium dioxide, makes germanium dioxide have certain water solubility, can be dissolved in water.
Claims (5)
- A kind of 1. catalyst type high pu-rity germanium production method, it is characterised in that including：1）, to germanium concentrate add concentrated hydrochloric acid prepare germanium tetrachloride, by the use of hydrogen chloride as protection gas use rectifying column to germanium tetrachloride Distilation is carried out, second distillation purification is carried out to the germanium tetrachloride after purification, further improves the concentration of germanium tetrachloride；2）, germanium tetrachloride under cryogenic by being hydrolyzed in the totally-enclosed hydrolysis kettle with agitating device, to hydrolysate Washing, stands clarification, using vacuum filter after the completion of washing；3）, secondary washing, clarification, filtering are carried out to the germanium dioxide after vacuum filter, the germanium dioxide after filtering is carried out true Sky is dry, carries out crushing packing after dry, obtains catalyst type high-purity germanium dioxide.
- A kind of 2. catalyst type high pu-rity germanium production method according to claim 1, it is characterised in that：The hydrolysis temperature Degree control is at 1-10 DEG C.
- A kind of 3. catalyst type high pu-rity germanium production method according to claim 1, it is characterised in that：The germanium tetrachloride essence Evaporate 84-86 DEG C of temperature of purification.
- A kind of 4. catalyst type high pu-rity germanium production method according to claim 1, it is characterised in that：The settling time is 24 it is small when.
- A kind of 5. catalyst type high pu-rity germanium production method according to claim 1, it is characterised in that：The hydrolysis is pure For water using adding twice, second of addition is twice of first time addition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201711389191.5A CN107935028A (en) | 2017-12-21 | 2017-12-21 | A kind of catalyst type high pu-rity germanium production method |
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| CN201711389191.5A CN107935028A (en) | 2017-12-21 | 2017-12-21 | A kind of catalyst type high pu-rity germanium production method |
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| CN107935028A true CN107935028A (en) | 2018-04-20 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109279646A (en) * | 2018-11-26 | 2019-01-29 | 广东先导稀材股份有限公司 | The production method of catalyst grade germanium dioxide |
| CN111484069A (en) * | 2020-04-20 | 2020-08-04 | 湖北联合贵稀资源再生科技有限公司 | Preparation method of germanium dioxide powder |
| CN115404364A (en) * | 2022-09-24 | 2022-11-29 | 昆明理工大学 | Method for preparing germanium hydroxide from zinc hydrometallurgy inorganic germanium slag |
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| CN101066777A (en) * | 2007-06-08 | 2007-11-07 | 东南大学 | Prepn process of germanium dioxide powder |
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| CN104818396A (en) * | 2015-05-19 | 2015-08-05 | 河北工程大学 | Technique for recovering germanium from electric furnace germanium slag |
| CN106564933A (en) * | 2016-11-22 | 2017-04-19 | 云南临沧鑫圆锗业股份有限公司 | Preparation method of low-chloride high-purity germanium dioxide |
| CN107324376A (en) * | 2017-08-02 | 2017-11-07 | 昆明汇泉高纯半导材料有限公司 | It is a kind of to utilize the method that germanium dioxide is produced containing germanium waste material |
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2017
- 2017-12-21 CN CN201711389191.5A patent/CN107935028A/en active Pending
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| CN102774877A (en) * | 2012-08-03 | 2012-11-14 | 云南驰宏锌锗股份有限公司 | Novel process for preparing germanium dioxide (GeO2) |
| CN104818396A (en) * | 2015-05-19 | 2015-08-05 | 河北工程大学 | Technique for recovering germanium from electric furnace germanium slag |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109279646A (en) * | 2018-11-26 | 2019-01-29 | 广东先导稀材股份有限公司 | The production method of catalyst grade germanium dioxide |
| CN109279646B (en) * | 2018-11-26 | 2020-12-22 | 广东先导稀材股份有限公司 | Production method of catalyst-grade germanium dioxide |
| CN111484069A (en) * | 2020-04-20 | 2020-08-04 | 湖北联合贵稀资源再生科技有限公司 | Preparation method of germanium dioxide powder |
| CN111484069B (en) * | 2020-04-20 | 2023-09-29 | 湖北联合贵稀资源再生科技有限公司 | Preparation method of germanium dioxide powder |
| CN115404364A (en) * | 2022-09-24 | 2022-11-29 | 昆明理工大学 | Method for preparing germanium hydroxide from zinc hydrometallurgy inorganic germanium slag |
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