CN116199251A - Method for efficiently preparing gallium oxyhydroxide - Google Patents
Method for efficiently preparing gallium oxyhydroxide Download PDFInfo
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- CN116199251A CN116199251A CN202310054518.2A CN202310054518A CN116199251A CN 116199251 A CN116199251 A CN 116199251A CN 202310054518 A CN202310054518 A CN 202310054518A CN 116199251 A CN116199251 A CN 116199251A
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- gallium
- oxyhydroxide
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- gallium oxyhydroxide
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- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title claims abstract description 122
- 229910052733 gallium Inorganic materials 0.000 title claims abstract description 122
- 238000000034 method Methods 0.000 title claims abstract description 49
- 229910052751 metal Inorganic materials 0.000 claims abstract description 45
- 239000002184 metal Substances 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 20
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000008367 deionised water Substances 0.000 claims description 29
- 229910021641 deionized water Inorganic materials 0.000 claims description 29
- 229910021513 gallium hydroxide Inorganic materials 0.000 claims description 24
- DNUARHPNFXVKEI-UHFFFAOYSA-K gallium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Ga+3] DNUARHPNFXVKEI-UHFFFAOYSA-K 0.000 claims description 24
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 15
- 238000010907 mechanical stirring Methods 0.000 claims description 15
- 239000001301 oxygen Substances 0.000 claims description 15
- 229910052760 oxygen Inorganic materials 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 239000011268 mixed slurry Substances 0.000 claims description 8
- 238000007664 blowing Methods 0.000 claims description 6
- 230000005587 bubbling Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 6
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 10
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 8
- 229910001195 gallium oxide Inorganic materials 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000004090 dissolution Methods 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 239000003513 alkali Substances 0.000 description 5
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- CHPZKNULDCNCBW-UHFFFAOYSA-N gallium nitrate Chemical compound [Ga+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CHPZKNULDCNCBW-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910000373 gallium sulfate Inorganic materials 0.000 description 3
- SBDRYJMIQMDXRH-UHFFFAOYSA-N gallium;sulfuric acid Chemical compound [Ga].OS(O)(=O)=O SBDRYJMIQMDXRH-UHFFFAOYSA-N 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229940044658 gallium nitrate Drugs 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- FZHLWVUAICIIPW-UHFFFAOYSA-M sodium gallate Chemical compound [Na+].OC1=CC(C([O-])=O)=CC(O)=C1O FZHLWVUAICIIPW-UHFFFAOYSA-M 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 description 1
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 150000002258 gallium Chemical class 0.000 description 1
- UPWPDUACHOATKO-UHFFFAOYSA-K gallium trichloride Chemical compound Cl[Ga](Cl)Cl UPWPDUACHOATKO-UHFFFAOYSA-K 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to the technical field of nonferrous metal metallurgy, and particularly relates to a method for efficiently preparing gallium oxyhydroxide. The technical scheme of the invention can solve the problems of long process flow, large reagent consumption, high requirement on equipment, difficult achievement of standards of product purity and physical specification and the like of the existing gallium oxyhydroxide preparation process, has the characteristics of low requirement on equipment, simple operation, low energy consumption, short process, high efficiency, low cost and the like, and can realize the high-efficiency short-process preparation of high-purity gallium oxyhydroxide powder materials.
Description
Technical Field
The invention belongs to the technical field of nonferrous metal metallurgy, and particularly relates to a method for efficiently preparing gallium oxyhydroxide.
Background
Gallium oxide (Ga) 2 O 3 ) Is an ultra-wide band-gap semiconductor, is the most novel fourth-generation semiconductor material at present, and has a band gap of up to 4.9-5.3eV. In contrast, the band gap of semiconductors such as silicon carbide (SiC) and gallium nitride (GaN) is 3.25eV and 3.4eV, respectively, whereas the band gap of silicon is only 1.1eV. Ultra-high forbidden band width enables Ga 2 O 3 The prepared device can be kept stable under extreme environments such as high temperature, low temperature, strong radiation and the like, and the performance of a power semiconductor is several times that of Si, siC and GaN, so that the device is a preferable material for preparing high-power semiconductor electronic devices, and has very important application value in the aspects of high-power electronic devices, ultraviolet transparent conduction, solar blind detection, gas sensing and the like.
With the rapid development of the fields of high and new technologies such as information, energy, traffic, national defense and the like, the demand of industries for gallium oxide is increasing. In the production of high-purity gallium oxide, high-purity gallium metal or gallium salt is generally used as a raw material, firstly, a gallium hydroxide precursor with the purity and the size and shape meeting the requirements is prepared, and then, the high-purity gallium oxide is obtained through high-temperature calcination. Thus, the preparation of acceptable gallium oxyhydroxide is a necessary condition and technical core for the production of gallium oxide.
Through retrieval, the application of Chinese patent application number 201810752162.9 discloses a method for preparing gallium oxide, which comprises the steps of reacting sulfuric acid and hydrogen peroxide serving as a dissolving agent with gallium metal to generate a gallium sulfate solution, further crystallizing to separate gallium sulfate crystals, and calcining at high temperature to obtain gallium oxide powder. The solution adopts sulfuric acid with relatively low reactivity, hydrogen peroxide is added to promote the dissolution process of gallium metal during leaching, the reagent cost is high, and SO is generated during the preparation of gallium oxide by high-temperature calcination of gallium sulfate 2 The smoke and the environmental protection pressure are high.
The Chinese patent application Nos. 201711418839.7 and 201710311705.9 disclose a method for preparing gallium oxyhydroxide from gallium metal, preferably nitric acid is used as a dissolving agent to react with gallium metal to generate gallium nitrate solution, then alkali solution is further added dropwise into the solution for neutralization, and the gallium oxyhydroxide powder is obtained after aging; the application of Chinese patent application No. 202010436819.8 proposes adding surface active agents such as dodecylbenzene sulfonic acid and the like in the preparation stage of gallium nitrate solution so as to promote the next stage of neutralizing and precipitating the gallium hydroxide; all three applications are based on the basic ideas of dissolution of gallium metal and neutralization of alkali to prepare gallium oxyhydroxide, and involve consumption of a large amount of acid, alkali and other reagents, so that the cost of the reagents is high, impurities are easy to introduce, the purity of the product is affected, acid and alkali cannot be recovered, and high-salt wastewater is difficult to treat.
The application of Chinese patent application No. 201210542115.4 discloses a method for preparing gallium oxyhydroxide by electrochemistry, wherein gallium metal is taken as an anode, three-stage electrolysis is carried out in alkaline electrolyte to obtain sodium gallate solution, and further neutralization, washing and drying are carried out to obtain gallium oxyhydroxide. Although the method can obtain a high-purity product, the method for obtaining the sodium gallate solution by electrolyzing the gallium metal has the advantages of long flow, complex operation, high energy consumption and poor economy.
The application of Chinese patent application No. 201210313080.7 discloses a preparation method of gallium hydroxide nanocrystals, which takes saturated benzene solution of gallium chloride and cetyltrimethylammonium bromide as raw materials, and the gallium hydroxide nanocrystals are successfully obtained by reacting for 10-18 hours at 160-200 ℃ in a high-pressure reaction kettle, but the method has high energy consumption, high requirements on equipment, easy production of organic wastewater which is difficult to treat and high environmental protection pressure.
The application of Chinese patent application Nos. 201910971014.0 and 201510835364.6 discloses a method for preparing gallium oxyhydroxide based on a short flow of hydrothermal reaction, gallium metal is used as a raw material to directly react with water to obtain gallium oxyhydroxide powder, but the reaction of gallium metal and water needs to be carried out under the conditions of high temperature and high pressure above 150 ℃, so that the energy consumption is high, high-cost pressure reaction equipment is needed, and liquid gallium cannot be sufficiently scattered and stirred in a mechanical stirring mode, so that the hydrothermal reaction is difficult to thoroughly proceed, and gallium oxyhydroxide powder materials with uniform morphology and size cannot be obtained.
In summary, the existing gallium oxyhydroxide preparation process still has a large space for optimization and improvement, and further development of a gallium oxyhydroxide preparation process technology which is simple to operate, short in flow, low in cost and environment-friendly is necessary, so that high-quality development of the fourth-generation semiconductor industry is supported.
Disclosure of Invention
The invention aims to solve the problems of long process flow, large reagent consumption, high equipment requirement, difficult standard reaching of product purity and physical specification and the like of the existing gallium oxyhydroxide preparation process, and provides a method for efficiently preparing gallium oxyhydroxide. The process technology has the characteristics of low equipment requirement, simple operation, low energy consumption, short flow, high efficiency, low cost and the like, and can realize the high-efficiency short-flow preparation of the high-purity gallium hydroxide powder material.
In order to achieve the technical purpose and the technical effect, the invention is realized by the following technical scheme:
a method for preparing gallium oxyhydroxide efficiently, under normal pressure, adds gallium metal into deionized water, and simultaneously blows oxygen or air into the system, under the condition of mechanical stirring, the gallium metal is converted into gallium oxyhydroxide, thus realizing the efficient short-flow preparation of high-purity gallium oxyhydroxide powder material.
Further, the method for efficiently preparing the gallium oxyhydroxide comprises the following specific process operations:
1) Adding gallium metal into deionized water according to a proportion;
2) Under the normal pressure condition, heating the system to a preset temperature, simultaneously blowing oxygen or air into the system, and converting the gallium metal into gallium oxyhydroxide under the mechanical stirring condition;
3) Filtering the obtained mixed slurry after the reaction is finished to realize solid-liquid separation;
4) And drying the filter residues to obtain the high-purity gallium hydroxide powder material.
Further, in the method for efficiently preparing the gallium oxyhydroxide as described above, in the step 1), the purity of the gallium metal is more than 4N, and the mass ratio of deionized water to the gallium metal is controlled to be 5-50:1.
Further, in the method for efficiently preparing the gallium oxyhydroxide, as described above, in the step 2), the reaction temperature is controlled to be 25-95 ℃, and the reaction time is controlled to be 2-12 hours.
Further, in the method for efficiently preparing gallium oxyhydroxide as described above, in the step 2), the bubbling speed of oxygen or air is controlled to be 1-20L/min.
Further, in the method for efficiently preparing the gallium oxyhydroxide as described above, in the step 2), the mechanical stirring speed is controlled to be 300-1200r/min.
Further, in the method for efficiently preparing the gallium oxyhydroxide as described above, in the step 3), the solid-liquid separation temperature is consistent with the chemical reaction temperature in the step 2), and the filter residues are washed with deionized water for 3-8 times.
Further, in the method for efficiently preparing the gallium oxyhydroxide as described above, in the step 4), the filter residue is dried for 12-48 hours at 120-180 ℃ to obtain the high-purity gallium oxyhydroxide powder material.
The beneficial effects of the invention are as follows:
1. according to the invention, the high-purity gallium hydroxide powder material is prepared by taking gallium, deionized water and oxygen or air as raw materials through a gas-liquid reaction in one step, so that the process is short, the efficiency is high, no chemical reagents such as acid, alkali and the like are required to be consumed, the risk of introducing impurities into the raw materials is greatly reduced, the high-purity product is facilitated to be obtained, the production process is environment-friendly, and the production cost is low.
2. The invention takes deionized water as a reaction medium, and generates the gallium hydroxide by directly reacting with liquid gallium through blowing oxygen or air, thereby greatly strengthening the thermodynamic and kinetic conditions of the reaction. Compared with the traditional gallium hydrothermal reaction without introducing oxygen/air, the initial temperature of the generated gallium hydroxide is reduced from the original temperature of >150 ℃ (preferably more than 200 ℃) to the temperature below the boiling point of water (< 100 ℃), so that the reaction can be carried out under normal pressure, the energy consumption required by the reaction is greatly reduced, high-pressure reaction equipment with higher investment and maintenance cost is not required, the production cost can be effectively reduced, and the economic benefit of a production enterprise is improved.
3. According to the invention, the conversion process of family gallium to gallium oxyhydroxide is enhanced by blowing oxygen/air and mechanical stirring, so that the temperature and pressure required by the reaction can be effectively reduced, liquid gallium can be fully dispersed and stirred in the reaction process to form highly dispersed nano gallium metal particles with uniform size, the particles are high in surface activity and large in reactivity, the reaction process is efficiently and thoroughly carried out, and gallium oxyhydroxide powder with uniform micro morphology and particle size can be formed, so that the gallium oxyhydroxide precursor for producing the fourth-generation semiconductor material, which meets the requirements on chemical purity and physical specification, is finally obtained, and the high-efficiency short-process preparation of high-purity gallium oxyhydroxide is realized.
Of course, it is not necessary for any one product to practice the invention to achieve all of the advantages set forth above at the same time.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention discloses a method for efficiently preparing gallium oxyhydroxide, which comprises the steps of adding gallium metal into deionized water under normal pressure, simultaneously blowing oxygen or air into a system, and converting the gallium metal into gallium oxyhydroxide under the condition of mechanical stirring. The technical scheme of the invention has the characteristics of low equipment requirement, simple operation, low energy consumption, short flow, high efficiency, low cost and the like, and can realize the high-efficiency short-flow preparation of the high-purity gallium hydroxide powder material.
The production process specifically comprises the following steps:
1) Adding metal gallium with the purity of more than 4N into deionized water in proportion, and controlling the mass ratio of the deionized water to the metal gallium to be between 2:1 and 15:1.
2) Under normal pressure, the system is heated to 25-95 ℃, oxygen or air is blown into the system at the speed of 1-20L/min, and the reaction is carried out for 2-12h under the condition of mechanical stirring with the rotating speed of 300-1200r/min, so that the gallium metal is converted into gallium hydroxide.
3) After the reaction is finished, filtering the obtained mixed slurry at the temperature of 25-95 ℃ which is consistent with the temperature of the previous reaction step, realizing solid-liquid separation, and washing filter residues with deionized water for 3-8 times.
4) Drying the filter residue at 120-180 ℃ for 12-48h to obtain the high-purity gallium hydroxide powder material.
The invention is further described below in connection with specific embodiments.
Example 1
The embodiment provides a method for efficiently preparing gallium oxyhydroxide, which specifically comprises the following steps:
1) And adding the metal gallium with the purity of 4N into deionized water according to a proportion, and controlling the mass ratio of the deionized water to the metal gallium to be 2:1.
2) Under normal pressure, the system is heated to 25 ℃, oxygen is blown into the system at the speed of 1L/min, and the reaction is carried out for 12 hours under the condition of mechanical stirring with the rotating speed of 300r/min, so that the gallium metal is converted into gallium hydroxide.
3) After the reaction is finished, filtering the obtained mixed slurry at the temperature of 25 ℃ to realize solid-liquid separation, and washing filter residues with deionized water for 3 times.
4) And drying the filter residue at 120 ℃ for 48 hours to obtain the high-purity gallium hydroxide powder material.
By adopting the treatment method of the embodiment, the conversion rate and the product purity of the gallium oxyhydroxide are analyzed by combining aqua regia dissolution with inductively coupled plasma mass spectrometry (ICP-MS), and the result is that the conversion rate of gallium metal to gallium oxyhydroxide is 99.71%, and the product purity of gallium oxyhydroxide is 99.995%.
Example 2
The embodiment provides a method for efficiently preparing gallium oxyhydroxide, which specifically comprises the following steps:
1) And adding the gallium with the purity of 4N into deionized water according to a proportion, and controlling the mass ratio of the deionized water to the gallium to be 15:1.
2) Under normal pressure, the system is heated to 95 ℃, air is blown into the system at the speed of 20L/min, and the reaction is carried out for 2 hours under the condition of mechanical stirring with the rotating speed of 1200r/min, so that the gallium metal is converted into gallium hydroxide.
3) After the reaction is finished, filtering the obtained mixed slurry at the temperature of 95 ℃ to realize solid-liquid separation, and washing filter residues with deionized water for 8 times.
4) And drying the filter residue at 180 ℃ for 12 hours to obtain the high-purity gallium hydroxide powder material.
By adopting the treatment method of the embodiment, the conversion rate and the product purity of the gallium oxyhydroxide are analyzed by combining aqua regia dissolution with inductively coupled plasma mass spectrometry (ICP-MS), and the result is that the conversion rate of gallium metal to gallium oxyhydroxide is 99.53%, and the product purity of gallium oxyhydroxide is 99.998%.
Example 3
The embodiment provides a method for efficiently preparing gallium oxyhydroxide, which specifically comprises the following steps:
1) And adding the metal gallium with the purity of 4N into deionized water according to a proportion, and controlling the mass ratio of the deionized water to the metal gallium to be 4:1.
2) Under normal pressure, the system is heated to 45 ℃, oxygen is blown into the system at the speed of 5L/min, and the reaction is carried out for 4 hours under the condition of mechanical stirring with the rotating speed of 450r/min, so that the gallium metal is converted into gallium hydroxide.
3) After the reaction is finished, filtering the obtained mixed slurry at the temperature of 45 ℃ to realize solid-liquid separation, and washing filter residues with deionized water for 4 times.
4) And drying the filter residue at 130 ℃ for 18 hours to obtain the high-purity gallium hydroxide powder material.
By adopting the treatment method of the embodiment, the conversion rate and the product purity of the gallium oxyhydroxide are analyzed by combining aqua regia dissolution with inductively coupled plasma mass spectrometry (ICP-MS), and the result is that the conversion rate of gallium metal to gallium oxyhydroxide is 99.23%, and the product purity of gallium oxyhydroxide is 99.996%.
Example 4
The embodiment provides a method for efficiently preparing gallium oxyhydroxide, which specifically comprises the following steps:
1) And adding the metal gallium with the purity of 4N into deionized water according to a proportion, and controlling the mass ratio of the deionized water to the metal gallium to be 8:1.
2) Under normal pressure, the system is heated to 55 ℃, air is blown into the system at the speed of 10L/min, and the metal gallium is converted into gallium hydroxide under the condition of mechanical stirring with the rotating speed of 600r/min for 8 hours.
3) After the reaction is finished, filtering the obtained mixed slurry at the temperature of 55 ℃ to realize solid-liquid separation, and washing filter residues with deionized water for 5 times.
4) And drying the filter residue at 140 ℃ for 24 hours to obtain the high-purity gallium hydroxide powder material.
By adopting the treatment method of the embodiment, the conversion rate and the product purity of the gallium oxyhydroxide are analyzed by combining aqua regia dissolution with inductively coupled plasma mass spectrometry (ICP-MS), and the result is that the conversion rate of gallium metal to gallium oxyhydroxide is 99.37 percent and the product purity of gallium oxyhydroxide is 99.997 percent.
Example 5
The embodiment provides a method for efficiently preparing gallium oxyhydroxide, which specifically comprises the following steps:
1) And adding the metal gallium with the purity of 4N into deionized water according to a proportion, and controlling the mass ratio of the deionized water to the metal gallium to be 12:1.
2) Under normal pressure, the system is heated to 70 ℃, oxygen is blown into the system at the speed of 15L/min, and the reaction is carried out for 10 hours under the condition of mechanical stirring with the rotating speed of 800r/min, so that the gallium metal is converted into gallium hydroxide.
3) After the reaction is finished, filtering the obtained mixed slurry at the temperature of 70 ℃ to realize solid-liquid separation, and washing filter residues with deionized water for 6 times.
4) And drying the filter residue at 160 ℃ for 36 hours to obtain the high-purity gallium hydroxide powder material.
By adopting the treatment method of the embodiment, the conversion rate and the product purity of the gallium oxyhydroxide are analyzed by combining aqua regia dissolution with inductively coupled plasma mass spectrometry (ICP-MS), and the result is that the conversion rate of gallium metal to gallium oxyhydroxide is 99.42%, and the product purity of gallium oxyhydroxide is 99.996%.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (8)
1. A method for efficiently preparing gallium oxyhydroxide is characterized in that: under normal pressure, adding gallium metal into deionized water, and simultaneously blowing oxygen or air into the system, and converting the gallium metal into gallium oxyhydroxide under the condition of mechanical stirring, thereby realizing the efficient short-flow preparation of the high-purity gallium oxyhydroxide powder material.
2. The method for efficiently preparing gallium oxyhydroxide according to claim 1, wherein: the specific process comprises the following steps:
1) Adding gallium metal into deionized water according to a proportion;
2) Under the normal pressure condition, heating the system to a preset temperature, simultaneously blowing oxygen or air into the system, and converting the gallium metal into gallium oxyhydroxide under the mechanical stirring condition;
3) Filtering the obtained mixed slurry after the reaction is finished to realize solid-liquid separation;
4) And drying the filter residues to obtain the high-purity gallium hydroxide powder material.
3. The method for efficiently preparing gallium oxyhydroxide according to claim 2, wherein: in the step 1), the purity of the gallium is more than 4N, and the mass ratio of the deionized water to the gallium is controlled to be 5-50:1.
4. The method for efficiently preparing gallium oxyhydroxide according to claim 2, wherein: in the step 2), the reaction temperature is controlled to be 25-95 ℃ and the reaction time is controlled to be 2-12h.
5. The method for efficiently preparing gallium oxyhydroxide according to claim 2, wherein: in the step 2), the bubbling speed of oxygen or air is controlled to be 1-20L/min.
6. The method for efficiently preparing gallium oxyhydroxide according to claim 2, wherein: in the step 2), the mechanical stirring speed is controlled to be 300-1200r/min.
7. The method for efficiently preparing gallium oxyhydroxide according to claim 2, wherein: in the step 3), the solid-liquid separation temperature is consistent with the chemical reaction temperature in the step 2), and filter residues are washed with deionized water for 3-8 times.
8. The method for efficiently preparing gallium oxyhydroxide according to claim 2, wherein: in the step 4), the filter residue is dried for 12-48 hours at the temperature of 120-180 ℃ to obtain the high-purity gallium hydroxide powder material.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011144080A (en) * | 2010-01-15 | 2011-07-28 | Sumitomo Chemical Co Ltd | Method for producing gallium oxide |
| CN102786078A (en) * | 2012-08-29 | 2012-11-21 | 吉林大学 | Preparation method of hydroxyl gallium oxide nanometer crystal |
| CN102976393A (en) * | 2012-12-06 | 2013-03-20 | 吉林大学 | Preparation method of gallium oxide hydroxide nano-crystals |
| CN106744730A (en) * | 2015-11-19 | 2017-05-31 | 上饶师范学院 | Gallium oxide, gallium nitride nano-powder are prepared by raw material two-step method of gallium |
| CN108046311A (en) * | 2017-12-25 | 2018-05-18 | 清远先导材料有限公司 | The preparation method of high-purity gallium oxide |
| CN110627112A (en) * | 2019-10-12 | 2019-12-31 | 成都中建材光电材料有限公司 | Preparation method and preparation device of high-purity gallium oxide |
-
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- 2023-02-03 CN CN202310054518.2A patent/CN116199251B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011144080A (en) * | 2010-01-15 | 2011-07-28 | Sumitomo Chemical Co Ltd | Method for producing gallium oxide |
| CN102786078A (en) * | 2012-08-29 | 2012-11-21 | 吉林大学 | Preparation method of hydroxyl gallium oxide nanometer crystal |
| CN102976393A (en) * | 2012-12-06 | 2013-03-20 | 吉林大学 | Preparation method of gallium oxide hydroxide nano-crystals |
| CN106744730A (en) * | 2015-11-19 | 2017-05-31 | 上饶师范学院 | Gallium oxide, gallium nitride nano-powder are prepared by raw material two-step method of gallium |
| CN108046311A (en) * | 2017-12-25 | 2018-05-18 | 清远先导材料有限公司 | The preparation method of high-purity gallium oxide |
| CN110627112A (en) * | 2019-10-12 | 2019-12-31 | 成都中建材光电材料有限公司 | Preparation method and preparation device of high-purity gallium oxide |
Non-Patent Citations (2)
| Title |
|---|
| YUJ IE DING ET AL.: "Bulk Expansion Effect of Gallium-Based Thermal Interface Material", INT J THERMOPHYS, 27 May 2017 (2017-05-27), pages 1 - 10 * |
| 马超;李宇兴;赖永勤;李学如;: "纳米氧化镓的制备及其抗菌活性的研究", 化学与生物工程, no. 09, 25 September 2015 (2015-09-25) * |
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