CN109437283A - A kind of nanometer titanium dioxide germanium production technology new process - Google Patents
A kind of nanometer titanium dioxide germanium production technology new process Download PDFInfo
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- CN109437283A CN109437283A CN201811398986.7A CN201811398986A CN109437283A CN 109437283 A CN109437283 A CN 109437283A CN 201811398986 A CN201811398986 A CN 201811398986A CN 109437283 A CN109437283 A CN 109437283A
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- germanium
- titanium dioxide
- production technology
- nanometer titanium
- new process
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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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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of germanium dioxide production technologies, more particularly to a kind of nanometer titanium dioxide germanium production technology new process, include the following steps: to be put into ammonium hydroxide and distilled water in agitator tank, and heating stirring, germanium tetrachloride powder is added in agitator tank in whipping process, is heated and is stirred in agitator tank；It keeps stirring during heating, germanium tetrachloride is reacted with ammonium hydroxide and distilled water, generate germanic acid radical ion aqueous solution, after the solution of homogeneous transparent to be formed, stop heating, compared with prior art, the beneficial effects of the present invention are: by mix, react, cooling down and etc. processed, and additive is added in process, the crystal of precipitation is purer, avoids impurity.
Description
Technical field
The present invention relates to a kind of germanium dioxide production technologies, and in particular to a kind of new work of nanometer titanium dioxide germanium production technology
Skill.
Background technique
Germanium dioxide is the dioxide of germanium, and electronic type is identical as carbon dioxide, is white powder or colourless crystallization, has
Slightly be dissolved in water hexagonal crystal system (low-temperature stabilization) and two kinds of insoluble tetragonal system, transition temperature be 1033 DEG C, be mainly used for
Germanium metal processed also serves as spectrum analysis and semiconductor material.
Germanium dioxide is tetragonal crystal system, hexagonal crystal system or amorphous body.Six sides crystallization and β-quartz isomorphism, germanium are matched for four
Position, four directions crystallization have stipoverite type structure, are similar to rutile, and wherein germanium is hexa-coordinate.Under high pressure, amorphous germanium dioxide
It is changed into hexa-coordinate structure；With pressure reduction, germanium dioxide also gradually becomes the structure of four-coordination, class Rutile structure
Germanium dioxide can be changed into another rhombic system chloride-calcium type structure under high pressure.
Existing germanium dioxide processing is cumbersome, and is easy to mix the more impurity of dye, therefore, the crystalline substance of precipitation when crystal is precipitated
Body needs to process essence again.
Therefore, a kind of new nanometer titanium dioxide germanium production technology new process is developed, not only there is urgent researching value, also have
There are good economic benefit and commercial application potentiality, where this power exactly of the invention being accomplished and basis.
Summary of the invention
In order to overcome the defect of the prior art as indicated above, the present inventor has made intensive studies this, is paying
After a large amount of creative works, so as to complete the present invention.
Specifically, the technical problems to be solved by the present invention are: providing a kind of new work of nanometer titanium dioxide germanium production technology
Skill processes cumbersome technical problem to solve existing germanium dioxide.
To achieve the above object, the invention provides the following technical scheme:
A kind of nanometer titanium dioxide germanium production technology new process, includes the following steps:
(1) it mixes
It is put into ammonium hydroxide and distilled water, and heating stirring in agitator tank, germanium tetrachloride powder is added in whipping process
In agitator tank, is heated and stirred in agitator tank；
(2) it reacts
It keeping stirring during heating, germanium tetrachloride is reacted with ammonium hydroxide and distilled water, germanic acid radical ion aqueous solution is generated,
After the solution of homogeneous transparent to be formed, stop heating；
(3) cooling
Germanic acid radical ion aqueous solution is poured out to container, and places and cools down indoors, until being cooled to room temperature, or is used
Cooling device is cooled to room temperature；
(4) additive is prepared
Lysine water-soluble glue is prepared using sol-gel technique；
(5) it is precipitated
After germanic acid radical ion aqueous solution is cooled to room temperature, lysine water-soluble glue is added, heats and stirs, germanic acid radical ion
For germanium tetrachloride in aqueous solution under the action of ammonium ion and lysine, hydrolysis rapidly in water, unformed germanium oxide is certainly
Hair aggregation roughening, recrystallization form crystal；
(6) dry
Gained crystal and amorphous liquid solution are placed on drying in drying box, obtain dry solidifying crystal, dry will coagulate crystal in sky
Atmosphere bakes 1 hour in enclosing, and is ground to obtain a nanometer GeO2Powder.
In the present invention, as an improvement, the mass percent that ammonium hydroxide is added in the step (1) is 3-6%, described
The mass percent of distilled water is 94-97%.
In the present invention, as an improvement, the heating temperature that agitator tank stirs in the step (1) is 60-80 DEG C.
In the present invention, as an improvement, the stirring duration in the step (5) is greater than 10 minutes.
In the present invention, as an improvement, the drying temperature of drying box is controlled at 50-55 DEG C in the step (6).
In the present invention, as an improvement, maturing temperature is 550-600 DEG C in the step (6).
In the present invention, as an improvement, in the step (4) in lysine water-soluble glue lysine mass percent
For 15%-20%.
In the present invention, as an improvement, the oxidation germanium solution of the amorphousness continues to be precipitated in the drying process
Crystal habit.
Compared with prior art, the beneficial effects of the present invention are:
(1) by mix, react, cooling down and etc. processed, and additive is added in process, the crystalline substance of precipitation
Body is purer, avoids impurity.
(2) crystal obtained after the reaction was completed is dry by drying steps, and germanium dioxide powder, processing step are obtained after dry
It is rapid simple and more efficient.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described.In all the appended drawings, similar element
Or part is generally identified by similar appended drawing reference.In attached drawing, each element or part might not be drawn according to actual ratio.
Fig. 1 is process flow chart of the invention；
Specific embodiment
It is described in detail below in conjunction with embodiment of the attached drawing to technical solution of the present invention.Following embodiment is only used for
Clearly illustrate technical solution of the present invention, therefore be only used as example, and cannot be used as a limitation and limit protection model of the invention
It encloses.
Embodiment one: as shown in Figure 1, a kind of nanometer titanium dioxide germanium production technology new process, includes the following steps:
(1) it mixes
It is put into the distilled water that mass percent is 3% ammonium hydroxide and mass percent is 97% in agitator tank, and heats and stirs
It mixes, the germanium tetrachloride powder that mass percent is 3% is added in agitator tank in whipping process, is heated in agitator tank
And stirring, the heating temperature of the agitator tank stirring is 60 DEG C；
(2) it reacts
It keeping stirring during heating, germanium tetrachloride is reacted with ammonium hydroxide and distilled water, germanic acid radical ion aqueous solution is generated,
After the solution of homogeneous transparent to be formed, stop heating；
(3) cooling
Germanic acid radical ion aqueous solution is poured out to container, and places and cools down indoors, until being cooled to room temperature, or is used
Cooling device is cooled to room temperature；
(4) additive is prepared
Lysine water-soluble glue is prepared using sol-gel technique, the mass percent of lysine is in lysine water-soluble glue
15%；
(5) it is precipitated
After germanic acid radical ion aqueous solution is cooled to room temperature, the hydrosol that lysine mass fraction is 15% is added, heating
And stir, stirring duration is greater than 10 minutes, and the germanium tetrachloride in germanic acid radical ion aqueous solution is in ammonium ion and the work of lysine
Under, hydrolysis rapidly in water, unformed germanium oxide self-assemble roughening recrystallizes and forms crystal；
(6) dry
Gained crystal and amorphous liquid solution are placed on drying in drying box, the drying temperature of drying box is controlled at 50 DEG C,
Dry solidifying crystal is obtained, dry solidifying crystal is baked 1 hour in air atmosphere, maturing temperature is 550 DEG C, and is ground and received
Rice GeO2Powder.
Embodiment two: a kind of nanometer titanium dioxide germanium production technology new process includes the following steps:
(1) it mixes
It is put into the distilled water that mass percent is 6% ammonium hydroxide and mass percent is 94% in agitator tank, and heats and stirs
It mixes, the germanium tetrachloride powder that mass percent is 6% is added in agitator tank in whipping process, is heated in agitator tank
And stirring, the heating temperature of the agitator tank stirring is 65 DEG C；
(2) it reacts
It keeping stirring during heating, germanium tetrachloride is reacted with ammonium hydroxide and distilled water, germanic acid radical ion aqueous solution is generated,
After the solution of homogeneous transparent to be formed, stop heating；
(3) cooling
Germanic acid radical ion aqueous solution is poured out to container, and places and cools down indoors, until being cooled to room temperature, or is used
Cooling device is cooled to room temperature；
(4) additive is prepared
Lysine water-soluble glue is prepared using sol-gel technique, the mass percent of lysine is in lysine water-soluble glue
15%；
(5) it is precipitated
After germanic acid radical ion aqueous solution is cooled to room temperature, the hydrosol that lysine mass fraction is 20% is added, heating
And stir, stirring duration is greater than 10 minutes, and the germanium tetrachloride in germanic acid radical ion aqueous solution is in ammonium ion and the work of lysine
Under, hydrolysis rapidly in water, unformed germanium oxide self-assemble roughening recrystallizes and forms crystal；
(6) dry
Gained crystal and amorphous liquid solution are placed on drying in drying box, the drying temperature of drying box is controlled at 55 DEG C,
Dry solidifying crystal is obtained, dry solidifying crystal is baked 1 hour in air atmosphere, maturing temperature is 600 DEG C, and is ground and received
Rice GeO2Powder.
Embodiment three: a kind of nanometer titanium dioxide germanium production technology new process includes the following steps:
(1) it mixes
It is put into the distilled water that mass percent is 4.5% ammonium hydroxide and mass percent is 95.5% in agitator tank, and adds
The germanium tetrachloride powder that mass percent is 5% is added in agitator tank in whipping process, carries out in agitator tank by thermal agitation
The heating temperature of heating and stirring, the agitator tank stirring is 63 DEG C；
(2) it reacts
It keeping stirring during heating, germanium tetrachloride is reacted with ammonium hydroxide and distilled water, germanic acid radical ion aqueous solution is generated,
After the solution of homogeneous transparent to be formed, stop heating；
(3) cooling
Germanic acid radical ion aqueous solution is poured out to container, and places and cools down indoors, until being cooled to room temperature, or is used
Cooling device is cooled to room temperature；
(4) additive is prepared
Lysine water-soluble glue is prepared using sol-gel technique, the mass percent of lysine is in lysine water-soluble glue
15%；
(5) it is precipitated
After germanic acid radical ion aqueous solution is cooled to room temperature, the hydrosol that lysine mass fraction is 17% is added, heating
And stir, stirring duration is greater than 10 minutes, and the germanium tetrachloride in germanic acid radical ion aqueous solution is in ammonium ion and the work of lysine
Under, hydrolysis rapidly in water, unformed germanium oxide self-assemble roughening recrystallizes and forms crystal；
(6) dry
Gained crystal and amorphous liquid solution are placed on drying in drying box, the drying temperature of drying box is controlled at 53 DEG C,
Dry solidifying crystal is obtained, dry solidifying crystal is baked 1 hour in air atmosphere, maturing temperature is 580 DEG C, and is ground and received
Rice GeO2Powder.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme should all cover within the scope of the claims and the description of the invention.
Claims (8)
1. a kind of nanometer titanium dioxide germanium production technology new process, which comprises the steps of:
(1) it mixes
It is put into ammonium hydroxide and distilled water, and heating stirring in agitator tank, germanium tetrachloride powder is added in whipping process and is stirred
In tank, is heated and stirred in agitator tank；
(2) it reacts
It keeps stirring during heating, germanium tetrachloride is reacted with ammonium hydroxide and distilled water, germanic acid radical ion aqueous solution is generated, to shape
After the solution of homogeneous transparent, stop heating；
(3) cooling
Germanic acid radical ion aqueous solution is poured out to container, and places and cools down indoors, until being cooled to room temperature, or using cooling
Device is cooled to room temperature；
(4) additive is prepared
Lysine water-soluble glue is prepared using sol-gel technique；
(5) it is precipitated
After germanic acid radical ion aqueous solution is cooled to room temperature, lysine water-soluble glue is added, heats and stirs, germanic acid radical ion is water-soluble
Germanium tetrachloride in liquid is under the action of ammonium ion and lysine, hydrolysis rapidly in water, and unformed germanium oxide is spontaneous poly-
Collection roughening, recrystallization form crystal；
(6) dry
Gained crystal and amorphous liquid solution are placed on drying in drying box, obtain dry solidifying crystal, dry will coagulate crystal in air atmosphere
It is baked in enclosing 1 hour, and is ground to obtain a nanometer GeO2Powder.
2. a kind of nanometer titanium dioxide germanium production technology new process according to claim 1, it is characterised in that: the step
(1) mass percent that ammonium hydroxide is added in is 3%, and the mass percent of the distilled water is 97%.
3. a kind of nanometer titanium dioxide germanium production technology new process according to claim 1, it is characterised in that: the step
(1) heating temperature that agitator tank stirs in is 60-80 DEG C.
4. a kind of nanometer titanium dioxide germanium production technology new process according to claim 1, it is characterised in that: the step
(5) the stirring duration in is greater than 10 minutes.
5. a kind of nanometer titanium dioxide germanium production technology new process according to claim 1, it is characterised in that: the step
(6) drying temperature of drying box is controlled at 50-55 DEG C in.
6. a kind of nanometer titanium dioxide germanium production technology new process according to claim 1, it is characterised in that: the step
(6) maturing temperature is 550-600 DEG C in.
7. a kind of nanometer titanium dioxide germanium production technology new process according to claim 1, it is characterised in that: the step
(4) mass percent of lysine is 15%-20% in lysine water-soluble glue in.
8. a kind of nanometer titanium dioxide germanium production technology new process according to claim 1, it is characterised in that: described amorphous
The oxidation germanium solution of state continues to precipitate crystal form in the drying process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811398986.7A CN109437283A (en) | 2018-11-22 | 2018-11-22 | A kind of nanometer titanium dioxide germanium production technology new process |
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| CN201811398986.7A CN109437283A (en) | 2018-11-22 | 2018-11-22 | A kind of nanometer titanium dioxide germanium production technology new process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111661872A (en) * | 2020-06-16 | 2020-09-15 | 华东师范大学 | Preparation method of nano germanium oxide |
| CN115536055A (en) * | 2022-09-27 | 2022-12-30 | 昆明理工大学 | Method for preparing germanium dioxide from zinc hydrometallurgy inorganic germanium slag |
-
2018
- 2018-11-22 CN CN201811398986.7A patent/CN109437283A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111661872A (en) * | 2020-06-16 | 2020-09-15 | 华东师范大学 | Preparation method of nano germanium oxide |
| CN111661872B (en) * | 2020-06-16 | 2022-10-04 | 华东师范大学 | Preparation method of nano germanium oxide |
| CN115536055A (en) * | 2022-09-27 | 2022-12-30 | 昆明理工大学 | Method for preparing germanium dioxide from zinc hydrometallurgy inorganic germanium slag |
| CN115536055B (en) * | 2022-09-27 | 2023-08-18 | 昆明理工大学 | Method for preparing germanium dioxide from zinc hydrometallurgy inorganic germanium slag |
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Application publication date: 20190308 |