CN103183382B - Method for preparing acicular bismuth oxide with bismuth metal - Google Patents
Method for preparing acicular bismuth oxide with bismuth metal Download PDFInfo
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- CN103183382B CN103183382B CN201310096837.6A CN201310096837A CN103183382B CN 103183382 B CN103183382 B CN 103183382B CN 201310096837 A CN201310096837 A CN 201310096837A CN 103183382 B CN103183382 B CN 103183382B
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- bismuth
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Abstract
The invention relates to a method for preparing an acicular bismuth oxide with bismuth metal. Under the action of electric arc and low temperature, bismuth raw materials are dissolved into a bismuth solution, a lot of bismuth steam is further formed, and in contact with the oxygen in air to product a spherical beta-bismuth oxide, then the spherical beta-bismuth oxide is added in nitric acid, the reaction time is controlled, and the separation is carried out to obtain a bismuth subnitrate powder; and then the bismuth subnitrate powder is calcined to obtain the acicular alfa-bismuth oxide. The method can save large amount of acid and base, greatly reduces the supplementary material consumption, and is easy to implement on the industrial production.
Description
Technical field
The present invention relates to the deep processing treatment technology of bismuth product, particularly a kind of method by bismuth preparation of metals needle-like bismuth oxide.
Background technology
The chemical formula Bi of bismuth oxide (Bismuth oxide)
20
3, molecular weight 465.96, fusing point 820 DEG C, boiling point 1890 DEG C, alpha-oxidation bismuth is yellow monoclinic system crystal, can be prepared into different-shape α bismuth oxide, as: pattern, like needle-like, claims needle-like bismuth oxide; Appearance is spherical, claims spherical bismuth oxide, etc.Its relative density is 8.9, and fusing point 825 DEG C, is dissolved in acid, water insoluble and alkali.Bismuth oxide, as a kind of electronic functional material, is widely used in voltage dependent resistor, zinc oxide lightning rod device, chromoscope, the manufacture of the electronic industrial products such as electrical condenser.In addition, the application of bismuth oxide is also had in battery industry and superconductor technology.The method that current traditional technology prepares needle-like bismuth oxide has: the first adopts bismuth metal to add nitric acid dissolve, then adds alkali and be prepared into bismuth subnitrate, then obtains needle-like bismuth oxide by high-temperature calcination; The second adds nitric acid dissolve with bismuth metal to become bismuth nitrate solution, then adjustment adds excessive alkali lye, adjust ph, is prepared into needle-like bismuth oxide; The second is on 04 06th, 2011, a kind of method for producing bismuth oxide by pyrogenic process disclosed in Chinese invention patent application publication No. CNl02001706A, broken for bismuth ingot, powder process is dropped into after sieving in horizontal rotary oxidized still and heats up, the temperature control to oxidized still is realized by ladder type of heating, the heating of this ladder comprises intensification and the repeating of constant temperature stage, and pass into dioxygen oxidation bismuth meal, oxidation stage is complete simultaneously, oxygen feeding stop is also come out of the stove after being cooled to room temperature, obtains bismuth oxide.This technique need be broken to bismuth ingot, powder process, and granularity is enough thin, and during oxidation, the material bed of material is enough thin, obtain bismuth oxide product and be often oxidized not exclusively, and processing step is many, is unfavorable for industrialization after oxidation.
Summary of the invention
Based on above-mentioned Problems existing, the present invention proposes a kind of method by bismuth preparation of metals needle-like bismuth oxide, the method is by electric arc direct production β-oxidation bismuth, alpha-oxidation bismuth is obtained again by calcining, a large amount of acid, alkali can be saved, greatly reduce supplementary product onsumption, and be easy to realize in industrial production.
Technical scheme of the present invention is: a kind of method by bismuth preparation of metals needle-like bismuth oxide, by under arcing and low temperature condition, bismuth raw material is made to melt into bismuth liquid, and then form a large amount of bismuth steam, by contacting with the oxygen in air, to generate pattern be spherical β-oxidation bismuth, then β-oxidation bismuth is added nitric acid, controls the reaction times, be separated, obtain bismuth subnitrate powder; Again by calcining bismuth subnitrate powder, be prepared into the alpha-oxidation bismuth that pattern is needle-like; Concrete technology condition step is as follows:
1. bismuth raw material is put into electric arc furnace, carry out negative pressure draws air to system, the bismuth raw material under arcing that is energized melts into bismuth liquid, and then forms a large amount of bismuth steam; By contacting with the oxygen in air, to generate pattern be spherical β-oxidation bismuth; In technological process, control furnace temperature 300 ~ 500 DEG C; Electric arc furnace operating voltage 32 ~ 64V, working current 1000 ~ 24000A;
2. get spherical β-oxidation bismuth, add nitric acid; In units of gram/gram, liquid-solid mass ratio is 1 ~ 10:1; Nitric acid and bismuth oxide mass ratio 0.1 ~ 1:1, temperature of reaction 85 ~ 100 DEG C, reaction times 3 ~ 4h; Reactant is bleached look;
3., to step white reaction thing 2., after solid-liquid separation, drying solid is bismuth subnitrate powder;
4. by calcining bismuth subnitrate powder, needle-like bismuth oxide is obtained, calcining temperature 500 ~ 800 DEG C.
Bismuth raw material of the present invention is bismuth ingot, bismuth pearl, bismuth meal and each eka-bismuth metal.
The present invention compares traditional technology following advantage:
1, bismuth raw material of the present invention is broken without the need to passing through, grinding, and the techniques such as powder process, take feeding mode to be directly enter stove;
2, cost advantage, the present invention compares traditional technology and saves a large amount of acid, alkali, greatly reduces supplementary product onsumption, especially more obvious to the local cost advantage that soda acid auxiliary material price is high.
3, be easy to realize in industrial production.
Accompanying drawing explanation
Fig. 1 is the X-ray diffraction analysis figure of embodiment.
Fig. 2 is the electronic scanning video picture figure in embodiment 1.
Fig. 3 is the X-ray diffraction analysis figure in embodiment 2.
Fig. 4 is the electronic scanning video picture figure in embodiment 2.
Fig. 5 is the X-ray diffraction analysis figure in embodiment 3.
Fig. 6 is the electronic scanning video picture figure in embodiment 3.
Embodiment
The present invention is described further below in conjunction with accompanying drawing and concrete enforcement, but is not restriction the present invention.
The present embodiment bismuth raw material is bismuth ingot metal.
By a method for bismuth preparation of metals needle-like bismuth oxide, be by under arcing and low temperature condition, make bismuth ingot metal melt into bismuth liquid, and then form a large amount of bismuth steam, by contacting with the oxygen in air, to generate pattern be spherical β-oxidation bismuth.Again β-oxidation bismuth is added nitric acid, control the reaction times, be separated, obtain bismuth subnitrate powder; Again by calcining bismuth subnitrate powder, be prepared into the alpha-oxidation bismuth that pattern is needle-like;
1, the present embodiment melts bismuth temperature 350 ~ 500 DEG C, operating voltage 32 ~ 64V, electric current 1000 ~ 24000A, negative pressure draws air, and 1t bismuth ingot output bismuth oxide 1.116t, Bi ~ 99.9% in gained bismuth oxide product, crystalline phase and Electronic Speculum are shown in accompanying drawing 1 and accompanying drawing 2.
2, β-oxidation bismuth is directly prepared into bismuth subnitrate; Get β-oxidation bismuth 30g and add 6.3 ~ 7.5g nitric acid, temperature 85 DEG C, reaction times 3h, products obtained therefrom is white powder, and crystalline phase and Electronic Speculum are shown in accompanying drawing 3 and accompanying drawing 4;
3, after the white powder product solid-liquid separation in step 2, dry solid, under 650 degrees Celsius, calcine to obtain needle-like bismuth oxide, crystalline phase and Electronic Speculum are shown in accompanying drawing 5 and accompanying drawing 6.
Claims (1)
1. the method by bismuth preparation of metals needle-like bismuth oxide, it is characterized in that: by under arcing and low temperature condition, bismuth raw material is made to melt into bismuth liquid, and then form a large amount of bismuth steam, by contacting with the oxygen in air, to generate pattern be spherical β-oxidation bismuth, then β-oxidation bismuth is added nitric acid, controls the reaction times, be separated, obtain bismuth subnitrate powder; Again by calcining bismuth subnitrate powder, be prepared into the alpha-oxidation bismuth that pattern is needle-like; Concrete technology condition step is as follows:
1. bismuth raw material is put into electric arc furnace, carry out negative pressure draws air to system, the bismuth raw material under arcing that is energized melts into bismuth liquid, and then forms a large amount of bismuth steam; By contacting with the oxygen in air, to generate pattern be spherical β-oxidation bismuth; In technological process, control furnace temperature 350 DEG C; Electric arc furnace operating voltage 32 ~ 64V, working current 1000 ~ 24000A;
2. get spherical β-oxidation bismuth, add nitric acid, in units of gram/gram, liquid-solid mass ratio is 1 ~ 10:1; Nitric acid and bismuth oxide mass ratio 0.1 ~ 1:1, temperature of reaction 85 ~ 100 DEG C, reaction times 3 ~ 4h; Reactant is bleached look;
3., to step white reaction thing 2., after solid-liquid separation, drying solid is bismuth subnitrate powder;
4. by calcining bismuth subnitrate powder, needle-like bismuth oxide is obtained, calcining temperature 800 DEG C.
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| 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 |
| CN104445398B (en) * | 2014-09-18 | 2016-04-20 | 株洲科能新材料有限责任公司 | The method of superfine bismuth oxide powder is prepared based on fluidized bed airflow pulverizer |
| CN107601560A (en) * | 2017-11-08 | 2018-01-19 | 湖南金旺铋业股份有限公司 | A kind of production technology of five water bismuth nitrate |
| CN112340776A (en) * | 2020-11-06 | 2021-02-09 | 铜仁学院 | Bismuth oxycarbonate nano material and preparation method and application thereof |
| CN112520707A (en) * | 2020-12-28 | 2021-03-19 | 广东先导稀贵金属材料有限公司 | Preparation method of tellurium dioxide |
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| CN101628735B (en) * | 2009-08-24 | 2011-11-16 | 长沙金堂铋业有限公司 | Method for preparing bismuth-series chemical product |
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