CN105905937B - The technique of micro chlorine in a kind of removal gallium trichloride - Google Patents
The technique of micro chlorine in a kind of removal gallium trichloride Download PDFInfo
- Publication number
- CN105905937B CN105905937B CN201610256992.3A CN201610256992A CN105905937B CN 105905937 B CN105905937 B CN 105905937B CN 201610256992 A CN201610256992 A CN 201610256992A CN 105905937 B CN105905937 B CN 105905937B
- Authority
- CN
- China
- Prior art keywords
- chlorine
- gallium
- reaction
- technique
- gallium trichloride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of purifying process of gallium trichloride, the technique is excessively to judge reaction end by chlorine, then by the way that instead plus gallium consumes unnecessary chlorine to remove dechlorination impurity, its processing step is：The g galliums of 500g 3000 are put into reactor, reaction temperature is 180 DEG C, logical chlorine reaction, when gallium trichloride is reacted to terminal, i.e. reaction solution present pistac when, stopping is passed through chlorine, opens nitrogen purging, 1.0g 2.0g gallium is added into reactor, and continues to keep 180 DEG C until reaction solution becomes colourless by yellow green；The technique is excessively to judge reaction end by chlorine, then by instead plus gallium consumes unnecessary chlorine to remove dechlorination impurity, making chlorine impurity content in gallium trichloride be reduced to below 1ppm, and have very high product yield.
Description
Technical field
It is particularly a kind of to remove micro chlorine in gallium trichloride the present invention relates to a kind of purifying process of gallium trichloride
Technique, belong to chemical technology field.
Background technology
Due to being reacted in gallium trichloride production technology using chlorine, the reaction mechanism mechanism of reaction generates after gallium dichloride transition
Gallium trichloride, the judgement in reaction end judged by color change, when color by it is colourless become pistac when, i.e.,
Reaction reaches terminal, and now chlorine is excessive.So often contain micro chlorine in gallium trichloride product, and micro chlorine meeting
Cause product colour partially yellow.In the practical application of electronic grade high-purity gallium trichloride, chlorine is a kind of objectionable impurities, therefore right
The requirement of chlorine content is typically less than 1ppm.
Required to touch the mark, mostly selection carries out rectification and purification using rectifying column at present, but because chlorine is in trichlorine
Changing has certain solubility in gallium, simple rectification and purification is extremely difficult to purification and required.
The content of the invention
In view of the defects of above-mentioned technology is present, micro chlorine in gallium trichloride is removed it is an object of the invention to provide a kind of
Technique, the excessive chlorine for making to contain in gallium trichloride are reduced to 1ppm once, its index is reached electronic grade high-purity gallium trichloride
Requirement.
The technical scheme is that：The technique of micro chlorine, the technique are to pass through chlorine in a kind of removal gallium trichloride
Excess consumes unnecessary chlorine to remove dechlorination impurity to judge reaction end, then by instead adding gallium, and its processing step is：To
500g-3000 g galliums are put into reactor, reaction temperature is 180 DEG C, leads to chlorine reaction, terminal is reacted in gallium trichloride
When, i.e., reaction solution present pistac when, stopping is passed through chlorine, opens nitrogen purging, 1.0g-2.0g is added into reactor
Gallium, and continue keep 180 DEG C until reaction solution become colourless by yellow green.The present invention is to be sentenced former by color
On the basis of disconnected terminal, then minimal amount of gallium is added into reactor, reaction solution color is become again again colourless, it is more to consume
Remaining chlorine.Because gallium trichloride differs larger with the boiling point of in-between state monochlor(in)ate gallium and gallium dichloride, by simply subtracting
Pressure distillation can just separate well, the gallium total overall reaction generation gallium trichloride before so both ensureing in reactor,
And unnecessary chlorine is consumed.It can not only ensure that product has very high yield, also ensures by the method
The purity requirement of product.
The beneficial effects of the present invention are：The technique is excessively to judge reaction end by chlorine, then by instead plus gold
Belong to gallium to consume unnecessary chlorine to remove dechlorination impurity, chlorine impurity content in gallium trichloride is reduced to below 1ppm, and have
Very high product yield.
Embodiment
With reference to specific embodiment, the present invention is carried out using chlorine content different gallium trichloride purification experiment detailed
Explanation.
Embodiment 1：
500g galliums are put into, 180 DEG C, lead to chlorine reaction.When gallium trichloride is reacted to terminal, i.e., reaction solution is presented light
Yellow green when, stopping is passed through chlorine, opens nitrogen purging, 1.0g gallium is added into reactor, and continue holding 180
DEG C until reaction solution become colourless by yellow green.
Chlorine content contrast is as follows after before purification：
| Chlorine content（ppm） | |
| Chlorine is excessive | 15.8 |
| After adding gallium | 0.4 |
Embodiment 2：
1000g galliums are put into, 180 DEG C, lead to chlorine reaction.When gallium trichloride is reacted to terminal, i.e., reaction solution is presented
Pistac when, stopping is passed through chlorine, opens nitrogen purging, 1.0g gallium is added into reactor, and continue to keep
180 DEG C until reaction solution becomes colourless by yellow green.
Chlorine content contrast is as follows after before purification：
| Chlorine content（ppm） | |
| Chlorine is excessive | 20.5 |
| After adding gallium | 0.6 |
Embodiment 3：
3000g galliums are put into, 180 DEG C, lead to chlorine reaction.When gallium trichloride is reacted to terminal, i.e., reaction solution is presented
Pistac when, stopping is passed through chlorine, opens nitrogen purging, 2.0g gallium is added into reactor, and continue to keep
180 DEG C until reaction solution becomes colourless by yellow green.
Chlorine content contrast is as follows after before purification：
| Chlorine content（ppm） | |
| Chlorine is excessive | 18.6 |
| After adding gallium | 0.5 |
Claims (1)
1. a kind of technique for removing micro chlorine in gallium trichloride, it is characterised in that the technique is excessively judged by chlorine
Reaction end, then unnecessary chlorine is consumed to remove dechlorination impurity by instead adding gallium, its processing step is：Thrown into reactor
Entering 500g-3000g galliums, reaction temperature is 180 DEG C, leads to chlorine reaction, when gallium trichloride is reacted to terminal, i.e. reaction solution
Present pistac when, stopping is passed through chlorine, opens nitrogen purging, initial reaction gallium is added into reactor
0.67 ‰ -2 ‰ gallium, and continue to keep 180 DEG C until reaction solution becomes colourless by yellow green.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610256992.3A CN105905937B (en) | 2016-04-25 | 2016-04-25 | The technique of micro chlorine in a kind of removal gallium trichloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610256992.3A CN105905937B (en) | 2016-04-25 | 2016-04-25 | The technique of micro chlorine in a kind of removal gallium trichloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105905937A CN105905937A (en) | 2016-08-31 |
| CN105905937B true CN105905937B (en) | 2017-12-05 |
Family
ID=56752867
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610256992.3A Active CN105905937B (en) | 2016-04-25 | 2016-04-25 | The technique of micro chlorine in a kind of removal gallium trichloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105905937B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111072058B (en) * | 2019-12-20 | 2022-02-22 | 广东先导稀材股份有限公司 | Preparation method and equipment of gallium trichloride |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4372923A (en) * | 1980-12-05 | 1983-02-08 | Rhone-Poulenc Industries | Purification of solutions of gallium values by liquid/liquid extraction |
| EP0335147A1 (en) * | 1988-03-26 | 1989-10-04 | Hoechst Aktiengesellschaft | Process and apparatus for manufacturing of galliumchloride from gallium-containing compounds |
| RU2036150C1 (en) * | 1992-08-05 | 1995-05-27 | Научно-внедренческое предприятие "Ноосфера-центр" | Method for manufacture of highly pure gallium trichloride |
| CN1778683A (en) * | 2005-09-07 | 2006-05-31 | 中国铝业股份有限公司 | Production of gallium chloride |
| CN101413067A (en) * | 2008-10-29 | 2009-04-22 | 南京金美镓业有限公司 | Chemical extraction method and apparatus for metal gallium |
| CN101792174A (en) * | 2010-03-12 | 2010-08-04 | 韶关市锦源实业有限公司 | Anhydrous indium chloride synthesizing method |
| EP2570523A1 (en) * | 2010-05-12 | 2013-03-20 | National University Corporation Tokyo University Of Agriculture and Technology | Method for producing gallium trichloride gas and method for producing nitride semiconductor crystal |
| RU2573510C1 (en) * | 2014-09-16 | 2016-01-20 | Общество с ограниченной ответственностью "Инновации и разработки" (ООО "Иннова-Р") | Apparatus and method of producing high-purity gallium trichloride |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5474298A (en) * | 1977-11-24 | 1979-06-14 | Fujitsu Ltd | Purification of gallium trichloride |
| JPS6425922A (en) * | 1987-07-20 | 1989-01-27 | Mitsubishi Metal Corp | Method for reducing gallium chloride |
-
2016
- 2016-04-25 CN CN201610256992.3A patent/CN105905937B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4372923A (en) * | 1980-12-05 | 1983-02-08 | Rhone-Poulenc Industries | Purification of solutions of gallium values by liquid/liquid extraction |
| EP0335147A1 (en) * | 1988-03-26 | 1989-10-04 | Hoechst Aktiengesellschaft | Process and apparatus for manufacturing of galliumchloride from gallium-containing compounds |
| RU2036150C1 (en) * | 1992-08-05 | 1995-05-27 | Научно-внедренческое предприятие "Ноосфера-центр" | Method for manufacture of highly pure gallium trichloride |
| CN1778683A (en) * | 2005-09-07 | 2006-05-31 | 中国铝业股份有限公司 | Production of gallium chloride |
| CN101413067A (en) * | 2008-10-29 | 2009-04-22 | 南京金美镓业有限公司 | Chemical extraction method and apparatus for metal gallium |
| CN101792174A (en) * | 2010-03-12 | 2010-08-04 | 韶关市锦源实业有限公司 | Anhydrous indium chloride synthesizing method |
| EP2570523A1 (en) * | 2010-05-12 | 2013-03-20 | National University Corporation Tokyo University Of Agriculture and Technology | Method for producing gallium trichloride gas and method for producing nitride semiconductor crystal |
| RU2573510C1 (en) * | 2014-09-16 | 2016-01-20 | Общество с ограниченной ответственностью "Инновации и разработки" (ООО "Иннова-Р") | Apparatus and method of producing high-purity gallium trichloride |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105905937A (en) | 2016-08-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105905937B (en) | The technique of micro chlorine in a kind of removal gallium trichloride | |
| CN101700466A (en) | Process for treating residual liquid and tail gas in polysilicon production by improved Siemens method | |
| KR100729320B1 (en) | High purity phosphoric acid and method for production thereof | |
| CN110589770A (en) | Preparation method of electronic-grade hydrofluoric acid | |
| CN102328951A (en) | Method and device for removing hydrogen-containing impurities from germanium tetrachloride | |
| CN106255666A (en) | The processing method of fluoride water and processing means | |
| CN108502888A (en) | The purification system and silicon crystal of trichlorosilane | |
| MX2016008431A (en) | Novel purification processes. | |
| CN101780957A (en) | Method for refining trichlorosilane | |
| CN109678114B (en) | Method for removing arsenic impurity in electronic grade hydrochloric acid | |
| CN105502409B (en) | The method and device of infinite reflux rectification and purification optical fiber level silicon tetrachloride | |
| KR102310763B1 (en) | Purification method and apparatus for ultra-high purity hydrogen fluoride | |
| CN103088421A (en) | Method for chemically synthesizing high-purity hexagonal monocrystal calcium fluoride | |
| CN109081821B (en) | Furfural recovery device and recovery method for condensate liquid in ceramic production | |
| CN102502530A (en) | Method for producing electronic-grade sulfuric acid by static fusion crystallization | |
| KR102176381B1 (en) | Method for reprocessing wastewater from nitrobenzene production | |
| CN106699522A (en) | Production process of high-quality trimethyl orthoacetate | |
| CN113999094A (en) | Method for directly producing electronic grade hydrogen peroxide and acetone | |
| US20190352179A1 (en) | Method and system for producing purified aqueous hydrogen peroxide solution | |
| WO2015159893A1 (en) | Method for manufacturing fatty acid chloride and fatty acid chloride | |
| CN105399067B (en) | A kind of method for improving ketazine yield in ketazine process hydrazine hydrate still-process | |
| CN106187676B (en) | The recovery method of distillation residual liquid in a kind of production of tetrachloro-ethylene | |
| CN109503331B (en) | Method for preparing high-purity hydrogen chloride gas from 2, 4-dichlorophenol byproduct | |
| CN107381877B (en) | Nitromethane high-salinity wastewater treatment method | |
| KR20070028734A (en) | Purification method of nitrogen trifluoride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Zhao Yi Inventor after: Zhao Chao Inventor after: Wang Tianyuan Inventor after: Pei Kai Inventor after: Ji Yanqiu Inventor after: Liu Ying Inventor before: Zhao Yi Inventor before: Pei Kai Inventor before: Ji Yanqiu Inventor before: Liu Ying |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |