CN110344081A - A kind of method that wet chemistry-electrochemistry refining prepares high purity gallium - Google Patents
A kind of method that wet chemistry-electrochemistry refining prepares high purity gallium Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B58/00—Obtaining gallium or indium
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Abstract
A kind of method that wet chemistry-electrochemistry refining prepares high purity gallium, comprising the following steps: in 5-20% excellent pure grade NaOH solution, at 30-50 DEG C, using 99.99% thick gallium as anode, in 0.05-1A/cm2Electrochemistry liquid making is carried out under anodic current density, and preelectrolysis is carried out under cathode-current density, prepares 50-100g/L sodium solution gallate, as gallium electrorefining electrolyte；It using 99.99% thick gallium as raw material, is washed using the chemistry that pure acid carries out 2-30 minutes at 30-50 DEG C, then uses high purity water gradually dilute acid, and clean 5-15 times, obtain electrorefining anode gallium；Platinized platinum is cathode, progress electrorefining, 30-50 DEG C of temperature, cathode-current density 0.01-0.1A/cm2, anode gallium stirring rate 100-400rpm, in cathodic region acquisition gallium-purifying；Two sections of chemistry are carried out at 30-40 DEG C using excellent pure grade acid to wash, time 2-10 minute, cleaning 5-12 times is then gradually diluted with high purity water, obtains 7N gallium.The invention has the advantages that thick gallium purification process uses Whote-wet method technique, equipment is simple, and investment is small, and operation is easy；The gallium refinery practice period is short, gallium loss late is small, at low cost.
Description
Technical field
The present invention relates to field of material preparation, in particular to a kind of ultra high pure metal gallium wet preparation method.
Background technique
It is only 29.8 DEG C of dissipated metal with aluminium fusing point of the same clan that gallium (Ga), which is a kind of, in the form of gallium nitride, GaAs
Semiconductor field is widely used.In recent years, with high-new skills such as new energy, 3D printing, flexible device, LED, 5G communications
The fast development of art industry, the demand to gallium increasingly increase, especially urgent need high purity metal gallium product.Currently, gallium
Mainly proposed from the circulating mother liquor of bauxite into alumina process, by Pro-concentration with ion exchange process and electrodeposition group technology,
99.99% thick gallium can be obtained.However, in order to meet Hi-tech Industry Development requirement, it is necessary to carry out refining to thick gallium and mention
It is pure, obtain high purity metal gallium.
Currently, the preparation of high purity metal gallium (> 99.9999%) substantially passes through wet process and pyrogenic process Alternative combines.Xu Kai
A kind of method that China equal (200310115208.X) proposes low-temperature electrolytic and zone refining combined purifying prepares high purity gallium, but area
Domain smelting equipment is complicated, and operating procedure is harsh, and it is long to purify the period；Wang Ling etc. (Sichuan non-ferrous metal, 2000,3:8-11) is established
A kind of chemical treatment, electrorefining, vacuum distillation, crystal-pulling high purity gallium production technology, equally exist that the period is long, production effect
The problems such as rate is low, equipment and technique requirement are harsh, at high cost.
In consideration of it, developing a kind of high purity metal gallium preparation method easy to operate, the period is short, at low cost, have important
Meaning will be expected to push the fast development of gallium and its application industry.
Summary of the invention
It is an object of the present invention to provide the methods that a kind of wet chemistry-electrochemistry refining prepares high purity gallium, have equipment
Simply, the feature that operation is easy, the purification period is short and at low cost.
To achieve the above object, the present invention the following technical schemes are provided:
A kind of method that wet chemistry-electrochemistry refining prepares high purity gallium, it is characterised in that the following steps are included:
(a) electrochemistry liquid making: in 5-20% excellent pure grade NaOH solution, at 30-50 DEG C, using 99.99% thick gallium as anode,
In 0.05-1A/cm2Electrochemistry liquid making is carried out under anodic current density, preelectrolysis is further carried out under cathode-current density, is made
It is standby to obtain 50-100g/L sodium solution gallate, as gallium electrorefining electrolyte；
(b) one section of chemistry is washed: using 99.99% thick gallium as raw material, being carried out at 30-50 DEG C using 0.1-0.8N excellent pure grade acid
One section of chemistry is washed, time 2-30 minute, high purity water gradually dilute acid is then used, and clean 5-15 times, until solution colour is by black
Color obtains electrorefining 5N anode gallium to clarifying；
(c) electrorefining: using the solution of step (a) as electrolyte, it is anode that step (b), which obtains 5N gallium, and platinized platinum is cathode,
Progress electrorefining, 30-50 DEG C of temperature, cathode-current density 0.01-0.1A/cm2, anode gallium stirring rate 100-400rpm,
6N gallium is obtained in cathodic region；
(d) two sections of chemistry are washed: the 6N gallium obtained using step (c) is raw material, using 0.05-0.5N excellent pure grade acid in 30-40
It carries out two sections of chemistry at DEG C to wash, then time 2-10 minute is gradually diluted using high purity water, and cleaned 5-12 times, 7N gallium is obtained.
The electrochemistry liquid making, the preferred 8-15% of solution NaOH content, the preferred 0.1-0.5A/cm of anodic current density2, in advance
Electrolysis cathode current density 0.4-0.8A/cm2；
The excellent pure grade acid is one or both of hydrochloric acid, nitric acid, hydrofluoric acid, phosphoric acid；
One section of chemistry is washed, and the preferred 0.3-0.6N of excellent pure grade acid concentration, the time is 3-10 minutes preferred, and wash number is preferred
8-10 times；
The electrorefining, preferred 35-45 DEG C of temperature, cathode-current density 0.02-0.05A/cm2, anode gallium stirring speed
Rate 200-300rpm；
Two sections of chemistry are washed, and the preferred 0.1-0.3N of excellent pure grade acid concentration, the time is 4-6 minutes preferred, and wash number is preferred
6-8 times.
Compared with the existing technology, advantages of the present invention is as follows: thick gallium purification process uses Whote-wet method technique, and equipment is simple,
Invest it is small, operation be easy；The gallium refinery practice period is short, gallium loss late is small, at low cost.
Detailed description of the invention
Fig. 1 is process flow chart of the invention,
Fig. 2 is 7N high purity gallium product photo.
Specific embodiment
The present invention is discussed in detail referring to specific embodiment, but embodiment below is only limitted to explain the present invention, it is of the invention
Protection scope should include the full content of claim, be not limited only to the present embodiment.
Table 1 is 7N high purity gallium impurity content table
Unit: ppm wt
| Element | Na | Mg | Si | Ca | Cr | Mn |
| Content | <0.001 | <0.001 | 0.002 | <0.005 | <0.001 | <0.001 |
| Element | Fe | Ni | Cu | Zn | Sn | Pb |
| Content | <0.001 | 0.001 | 0.03 | 0.04 | <0.005 | 0.02 |
Embodiment 1
In 5% excellent pure grade NaOH solution, at 50 DEG C, using 99.99% thick gallium as anode, in 0.05A/cm2Anode current
Electrochemistry liquid making is carried out under density, and preelectrolysis is further carried out under cathode-current density, it is molten to prepare 50g/L gallic acid sodium
Liquid, as gallium electrorefining electrolyte；Using 99.99% thick gallium as raw material, one is carried out at 50 DEG C using 0.1N excellent pure grade acid
Duan Huaxue is washed, and the time 30 minutes, then using high purity water gradually dilute acid, and is cleaned 5 times, until solution colour is by black to clear
Clearly, electrorefining anode gallium is obtained；Platinized platinum is cathode, progress electrorefining, 30 DEG C of temperature, cathode-current density 0.1A/
cm2, anode gallium stirring rate 100rpm, in cathodic region acquisition gallium-purifying；Two sections are carried out at 40 DEG C using 0.05N excellent pure grade acid
Chemistry is washed, and the time 10 minutes, is then gradually diluted using high purity water, and clean 5 times, is obtained 7N gallium.
Embodiment 2
In 20% excellent pure grade NaOH solution, at 30 DEG C, using 99.99% thick gallium as anode, in 1A/cm2Anode current is close
Degree is lower to carry out electrochemistry liquid making, and preelectrolysis is further carried out under cathode-current density, prepares 100g/L sodium solution gallate,
As gallium electrorefining electrolyte；Using 99.99% thick gallium as raw material, one section of change is carried out at 30 DEG C using 0.8N excellent pure grade acid
Wash, and the time 2 minutes, then uses high purity water gradually dilute acid, and clean 15 times, until solution colour is extremely clarified by black, obtains
Obtain electrorefining anode gallium；Platinized platinum is cathode, carries out electrorefining, temperature 50 C, cathode-current density 0.01A/cm2, sun
Pole gallium stirring rate 400rpm obtains gallium-purifying in cathodic region；Two sections of chemistry are carried out at 30 DEG C using 0.5N excellent pure grade acid to wash,
Then time 2- minute is gradually diluted using high purity water, and clean 12 times, obtains 7N gallium.
Embodiment 3
In 10% excellent pure grade NaOH solution, at 40 DEG C, using 99.99% thick gallium as anode, in 0.1A/cm2Anode current
Electrochemistry liquid making is carried out under density, and preelectrolysis is further carried out under cathode-current density, it is molten to prepare 80g/L gallic acid sodium
Liquid, as gallium electrorefining electrolyte；Using 99.99% thick gallium as raw material, one is carried out at 40 DEG C using 0.3N excellent pure grade acid
Duan Huaxue is washed, and the time 5 minutes, then uses high purity water gradually dilute acid, and clean 8 times, until solution colour is extremely clarified by black,
Obtain electrorefining anode gallium；Platinized platinum is cathode, progress electrorefining, 40 DEG C of temperature, cathode-current density 0.02A/cm2,
Anode gallium stirring rate 200rpm obtains gallium-purifying in cathodic region；Two sections of chemistry are carried out at 35 DEG C using 0.1N excellent pure grade acid
It washes, the time 6 minutes, is then gradually diluted using high purity water, and clean 6 times, obtain 7N gallium.
Embodiment 4
In 15% excellent pure grade NaOH solution, at 35 DEG C, using 99.99% thick gallium as anode, in 0.5A/cm2Anode current
Electrochemistry liquid making is carried out under density, and preelectrolysis is further carried out under cathode-current density, it is molten to prepare 100g/L gallic acid sodium
Liquid, as gallium electrorefining electrolyte；Using 99.99% thick gallium as raw material, one is carried out at 30 DEG C using 0.6N excellent pure grade acid
Duan Huaxue is washed, and the time 3 minutes, then using high purity water gradually dilute acid, and is cleaned 10 times, until solution colour is by black to clear
Clearly, electrorefining anode gallium is obtained；Platinized platinum is cathode, progress electrorefining, 35 DEG C of temperature, cathode-current density 0.05A/
cm2, anode gallium stirring rate 300rpm, in cathodic region acquisition gallium-purifying；Two sections are carried out at 35 DEG C using 0.3N excellent pure grade acid
Chemistry is washed, and the time 4 minutes, is then gradually diluted using high purity water, and clean 8 times, is obtained 7N gallium.
Embodiment 5
In 8% excellent pure grade NaOH solution, at 45 DEG C, using 99.99% thick gallium as anode, in 0.3A/cm2Anode current is close
Degree is lower to carry out electrochemistry liquid making, and preelectrolysis is further carried out under cathode-current density, prepares 60g/L sodium solution gallate,
As gallium electrorefining electrolyte；Using 99.99% thick gallium as raw material, one section of change is carried out at 40 DEG C using 0.4N excellent pure grade acid
Wash, and the time 10 minutes, then uses high purity water gradually dilute acid, and clean 8 times, until solution colour is extremely clarified by black, obtains
Obtain electrorefining anode gallium；Platinized platinum is cathode, progress electrorefining, 40 DEG C of temperature, cathode-current density 0.06A/cm2, sun
Pole gallium stirring rate 200rpm obtains gallium-purifying in cathodic region；Two sections of chemistry are carried out at 40 DEG C using 0.3N excellent pure grade acid to wash,
It time 5 minutes, is then gradually diluted, and cleaned 7 times using high purity water, obtain 7N gallium.
It should be noted that those skilled in the art are that this hair may be implemented completely according to the various embodiments described above of the present invention
Bright independent claims and the full scope of appurtenance, realize process and the same the various embodiments described above of method；And the present invention is not
It elaborates and partly belongs to techniques well known.
The above, part specific embodiment only of the present invention, but scope of protection of the present invention is not limited thereto, appoints
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of, should all cover by what those skilled in the art
Within protection scope of the present invention.
Claims (6)
1. the method that a kind of wet chemistry-electrochemistry refining prepares high purity gallium, it is characterised in that the following steps are included:
(a) electrochemistry liquid making: in 5-20% excellent pure grade NaOH solution, at 30-50 DEG C, using 99.99% thick gallium as anode,
0.05-1A/cm2Electrochemistry liquid making is carried out under anodic current density, preelectrolysis is further carried out under cathode-current density, is prepared
50-100g/L sodium solution gallate is obtained, as gallium electrorefining electrolyte；
(b) one section of chemistry is washed: using 99.99% thick gallium as raw material, one section is carried out at 30-50 DEG C using 0.1-0.8N excellent pure grade acid
Chemistry is washed, time 2-30 minute, then using high purity water gradually dilute acid, and is cleaned 5-15 times, until solution colour by black extremely
Clarification, obtains electrorefining anode gallium, and the molten loss rate of gallium is lower than 4%；
(c) electrorefining: using the solution of step (a) as electrolyte, it is anode that step (b), which obtains 5N gallium, and platinized platinum is cathode, is carried out
Electrorefining, 30-50 DEG C of temperature, cathode-current density 0.01-0.1A/cm2, anode gallium stirring rate 100-400rpm, in yin
Polar region obtains gallium-purifying；
(d) two sections of chemistry are washed: for step (c) obtain gallium-purifying, using 0.05-0.5N excellent pure grade acid at 30-40 DEG C into
Two sections of chemistry of row are washed, time 2-10 minute, are then gradually diluted using high purity water, and clean 5-12 times, and 7N gallium is obtained.
2. a kind of method that wet chemistry-electrochemistry refining prepares high purity gallium as described in claim 1, which is characterized in that
The electrochemistry liquid making, the preferred 8-15% of solution NaOH content, the preferred 0.1-0.5A/cm of anodic current density2, preelectrolysis cathode
Current density 0.4-0.8A/cm2。
3. a kind of method that wet chemistry-electrochemistry refining prepares high purity gallium as described in claim 1, which is characterized in that
The excellent pure grade acid is one or both of hydrochloric acid, nitric acid, hydrofluoric acid, phosphoric acid.
4. a kind of method that wet chemistry-electrochemistry refining prepares high purity gallium as described in claim 1, which is characterized in that
One section of chemistry is washed, and the preferred 0.3-0.6N of excellent pure grade acid concentration, the time is 3-10 minutes preferred, and wash number is 8-10 times preferred.
5. a kind of method that wet chemistry-electrochemistry refining prepares high purity gallium as described in claim 1, which is characterized in that
The electrorefining, preferred 35-45 DEG C of temperature, cathode-current density 0.02-0.05A/cm2, anode gallium stirring rate 200-
300rpm。
6. a kind of method that wet chemistry-electrochemistry refining prepares high purity gallium as described in claim 1, which is characterized in that
Two sections of chemistry are washed, and the preferred 0.1-0.3N of excellent pure grade acid concentration, the time is 4-6 minutes preferred, and wash number is 6-8 times preferred.
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Cited By (4)
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|---|---|---|---|---|
| CN111394751A (en) * | 2020-04-16 | 2020-07-10 | 广东省稀有金属研究所 | Method for purifying gallium by electrolysis, high-purity gallium and electrolysis device |
| CN112111758A (en) * | 2020-09-07 | 2020-12-22 | 中铝矿业有限公司 | Preparation process of low-iron 4N gallium |
| CN113549955A (en) * | 2021-07-08 | 2021-10-26 | 中南大学 | Crude gallium electrolytic refining device and method |
| RU2819851C2 (en) * | 2022-07-22 | 2024-05-27 | Федеральное государственное унитарное предприятие "Комбинат "Электрохимприбор" (ФГУП "Комбинат "Электрохимприбор") | Method for obtaining metallic gallium |
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| CN111394751A (en) * | 2020-04-16 | 2020-07-10 | 广东省稀有金属研究所 | Method for purifying gallium by electrolysis, high-purity gallium and electrolysis device |
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| RU2819851C2 (en) * | 2022-07-22 | 2024-05-27 | Федеральное государственное унитарное предприятие "Комбинат "Электрохимприбор" (ФГУП "Комбинат "Электрохимприбор") | Method for obtaining metallic gallium |
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| CN110344081B (en) | 2020-11-27 |
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