CN104030353A - Normal-pressure hydrothermal-method phase inversion process of bismuth oxide - Google Patents
Normal-pressure hydrothermal-method phase inversion process of bismuth oxide Download PDFInfo
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- CN104030353A CN104030353A CN201410278504.XA CN201410278504A CN104030353A CN 104030353 A CN104030353 A CN 104030353A CN 201410278504 A CN201410278504 A CN 201410278504A CN 104030353 A CN104030353 A CN 104030353A
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Abstract
The invention provides a normal-pressure hydrothermal-method phase inversion process of bismuth oxide. According to the process, beta bismuth oxide is directly converted into alpha bismuth oxide in an aqueous phase without medium/high-temperature calcined conversion; the reaction process is that beta bismuth oxide and H2O are converted into alpha bismuth oxide and H2O at the temperature of 100 DEG C. The process is a brand-new process and is energy-saving and environment-friendly; compared with other alpha bismuth oxide preparation processes, the process is simple and practical and is very environment-friendly; the product purity is very high, the content of bismuth oxide can reach 99.9%, and the content of all kinds of impurities is low; and the process is widely applied to the aspects of electronics, articles for daily use, war industry and the like.
Description
Technical field
The present invention is a kind of constant pressure hydro-thermal method phase transfer process of bismuth oxide, belongs to crystal preparing technology field.
Background technology
Bismuth oxide sterling has α type and β type.α type bismuth oxide is yellow monoclinic system crystal, and relative density is 8.9, and 825 DEG C of fusing points, are dissolved in acid, water insoluble and alkali.β type bismuth oxide is that glassy yellow is extremely orange, tetragonal spheroidal, and relative density 8.55,860 DEG C of fusing points, are dissolved in acid, water insoluble, and easily by hydrogen, hydro carbons etc. are reduced to bismuth metal.From Hu'nan Jinwang Bismuth Industry PLC take the lead in preparing by oxygen manufacture oxidation bismuth oxide for suitability for industrialized production after, α bismuth oxide has had new production technique; That is: being prepared into bismuth oxide by electric arc furnace direct oxidation is beta-oxidation bismuth, and existing market demand is generally α bismuth oxide, and traditional phase inversion is by chemical method, or middle high-temperature calcination phase inversion is realized.Described chemical method is to be dissolved in excessive nitric acid by bismuth ingot, then converts bismuth subnitrate to by adding alkali, carries out middle high-temperature calcination be prepared into α bismuth oxide by bismuth subnitrate solution; This technique supplementary product onsumption is high, and cost is high, and environment is unfriendly, and explained hereafter long flow path, and energy consumption is also high.Described middle high-temperature calcination phase inversion is to use arc process to be prepared into beta-oxidation bismuth, then carries out high-temperature calcination in 550～800 DEG C by beta-oxidation bismuth and obtain α bismuth oxide, and middle high-temperature calcination phase transfer process environmental friendliness is with low cost, but phase inversion still exists greater energy consumption.
On 02 13rd, 2013, Hu'nan Jinwang Bismuth Industry PLC is in Chinese invention patent application publication number CN102923772A, a kind of bismuth oxide hydrothermal method phase inversion method is disclosed, that beta-oxidation bismuth is processed into after the powder that granularity is 500～600 nanometers, in water, be directly changed into α bismuth oxide, transform without high-temperature calcination in process, reaction process is: β type bismuth oxide+H
2o
heat→ α type bismuth oxide+H
2o.This technique needs two conditions, and the one, beta-oxidation bismuth will be processed into the powder that granularity is 500～600 nanometers; The 2nd, phase inversion needs the pressure of 2atm～20atm.Thereby processing unit is proposed to harsh requirement.
Summary of the invention
Technical problem to be solved by this invention is to have overcome in aforesaid method not enough, a kind of constant pressure hydro-thermal method phase transfer process of bismuth oxide is provided, make beta-oxidation bismuth in water, be directly changed into α bismuth oxide, transform without high-temperature calcination in process, processing unit of the present invention is simple and practical, without sour supplementary product onsumption, very friendly to environment, product purity is very high, and bismuth oxide content can reach 99.9%.
The present invention realizes by the following technical solutions:
A kind of constant pressure hydro-thermal method phase transfer process of bismuth oxide, under normal pressure, convert β type bismuth oxide to α bismuth oxide by hydrothermal method, specifically: under 1atm pressure, get during KOH or NaOH be soluble in the aqueous phase, controlling in water KOH or NaOH mass percentage content is 1～1.1%; Beta-oxidation bismuth raw material is scattered in water with the ratio of mass volume ratio 1:3～5g/ml, at 85～100 DEG C, switching time 0.1h～5h, after reaction to be converted completes, adopt liquid-solid separation equipment separating alpha bismuth oxide and the waters such as centrifugation apparatus, press filtration, suction filtration, the α bismuth oxide product of the certain moisture of gained band is dried under 80～50 DEG C of conditions, separation containing OH
-water return system continue on for being converted to as beta-oxidation bismuth dispersion agent and the medium of α bismuth oxide; Reaction equation: β type bismuth oxide+OH
-(100 DEG C) → α type bismuth oxide+OH
-.
The hydrothermal growth of α type bismuth oxide crystal of the present invention, the hot water dissolving who utilizes normal atmosphere conditions, make to be scattered in the β type bismuth oxide in water, generate lysate by solubilizing reaction, and reach certain degree of supersaturation and carry out crystallization and be grown to α type bismuth oxide crystal.
Compared with the prior art: the present invention makes β type bismuth oxide in water, be directly changed into α type bismuth oxide, transform without high-temperature calcination in process, phase inversion of the present invention is using water molecules as medium, not using other any chemical assistants, is a kind of brand-new technique, and production technique is simple, equipment is simple, with low cost, energy consumption is low, and phase inversion temperature is low.The water of the separation producing remains containing OH
-water, very friendly to environment without outer row.By XRD crystalline phase, figure can observe, and the present invention is prepared into bar-shaped α type bismuth oxide, and pattern is even, good dispersity, and product purity is very high, and bismuth oxide content can reach 99.9%, and all kinds of impurity is low.
The positive effect of the present invention and CN102923772A comparison is, under normal pressure, produce, normal temperature or≤100 DEG C, equipment, technique are simple, with low cost, energy consumption is low, phase inversion temperature is low, this products material is that arc process is prepared into beta-oxidation bismuth.Do not need beta-oxidation bismuth will be processed into the powder that granularity is 500～600 nanometers; To processing unit without harsh requirement.Therefore production cost is obviously demoted more than 80% than CN102923772A, is that those skilled in the art cannot expect.
Brief description of the drawings
Fig. 1 is β type bismuth oxide XRD figure before phase inversion of the present invention.
Fig. 2 is α type bismuth oxide XRD figure after phase inversion of the present invention.
Embodiment
Below by embodiment, the present invention is specifically described, the present embodiment is to further illustrate of the present invention, is not limiting the scope of the invention, and the person skilled in the art in this field can carry out nonessential improvement and adjustment according to content of the present invention.
The β type bismuth oxide of the present embodiment is prepared by arc process, and before phase inversion, β type bismuth oxide crystalline phase XRD is shown in accompanying drawing 1.Take 30.0g beta-oxidation bismuth, 1.0g sodium hydroxide, adds in the beaker that 90ml water is housed, and under normal temperature and pressure, stirs 3h, filters, at 105 DEG C, dries to obtain product 29.73g, reduces weight and be mainly material transfer loss after reaction; After hydrothermal method phase inversion, α type bismuth oxide crystalline phase XRD is shown in accompanying drawing 2.
Claims (1)
1. the constant pressure hydro-thermal method phase transfer process of a bismuth oxide, under normal pressure, convert β type bismuth oxide to α bismuth oxide by hydrothermal method, it is characterized in that: under 1atm pressure, get during KOH or NaOH be soluble in the aqueous phase, controlling in water KOH or NaOH mass percentage content is 1～1.1%; Beta-oxidation bismuth raw material is scattered in water with the ratio of mass volume ratio 1:3～5g/ml, at 85～100 DEG C, switching time 0.1h～5h, after reaction to be converted completes, adopt liquid-solid separation equipment separating alpha bismuth oxide and the waters such as centrifugation apparatus, press filtration, suction filtration, the α bismuth oxide product of the certain moisture of gained band is dried under 80～50 DEG C of conditions, separation containing OH
-water return system continue on for being converted to as beta-oxidation bismuth dispersion agent and the medium of α bismuth oxide; Reaction equation: β type bismuth oxide+OH
-(100 DEG C) → α type bismuth oxide+OH
-.
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| CN201410278504.XA CN104030353B (en) | 2014-06-20 | 2014-06-20 | A kind of constant pressure hydro-thermal method phase transfer process of bismuth oxide |
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| CN104030353A true CN104030353A (en) | 2014-09-10 |
| CN104030353B CN104030353B (en) | 2015-12-09 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107720821A (en) * | 2017-11-25 | 2018-02-23 | 贵溪三元金属有限公司 | A kind of constant pressure hydro-thermal method phase transfer process of bismuth oxide |
| CN108889292A (en) * | 2018-06-21 | 2018-11-27 | 河南师范大学 | A kind of growth in situ α/β-Bi2O3The method of composite photocatalyst material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311360A (en) * | 2008-04-16 | 2008-11-26 | 中国科学院上海光学精密机械研究所 | Synthetic method for one-dimensional single crystal bismuth oxide nano material |
| CN102320657A (en) * | 2011-08-04 | 2012-01-18 | 西南石油大学 | Method for preparing gamma-phase bismuth oxide |
| CN102923772A (en) * | 2012-11-12 | 2013-02-13 | 湖南金旺铋业股份有限公司 | Phase inversion method of bismuth oxide hydrothermal method |
| CN103145184A (en) * | 2013-03-25 | 2013-06-12 | 湖南金旺铋业股份有限公司 | Process for preparing needle-like bismuth oxide from bismuth by using wet method |
| CN103183382A (en) * | 2013-03-25 | 2013-07-03 | 湖南金旺铋业股份有限公司 | Method for preparing acicular bismuth oxide with bismuth metal |
-
2014
- 2014-06-20 CN CN201410278504.XA patent/CN104030353B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311360A (en) * | 2008-04-16 | 2008-11-26 | 中国科学院上海光学精密机械研究所 | Synthetic method for one-dimensional single crystal bismuth oxide nano material |
| CN102320657A (en) * | 2011-08-04 | 2012-01-18 | 西南石油大学 | Method for preparing gamma-phase bismuth oxide |
| CN102923772A (en) * | 2012-11-12 | 2013-02-13 | 湖南金旺铋业股份有限公司 | Phase inversion method of bismuth oxide hydrothermal method |
| CN103145184A (en) * | 2013-03-25 | 2013-06-12 | 湖南金旺铋业股份有限公司 | Process for preparing needle-like bismuth oxide from bismuth by using wet method |
| CN103183382A (en) * | 2013-03-25 | 2013-07-03 | 湖南金旺铋业股份有限公司 | Method for preparing acicular bismuth oxide with bismuth metal |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107720821A (en) * | 2017-11-25 | 2018-02-23 | 贵溪三元金属有限公司 | A kind of constant pressure hydro-thermal method phase transfer process of bismuth oxide |
| CN108889292A (en) * | 2018-06-21 | 2018-11-27 | 河南师范大学 | A kind of growth in situ α/β-Bi2O3The method of composite photocatalyst material |
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| CN104030353B (en) | 2015-12-09 |
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