CN1762825A - Gallium nitrate preparation method - Google Patents
Gallium nitrate preparation method Download PDFInfo
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- CN1762825A CN1762825A CN 200510098704 CN200510098704A CN1762825A CN 1762825 A CN1762825 A CN 1762825A CN 200510098704 CN200510098704 CN 200510098704 CN 200510098704 A CN200510098704 A CN 200510098704A CN 1762825 A CN1762825 A CN 1762825A
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- China
- Prior art keywords
- solution
- gallium
- gallium nitrate
- crystal
- nitric acid
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- 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 title claims abstract description 68
- 229940044658 gallium nitrate Drugs 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000013078 crystal Substances 0.000 claims abstract description 45
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 32
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 22
- 238000001704 evaporation Methods 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000002425 crystallisation Methods 0.000 claims description 10
- 230000008025 crystallization Effects 0.000 claims description 10
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 9
- 238000001816 cooling Methods 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000007605 air drying Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 6
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 229910001195 gallium oxide Inorganic materials 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 4
- 239000012498 ultrapure water Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 1
- JJBNCYLBHKHXAH-UHFFFAOYSA-N O.O.O.[Ga] Chemical compound O.O.O.[Ga] JJBNCYLBHKHXAH-UHFFFAOYSA-N 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229910021513 gallium hydroxide Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 208000030208 low-grade fever Diseases 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The present invention relates to gallium nitrate preparing process. The preparation process includes: dissolving 6N metal gallium in high purity nitric acid at 50-80 deg.c, evaporating the solution at 80-100 deg.c until no bad smell of nitric acid, cooling the solution to -20 deg.c to 0 deg.c, adding gallium nitrate crystal seed into the solution with the weight ratio between the added gallium nitrate crystal seed and gallium nitrate inside the solution being 0.01-0.1, separating crystal, filtering to separate gallium nitrate crystal hydrate, and air drying to obtain gallium nitrate crystal. Owing to the controlled acid dissolving and separation, the process has shortened acid dissolving time and crystal separating time, effectively raised production efficiency, simple operation and easy embodiment. Owing to the high purity of the material, the product has high purity up to 4N.
Description
Technical field
The present invention relates to a kind of preparation method of gallium nitrate.
Background technology
About the preparation technology of gallium nitrate, document announcement is less.In that " mineral compound synthesizes in the handbook (Japanization association compile, translate in the coltfoal of settling down, old river, Chemical Industry Press, 1986), and disclosed gallium nitrate preparation method has two kinds.Method one is that gallium or Gallium trioxide are dissolved in the nitric acid, and evaporating solns after concentrating, adds water.Carry out this operation repeatedly, in solution till the stink of no nitric acid.Dilute strong solution then and to 100ml solution, contain gallium 26g.From then on can separate out Ga (NO in the viscous soln
3)
3XH
2The solid of O.Behind the suction strainer, leave standstill a moment.Drying is carried out in crystallization in drying air stream, then,, promptly get anhydride under room temperature 40 ℃ of dryings 2 days.
Method two: gallium or gallium hydroxide are dissolved in the concentrated nitric acid of heat, again solution are put coldly, can make the granular crystal of eight hydrates.
In above-mentioned sour molten technology, when Gallium trioxide was dissolved in concentrated nitric acid at normal temperatures, dissolving is difficulty very.Following and the nitric acid reaction of gallium normal temperature, the surface generates one deck oxide passivation film, can stop the further reaction of gallium and nitric acid, sour molten difficulty.And comparatively difficulty is separated out in the aforesaid method crystallization, and it is longer that the time is separated out in crystallization, and preparation cycle is long.
Summary of the invention
Purpose of the present invention is exactly the deficiency that exists at above-mentioned prior art, provides a kind of and can effectively shorten the sour molten time and the time is separated out in crystallization, improves the preparation method of the gallium nitrate of product purity.
The objective of the invention is to be achieved through the following technical solutions.
A kind of preparation method of gallium nitrate, it is characterized in that preparation process is followed successively by: the 6N gallium is dissolved in 50～80 ℃ high pure nitric acid, after dissolving is finished, solution is filtered, under 80～100 ℃ of temperature, add water evaporating surplus nitric acid cleansing soln again, again solution is cooled to 0～-20 ℃, in cooled solution, add the gallium nitrate crystal seed, wherein the seed ratio of gallium nitrate weight ratio is 0.01～0.1 in crystal seed and the solution, after crystallization is separated out, separate after filtration, obtain nitric hydrate gallium crystal, through the air-dry gallium nitrate crystal that gets.
A kind of preparation method of gallium nitrate is characterized in that preparation process is the α-Ga with 5N
2O
3Add down at 60～95 ℃ and press nitric acid: the nitric acid preparation dissolving of the dilution proportion of water=1: 1～1: 2 prepares gallium nitrate solution.
Method of the present invention is selected α-Ga for use
2O
3, under 60～95 ℃, being dissolved in rare nitric acid of low-grade fever, the sour molten time is shorter, and 1 hour is that solubilized is complete.
Method of the present invention is separated out technology because employing adds crystal seed, has shortened inductive phase, has quickened the product speed of separating out, and behind the adding crystal seed, 15～30min can separate out crystal.If do not add crystal seed, the time of separating out is the longest to reach 10 days～30 days.The crystal seed of this technology time of separating out obviously shortens; Because raw materials used is commercial highly purified high purity reagent and high purity water, and in preparation process, the solution after the acid dissolving is filtered cleansing soln.The purity of prepared product is higher, can reach more than the 4N.
Description of drawings
Fig. 1 is the process flow sheet of method of the present invention.
Embodiment
A kind of preparation method of gallium nitrate, its preparation process is followed successively by: a. prepares gallium nitrate solution: the 6N gallium is dissolved in 50～80 ℃ high pure nitric acid or with 5N α-Ga
2O
3Under 60～95 ℃, be dissolved in nitric acid: in rare nitric acid of water=1: 1～1: 2, treat the dissolving fully of gallium or gallium oxide after, solution is filtered, make gallium nitrate solution; B. the redundant nitric acid in the evaporating solution: add high purity water in solution, evaporating solns under 80～100 ℃ of temperature carries out this operation repeatedly, till the no nitric acid stink, solution is cooled to 0～-20 ℃ to the solution again; C. crystallization is separated out: add the gallium nitrate crystal seed in cooled solution, wherein the seed ratio of gallium nitrate weight ratio is 0.01～0.1 in crystal seed and the solution, separates out the gallium nitrate crystal from solution; D. product is air-dry: after crystallization is separated out, filtering separation, through 30～40 ℃ after air-dry 1～2 day, the gallium nitrate crystal.
Embodiment 1
Gallium is dissolved in 50 ℃ of concentrated nitric acids of heat, treat that the gallium dissolving finishes, evaporating solns, keep temperature of reaction at 100 ℃, add water after concentrating, concentrate repeatedly, be evaporated to till the stink of no nitric acid in the solution, cooling solution adds crystal seed simultaneously to-20 ℃, contains the gallium nitrate weight ratio in the crystal seed weight of adding and the solution, be that the crystal seed coefficient is 0.03, carry out seed and stir decomposition, can make nitric hydrate gallium crystal through separating, air-dry 2 days through 30 ℃, adopt the ICP-MS analysis and detection technology, quality product can reach more than 99.99%.
Embodiment 2
With gallium be dissolved in 65 ℃ hot concentrated in, treat that gallium dissolving finishes evaporating solns, keep temperature of reaction about 90 ℃, solution is little boils in control, after concentrating, add water, be concentrated into till the stink of no nitric acid in the solution, cooling solution to 0 ℃ adds crystal seed (the crystal seed coefficient is 0.01) simultaneously and carries out seed and stir and decompose, can make nitric hydrate gallium crystal through separating, through 40 ℃ air-dry 1 day, adopt the ICP-MS analysis and detection technology, quality product can reach more than 99.99%.
Embodiment 3
Adopt high purity water and high purity reagent to carry out preparation of raw material, and the suitable sour molten and crystallization condition of control: gallium is dissolved in 85 ℃ hot concentrated, treat that the gallium dissolving finishes, evaporating solns, keep temperature of reaction at 80 ℃, after concentrating, add water, be concentrated into till the stink of no nitric acid in the solution, cool off this solution-10 ℃, add crystal seed (the crystal seed coefficient is 0.05) simultaneously and carry out seed and stir and decompose, can make nitric hydrate gallium crystal through separating, through 40 ℃ air-dry 2 days, adopt the ICP-MS analysis and detection technology, quality product can reach more than 99.99%.
Embodiment 4
Adopt high purity water and high purity reagent to carry out preparation of raw material, and the suitable sour molten and crystallization condition of control: Gallium trioxide is dissolved in rare nitric acid of 1: 1 and heats, under 85 ℃ of temperature, dissolve, treat that the gallium oxide dissolving finishes, evaporating solns, control 85 ℃, after concentrating, add water, be concentrated into repeatedly till the stink of no nitric acid in the solution, cooling solution-5 ℃, add crystal seed (the crystal seed coefficient is 0.08) simultaneously and carry out seed stirring decomposition, can make nitric hydrate gallium crystal through separating, air-dry 1 day through 35 ℃, adopt the ICP-MS analysis and detection technology, quality product can reach more than 99.99%.
Embodiment 5
Gallium trioxide is added by nitric acid: the volume ratio of water is in the nitric acid of 1: 2 dilution proportion, being heated to 60 ℃ dissolves, treat that the gallium oxide dissolving finishes, control reaction temperature is at 95 ℃ of evaporating solnss, add water after concentrating, repeatedly to the solution till the stink of no nitric acid, stop the heating cooling, add gallium nitrate crystal crystal seed simultaneously, carry out seed and stir decomposition, can make nitric hydrate gallium crystal through separating, contain the gallium nitrate weight ratio in crystal seed amount that adds and the solution, promptly the crystal seed coefficient is 0.10, and is air-dry 2 days through 35 ℃, adopt the ICP-MS analysis and detection technology, quality product can reach more than 99.99%.
Embodiment 6
Gallium trioxide is dissolved in 1: 1 by volume to be heated to temperature of reaction and to dissolve for 95 ℃ in the nitric acid after the dilution, the gallium oxide dissolving finishes, evaporating solns, control reaction temperature is at 100 ℃, add water after concentrating, be concentrated into till the stink of no nitric acid in the solution, cool off this solution, add crystal seed simultaneously, the crystal seed coefficient is 0.06, carries out seed and stirs decomposition, can make nitric hydrate gallium crystal through separating, through 40 ℃ air-dry 1 day, adopt the ICP-MS analysis and detection technology, quality product can reach more than 99.99%.
Claims (2)
1. the preparation method of a gallium nitrate, it is characterized in that preparation process is followed successively by: the 6N gallium is dissolved in 50～80 ℃ high pure nitric acid, after dissolving is finished, solution is filtered, under 80～100 ℃ of temperature, add water evaporating surplus nitric acid cleansing soln again, again solution is cooled to 0～-20 ℃, in cooled solution, add the gallium nitrate crystal seed, wherein the seed ratio of gallium nitrate weight ratio is 0.01～0.1 in crystal seed and the solution, after crystallization is separated out, separate after filtration, obtain nitric hydrate gallium crystal, through the air-dry gallium nitrate crystal that gets.
2. the preparation method of a kind of gallium nitrate according to claim 1 is characterized in that preparation process is the α-Ga with 5N
2O
3Add down at 60～95 ℃ and press nitric acid: the nitric acid preparation dissolving of the dilution proportion of water=1: 1～1: 2 prepares gallium nitrate solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510098704 CN1762825A (en) | 2005-09-07 | 2005-09-07 | Gallium nitrate preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510098704 CN1762825A (en) | 2005-09-07 | 2005-09-07 | Gallium nitrate preparation method |
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| Publication Number | Publication Date |
|---|---|
| CN1762825A true CN1762825A (en) | 2006-04-26 |
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ID=36747191
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|---|---|---|---|
| CN 200510098704 Pending CN1762825A (en) | 2005-09-07 | 2005-09-07 | Gallium nitrate preparation method |
Country Status (1)
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|---|---|
| CN (1) | CN1762825A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102963923A (en) * | 2012-11-28 | 2013-03-13 | 南京金美镓业有限公司 | Large-scale production method for preparing gallium nitrate by using gallium |
| JP2014019590A (en) * | 2012-07-13 | 2014-02-03 | Dowa Electronics Materials Co Ltd | Method for manufacturing aqueous gallium nitrate solution |
| CN107973336A (en) * | 2017-12-25 | 2018-05-01 | 清远先导材料有限公司 | The preparation method of gallium nitrate solution |
-
2005
- 2005-09-07 CN CN 200510098704 patent/CN1762825A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014019590A (en) * | 2012-07-13 | 2014-02-03 | Dowa Electronics Materials Co Ltd | Method for manufacturing aqueous gallium nitrate solution |
| CN102963923A (en) * | 2012-11-28 | 2013-03-13 | 南京金美镓业有限公司 | Large-scale production method for preparing gallium nitrate by using gallium |
| CN102963923B (en) * | 2012-11-28 | 2015-04-15 | 南京金美镓业有限公司 | Large-scale production method for preparing gallium nitrate by using gallium |
| CN107973336A (en) * | 2017-12-25 | 2018-05-01 | 清远先导材料有限公司 | The preparation method of gallium nitrate solution |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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