CN101987746A - Method for preparing high-purity bismuth oxide - Google Patents
Method for preparing high-purity bismuth oxide Download PDFInfo
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- CN101987746A CN101987746A CN2009103052401A CN200910305240A CN101987746A CN 101987746 A CN101987746 A CN 101987746A CN 2009103052401 A CN2009103052401 A CN 2009103052401A CN 200910305240 A CN200910305240 A CN 200910305240A CN 101987746 A CN101987746 A CN 101987746A
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Abstract
The invention belongs to a method for preparing high-purity bismuth oxide, which comprises the steps: (1) metal bismuth is added to a stainless steel reaction vessel after being washed by high-purity water, the high-purity water and high-purity nitric acid are added to carry out a heating reaction; the reactant is filtered after being cooled; the filtrate is condensed and cooled to obtain crystals; (2) the crystals in the step (1) are dissolved into a saturated solution by high-purity water; the saturated solution is added to the stainless steel reaction vessel and hydrolyzed under the stirring for standing; the bismuth subnitrate is completely precipitated; the supernatant liquor is eliminated; the precipitation is pumped; the pumped precipitation is washed by high-purity water, pumped and dried; the dried bismuth subnitrate is pulverized and added to a ceramic evaporating dish; then the pulverized bismuth subnitrate is transferred to a muffle furnace to be baked; the baked bismuth subnitrate is pulverized after being cooled; and the pulverized bismuth subnitrate is added to the muffle furnace to be baked and cooled so as to obtain the high-purity bismuth oxide finished product. The method for preparing the high-purity bismuth oxide has the advantages of simple process step and high production efficiency, and the high-purity bismuth oxide has the advantages of low impurity content and high purity.
Description
Technical field
The invention belongs to the mineral compound field, especially a kind of preparation method of high-purity bismuth oxide.
Background technology
High-purity bismuth oxide is applied in the manufacturing of resistance element and bismuth germanium oxide class monocrystalline widely.The method of preparation is as in the porcelain dish with Bismuth trinitrate at present, 400 ℃～500 ℃ calcinations 3～4 hours, calcination thing cooling, i.e. bismuth oxide, the bismuth oxide that this preparation method obtains is a lemon yellow, with the high-purity bismuth oxide yellow certain gap is arranged, purity is lower, and foreign matter content is higher, and technology is more loaded down with trivial details, production efficiency is lower, does not have competitive power on market.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of processing step simple, production efficiency is higher, foreign matter content is low, the preparation method of the high-purity bismuth oxide that purity is high.
The present invention is achieved through the following technical solutions:
A kind of preparation method of high-purity bismuth oxide the steps include:
(1), bismuth metal is put into the stainless steel reaction pot with after the high purity water washing, add high purity water and high pure nitric acid, carried out reacting by heating 1～2 hour, temperature is controlled at 60～65 ℃, and cooled and filtered is concentrated into 20～22Be with filtrate, and cooling obtains crystallization;
(2), the crystallization in the step (1) is dissolved as saturated solution with high purity water, put into the stainless steel reaction pot, under agitation be hydrolyzed, left standstill 10～15 minutes, bismuth subnitrate is precipitated fully, discard supernatant liquid, drain throw out, again with high purity water washing 3～6 times, drain, dry down at 80～85 ℃, the exsiccant bismuth subnitrate is ground, put into the furnace pot of porcelain, move to retort furnace, carry out 500～550 ℃ of calcinations 3～6 hours, grind again after the cooling, put into retort furnace again and carry out 500～550 ℃ of calcinations 3～6 hours, cooling obtains the high-purity bismuth oxide finished product.
And described high purity water is 1: 1 with the ratio of the weight of high pure nitric acid.
Advantage of the present invention and beneficial effect are:
1, the preparation method of this high-purity bismuth oxide reacts high pure nitric acid and bismuth metal in high purity water, makes bismuth subnitrate and generates the high-purity bismuth oxide finished product through grinding calcination repeatedly, and this preparation method is simple, can access the high bismuth oxide of purity.
2, processing step of the present invention is simple, and production efficiency is higher, foreign matter content is low, the preparation method of the high-purity bismuth oxide that purity is high.
Embodiment
The present invention is described in further detail by following examples.Need to prove: following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1
A kind of preparation method of high-purity bismuth oxide the steps include:
(1), the 1.5Kg bismuth metal is put into the stainless steel reaction pot with after the high purity water washing, add 2Kg high purity water and 2Kg high pure nitric acid, carried out reacting by heating 1 hour 10 minutes, temperature is controlled at 60 ℃, and cooled and filtered is concentrated into 20Be with filtrate, and cooling obtains crystallization;
(2), the crystallization in the step (1) is dissolved as saturated solution with high purity water, put into the stainless steel reaction pot, under agitation be hydrolyzed, left standstill 10 minutes, bismuth subnitrate is precipitated fully, discard supernatant liquid, drain throw out, again with high purity water washing 4 times, drain again, dry down at 80 ℃, the exsiccant bismuth subnitrate is ground, put into the furnace pot of porcelain, move to retort furnace, carry out 500 ℃ of calcinations 6 hours, grind again after the cooling, put into retort furnace again and carry out 520 ℃ of calcinations 4 hours, cooling obtains the high-purity bismuth oxide finished product.
Embodiment 2
A kind of preparation method of high-purity bismuth oxide the steps include:
(1), the 2Kg bismuth metal is put into the stainless steel reaction pot with after the high purity water washing, slowly add 2.5Kg high purity water and 2.5Kg high pure nitric acid, carried out reacting by heating 1 hour 15 minutes, temperature is controlled at 62 degree, cooled and filtered, filtrate is put into Stainless Steel Kettle concentrate, be concentrated into 22Be, cooling obtains crystallization;
(2), the crystallization in the step (1) is dissolved as saturated solution with high purity water, put into the stainless steel reaction pot, under agitation be hydrolyzed, left standstill 15 minutes, bismuth subnitrate is precipitated fully, discard supernatant liquid, throw out drained, again with high purity water washing 5 times, drain, place 85 ℃ of stainless steel vessels dry again, the exsiccant bismuth subnitrate is ground, put into the furnace pot of porcelain, move to retort furnace, carry out 550 ℃ of calcinations 5 hours, grind again after the cooling, put into retort furnace again and carry out 530 ℃ of calcinations 3.5 hours, cooling obtains the high-purity bismuth oxide finished product.
Claims (2)
1. the preparation method of a high-purity bismuth oxide, it is characterized in that: this preparation method's step is:
(1), bismuth metal is put into the stainless steel reaction pot with after the high purity water washing, add high purity water and high pure nitric acid, carried out reacting by heating 1～2 hour, temperature is controlled at 60～65 ℃, and cooled and filtered is concentrated into 20～22Be with filtrate, and cooling obtains crystallization;
(2), the crystallization in the step (1) is dissolved as saturated solution with high purity water, put into the stainless steel reaction pot, under agitation be hydrolyzed, left standstill 10～15 minutes, bismuth subnitrate is precipitated fully, discard supernatant liquid, drain throw out, again with high purity water washing 3～6 times, drain, dry down at 80～85 ℃, the exsiccant bismuth subnitrate is ground, put into the furnace pot of porcelain, move to retort furnace, carry out 500～550 ℃ of calcinations 3～6 hours, grind again after the cooling, put into retort furnace again and carry out 500～550 ℃ of calcinations 3～6 hours, cooling obtains the high-purity bismuth oxide finished product.
2. the preparation method of high-purity bismuth oxide according to claim 1, it is characterized in that: described high purity water is 1: 1 with the ratio of the weight of high pure nitric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103052401A CN101987746A (en) | 2009-08-05 | 2009-08-05 | Method for preparing high-purity bismuth oxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009103052401A CN101987746A (en) | 2009-08-05 | 2009-08-05 | Method for preparing high-purity bismuth oxide |
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| CN101987746A true CN101987746A (en) | 2011-03-23 |
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| CN2009103052401A Pending CN101987746A (en) | 2009-08-05 | 2009-08-05 | Method for preparing high-purity bismuth oxide |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992401A (en) * | 2012-12-27 | 2013-03-27 | 湖南金旺铋业股份有限公司 | Process for producing bismuth aluminate by using crude bismuth oxide |
| CN103011284A (en) * | 2012-12-27 | 2013-04-03 | 湖南金旺铋业股份有限公司 | Method for removing impurities from crude bismuth oxide |
| CN110330054A (en) * | 2019-07-19 | 2019-10-15 | 广东先导稀材股份有限公司 | A kind of preparation method of crystal grade high-purity bismuth oxide |
-
2009
- 2009-08-05 CN CN2009103052401A patent/CN101987746A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992401A (en) * | 2012-12-27 | 2013-03-27 | 湖南金旺铋业股份有限公司 | Process for producing bismuth aluminate by using crude bismuth oxide |
| CN103011284A (en) * | 2012-12-27 | 2013-04-03 | 湖南金旺铋业股份有限公司 | Method for removing impurities from crude bismuth oxide |
| CN110330054A (en) * | 2019-07-19 | 2019-10-15 | 广东先导稀材股份有限公司 | A kind of preparation method of crystal grade high-purity bismuth oxide |
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Application publication date: 20110323 |