CN109264782A - A kind of method that low pressure doping prepares pucherite - Google Patents
A kind of method that low pressure doping prepares pucherite Download PDFInfo
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- CN109264782A CN109264782A CN201811088000.6A CN201811088000A CN109264782A CN 109264782 A CN109264782 A CN 109264782A CN 201811088000 A CN201811088000 A CN 201811088000A CN 109264782 A CN109264782 A CN 109264782A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/006—Compounds containing, besides vanadium, two or more other elements, with the exception of oxygen or hydrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Abstract
The invention discloses a kind of methods that low pressure doping prepares pucherite, including sorting, it is primary to prepare, primary stirring, secondary preparation, secondary agitation, low pressure reaction, washing, dry and liquid waste processing, structure of the invention is scientific and reasonable, it is safe and convenient to use, different elements can be added as needed, so as to adjust the performance of product, by to the ammonium metavanadate solution being configured to, sodium hydroxide is added, it is stirred strongly, it is sufficiently mixed ammonium metavanadate solution with sodium hydroxide, the first solution is made, then to addition bismuth nitrate solid in another mixing kettle, concentrated nitric acid is added, obtain the second solution, first solution and the second solution are mixed, acquired solution is moved into agitator and is stirred, obtain presoma, presoma is moved into reaction kettle and is reacted, obtain pucherite crystal, reaction rate is fast, less energy consumption, yield is high, it is suitble to low cost Large-scale production, pucherite crystal repeatedly wash, to remove the byproduct of reaction of pucherite plane of crystal attachment.
Description
Technical field
The present invention relates to pucherite preparation technical field, specially a kind of method that low pressure doping prepares pucherite.
Background technique
Pucherite be otherwise known as in the world 184 Huang, at first with German BASF R&D and production Success Flag a new generation
The birth of environment-friendly materials, pucherite are a kind of glassy yellow inorganic chemicals, and it is one that it, which is free of the heavy metal element being harmful to the human body,
The metal oxide matter of the environmentally friendly low-carbon of kind.Pucherite has a variety of crystal phases, the pucherites of different crystal phases have different property and
Using, pucherite in addition to the property as colorant, it also has a photocatalysis performance, and pucherite is in the contact sun and fluorescent lamp
It can promote to chemically react when light, it can kill Escherichia coli, staphylococcus aureus etc., in addition to this, pucherite
It is also applied in office or domestic environment, decomposes organic compound and noxious material in air, pucherite can not only acceleration
Reaction is learned, also Lu can be determined with nature, not result in waste of resources and formed with additional pollution, this is the hair for meeting low-carbon economy
Exhibition demand, at this stage, the main method for preparing pucherite nano material has solid phase method, hydro-thermal method, the precipitation method, metal alkoxide water
Solution, template, sonochemical method, microwave-hydrothermal method etc., but these methods in material structure control there are still some shortcomings,
Reaction needed for temperature it is higher, equipment is complex, energy consumption is high, reaction time is long, yield is relatively low, preparation product morphology compared with
It is single etc..
Summary of the invention
The present invention provides a kind of method that low pressure doping prepares pucherite, can effectively solve to propose in above-mentioned background technique
These methods material structure control on there are still some shortcomings, the temperature for reacting required is higher, equipment is complex, energy consumption
It is big etc., the problem of reaction time is long, yield is relatively low, the product morphology of preparation is more single etc..
To achieve the above object, the invention provides the following technical scheme: a kind of method that low pressure doping prepares pucherite, packet
Include following steps:
S1, sorting: ammonium metavanadate and bismuth nitrate are chosen, needs to choose other compounds according to preparation；
S2, primary preparation: ammonium metavanadate solid is weighed, distilled water is added, is configured to ammonium metavanadate solution；
S3, primary stirring: sodium hydroxide will be added in step 2 in acquired solution and stirred strongly, be uniformly mixed
The first solution；
S4, secondary preparation: bismuth nitrate solid being added into mixing kettle, and concentrated nitric acid dissolution is added, obtains the second solution；
S5, secondary agitation: the first solution obtained in step 3 is mixed with the solution in step 4, uses sodium hydroxide tune
Solution PH is saved, insulated and stirred obtains presoma；
S6, low pressure reaction: acquired solution in step 5 is added in reaction kettle and carries out low pressure reaction, obtains pucherite crystal；
S7, washing: pucherite crystal obtained in step 6 is washed using distilled water, is then carried out using ethyl alcohol
Washing；
S8, drying: the pucherite crystal after washing being placed in dryer and is dried, and can be prepared pucherite and be received
Rice material；
S9, liquid waste processing: the waste liquid in reaction kettle is screened, and removes wherein solid impurity, is carried out to residual waste solution
It is discharged after oxidation processes.
It according to the above technical scheme,, can be by vibrating screen to inclined after ammonium metavanadate and bismuth nitrate sorting in the step S1
Ammonium vanadate and bismuth nitrate are screened, and wherein impurity is removed, and the aperture of the sieve is 50 mesh.
According to the above technical scheme, in the step S2, ammonium metavanadate solid is added in mixing kettle, distilled water is added,
It is configured to the ammonium metavanadate solution of 1mol/L.
According to the above technical scheme, in the step S3, the 1mol/L ammonium metavanadate solution that will be configured to is put into agitator
It is interior, the sodium hydroxide of 2-6 times of molal quantity of vanadium is added, carries out strong stirring in 15 minutes, obtains the first solution blender
Revolving speed is 3000r/min.
According to the above technical scheme, in the step S4, metavanadic acid in the bismuth nitrate solid in mixing kettle and step 3 is added
Ammonium vanadium equimolar ratio is added concentrated nitric acid and dissolves to bismuth nitrate solid, obtains the second solution.
According to the above technical scheme, it in the step S5, will be configured to configure in the first solution and step S4 in step S3
The second solution out is mixed, and solution pH value is adjusted to PH=8 from PH=3 with 1mol sodium hydroxide, is moved into agitator,
75 degree of constant temperature are kept, stirs 1 hour, obtains presoma.
According to the above technical scheme, in the step S6, gained presoma in step S5 is moved into reaction kettle, control is anti-
Answering temperature constant is 125 degree, pressure 0.5MPa, reacts 5 hours, obtains pucherite crystal.
According to the above technical scheme, in the step S7, gained pucherite crystal makes to be washed with distilled water 3 times in step S6
With use ethanol washing 2 times, remove pucherite plane of crystal attachment byproduct of reaction.
According to the above technical scheme, in the step S8, the vanadic acid sodium crystal after washing in step S7 is put into dryer
Interior, the drying temperature for adjusting dryer is 105 degree, and the drying time of the dryer is 4 hours.
According to the above technical scheme, in the step S9, the solid impurity filtered in waste liquid is subjected to unified recycle and is stored,
Convenient for the unified recycling and reusing of byproduct of reaction.
Compared with prior art, beneficial effects of the present invention:
The present invention is when low pressure doping prepares pucherite, when sorting, can add different elements, as needed so as to adjust production
The sodium hydroxide of 2-6 times of molal quantity of vanadium is added by the ammonium metavanadate solution to the 1mol/L being configured in the performance of product,
The strong stirring for carrying out 15 minutes, is sufficiently mixed ammonium metavanadate solution with sodium hydroxide, the first solution is made, then to another
The bismuth nitrate solid with ammonium metavanadate vanadium equimolar ratio in step 3 is added in mixing kettle, it is solid to bismuth nitrate that concentrated nitric acid is added
Body is dissolved, and the second solution is obtained, and the first solution and the second solution are mixed, and acquired solution is moved into agitator, is kept
75 degree of constant temperature stir 1 hour, obtain presoma, and presoma is moved into reaction kettle, and constant reaction temperature is 125 degree, reacts and is
Pressure 0.5Mpa reacts 5 hours, obtains pucherite crystal, and reaction rate is fast, less energy consumption, yield are high, is suitble to low-coat scale raw
It produces, pucherite crystal passes through 3 distillation water washings, 2 ethanol washings, to remove the reaction pair of pucherite plane of crystal attachment
Product.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is step schematic diagram of the invention.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1: as shown in Figure 1, the present invention provides the method and technology scheme that a kind of low pressure doping prepares pucherite, it is a kind of
The method that low pressure doping prepares pucherite, includes the following steps:
S1, sorting: ammonium metavanadate and bismuth nitrate are chosen, needs to choose other compounds according to preparation；
S2, primary preparation: ammonium metavanadate solid is weighed, distilled water is added, is configured to ammonium metavanadate solution；
S3, primary stirring: sodium hydroxide will be added in step 2 in acquired solution and stirred strongly, be uniformly mixed
The first solution；
S4, secondary preparation: bismuth nitrate solid being added into mixing kettle, and concentrated nitric acid dissolution is added, obtains the second solution；
S5, secondary agitation: the first solution obtained in step 3 is mixed with the solution in step 4, uses sodium hydroxide tune
Solution PH is saved, insulated and stirred obtains presoma；
S6, low pressure reaction: acquired solution in step 5 is added in reaction kettle and carries out low pressure reaction, obtains pucherite crystal；
S7, washing: pucherite crystal obtained in step 6 is washed using distilled water, is then carried out using ethyl alcohol
Washing；
S8, drying: the pucherite crystal after washing being placed in dryer and is dried, and can be prepared pucherite and be received
Rice material；
S9, liquid waste processing: the waste liquid in reaction kettle is screened, and removes wherein solid impurity, is carried out to residual waste solution
It is discharged after oxidation processes.
It according to the above technical scheme,, can be by vibrating screen to metavanadic acid after ammonium metavanadate and bismuth nitrate sorting in step S1
Ammonium and bismuth nitrate are screened, and wherein impurity is removed, and the aperture of sieve is 50 mesh
According to the above technical scheme, in step S2, ammonium metavanadate solid is added in mixing kettle, distilled water is added, is prepared
At the ammonium metavanadate solution of 1mol/L
According to the above technical scheme, in step S3, the 1mol/L ammonium metavanadate solution that will be configured to is put into agitator, is added
Enter the sodium hydroxide of 2-6 times of molal quantity of vanadium, carry out strong stirring in 15 minutes, the revolving speed for obtaining the first solution blender is
3000r/min。
According to the above technical scheme, in step S4, ammonium metavanadate vanadium in the bismuth nitrate solid in mixing kettle and step 3 is added
Element equimolar ratio is added concentrated nitric acid and dissolves to bismuth nitrate solid, obtains the second solution.
According to the above technical scheme, in step S5, by be configured to configure in the first solution and step S4 in step S3
Second solution is mixed, and solution pH value is adjusted to PH=8 from PH=3 with 1mol sodium hydroxide, moves into agitator, keeps
75 degree of constant temperature stir 1 hour, obtain presoma.
According to the above technical scheme, in step S6, gained presoma in step S5 is moved into reaction kettle, control reaction temperature
Spending constant is 125 degree, pressure 0.5MPa, reacts 5 hours, obtains pucherite crystal.
According to the above technical scheme, in step S7, gained pucherite crystal makes to be washed with distilled water 3 times and make in step S6
With ethanol washing 2 times, the byproduct of reaction of pucherite plane of crystal attachment is removed.
According to the above technical scheme, in step S8, the vanadic acid sodium crystal after washing in step S7 is put into dryer, is adjusted
The drying temperature of whole dryer is 105 degree, and the drying time of dryer is 4 hours.
According to the above technical scheme, in step S9, the solid impurity filtered in waste liquid is subjected to unified recycle and is stored, is convenient for
The unified recycling and reusing of byproduct of reaction.
Embodiment 2: as shown in Figure 1, the present invention provides the method and technology scheme that a kind of low pressure doping prepares pucherite, it is a kind of
The method that low pressure doping prepares pucherite, includes the following steps:
S1, sorting: ammonium metavanadate and bismuth nitrate are chosen, needs to choose other compounds according to preparation；
S2, primary preparation: ammonium metavanadate solid is weighed, distilled water is added, is configured to ammonium metavanadate solution；
S3, primary stirring: sodium hydroxide will be added in step 2 in acquired solution and stirred strongly, be uniformly mixed
The first solution；
S4, secondary preparation: bismuth nitrate solid being added into mixing kettle, and concentrated nitric acid dissolution is added, obtains the second solution；
S5, secondary agitation: the first solution obtained in step 3 is mixed with the solution in step 4, uses sodium hydroxide tune
Solution PH is saved, insulated and stirred obtains presoma；
S6, low pressure reaction: acquired solution in step 5 is added in reaction kettle and carries out low pressure reaction, obtains pucherite crystal；
S7, washing: pucherite crystal obtained in step 6 is washed using distilled water, is then carried out using ethyl alcohol
Washing；
S8, drying: the pucherite crystal after washing being placed in dryer and is dried, and can be prepared pucherite and be received
Rice material；
S9, liquid waste processing: the waste liquid in reaction kettle is screened, and removes wherein solid impurity, is carried out to residual waste solution
It is discharged after oxidation processes.
It according to the above technical scheme,, can be by vibrating screen to metavanadic acid after ammonium metavanadate and bismuth nitrate sorting in step S1
Ammonium and bismuth nitrate are screened, and wherein impurity is removed, and the aperture of sieve is 50 mesh.
According to the above technical scheme, in step S2, ammonium metavanadate solid is added in mixing kettle, distilled water is added, is prepared
At the ammonium metavanadate solution of 1mol/L
According to the above technical scheme, in step S3, the 1mol/L ammonium metavanadate solution that will be configured to is put into agitator, is added
Enter the sodium hydroxide of 2-6 times of molal quantity of vanadium, carry out strong stirring in 15 minutes, the revolving speed for obtaining the first solution blender is
3000r/min。
According to the above technical scheme, in step S4, ammonium metavanadate vanadium in the bismuth nitrate solid in mixing kettle and step 3 is added
Element equimolar ratio is added concentrated nitric acid and dissolves to bismuth nitrate solid, obtains the second solution.
According to the above technical scheme, in step S5, by be configured to configure in the first solution and step S4 in step S3
Second solution is mixed, and solution pH value is adjusted to PH=8 from PH=3 with 1mol sodium hydroxide, moves into agitator, keeps
75 degree of constant temperature stir 1 hour, obtain presoma.
According to the above technical scheme, in step S6, gained presoma in step S5 is moved into reaction kettle, control reaction temperature
Spending constant is 75 degree, pressure 0.3MPa, reacts 4 hours, obtains pucherite crystal.
According to the above technical scheme, in step S7, gained pucherite crystal makes to be washed with distilled water 3 times and make in step S6
With ethanol washing 2 times, the byproduct of reaction of pucherite plane of crystal attachment is removed.
According to the above technical scheme, in step S8, the vanadic acid sodium crystal after washing in step S7 is put into dryer, is adjusted
The drying temperature of whole dryer is 105 degree, and the drying time of dryer is 4 hours.
According to the above technical scheme, in step S9, the solid impurity filtered in waste liquid is subjected to unified recycle and is stored, is convenient for
The unified recycling and reusing of byproduct of reaction.
Embodiment 3: as shown in Figure 1, the present invention provides the method and technology scheme that a kind of low pressure doping prepares pucherite, it is a kind of
The method that low pressure doping prepares pucherite, includes the following steps:
S1, sorting: ammonium metavanadate and bismuth nitrate are chosen, needs to choose other compounds according to preparation；
S2, primary preparation: ammonium metavanadate solid is weighed, distilled water is added, is configured to ammonium metavanadate solution；
S3, primary stirring: sodium hydroxide will be added in step 2 in acquired solution and stirred strongly, be uniformly mixed
The first solution；
S4, secondary preparation: bismuth nitrate solid being added into mixing kettle, and concentrated nitric acid dissolution is added, obtains the second solution；
S5, secondary agitation: the first solution obtained in step 3 is mixed with the solution in step 4, uses sodium hydroxide tune
Solution PH is saved, insulated and stirred obtains presoma；
S6, low pressure reaction: acquired solution in step 5 is added in reaction kettle and carries out low pressure reaction, obtains pucherite crystal；
S7, washing: pucherite crystal obtained in step 6 is washed using distilled water, is then carried out using ethyl alcohol
Washing；
S8, drying: the pucherite crystal after washing being placed in dryer and is dried, and can be prepared pucherite and be received
Rice material；
S9, liquid waste processing: the waste liquid in reaction kettle is screened, and removes wherein solid impurity, is carried out to residual waste solution
It is discharged after oxidation processes.
It according to the above technical scheme,, can be by vibrating screen to metavanadic acid after ammonium metavanadate and bismuth nitrate sorting in step S1
Ammonium and bismuth nitrate are screened, and wherein impurity is removed, and the aperture of sieve is 50 mesh.
According to the above technical scheme, in step S2, ammonium metavanadate solid is added in mixing kettle, distilled water is added, is prepared
At the ammonium metavanadate solution of 1mol/L.
According to the above technical scheme, in step S3, the 1mol/L ammonium metavanadate solution that will be configured to is put into agitator, is added
Enter the sodium hydroxide of 2-6 times of molal quantity of vanadium, carry out strong stirring in 15 minutes, the revolving speed for obtaining the first solution blender is
3000r/min。
According to the above technical scheme, in step S4, ammonium metavanadate vanadium in the bismuth nitrate solid in mixing kettle and step 3 is added
Element equimolar ratio is added concentrated nitric acid and dissolves to bismuth nitrate solid, obtains the second solution.
According to the above technical scheme, in step S5, by be configured to configure in the first solution and step S4 in step S3
Second solution is mixed, and solution pH value is adjusted to PH=8 from PH=3 with 1mol sodium hydroxide, moves into agitator, keeps
75 degree of constant temperature stir 1 hour, obtain presoma.
According to the above technical scheme, in step S6, gained presoma in step S5 is moved into reaction kettle, control reaction temperature
Spending constant is 175 degree, pressure 0.7MPa, reacts 7 hours, obtains pucherite crystal.
According to the above technical scheme, in step S7, gained pucherite crystal makes to be washed with distilled water 3 times and make in step S6
With ethanol washing 2 times, the byproduct of reaction of pucherite plane of crystal attachment is removed.
According to the above technical scheme, in step S8, the vanadic acid sodium crystal after washing in step S7 is put into dryer, is adjusted
The drying temperature of whole dryer is 105 degree, and the drying time of dryer is 4 hours.
According to the above technical scheme, in step S9, the solid impurity filtered in waste liquid is subjected to unified recycle and is stored, is convenient for
The unified recycling and reusing of byproduct of reaction.
The sodium vanadate nano material that the present invention is prepared according to embodiment 1-3 detects, as a result such as table 1,
1 testing result of table
| Inspection project | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Reaction temperature (degree) | 125 | 75 | 175 |
| Pressure (Mpa) | 0.5 | 0.3 | 0.7 |
| Reaction time (h) | 5 | 4 | 7 |
| Color saturation | Saturation degree is high | Saturation degree is lower | Saturation degree is higher |
| Tinting strength, tinting power | Tinting strength, tinting power is high | Saturation degree is lower | Saturation degree is higher |
By testing result it can be found that when ammonium metavanadate and bismuth nitrate low pressure reaction is added, reaction temperature is 125 degree,
Reaction pressure is 0.5Mpa, when the reaction time is 5 hours, the sodium vanadate nano material color saturation and tinting strength, tinting power highest of preparation.
The working principle of the invention and process for using: the present invention chooses ammonium metavanadate when low pressure doping prepares pucherite
After bismuth nitrate, ammonium metavanadate and bismuth nitrate can be screened by vibrating screen, remove the impurity that raw material wherein adulterates, pass through
Ammonium metavanadate solid is added in mixing kettle, distilled water is added, is configured to the ammonium metavanadate solution of 1mol/L, it and then will configuration
At the ammonium metavanadate solution of 1mol/L be put into agitator, the sodium hydroxide of 2-6 times of molal quantity of vanadium is added, carries out 15 points
The strong stirring of clock, is sufficiently mixed ammonium metavanadate solution with sodium hydroxide, the first solution is made, then in another mixing kettle
The bismuth nitrate solid with ammonium metavanadate vanadium equimolar ratio in step 3 is added, it is molten to the progress of bismuth nitrate solid that concentrated nitric acid is added
Solution, obtains the second solution, will be configured to the first solution and the second solution is mixed, using 1mol sodium hydroxide by solution from PH
=3 are adjusted to PH=8, by acquired solution move into agitator in, keep 75 degree constant temperature, stirring 1 hour, obtain presoma, will before
It drives body to move into reaction kettle, it is 125 degree that it is constant, which to control reaction temperature, and keeping reaction is pressure 0.5MPa, reacts 5 hours, obtains
Pucherite crystal takes out the pucherite crystal prepared, and 3 washings are carried out using distilled water, then carry out 2 using ethyl alcohol
Vanadic acid sodium crystal after washing is put into drying to remove the byproduct of reaction of pucherite plane of crystal attachment by secondary washing
In machine, the drying temperature for adjusting dryer is 105 degree, and the drying of 4 hours is carried out to the vanadic acid sodium crystal of preparation, can be prepared
Remaining liq in reaction kettle is filtered by pucherite nano material out by filter screen, and the solid impurity that will filter out carries out
Unified recycling storage, is discharged after then being aoxidized waste reaction solution.
Finally, it should be noted that being not intended to restrict the invention the above is only preferred embodiment of the invention, although ginseng
According to previous embodiment, invention is explained in detail, for those skilled in the art, still can be to preceding
Technical solution documented by each embodiment is stated to modify or equivalent replacement of some of the technical features.It is all this
Within the spirit and principle of invention, any modification, equivalent replacement, improvement and so on should be included in protection model of the invention
Within enclosing.
Claims (10)
1. a kind of method that low pressure doping prepares pucherite, characterized by the following steps:
S1, sorting: ammonium metavanadate and bismuth nitrate are chosen, needs to choose other compounds according to preparation；
S2, primary preparation: ammonium metavanadate solid is weighed, distilled water is added, is configured to ammonium metavanadate solution；
S3, primary stirring: will be added sodium hydroxide and be stirred strongly in acquired solution in step 2, obtain uniformly mixed the
One solution；
S4, secondary preparation: bismuth nitrate solid being added into mixing kettle, and concentrated nitric acid dissolution is added, obtains the second solution；
S5, secondary agitation: the first solution obtained in step 3 is mixed with the solution in step 4, is adjusted using sodium hydroxide molten
Liquid PH, insulated and stirred obtain presoma；
S6, low pressure reaction: acquired solution in step 5 is added in reaction kettle and carries out low pressure reaction, obtains pucherite crystal；
S7, washing: pucherite crystal obtained in step 6 is washed using distilled water, is then washed using ethyl alcohol；
S8, drying: the pucherite crystal after washing being placed in dryer and is dried, and can prepare pucherite nanometer material
Material；
S9, liquid waste processing: the waste liquid in reaction kettle is screened, and is removed wherein solid impurity, is aoxidized to residual waste solution
It is discharged after processing.
2. the method that a kind of low pressure doping according to claim 1 prepares pucherite, it is characterised in that: the step S1
In, after ammonium metavanadate and bismuth nitrate sorting, ammonium metavanadate and bismuth nitrate can be screened by vibrating screen, be removed wherein miscellaneous
Matter, the aperture of the sieve are 50 mesh.
3. the method that a kind of low pressure doping according to claim 1 prepares pucherite, it is characterised in that: the step S2
In, ammonium metavanadate solid is added in mixing kettle, distilled water is added, is configured to the ammonium metavanadate solution of 1mol/L.
4. the method that a kind of low pressure doping according to claim 1 prepares pucherite, it is characterised in that: the step S3
In, the 1mol/L ammonium metavanadate solution that will be configured to is put into agitator, the sodium hydroxide of 2-6 times of molal quantity of vanadium is added,
The strong stirring for carrying out 15 minutes, the revolving speed for obtaining the first solution blender is 3000r/min.
5. the method that a kind of low pressure doping according to claim 1 prepares pucherite, it is characterised in that: the step S4
In, ammonium metavanadate vanadium equimolar ratio in the bismuth nitrate solid in mixing kettle and step 3 is added, concentrated nitric acid is added to bismuth nitrate
Solid is dissolved, and the second solution is obtained.
6. the method that a kind of low pressure doping according to claim 1 prepares pucherite, it is characterised in that: the step S5
In, the second solution for being configured to configure in the first solution and step S4 in step S3 is mixed, solution pH value is used
1mol sodium hydroxide is adjusted to PH=8 from PH=3, moves into agitator, keeps 75 degree of constant temperature, stirs 1 hour, obtains forerunner
Body.
7. the method that a kind of low pressure doping according to claim 1 prepares pucherite, it is characterised in that: the step S6
In, gained presoma in step S5 is moved into reaction kettle, it is 125 degree that it is constant, which to control reaction temperature, pressure 0.5MPa, reaction 5
Hour, obtain pucherite crystal.
8. the method that a kind of low pressure doping according to claim 1 prepares pucherite, it is characterised in that: the step S7
In, gained pucherite crystal makes to be washed with distilled water 3 times and use ethanol washing 2 times in step S6, removes pucherite crystal table
The byproduct of reaction of face attachment.
9. the method that a kind of low pressure doping according to claim 1 prepares pucherite, it is characterised in that: the step S8
In, the vanadic acid sodium crystal after washing in step S7 is put into dryer, the drying temperature for adjusting dryer is 105 degree, described
The drying time of dryer is 4 hours.
10. the method that a kind of low pressure doping according to claim 1 prepares pucherite, it is characterised in that: the step S9
In, the solid impurity filtered in waste liquid is subjected to unified recycle and is stored, convenient for the unified recycling and reusing of byproduct of reaction.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110760202A (en) * | 2019-09-18 | 2020-02-07 | 湖南柿竹园有色金属有限责任公司 | Preparation method of bismuth vanadate fluorescent pigment |
| CN110760203A (en) * | 2019-09-18 | 2020-02-07 | 湖南柿竹园有色金属有限责任公司 | Preparation process of novel bismuth temperature-resistant environment-friendly pigment |
| CN114031114A (en) * | 2021-11-12 | 2022-02-11 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing bismuth vanadate powder by using failure electrolyte of vanadium battery |
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| CN102295311A (en) * | 2011-07-22 | 2011-12-28 | 河北联合大学 | Method for preparing bismuth vanadate nano-material by microwave radiation method |
| CN102951682A (en) * | 2012-11-14 | 2013-03-06 | 陕西科技大学 | Preparation method of cellular spherical bismuth vanadate microcrystalline |
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2018
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295311A (en) * | 2011-07-22 | 2011-12-28 | 河北联合大学 | Method for preparing bismuth vanadate nano-material by microwave radiation method |
| CN102951682A (en) * | 2012-11-14 | 2013-03-06 | 陕西科技大学 | Preparation method of cellular spherical bismuth vanadate microcrystalline |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110760202A (en) * | 2019-09-18 | 2020-02-07 | 湖南柿竹园有色金属有限责任公司 | Preparation method of bismuth vanadate fluorescent pigment |
| CN110760203A (en) * | 2019-09-18 | 2020-02-07 | 湖南柿竹园有色金属有限责任公司 | Preparation process of novel bismuth temperature-resistant environment-friendly pigment |
| CN114031114A (en) * | 2021-11-12 | 2022-02-11 | 成都先进金属材料产业技术研究院股份有限公司 | Method for preparing bismuth vanadate powder by using failure electrolyte of vanadium battery |
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