CN109368689A - Tetragonal structure germanium oxide is converted into the production technology of the molten germanium of six squares acid - Google Patents
Tetragonal structure germanium oxide is converted into the production technology of the molten germanium of six squares acid Download PDFInfo
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- CN109368689A CN109368689A CN201811399994.3A CN201811399994A CN109368689A CN 109368689 A CN109368689 A CN 109368689A CN 201811399994 A CN201811399994 A CN 201811399994A CN 109368689 A CN109368689 A CN 109368689A
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- C01G17/00—Compounds of germanium
- C01G17/02—Germanium dioxide
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Abstract
Tetragonal structure germanium oxide is converted into the production technology of the molten germanium of six squares acid, includes the following steps: the first step, takes the raw material containing tetragonal structure germanium oxide, is added in reaction kettle, and water is added, sodium hydroxide is then added thereto, stirs, and reacts 2-3 hours;Second step, the material that the first step is obtained carry out heating evaporation, obtain concentrate, concentrate are reduced temperature, and be 4.5-6.0 using hydrochloric acid adjustment pH;Third step is added sodium chlorate, stirs evenly, and heat up, be kept stirring 3-5 hours;Hydrochloric acid is added into the material of third step for 4th step, then carries out heating distillation, collects fraction;Fraction is added the distilled water of 6.5 times of volumes and places a period of time after stirring 2-3 hour, be during which passed through oxygen, generates precipitating by the 5th step, is washed with cold water and is precipitated to washing lotion not until chloride ion-containing, the sour molten germanium product of six squares is dried to obtain in 200 DEG C.The present invention provides a kind of reasonable techniques, convert the molten germanium of six squares acid for tetragonal structure germanium oxide.
Description
Technical field
The present invention relates to metallurgical technology fields, and in particular to a kind of tetragonal structure germanium oxide is converted into the molten germanium of six squares acid
Production technology.
Background technique
The chemical property of germanium is stablized, but does not give birth to quickly at 600~700 DEG C with air or water vapor acting at normal temperature
At germanium dioxide.When not working with dilute sulfuric acid, hydrochloric acid, but heating in concentrated sulfuric acid, germanium will be slow dissolution.Germanium is in nitric acid, king
It is soluble in water.The effect of germanium and alkaline solution is very weak, but the alkali melted can be such that germanium dissolves rapidly in air.Germanium does not rise with carbon
Effect, so germanium melts in graphite crucible, will not be polluted by carbon.
Germanium dioxide is widely used in industrial production and science and technology field.Such as optical fluorescence powder, fiber optic materials, because
The glass of doping germanium oxide has higher refractive index and dispersion, can make pantoscope and micro- lens head.In recent years
Come, with the development of science and technology, germanium dioxide be widely used in make high pure metal germanium, germanium compound, chemical catalyst and
Conversion, the adjustment of dehydrogenation, gasoline fraction, colour film and polyester fiber when medical industry can be used as catalyst for Petroleum refining
Among production.Moreover, germanium dioxide or the catalyst of polymerization reaction, the glass containing germanium dioxide, resin, electronic device
Deng as semiconductor material.
There are two types of crystal forms for germanium dioxide tool, wherein the germanium dioxide of tetragonal structure is not soluble in water, it is difficult to carry out preferably benefit
With.And its purity of the germanium dioxide of tetragonal structure is poor, majority can adulterate plurality of impurities, currently without effective method by its
It is converted into another crystal form.
Therefore, the production technology that the new tetragonal structure germanium oxide of one kind is converted into the molten germanium of six squares acid is developed, is not only had
Urgent researching value, it may have good economic benefit and commercial application potentiality, this power exactly of the invention being accomplished
Place and basis.
Summary of the invention
For the defects in the prior art, the present invention provides the production that tetragonal structure germanium oxide is converted into the molten germanium of six squares acid
Technique.
Tetragonal structure germanium oxide is converted into the production technology of the molten germanium of six squares acid, includes the following steps:
The first step takes the raw material containing tetragonal structure germanium oxide, is added in reaction kettle, and water is added, is then added thereto
Sodium hydroxide, stirring are reacted 2-3 hours;
Second step, the material that the first step is obtained carry out heating evaporation, obtain concentrate, concentrate is reduced temperature, and
It is 4.5-6.0 using hydrochloric acid adjustment pH;
Third step is added sodium chlorate, stirs evenly, and heat up, be kept stirring 3-5 hours;
Hydrochloric acid is added into the material of third step for 4th step, then carries out heating distillation, collects fraction;
Fraction is added the distilled water of 6.5 times of volumes and places a period of time after stirring 2-3 hours, during which led to by the 5th step
Enter oxygen, generate precipitating, is washed with cold water and be precipitated to washing lotion not until chloride ion-containing, it is molten that six square acid are dried to obtain in 200 DEG C
Germanium product.
In the present invention, as a kind of perferred technical scheme, in the first step, the mass volume ratio of raw material and water is 1kg:
15-18L。
In the present invention, as a kind of perferred technical scheme, in the first step, the weight of weight and raw material is added in sodium hydroxide
Than for 0.3-0.7:1.
In the present invention, as a kind of perferred technical scheme, in the first step, sodium hydroxide is added in three times, adds for the first time
Enter the 1/5 of total weight, the 1/2 of second of addition total weight, it is all added remaining for the third time.
In the present invention, as a kind of perferred technical scheme, in the first step, control reaction kettle reaction temperature be 80 DEG C~
85℃。
In the present invention, as a kind of perferred technical scheme, in second step, evaporates the first step and water total volume 1/2- is added
2/3 water.
In the present invention, as a kind of perferred technical scheme, in second step, concentrate is reduced into temperature to 35-45 DEG C.
In the present invention, as a kind of perferred technical scheme, in second step, the molar concentration of hydrochloric acid is 12-15mol/L.
In the present invention, as a kind of perferred technical scheme, in third step, it is warming up to 50-60 DEG C.
In the present invention, as a kind of perferred technical scheme, in the 4th step, the hydrochloric acid molar concentration 5-9mol/L of addition,
90-100 DEG C is heated to be distilled.
In the present invention, as a kind of perferred technical scheme, in the 5th step, standing time is 20-28 hours.
Due to using the technology described above, the invention has the following beneficial effects:
The present invention first the raw material containing tetragonal structure germanium oxide is added in reaction kettle, and water is added, and then adds thereto
Enter sodium hydroxide, stir, reacts 2-3 hours;And heating evaporation is carried out, concentrate is obtained, concentrate is reduced into temperature, and utilize
It is 4.5-6.0 that hydrochloric acid, which adjusts pH,.Based on the step, technique of the invention can fill the tetragonal structure germanium oxide contained in raw material
Divide alkali soluble, and be enriched with, provides advantageous condition for subsequent conversion.
Sodium chlorate is added in the present invention, stirs evenly, and heat up, is kept stirring 3-5 hours, can will contain tetragonal
The impurity (predominantly arsenic) contained in the raw material of type germanium oxide is converted to the higher substance of boiling point, it is ensured that next step is in distillation
Impurity remains in mother liquor, improves the recovery rate and DNA purity of germanium.
Fraction is added the distilled water of 6.5 times of volumes and places a period of time after stirring 2-3 hours, be during which passed through by the present invention
Oxygen generates precipitating, wash with cold water and is precipitated to washing lotion not until chloride ion-containing, the sour molten germanium of six squares is dried to obtain in 200 DEG C
Product.Using the step, the crystal transfer of germanium oxide can be realized under the premise of oxygen abundance.
In conclusion it is molten to convert six square acid for tetragonal structure germanium oxide the present invention provides a kind of reasonable technique
Germanium.
Specific embodiment
Technical solution of the present invention is described in detail below in conjunction with specific embodiment.Following embodiment is only used for more
Add and clearly demonstrate technical solution of the present invention, therefore be only used as example, and not intended to limit the protection scope of the present invention.
Embodiment 1
Tetragonal structure germanium oxide is converted into the production technology of the molten germanium of six squares acid, includes the following steps:
The first step takes the raw material containing tetragonal structure germanium oxide, is added in reaction kettle, and water, the quality of raw material and water is added
Volume ratio is 1kg:15L, and sodium hydroxide is then added thereto, and it is 0.3:1 that weight and the weight ratio of raw material, which is added, in sodium hydroxide,
Sodium hydroxide is added in three times, and the 1/5 of total weight is added for the first time, just starts to be added reacting, second of addition total weight
1/2, react 30 minutes when be added, for the third time by it is remaining all be added, reaction 1.5 hours after be added, step by step
Adding manner, it can be ensured that the germanium oxide in raw material is stirred with 60 revs/min of rate adequately by alkali soluble, controls reaction kettle
Reaction temperature be 80 DEG C, react 2 hours;
Second step, the material that the first step is obtained carry out heating evaporation, evaporate the first step and water total volume 1/2 is added
Water obtains concentrate, and concentrate is reduced temperature to 35 DEG C, and is 4.5 using hydrochloric acid adjustment pH, and the molar concentration of hydrochloric acid is
12mol/L;
Third step is added sodium chlorate, stirs evenly, and be warming up to 50 DEG C, be kept stirring 3 hours;
4th step, hydrochloric acid is added into the material of third step, and the hydrochloric acid molar concentration 5mol/L of addition is then heated to 90
It DEG C is distilled, collects fraction;
Fraction is added the distilled water of 6.5 times of volumes and places 20 hours after stirring 2 hours, be during which passed through oxygen by the 5th step
Gas generates precipitating, wash with cold water and is precipitated to washing lotion not until chloride ion-containing, the molten germanium production of six squares acid is dried to obtain in 200 DEG C
Product.
In the present embodiment, the relative density of raw material about 6.31 (25 DEG C) is about 1086 DEG C of fusing point, not soluble in water;Obtained production
Product relative density 4.22 (25 DEG C), it is about 1116 DEG C of fusing point, water-soluble.
Embodiment 2
Tetragonal structure germanium oxide is converted into the production technology of the molten germanium of six squares acid, includes the following steps:
The first step takes the raw material containing tetragonal structure germanium oxide, is added in reaction kettle, and water, the quality of raw material and water is added
Volume ratio is 1kg:18L, and sodium hydroxide is then added thereto, and it is 0.7:1 that weight and the weight ratio of raw material, which is added, in sodium hydroxide,
Sodium hydroxide is added in three times, and the 1/5 of total weight is added for the first time, just starts to be added reacting, second of addition total weight
1/2, react 30 minutes when be added, for the third time by it is remaining all be added, reaction 1.5 hours after be added, step by step
Adding manner, it can be ensured that the germanium oxide in raw material is stirred with 60 revs/min of rate adequately by alkali soluble, controls reaction kettle
Reaction temperature be 85 DEG C, react 3 hours;
Second step, the material that the first step is obtained carry out heating evaporation, evaporate the first step and water total volume 2/3 is added
Water obtains concentrate, and concentrate is reduced temperature to 45 DEG C, and is 6.0 using hydrochloric acid adjustment pH, and the molar concentration of hydrochloric acid is
15mol/L;
Third step is added sodium chlorate, stirs evenly, and be warming up to 60 DEG C, be kept stirring 5 hours;
4th step, hydrochloric acid is added into the material of third step, and the hydrochloric acid molar concentration 9mol/L of addition is then heated to
100 DEG C are distilled, and fraction is collected;
Fraction is added the distilled water of 6.5 times of volumes and places 28 hours after stirring 3 hours, be during which passed through oxygen by the 5th step
Gas generates precipitating, wash with cold water and is precipitated to washing lotion not until chloride ion-containing, the molten germanium production of six squares acid is dried to obtain in 200 DEG C
Product.
In the present embodiment, the relative density of raw material about 6.31 (25 DEG C) is about 1086 DEG C of fusing point, not soluble in water;Obtained production
Product relative density 4.26 (25 DEG C), it is about 1114 DEG C of fusing point, water-soluble.
Embodiment 3
Tetragonal structure germanium oxide is converted into the production technology of the molten germanium of six squares acid, includes the following steps:
The first step takes the raw material containing tetragonal structure germanium oxide, is added in reaction kettle, and water, the quality of raw material and water is added
Volume ratio is 1kg:16L, and sodium hydroxide is then added thereto, and it is 0.5:1 that weight and the weight ratio of raw material, which is added, in sodium hydroxide,
Sodium hydroxide is added in three times, and the 1/5 of total weight is added for the first time, just starts to be added reacting, second of addition total weight
1/2, react 30 minutes when be added, for the third time by it is remaining all be added, reaction 1.5 hours after be added, step by step
Adding manner, it can be ensured that the germanium oxide in raw material is stirred with 60 revs/min of rate adequately by alkali soluble, controls reaction kettle
Reaction temperature be 83 DEG C, react 2.5 hours;
Second step, the material that the first step is obtained carry out heating evaporation, evaporate the first step and water total volume 2/3 is added
Water obtains concentrate, and concentrate is reduced temperature to 40 DEG C, and is 5.0 using hydrochloric acid adjustment pH, and the molar concentration of hydrochloric acid is
14mol/L;
Third step is added sodium chlorate, stirs evenly, and be warming up to 55 DEG C, be kept stirring 4 hours;
4th step, hydrochloric acid is added into the material of third step, and the hydrochloric acid molar concentration 7mol/L of addition is then heated to 95
It DEG C is distilled, collects fraction;
Fraction is added the distilled water of 6.5 times of volumes and places 24 hours, be during which passed through after stirring 2.5 hours by the 5th step
Oxygen generates precipitating, wash with cold water and is precipitated to washing lotion not until chloride ion-containing, the sour molten germanium of six squares is dried to obtain in 200 DEG C
Product.
In the present embodiment, the relative density of raw material about 6.31 (25 DEG C) is about 1086 DEG C of fusing point, not soluble in water;Obtained production
Product relative density 4.23 (25 DEG C), it is about 1115 DEG C of fusing point, water-soluble.
Embodiment 4
Tetragonal structure germanium oxide is converted into the production technology of the molten germanium of six squares acid, includes the following steps:
The first step takes the raw material containing tetragonal structure germanium oxide, is added in reaction kettle, and water, the quality of raw material and water is added
Volume ratio is 1kg:15L, and sodium hydroxide is then added thereto, and it is 0.7:1 that weight and the weight ratio of raw material, which is added, in sodium hydroxide,
Sodium hydroxide is added in three times, and the 1/5 of total weight is added for the first time, just starts to be added reacting, second of addition total weight
1/2, react 30 minutes when be added, for the third time by it is remaining all be added, reaction 1.5 hours after be added, step by step
Adding manner, it can be ensured that the germanium oxide in raw material is stirred with 60 revs/min of rate adequately by alkali soluble, controls reaction kettle
Reaction temperature be 80 DEG C, react 3 hours;
Second step, the material that the first step is obtained carry out heating evaporation, evaporate the first step and water total volume 1/2 is added
Water obtains concentrate, and concentrate is reduced temperature to 45 DEG C, and is 4.5 using hydrochloric acid adjustment pH, and the molar concentration of hydrochloric acid is
15mol/L;
Third step is added sodium chlorate, stirs evenly, and be warming up to 50 DEG C, be kept stirring 5 hours;
4th step, hydrochloric acid is added into the material of third step, and the hydrochloric acid molar concentration 5mol/L of addition is then heated to
100 DEG C are distilled, and fraction is collected;
Fraction is added the distilled water of 6.5 times of volumes and places 28 hours after stirring 2 hours, be during which passed through oxygen by the 5th step
Gas generates precipitating, wash with cold water and is precipitated to washing lotion not until chloride ion-containing, the molten germanium production of six squares acid is dried to obtain in 200 DEG C
Product.
In the present embodiment, the relative density of raw material about 6.31 (25 DEG C) is about 1086 DEG C of fusing point, not soluble in water;Obtained production
Product relative density 4.22 (25 DEG C), it is about 1116 DEG C of fusing point, water-soluble.
Embodiment 5
Tetragonal structure germanium oxide is converted into the production technology of the molten germanium of six squares acid, includes the following steps:
The first step takes the raw material containing tetragonal structure germanium oxide, is added in reaction kettle, and water, the quality of raw material and water is added
Volume ratio is 1kg:18L, and sodium hydroxide is then added thereto, and it is 0.4:1 that weight and the weight ratio of raw material, which is added, in sodium hydroxide,
Sodium hydroxide is added in three times, and the 1/5 of total weight is added for the first time, just starts to be added reacting, second of addition total weight
1/2, react 30 minutes when be added, for the third time by it is remaining all be added, reaction 1.5 hours after be added, step by step
Adding manner, it can be ensured that the germanium oxide in raw material is stirred with 60 revs/min of rate adequately by alkali soluble, controls reaction kettle
Reaction temperature be 84 DEG C, react 2-3 hours;
Second step, the material that the first step is obtained carry out heating evaporation, evaporate the first step and water total volume 2/3 is added
Water obtains concentrate, and concentrate is reduced temperature to 37 DEG C, and is 5.7 using hydrochloric acid adjustment pH, and the molar concentration of hydrochloric acid is
13mol/L;
Third step is added sodium chlorate, stirs evenly, and be warming up to 60 DEG C, be kept stirring 3.5 hours;
4th step, hydrochloric acid is added into the material of third step, and the hydrochloric acid molar concentration 8mol/L of addition is then heated to 92
It DEG C is distilled, collects fraction;
Fraction is added the distilled water of 6.5 times of volumes and places 21 hours after stirring 3 hours, be during which passed through oxygen by the 5th step
Gas generates precipitating, wash with cold water and is precipitated to washing lotion not until chloride ion-containing, the molten germanium production of six squares acid is dried to obtain in 200 DEG C
Product.
In the present embodiment, the relative density of raw material about 6.31 (25 DEG C) is about 1086 DEG C of fusing point, not soluble in water;Obtained production
Product relative density 4.22 (25 DEG C), it is about 1115 DEG C of fusing point, water-soluble.
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 (10)
1. the production technology that tetragonal structure germanium oxide is converted into the molten germanium of six squares acid, characterized by the following steps:
The first step takes the raw material containing tetragonal structure germanium oxide, is added in reaction kettle, and water is added, hydrogen-oxygen is then added thereto
Change sodium, stirring is reacted 2-3 hours;
Second step, the material that the first step is obtained carry out heating evaporation, obtain concentrate, concentrate is reduced temperature, and utilize
It is 4.5-6.0 that hydrochloric acid, which adjusts pH,;
Third step is added sodium chlorate, stirs evenly, and heat up, be kept stirring 3-5 hours;
Hydrochloric acid is added into the material of third step for 4th step, then carries out heating distillation, collects fraction;
Fraction is added the distilled water of 6.5 times of volumes and places a period of time after stirring 2-3 hours, be during which passed through oxygen by the 5th step
Gas generates precipitating, wash with cold water and is precipitated to washing lotion not until chloride ion-containing, the molten germanium production of six squares acid is dried to obtain in 200 DEG C
Product.
2. the production technology that tetragonal structure germanium oxide as described in claim 1 is converted into the molten germanium of six squares acid, it is characterised in that:
In the first step, the mass volume ratio of raw material and water is 1kg:15-18L.
3. the production technology that tetragonal structure germanium oxide as claimed in claim 2 is converted into the molten germanium of six squares acid, it is characterised in that:
In the first step, it is 0.3-0.7:1 that weight and the weight ratio of raw material, which is added, in sodium hydroxide.
4. the production technology that tetragonal structure germanium oxide as claimed in claim 3 is converted into the molten germanium of six squares acid, it is characterised in that:
In the first step, sodium hydroxide is added in three times, the 1/5 of total weight, the 1/2 of second of addition total weight is added for the first time, third
It is secondary to be all added remaining.
5. the production technology that tetragonal structure germanium oxide as claimed in claim 4 is converted into the molten germanium of six squares acid, it is characterised in that:
In the first step, the reaction temperature for controlling reaction kettle is 80 DEG C~85 DEG C.
6. the production technology that tetragonal structure germanium oxide as described in claim 1 is converted into the molten germanium of six squares acid, it is characterised in that:
In second step, the water that water total volume 1/2-2/3 is added in the first step is evaporated.
7. the production technology that tetragonal structure germanium oxide as claimed in claim 6 is converted into the molten germanium of six squares acid, it is characterised in that:
In second step, concentrate is reduced into temperature to 35-45 DEG C.
8. the production technology that tetragonal structure germanium oxide as claimed in claim 7 is converted into the molten germanium of six squares acid, it is characterised in that:
In second step, the molar concentration of hydrochloric acid is 12-15mol/L.
9. the production technology that tetragonal structure germanium oxide as described in claim 1 is converted into the molten germanium of six squares acid, it is characterised in that:
In third step, it is warming up to 50-60 DEG C.
10. tetragonal structure germanium oxide as described in claim 1 is converted into the production technology of the molten germanium of six squares acid, feature exists
In: the hydrochloric acid molar concentration 5-9mol/L of addition is heated to 90-100 DEG C and is distilled.
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Cited By (1)
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CN117607080A (en) * | 2024-01-22 | 2024-02-27 | 昆明理工大学 | Analysis method of germanium chemical phase in germanium-containing complex minerals |
-
2018
- 2018-11-22 CN CN201811399994.3A patent/CN109368689A/en active Pending
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CN117607080A (en) * | 2024-01-22 | 2024-02-27 | 昆明理工大学 | Analysis method of germanium chemical phase in germanium-containing complex minerals |
CN117607080B (en) * | 2024-01-22 | 2024-03-29 | 昆明理工大学 | Analysis method of germanium chemical phase in germanium-containing complex minerals |
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