CN113003605A - Method for directly preparing high-purity bismuth oxide from crude bismuth - Google Patents
Method for directly preparing high-purity bismuth oxide from crude bismuth Download PDFInfo
- Publication number
- CN113003605A CN113003605A CN202110250557.0A CN202110250557A CN113003605A CN 113003605 A CN113003605 A CN 113003605A CN 202110250557 A CN202110250557 A CN 202110250557A CN 113003605 A CN113003605 A CN 113003605A
- Authority
- CN
- China
- Prior art keywords
- bismuth
- mol
- concentration
- purity
- crude
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 55
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 44
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910000416 bismuth oxide Inorganic materials 0.000 title claims abstract description 40
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 title claims abstract description 40
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 56
- 238000001035 drying Methods 0.000 claims abstract description 44
- 238000000967 suction filtration Methods 0.000 claims abstract description 41
- 239000007853 buffer solution Substances 0.000 claims abstract description 39
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 36
- 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 33
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 14
- 239000003513 alkali Substances 0.000 claims abstract description 8
- HWSISDHAHRVNMT-UHFFFAOYSA-N Bismuth subnitrate Chemical compound O[NH+]([O-])O[Bi](O[N+]([O-])=O)O[N+]([O-])=O HWSISDHAHRVNMT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 7
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229960001482 bismuth subnitrate Drugs 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 22
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- FWABRVJYGBOLEM-UHFFFAOYSA-N diazanium;azane;carbonate Chemical compound N.[NH4+].[NH4+].[O-]C([O-])=O FWABRVJYGBOLEM-UHFFFAOYSA-N 0.000 claims description 19
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 16
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- 239000012535 impurity Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000010306 acid treatment Methods 0.000 abstract description 2
- 238000003837 high-temperature calcination Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000010335 hydrothermal treatment Methods 0.000 abstract description 2
- 238000006386 neutralization reaction Methods 0.000 abstract description 2
- 238000004140 cleaning Methods 0.000 description 18
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 150000001621 bismuth Chemical class 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a method for directly preparing high-purity bismuth oxide from crude bismuth. Providing crude bismuth, placing the crude bismuth into a nitric acid solution with the concentration of 2.0-5.0 mol/L, stirring for 30-60min at the temperature of 30-40 ℃, and performing suction filtration and drying treatment to obtain bismuth suboxide nitrate solid; and then placing the prepared bismuth subnitrate solid in an ammonia water-ammonium carbonate buffer solution with the pH value of 9-10, uniformly mixing, carrying out ultrasonic treatment for 3-5h at normal temperature to prepare a mixed solution, placing the mixed solution in a high-pressure reaction kettle, reacting for 3-5h at the temperature of 50-70 ℃, and carrying out suction filtration and drying treatment after the reaction is finished to prepare the high-purity bismuth oxide. The method for directly preparing high-purity bismuth oxide from crude bismuth sequentially comprises acid treatment, alkali neutralization and hydrothermal treatment, the purity of purified bismuth oxide is over 99.98%, a hydrothermal method is adopted to replace a high-temperature calcination method in the preparation method, energy consumption is reduced, energy is saved, the preparation method is simple and easy to implement, and the method is an environment-friendly process.
Description
Technical Field
The application relates to a method for directly preparing high-purity bismuth oxide from crude bismuth, belonging to the field of bismuth oxide preparation.
Background
The high-purity bismuth oxide can be used for preparing bismuth salt, and is widely applied to the fields of ceramic coloring, fireproof paper manufacturing, catalysts and the like. In the prior art, bismuth oxide is generally purified by a calcination method, but the prepared bismuth oxide is lemon yellow, and has lower purity, higher impurity content, large energy consumption, more complicated preparation process and lower efficiency compared with high-purity bismuth oxide. Therefore, how to provide a high-purity bismuth oxide preparation process which has high purity, saves energy and is simple in preparation method is an urgent problem to be solved.
Disclosure of Invention
The invention aims to provide a method for directly preparing high-purity bismuth oxide from crude bismuth, which overcomes the defects of low purity, high impurity content, high energy consumption and complicated preparation process of the high-purity bismuth oxide in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the method for directly preparing high-purity bismuth oxide from crude bismuth comprises the following steps:
(1) nitric acid impurity treatment: providing crude bismuth, placing the crude bismuth into a nitric acid solution with the concentration of 2.0-5.0 mol/L, stirring for 30-60min at the temperature of 30-40 ℃, and performing suction filtration and drying treatment to obtain bismuth suboxide nitrate solid;
(2) alkali treatment: putting the bismuth subnitrate solid prepared in the step (1) into an ammonia water-ammonium carbonate buffer solution with the pH value of 9-10, uniformly mixing, and carrying out ultrasonic treatment for 3-5h at normal temperature to prepare a mixed solution;
(3) and (3) placing the mixed solution prepared in the step (2) into a high-pressure reaction kettle, reacting for 3-5 hours at the temperature of 50-70 ℃, and performing suction filtration and drying treatment after the reaction is finished to obtain the high-purity bismuth oxide.
Optionally, the concentration upper limit of the nitric acid solution in the step (1) is selected from 2.5mol/L, 3.0mol/L, 3.5mol/L, 4.0mol/L, 4.5mol/L and 5.0 mol/L; the lower limit of the concentration of the nitric acid solution in the step (1) is selected from 2.0mol/L, 2.5mol/L, 3.0mol/L, 3.5mol/L, 4.0mol/L and 4.5 mol/L.
Optionally, in the suction filtration treatment process in the step (1), a dilute nitric acid concentrated solution with a concentration of 0.1mol/L-1.0mol/L is used for cleaning for 2-3 times, and then deionized water is used for cleaning for 3-5 times.
Optionally, the upper limit of the concentration of the dilute nitric acid in the suction filtration treatment process in the step (1) is selected from 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L, 0.9mol/L and 1.0 mol/L; the lower limit of the concentration of the dilute nitric acid in the suction filtration treatment process in the step (1) is selected from 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L and 0.9 mol/L.
Optionally, in the suction filtration treatment process in the step (1), the diluted nitric acid concentrated solution is adopted to wash the solution for 2 times, and then the solution is washed by deionized water for 5 times.
Optionally, in the suction filtration treatment process in the step (1), the diluted nitric acid concentrated solution is used for cleaning 3 times, and then the deionized water is used for cleaning 3 times.
Optionally, the drying treatment temperature in the step (1) is 30-35 ℃.
Optionally, the drying treatment temperature in the step (1) is 30 ℃.
Optionally, the drying treatment temperature in the step (1) is 31 ℃.
Optionally, the drying treatment temperature in the step (1) is 32 ℃.
Optionally, the drying treatment temperature in the step (1) is 33 ℃.
Optionally, the drying treatment temperature in the step (1) is 34 ℃.
Optionally, the drying treatment temperature in the step (1) is 35 ℃.
Optionally, the concentration of the ammonia in the ammonia-ammonium carbonate buffer solution is 0.1mol/L-1.0 mol/L.
Optionally, the upper limit of the concentration of the ammonia water in the ammonia water-ammonium carbonate buffer solution is selected from 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L, 0.9mol/L and 1.0 mol/L; the lower limit of the concentration of the ammonia water in the ammonia water-ammonium carbonate buffer solution is selected from 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L and 0.9 mol/L.
Optionally, the concentration of ammonium carbonate in the ammonia-ammonium carbonate buffer solution is 1.0mol/L to 2.0 mol/L.
Optionally, the upper limit of the concentration of ammonium carbonate in the ammonia-ammonium carbonate buffer solution is selected from 1.1mol/L, 1.2mol/L, 1.3mol/L, 1.4mol/L, 1.5mol/L, 1.6mol/L, 1.7mol/L, 1.8mol/L, 1.9mol/L, 2.0 mol/L; the lower limit of the concentration of ammonium carbonate in the ammonia water-ammonium carbonate buffer solution is selected from 1.0mol/L, 1.1mol/L, 1.2mol/L, 1.3mol/L, 1.4mol/L, 1.5mol/L, 1.6mol/L, 1.7mol/L, 1.8mol/L and 1.9 mol/L.
Optionally, the concentration of the ammonia in the ammonia-ammonium carbonate buffer solution is 0.5mol/L-1.0 mol/L.
Optionally, the concentration of the ammonia in the ammonia-ammonium carbonate buffer solution is 0.6mol/L-0.8 mol/L.
Optionally, the concentration of ammonium carbonate in the ammonia-ammonium carbonate buffer solution is 1.0mol/L to 1.5 mol/L.
Optionally, the concentration of ammonium carbonate in the ammonia-ammonium carbonate buffer solution is 1.2mol/L to 1.4 mol/L.
Optionally, in the suction filtration treatment process in the step (3), ammonia water concentrated solution with a concentration of 0.1mol/L-1.0mol/L is adopted for cleaning for 3-5 times, and then deionized water is used for cleaning for 3-5 times.
Optionally, the upper limit of the concentration of ammonia water in the suction filtration treatment process in the step (3) is selected from 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L and 0 ℃; 8mol/L, 0.9mol/L and 1.0 mol/L; the lower limit of the concentration of ammonia water in the suction filtration treatment process in the step (3) is selected from 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L and 0; 8mol/L and 0.9 mol/L.
Optionally, in the suction filtration treatment process in the step (3), ammonia water is used for washing for 3 times, and then deionized water is used for washing for 4 times.
Optionally, in the suction filtration treatment process in the step (3), ammonia water is used for washing for 5 times, and then deionized water is used for washing for 3 times.
Optionally, the drying treatment temperature in the step (3) is 40-50 ℃, and the drying time is 3-5 h.
Optionally, placing the mixed solution prepared in the step (2) into a high-pressure reaction kettle, and reacting for 3-4h at the temperature of 50-60 ℃.
Compared with the prior art, the invention has the advantages that: the method for directly preparing high-purity bismuth oxide from crude bismuth sequentially comprises acid treatment, alkali neutralization and hydrothermal treatment, the purity of purified bismuth oxide is over 99.98%, a hydrothermal method is adopted to replace a high-temperature calcination method in the preparation method, energy consumption is reduced, energy is saved, the preparation method is simple and easy to implement, and the method is an environment-friendly process.
Detailed Description
In view of the deficiencies in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide technical solutions of the present invention. The technical solution, its implementation and principles, etc. will be further explained as follows.
The method for directly preparing high-purity bismuth oxide from crude bismuth comprises the following steps:
(1) nitric acid impurity treatment: providing crude bismuth, placing the crude bismuth into a nitric acid solution with the concentration of 2.0-5.0 mol/L, stirring for 30-60min at the temperature of 30-40 ℃, and performing suction filtration and drying treatment to obtain bismuth suboxide nitrate solid;
(2) alkali treatment: putting the bismuth subnitrate solid prepared in the step (1) into an ammonia water-ammonium carbonate buffer solution with the pH value of 9-10, uniformly mixing, and carrying out ultrasonic treatment for 3-5h at normal temperature to prepare a mixed solution;
(3) and (3) placing the mixed solution prepared in the step (2) into a high-pressure reaction kettle, reacting for 3-5 hours at the temperature of 50-70 ℃, and performing suction filtration and drying treatment after the reaction is finished to obtain the high-purity bismuth oxide.
Optionally, the concentration upper limit of the nitric acid solution in the step (1) is selected from 2.5mol/L, 3.0mol/L, 3.5mol/L, 4.0mol/L, 4.5mol/L and 5.0 mol/L; the lower limit of the concentration of the nitric acid solution in the step (1) is selected from 2.0mol/L, 2.5mol/L, 3.0mol/L, 3.5mol/L, 4.0mol/L and 4.5 mol/L.
Optionally, in the suction filtration treatment process in the step (1), a dilute nitric acid concentrated solution with a concentration of 0.1mol/L-1.0mol/L is used for cleaning for 2-3 times, and then deionized water is used for cleaning for 3-5 times.
Optionally, the upper limit of the concentration of the dilute nitric acid in the suction filtration treatment process in the step (1) is selected from 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L, 0.9mol/L and 1.0 mol/L; the lower limit of the concentration of the dilute nitric acid in the suction filtration treatment process in the step (1) is selected from 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L and 0.9 mol/L.
Optionally, in the suction filtration treatment process in the step (1), the diluted nitric acid concentrated solution is adopted to wash the solution for 2 times, and then the solution is washed by deionized water for 5 times.
Optionally, in the suction filtration treatment process in the step (1), the diluted nitric acid concentrated solution is used for cleaning 3 times, and then the deionized water is used for cleaning 3 times.
Optionally, the drying treatment temperature in the step (1) is 30-35 ℃.
Optionally, the drying treatment temperature in the step (1) is 30 ℃.
Optionally, the drying treatment temperature in the step (1) is 31 ℃.
Optionally, the drying treatment temperature in the step (1) is 32 ℃.
Optionally, the drying treatment temperature in the step (1) is 33 ℃.
Optionally, the drying treatment temperature in the step (1) is 34 ℃.
Optionally, the drying treatment temperature in the step (1) is 35 ℃.
Optionally, the concentration of the ammonia in the ammonia-ammonium carbonate buffer solution is 0.1mol/L-1.0 mol/L.
Optionally, the upper limit of the concentration of the ammonia water in the ammonia water-ammonium carbonate buffer solution is selected from 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L, 0.9mol/L and 1.0 mol/L; the lower limit of the concentration of the ammonia water in the ammonia water-ammonium carbonate buffer solution is selected from 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L and 0.9 mol/L.
Optionally, the concentration of ammonium carbonate in the ammonia-ammonium carbonate buffer solution is 1.0mol/L to 2.0 mol/L.
Optionally, the upper limit of the concentration of ammonium carbonate in the ammonia-ammonium carbonate buffer solution is selected from 1.1mol/L, 1.2mol/L, 1.3mol/L, 1.4mol/L, 1.5mol/L, 1.6mol/L, 1.7mol/L, 1.8mol/L, 1.9mol/L, 2.0 mol/L; the lower limit of the concentration of ammonium carbonate in the ammonia water-ammonium carbonate buffer solution is selected from 1.0mol/L, 1.1mol/L, 1.2mol/L, 1.3mol/L, 1.4mol/L, 1.5mol/L, 1.6mol/L, 1.7mol/L, 1.8mol/L and 1.9 mol/L.
Optionally, the concentration of the ammonia in the ammonia-ammonium carbonate buffer solution is 0.5mol/L-1.0 mol/L.
Optionally, the concentration of the ammonia in the ammonia-ammonium carbonate buffer solution is 0.6mol/L-0.8 mol/L.
Optionally, the concentration of ammonium carbonate in the ammonia-ammonium carbonate buffer solution is 1.0mol/L to 1.5 mol/L.
Optionally, the concentration of ammonium carbonate in the ammonia-ammonium carbonate buffer solution is 1.2mol/L to 1.4 mol/L.
Optionally, in the suction filtration treatment process in the step (3), ammonia water concentrated solution with a concentration of 0.1mol/L-1.0mol/L is adopted for cleaning for 3-5 times, and then deionized water is used for cleaning for 3-5 times.
Optionally, the upper limit of the concentration of ammonia water in the suction filtration treatment process in the step (3) is selected from 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L and 0 ℃; 8mol/L, 0.9mol/L and 1.0 mol/L; the lower limit of the concentration of ammonia water in the suction filtration treatment process in the step (3) is selected from 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L and 0; 8mol/L and 0.9 mol/L.
Optionally, in the suction filtration treatment process in the step (3), ammonia water is used for washing for 3 times, and then deionized water is used for washing for 4 times.
Optionally, in the suction filtration treatment process in the step (3), ammonia water is used for washing for 5 times, and then deionized water is used for washing for 3 times.
Optionally, the drying treatment temperature in the step (3) is 40-50 ℃, and the drying time is 3-5 h.
Optionally, placing the mixed solution prepared in the step (2) into a high-pressure reaction kettle, and reacting for 3-4h at the temperature of 50-60 ℃.
The technical solution of the present invention is further explained below with reference to several examples.
Each of the substances in the examples of the present application is commercially available.
Example 1
The method for directly preparing high-purity bismuth oxide from crude bismuth comprises the following steps:
(1) nitric acid impurity treatment: providing crude bismuth, placing the crude bismuth into a nitric acid solution with the concentration of 2.0mol/L, stirring for 30-60min at the temperature of 30-40 ℃, and performing suction filtration and drying treatment to obtain bismuth suboxide nitrate solid;
(2) alkali treatment: putting the bismuth subnitrate solid prepared in the step (1) into an ammonia water-ammonium carbonate buffer solution with the pH value of 9, uniformly mixing, and carrying out ultrasonic treatment for 3-5h at normal temperature to prepare a mixed solution;
(3) and (3) placing the mixed solution prepared in the step (2) into a high-pressure reaction kettle, reacting for 3-5 hours at the temperature of 50-70 ℃, and performing suction filtration and drying treatment after the reaction is finished to obtain the high-purity bismuth oxide.
And (2) in the suction filtration treatment process in the step (1), washing the solution for 3 times by using deionized water after washing the solution for 3 times by using dilute nitric acid concentrated solution with the concentration of 0.1 mol/L.
The drying temperature in the step (1) is 30 ℃.
The concentration of the ammonia water in the ammonia water-ammonium carbonate buffer solution is 0.1 mol/L.
The concentration of ammonium carbonate in the ammonia water-ammonium carbonate buffer solution is 1.0 mol/L.
And (3) in the suction filtration treatment process in the step (3), ammonia water concentrated solution with the concentration of 0.1mol/L is adopted for cleaning for 3 times, and then deionized water is used for cleaning for 5 times.
The drying treatment temperature in the step (3) is 40 ℃, and the drying time is 3 h.
Example 2
The method for directly preparing high-purity bismuth oxide from crude bismuth comprises the following steps:
(1) nitric acid impurity treatment: providing crude bismuth, placing the crude bismuth into a nitric acid solution with the concentration of 3.0mol/L, stirring for 30-60min at the temperature of 30-40 ℃, and performing suction filtration and drying treatment to obtain bismuth suboxide nitrate solid;
(2) alkali treatment: putting the bismuth subnitrate solid prepared in the step (1) into an ammonia water-ammonium carbonate buffer solution with the pH value of 9.5, uniformly mixing, and carrying out ultrasonic treatment for 3-5h at normal temperature to prepare a mixed solution;
(3) and (3) placing the mixed solution prepared in the step (2) into a high-pressure reaction kettle, reacting for 3-5 hours at the temperature of 50-70 ℃, and performing suction filtration and drying treatment after the reaction is finished to obtain the high-purity bismuth oxide.
And (2) in the suction filtration treatment process in the step (1), washing with dilute nitric acid concentrated solution with the concentration of 0.5mol/L for 2 times, and then washing with deionized water for 4 times.
The drying treatment temperature in the step (1) is 32 ℃.
The concentration of the ammonia water in the ammonia water-ammonium carbonate buffer solution is 0.5 mol/L.
The concentration of ammonium carbonate in the ammonia water-ammonium carbonate buffer solution is 1.5 mol/L.
And (3) in the suction filtration treatment process in the step (3), ammonia water concentrated solution with the concentration of 0.5mol/L is adopted for cleaning for 3 times, and then deionized water is used for cleaning for 5 times.
The drying treatment temperature in the step (3) is 45 ℃, and the drying time is 4 h.
Example 3
The method for directly preparing high-purity bismuth oxide from crude bismuth comprises the following steps:
(1) nitric acid impurity treatment: providing crude bismuth, placing the crude bismuth into a nitric acid solution with the concentration of 4.0mol/L, stirring for 30-60min at the temperature of 30-40 ℃, and performing suction filtration and drying treatment to obtain bismuth suboxide nitrate solid;
(2) alkali treatment: putting the bismuth subnitrate solid prepared in the step (1) into an ammonia water-ammonium carbonate buffer solution with the pH value of 10, uniformly mixing, and carrying out ultrasonic treatment for 3-5h at normal temperature to prepare a mixed solution;
(3) and (3) placing the mixed solution prepared in the step (2) into a high-pressure reaction kettle, reacting for 3-5 hours at the temperature of 50-70 ℃, and performing suction filtration and drying treatment after the reaction is finished to obtain the high-purity bismuth oxide.
And (2) in the suction filtration treatment process in the step (1), washing with dilute nitric acid concentrated solution with the concentration of 1.0mol/L for 2 times, and then washing with deionized water for 5 times.
The drying temperature in the step (1) is 35 ℃.
The concentration of the ammonia water in the ammonia water-ammonium carbonate buffer solution is 1.0 mol/L.
The concentration of ammonium carbonate in the ammonia water-ammonium carbonate buffer solution is 2.0 mol/L.
And (3) in the suction filtration treatment process in the step (3), ammonia water concentrated solution with the concentration of 0.5mol/L is adopted for cleaning for 3 times, and then deionized water is used for cleaning for 5 times.
The drying treatment temperature in the step (3) is 50 ℃, and the drying time is 3 h.
The purity detection of the high-purity bismuth oxide prepared in the embodiments 1 to 3 shows that the purity of the bismuth oxide is over 99.98, and the preparation method is simple and feasible, energy-saving and environment-friendly.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present invention, which are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and therefore, the protection scope of the present invention is not limited thereby. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. The method for directly preparing high-purity bismuth oxide from crude bismuth is characterized by comprising the following steps of:
(1) nitric acid impurity treatment: providing crude bismuth, placing the crude bismuth into a nitric acid solution with the concentration of 2.0-5.0 mol/L, stirring for 30-60min at the temperature of 30-40 ℃, and performing suction filtration and drying treatment to obtain bismuth suboxide nitrate solid;
(2) alkali treatment: putting the bismuth subnitrate solid prepared in the step (1) into an ammonia water-ammonium carbonate buffer solution with the pH value of 9-10, uniformly mixing, and carrying out ultrasonic treatment for 3-5h at normal temperature to prepare a mixed solution;
(3) and (3) placing the mixed solution prepared in the step (2) into a high-pressure reaction kettle, reacting for 3-5 hours at the temperature of 50-70 ℃, and performing suction filtration and drying treatment after the reaction is finished to obtain the high-purity bismuth oxide.
2. The method for directly preparing high-purity bismuth oxide from crude bismuth according to claim 1, wherein in the suction filtration treatment in the step (1), the crude bismuth is washed with 0.1mol/L-1.0mol/L dilute nitric acid concentrated solution for 2-3 times and then washed with deionized water for 3-5 times.
3. The method for directly preparing high-purity bismuth oxide from crude bismuth according to claim 1, wherein the concentration of nitric acid in the step (1) is 2.0 mol/L-4.0 mol/L;
preferably, the concentration of the nitric acid in the step (1) is 2.0 mol/L-3.0 mol/L.
4. The method for directly preparing high-purity bismuth oxide from crude bismuth according to claim 1, wherein the drying temperature in the step (1) is 30-35 ℃.
5. The method for directly preparing high-purity bismuth oxide from crude bismuth according to claim 1, wherein the concentration of ammonia in the ammonia-ammonium carbonate buffer solution is 0.1-1.0 mol/L;
preferably, the concentration of ammonium carbonate in the ammonia-ammonium carbonate buffer solution is 1.0mol/L-2.0 mol/L.
6. The method for directly preparing high-purity bismuth oxide from crude bismuth according to claim 5, wherein the concentration of ammonia in the ammonia-ammonium carbonate buffer solution is 0.5-1.0 mol/L;
preferably, the concentration of the ammonia water in the ammonia water-ammonium carbonate buffer solution is 0.6-0.8 mol/L.
7. The method for directly preparing high-purity bismuth oxide from crude bismuth according to claim 5, wherein the concentration of ammonium carbonate in the ammonia-ammonium carbonate buffer solution is 1.0mol/L-1.5 mol/L;
preferably, the concentration of ammonium carbonate in the ammonia-ammonium carbonate buffer solution is 1.2mol/L-1.4 mol/L.
8. The method for directly preparing high-purity bismuth oxide from crude bismuth according to claim 1, wherein the filtration treatment in the step (3) is performed by washing with 0.1mol/L-1.0mol/L ammonia water concentrated solution for 3-5 times, and then washing with deionized water for 3-5 times.
9. The method for directly preparing high-purity bismuth oxide from crude bismuth according to claim 1, wherein the drying treatment temperature in the step (3) is 40-50 ℃, and the drying time is 3-5 h.
10. The method for directly preparing high-purity bismuth oxide from crude bismuth according to claim 1, wherein the mixed solution obtained in the step (2) is placed in a high-pressure reaction kettle and reacts for 3-4 hours at the temperature of 50-60 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110250557.0A CN113003605A (en) | 2021-03-08 | 2021-03-08 | Method for directly preparing high-purity bismuth oxide from crude bismuth |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110250557.0A CN113003605A (en) | 2021-03-08 | 2021-03-08 | Method for directly preparing high-purity bismuth oxide from crude bismuth |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113003605A true CN113003605A (en) | 2021-06-22 |
Family
ID=76408278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110250557.0A Pending CN113003605A (en) | 2021-03-08 | 2021-03-08 | Method for directly preparing high-purity bismuth oxide from crude bismuth |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113003605A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113800561A (en) * | 2021-10-25 | 2021-12-17 | 烟台佳隆纳米产业有限公司 | Method for industrially producing bismuth oxide fibers |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049966A (en) * | 2007-03-28 | 2007-10-10 | 湖南金旺实业有限公司 | Method for producing powder in micron order of bismuth oxide |
| CN102242271A (en) * | 2011-06-15 | 2011-11-16 | 金川集团有限公司 | Method for preparing bismuth oxide from bismuth-containing solution with high concentration of copper |
-
2021
- 2021-03-08 CN CN202110250557.0A patent/CN113003605A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049966A (en) * | 2007-03-28 | 2007-10-10 | 湖南金旺实业有限公司 | Method for producing powder in micron order of bismuth oxide |
| CN102242271A (en) * | 2011-06-15 | 2011-11-16 | 金川集团有限公司 | Method for preparing bismuth oxide from bismuth-containing solution with high concentration of copper |
Non-Patent Citations (1)
| Title |
|---|
| 吴文伟等: "一种由粗铋直接制备高纯氧化铋的方法" * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113800561A (en) * | 2021-10-25 | 2021-12-17 | 烟台佳隆纳米产业有限公司 | Method for industrially producing bismuth oxide fibers |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2016180288A1 (en) | Methodsmethod for preparing nickel-cobalt-aluminum precursor material andor positive electrode material with gradient distribution of aluminum element | |
| CN102513085B (en) | Cerium oxide-zirconium oxide-based composite oxide and preparation method thereof | |
| EP4354548A1 (en) | Multi-element partition-doped cobalt-free positive electrode material and preparation method therefor | |
| CN113793927B (en) | Ternary cathode material of lithium ion battery and preparation method thereof | |
| CN102001835B (en) | Method for preparing modified glass microspheres | |
| CN106166487A (en) | A kind of quaternary composite oxides low-temperature SCR catalyst and preparation method thereof | |
| CN110898794A (en) | Preparation method of lithium ion sieve | |
| CN108031479A (en) | A kind of preparation method of beta bismuth oxide-bismoclite | |
| CN113003605A (en) | Method for directly preparing high-purity bismuth oxide from crude bismuth | |
| CN103165912A (en) | Catalytic agent for lithium-air battery cathode and preparation method | |
| CN114094080B (en) | Single crystal type lithium-rich layered-spinel composite positive electrode material and preparation method thereof | |
| CN102275984A (en) | Method for preparing pure anatase phase nano titanium dioxide | |
| CN116177625A (en) | Method for reducing residual alkali on surface of nickel-based positive electrode material and application thereof | |
| CN104043390B (en) | A kind of nano-heterogeneous structure hollow ball of small size high-specific surface area and preparation method thereof | |
| CN103706386A (en) | Ag2CO3 / SrCO3 visible light catalyst and preparation method thereof | |
| CN102557133B (en) | Method for preparing fishbone-shaped and firewood-shaped BiVO4 powder by microwave hydrothermal method | |
| CN101696032B (en) | Method for preparing chromium and nitrogen co-doping nano-titanium dioxide powders | |
| CN112591792A (en) | Simple preparation method of colored titanium dioxide for photocatalysis | |
| CN107265401A (en) | A kind of PDA/Bi AgIn5S8/TiO2Heterojunction photovoltaic pole and preparation method and purposes | |
| CN103447020A (en) | Composite metal oxide catalyst for preparing biodiesel | |
| CN108479842B (en) | Preparation method of Bi5O7NO3 or Ag/Bi5O7NO3 composite photocatalytic material | |
| CN116207318A (en) | All-vanadium redox flow battery electrolyte and preparation method thereof | |
| CN114084917B (en) | Nickel-cobalt-manganese ternary precursor with XRD diffraction bifurcation double peak and preparation method thereof | |
| CN101168453A (en) | Method for treating (SO4)2- impurity of spherical nickel hydroxide | |
| CN109888112A (en) | A method of efficient stable perovskite solar battery is prepared using cerium oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210622 |