CN103253706A - Preparation method of basic bismuth nitrate - Google Patents
Preparation method of basic bismuth nitrate Download PDFInfo
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- CN103253706A CN103253706A CN201310183160XA CN201310183160A CN103253706A CN 103253706 A CN103253706 A CN 103253706A CN 201310183160X A CN201310183160X A CN 201310183160XA CN 201310183160 A CN201310183160 A CN 201310183160A CN 103253706 A CN103253706 A CN 103253706A
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- reaction
- vikaline
- preparation
- bismuth oxide
- oxide powder
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Abstract
The invention discloses a preparation method of basic bismuth nitrate. Specifically, the preparation method comprises the steps of I, preparing ordinary bismuth oxide powder from refined bismuth; and II, adding the prepared ordinary bismuth oxide powder to a nitric acid water solution, implementing reaction, carrying out ball-milling or rod-milling in the reaction process, filtering after reaction to obtain a basic bismuth nitrate precipitate and filtrate, and recycling the obtained filtrate. The preparation method has the characteristics of rapid reaction speed and high conversion rate; the preparation method is free from the generation of nitric oxide and wastewater in the reaction process, thus being environment-friendly; and the preparation method has the remarkable advantages of low consumption of a chemical reagent, low energy consumption, low cost, simple equipment and operation, and the like.
Description
Technical field
The invention belongs to domain of inorganic chemistry, be specially a kind of preparation method of Vikaline.
Background technology
The traditional method of preparation Vikaline all is to be raw material with the Bismuth trinitrate, prepares Bismuth trinitrate by smart bismuth earlier, and concrete reaction formula is:
Bi+6HNO
3=Bi(NO
3)
3+3NO
2↑+3H
2O （1）
Bi+4HNO
3=Bi(NO
3)
3+NO↑+2H
2O （2）
And then adopt the pure water hydrolysis method to produce, or in order to ammoniacal liquor (volatile salt) for the neutralizing hydrolysis method of neutralizing agent is hydrolyzed into Vikaline with Bismuth trinitrate, specifically reaction formula is:
5Bi(NO
3)
3+10H
2O=4BiNO
3(OH)
2·BiO(OH)+11HNO
3 （3）
5Bi(NO
3)
3+11NH
4OH=4BiNO
3(OH)
2·BiO(OH)+11NH
4NO
3+H
2O （4）
5Bi(NO
3)
3+5.5(NH
4)
2CO
3+4.5H
2O=4BiNO
3(OH)
2·BiO(OH)+11NH
4NO
3+5.5CO
2 （5）
When the preparation Bismuth trinitrate, can produce a large amount of oxynitride and consume a large amount of nitric acid, produce a large amount of rare nitric acid or ammonium nitrate wastewater simultaneously.At this situation, ZL200910305977.3 " a kind of method for preparing bismuth-series chemical product " proposes to prepare Vikaline by common bismuth oxide:
5Bi
2O
3(Gu)+8HNO
3+ 5H
2O=2[4BiNO
3(OH)
2BiO (OH)] (Gu) (6)
This method does not produce oxynitrides and waste water, and required nitric acid has only 4/15ths of traditional method.But also there is certain shortcoming in above-mentioned reaction, Gu this reaction is solid-conversion reaction, reaction product is wrapped in the surface of reactant, hinders reaction and further carries out, and cause its long reaction time, and transformation efficiency is not high.Therefore the speed of response and the turnover ratio that how to improve this method become its key in application.
Summary of the invention
The object of the present invention is to provide a kind of method of rapidly and efficiently being produced Vikaline by common bismuth oxide.
The inventive method key step is as follows:
The first step: prepare the regular grade bismuth oxide powder by smart bismuth;
Second step: the regular grade bismuth oxide powder that the first step is produced adds in the salpeter solution, carries out ball milling or rod milling in reaction process, peels off the Vikaline solid product of parcel bismuth oxide, exposes new bismuth oxide reaction surface, significantly improves chemical conversion speed; After reaction is finished, filter, obtain Vikaline precipitation and filtrate; And with the filtrate cycle utilization that obtains.
In the first step, the granularity of regular grade bismuth oxide powder is smaller or equal to 0.154mm.
In second step, nitric acid dosage is 1～4 times of theoretical amount of the mol ratio of itself and bismuth oxide in the reaction, the quality of keeping salpeter solution is 1～20 with the ratio of the quality of regular grade bismuth oxide powder, make the concentration control of salpeter solution in suitable scope, and make conversion reaction (6) press equation generation bismuth subnitrate as far as possible.
The temperature of reaction in second step is 5～100 ℃, and the reaction times is 15～840 minutes.
Abrading-ball or frotton are 1～20 with the ratio of the quality of regular grade bismuth oxide powder, and the rotating speed in ball milling or the rod milling process is 5～500 rev/mins.
Adopt in second step and do not pollute the material of Vikaline as the material of ball milling or rod milling instrument and reactor wall.
The present invention adopts the mode of ball milling or rod milling, the quick and reactants separate with the reaction product that is wrapped in reaction-ure surface, thus reaction (6) can be carried out smoothly, speed of response is accelerated greatly, and transformation efficiency significantly improves.
It is fast that the present invention has speed of response, the characteristics that transformation efficiency is high; In reaction process, utilize mechanical force to carry out ball milling or rod milling, peel off the Vikaline solid product of parcel bismuth oxide, expose new bismuth oxide reaction surface, significantly improve chemical conversion speed, and advantages such as the remaining filtrate in reaction back can recycle, has environmental friendliness, and technology is simple.
Embodiment
Be described in further detail below in conjunction with the present invention of embodiment.
Embodiment 1
Prepare common bismuth oxide by smart bismuth oxidation, Bi in the product that wherein makes
2O
3Content greater than 99.98%.It is in 63% the chemical pure nitric acid that the above-mentioned common bismuth oxide of 124.1g is added the 46ml mass percent, and then toward wherein adding pure water 600ml, mixture behind the adding pure water is put into the stainless steel mill tube that 1000g zirconium dioxide abrading-ball is housed, ball milling transforms 1 hour under the temperature of 100 rev/mins rotating speeds and 25 ℃, reaction, after reaction is finished product is filtered, obtain Vikaline precipitation and filtrate, and then with the Vikaline drying that obtains, finally obtain 148.11g Vikaline and 578ml filtrate.Wherein, contain Bi71.84% in the Vikaline, contain Bi3.3g/L and nitric acid 0.2mol/L in the filtrate, filtrate is returned next time use.
Embodiment 2
Prepare common bismuth oxide by smart bismuth oxidation, Bi in the product that wherein makes
2O
3Content greater than 99.98%.It is in 63% the chemical pure nitric acid that this bismuth oxide of 121.85g is joined the 38ml mass percent, mix, and then toward wherein adding the mother liquor 570ml that contains Bi3.5g/L and nitric acid 0.2mol/L, mixture behind the adding pure water is put into the stainless steel mill tube that 1250g stainless steel frotton is housed, ball milling transforms 0.5 hour under the temperature of 150 rev/mins rotating speeds and 50 ℃, filtration, drying obtain 151.62g Vikaline and 578ml filtrate then.Wherein, contain Bi71.54% in the Vikaline of acquisition, the content of Bi is that the concentration of 3.3g/L and nitric acid is 0.22mol/L in the filtrate, filtrate is returned recycle next time.
Claims (6)
1. a method for preparing Vikaline is characterized in that, this method specifically comprises following step,
The first step: prepare the regular grade bismuth oxide powder by smart bismuth;
Second step: the regular grade bismuth oxide powder that the first step is made adds in the salpeter solution, reaction, in reaction process, carry out ball milling or rod milling, peel off the Vikaline solid product of parcel bismuth oxide, expose new bismuth oxide reaction surface, after reaction is finished, filter, obtain Vikaline precipitation and mother liquor; And with the mother liquid recycling that obtains.
2. the preparation method of Vikaline according to claim 1, it is characterized in that: in the first step, the granularity of regular grade bismuth oxide powder is less than or equal to 0.154mm.
3. the preparation method of Vikaline according to claim 1, it is characterized in that: in the first step, nitric acid dosage is 1～4 times of theoretical amount of the mol ratio of itself and bismuth oxide in the reaction, and the quality of salpeter solution is 1～20 with the ratio of the quality of regular grade bismuth oxide powder.
4. the preparation method of Vikaline according to claim 1 is characterized in that: the temperature of reaction in second step is 5～100 ℃, and the reaction times is 15～840 minutes.
5. the preparation method of Vikaline according to claim 1 is characterized in that: abrading-ball or frotton are 1～20 with the ratio of the quality of regular grade bismuth oxide powder in second step, and the rotating speed in ball milling or the rod milling process is 5～500 rev/mins.
6. the preparation method of Vikaline according to claim 1 is characterized in that: adopt in second step and do not pollute the material of Vikaline as the material of ball milling or rod milling instrument and reactor wall.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310183160XA CN103253706A (en) | 2013-05-17 | 2013-05-17 | Preparation method of basic bismuth nitrate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310183160XA CN103253706A (en) | 2013-05-17 | 2013-05-17 | Preparation method of basic bismuth nitrate |
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| CN103253706A true CN103253706A (en) | 2013-08-21 |
Family
ID=48957988
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109911936A (en) * | 2019-04-03 | 2019-06-21 | 上海应用技术大学 | A kind of sheet basic bismuth nitrate and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587063A (en) * | 2004-07-22 | 2005-03-02 | 中国地质大学（武汉） | Process for preparing nano alkaline bismuth nitrate by micro emulsion |
| CN101628735A (en) * | 2009-08-24 | 2010-01-20 | 中南大学 | Method for preparing bismuth-series chemical product |
-
2013
- 2013-05-17 CN CN201310183160XA patent/CN103253706A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587063A (en) * | 2004-07-22 | 2005-03-02 | 中国地质大学（武汉） | Process for preparing nano alkaline bismuth nitrate by micro emulsion |
| CN101628735A (en) * | 2009-08-24 | 2010-01-20 | 中南大学 | Method for preparing bismuth-series chemical product |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109911936A (en) * | 2019-04-03 | 2019-06-21 | 上海应用技术大学 | A kind of sheet basic bismuth nitrate and preparation method thereof |
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Application publication date: 20130821 |