CN102923772B - Phase inversion method of bismuth oxide hydrothermal method - Google Patents
Phase inversion method of bismuth oxide hydrothermal method Download PDFInfo
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- CN102923772B CN102923772B CN201210448157.1A CN201210448157A CN102923772B CN 102923772 B CN102923772 B CN 102923772B CN 201210448157 A CN201210448157 A CN 201210448157A CN 102923772 B CN102923772 B CN 102923772B
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Abstract
The invention provides a phase inversion method of a bismuth oxide hydrothermal method. The phase inversion method of the bismuth oxide hydrothermal method includes that beta bismuth oxide is directly converted to alpha bismuth oxide in aqueous phase without need for conversion through middle-high-temperature calcination. A reaction process includes that the beta bismuth oxide and H2O are heated to form the alpha bismuth oxide and the H2O. The phase inversion method of the bismuth oxide hydrothermal method is a brand-novel technology, energy-saving and environmental-friendly. Compared with other methods which are used for preparing of the alpha bismuth oxide, the phase inversion method of the bismuth oxide hydrothermal method is simple and practical in craft, quite good in environmental protection, quite high in product fitness, and low in various kinds of impurities, and can achieve 99.9% bismuth oxide content, and can be widely applied to electron, daily commodity, war industry and the like.
Description
Technical field
The present invention is a kind of bismuth oxide hydrothermal method phase inversion method, 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 ℃ 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 ℃ of fusing points, are dissolved in acid, water insoluble.Easily, by hydrogen, hydro carbons etc. are reduced to bismuth metal.α type bismuth oxide is than β type bismuth oxide excellent performance, applied range.If the aspects such as catalyzer, electric slurry, ceramic fabric, medicine, red glass Synergist S-421 95 are all to use α type bismuth oxide.But, the preparation of prior art electric arc pyrogenic process, what obtain is β type bismuth oxide, need to be converted to α type bismuth oxide.Traditional phase inversion is by chemical method, or in 550～800 ℃, high-temperature calcination realizes.Chemical method is produced α type bismuth oxide, and 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; Middle high-temperature calcination phase transfer process environmental friendliness, with low cost, but still there is greater energy consumption in phase inversion.
Summary of the invention
Technical problem to be solved by this invention is to have overcome in aforesaid method not enough, and a kind of bismuth oxide hydrothermal method phase inversion method is provided, and it is low that the present invention has energy consumption, and without soda acid supplementary product onsumption, manufacturing cost is all low, environmental protection.
The present invention is by being realized by following technical scheme:
A kind of bismuth oxide hydrothermal method phase inversion method, is to convert β type bismuth oxide to α type bismuth oxide by hydrothermal method, comprises the following steps:
1. by β type bismuth oxide routinely art breading to become granularity be the powder of 500～600 nanometers;
2. with the ratio of liquid-solid ratio 3～5:1ml/g, β type bismuth oxide is added in the autoclave that pure water is housed, dispersed with stirring, makes β type bismuth oxide be scattered in form slurry in water; Continue to stir heating, sealing pressing; Control condition is: 85～180 ℃ of pyroreaction still interior reaction temperatures, pressure 2atm～20atm, heating 0.2h～12h switching time;
Reaction equation: β type bismuth oxide+H
2o
heat→ α type bismuth oxide+H
2o
3. after reaction to be converted completes, adopt centrifugation apparatus, press filtration, suction filtration separating alpha type bismuth oxide and water, the α type bismuth oxide product of the certain moisture of gained band is dried 12h under 80～105 ℃ of conditions;
4. the water separating remains pure water, and return system continues on for being converted to as β type bismuth oxide the dispersion agent of α type bismuth oxide.
The hydrothermal growth of α type bismuth oxide crystal of the present invention, it is the water dissolution of utilizing High Temperature High Pressure, make the β type bismuth oxide being insoluble under normal atmosphere conditions, 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 pure 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.Be widely used in electronics, daily, the aspects such as military project.
Accompanying drawing explanation
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.
Embodiment 1
The β type bismuth oxide powder of the present embodiment is prepared by arc process, and granularity is 500;
Before phase inversion, β type bismuth oxide crystalline phase XRD is shown in accompanying drawing 1.Take 30.0g β type bismuth oxide powder and add in 90ml pure water, dispersed with stirring is boiled 12h under 2atm air pressure, 85 ℃ of temperature of reaction.Product is through filtering, and at 80 ℃, dry 12h, obtains α type bismuth oxide 29.75g.By analysis, gained α type bismuth oxide is bar-shaped, and bismuth oxide content can reach 99.9%; And pattern is even, after reaction, reduces weight and be mainly material transfer loss; After hydrothermal method phase inversion, α type bismuth oxide crystalline phase XRD is shown in accompanying drawing 2.
Embodiment 2
The β type bismuth oxide powder granularity of the present embodiment is 600;
Take 30.0g β type bismuth oxide and add in the autoclave that 90ml water is housed, pyroreaction still is placed in to baking oven, 120 ℃ of temperature of reaction; Under 10atm air pressure, heat 8h, take out after cooling autoclave, through filtering, drying 12h obtain product 29.83g at 105 ℃.By analysis, gained α type bismuth oxide is bar-shaped, and bismuth oxide content can reach 99.9%; And pattern is even, after reaction, reduces weight and be mainly material transfer loss.
Embodiment 3
The β type bismuth oxide powder granularity of the present embodiment is 550; Take 30.0g β type bismuth oxide and add in 90ml water, dispersed with stirring, 180 ℃ of temperature of reaction are boiled 0.2h under 20atm air pressure, and product entered filtration, 100 degrees Celsius of dry 12h, obtained α type bismuth oxide 29.8g.By analysis, gained α type bismuth oxide is bar-shaped, and bismuth oxide content can reach 99.9%; And pattern is even, after reaction, reduces weight and be mainly material transfer loss.
Claims (1)
1. a bismuth oxide hydrothermal method phase inversion method, is characterized in that converting β type bismuth oxide to α type bismuth oxide by hydrothermal method, comprises the following steps:
1. by β type bismuth oxide routinely art breading to become granularity be the powder of 500～600 nanometers;
2. with the ratio of liquid-solid ratio 3～5:1ml/g, β type bismuth oxide is added in the autoclave that pure water is housed, dispersed with stirring, makes β type bismuth oxide be scattered in form slurry in water; Continue to stir heating, sealing pressing; Control condition is: 85～180 ℃ of pyroreaction still interior reaction temperatures, pressure 2atm～20atm, heating 0.2h～12h switching time;
Reaction equation: β type bismuth oxide+H
2o
heat→ α type bismuth oxide+H
2o;
3. after reaction to be converted completes, adopt centrifugation apparatus, press filtration, suction filtration separating alpha type bismuth oxide and water, the α type bismuth oxide product of the certain moisture of gained band is dried 12h under 80～105 ℃ of conditions;
4. the water separating remains pure water, and return system continues on for being converted to as β type bismuth oxide the dispersion agent of α type bismuth oxide.
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| CN104030352B (en) * | 2014-06-20 | 2015-12-09 | 湖南金旺铋业股份有限公司 | A kind of constant pressure hydro-thermal method phase inversion process of bismuth oxide |
| CN104030353B (en) * | 2014-06-20 | 2015-12-09 | 湖南金旺铋业股份有限公司 | A kind of constant pressure hydro-thermal method phase transfer process of bismuth oxide |
| 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 |
Citations (1)
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| CN102320657A (en) * | 2011-08-04 | 2012-01-18 | 西南石油大学 | Method for preparing gamma-phase bismuth oxide |
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| CN102320657A (en) * | 2011-08-04 | 2012-01-18 | 西南石油大学 | Method for preparing gamma-phase bismuth oxide |
Non-Patent Citations (4)
| Title |
|---|
| Bi2O3制备方法的研究现状及发展趋势;吴绍华等;《湿法冶金》;20050930;摘要 * |
| O. Monnereau等.Synthesis of Bi2O3 by controlled transformation rate thermal analysis: a new route for this oxide?.《Solid State Ionics》.2003,摘要. |
| Synthesis of Bi2O3 by controlled transformation rate thermal analysis: a new route for this oxide?;O. Monnereau等;《Solid State Ionics》;20031231;摘要 * |
| 吴绍华等.Bi2O3制备方法的研究现状及发展趋势.《湿法冶金》.2005,摘要. |
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