CN110015687A - The production method of five nitric hydrate bismuths - Google Patents
The production method of five nitric hydrate bismuths Download PDFInfo
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- CN110015687A CN110015687A CN201910294160.4A CN201910294160A CN110015687A CN 110015687 A CN110015687 A CN 110015687A CN 201910294160 A CN201910294160 A CN 201910294160A CN 110015687 A CN110015687 A CN 110015687A
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- bismuth
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- C01—INORGANIC CHEMISTRY
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- C01G29/00—Compounds of bismuth
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The present invention relates to a kind of production methods of five nitric hydrate bismuths, it includes the following steps: S1, addition bismuth oxide, the pure nitric acid of analysis that mass fraction is 63% ~ 68%, deionized water into a stainless steel kettle, bismuth oxide, the mass ratio analyzed between pure nitric acid, deionized water are 1:1.45 ~ 1.7:1 ~ 1.8, and dissolution obtains bismuth nitrate solution under the conditions of 45 ~ 75 DEG C；S2, clear bismuth nitrate solution is obtained after filtering the bismuth nitrate solution that S1 is obtained by two-stage filter, clear bismuth nitrate solution is transferred to an evaporating kettle of resistance to nitric acid corrosion, it is 1.90 ~ 2.15 that bismuth nitrate solution, which is concentrated into gravity, under the conditions of normal pressure, 85 ~ 125 DEG C, obtains concentrate；S3, concentrate is then transferred to by a crystallization kettle with certain transfer rate, after transfer under certain holding temperature stirred crystallization and keep the temperature a period of time, material in crystallization kettle is then transferred to centrifuge, with discharging after certain centrifugation rate centrifugation a period of time, five nitric hydrate bismuths are obtained.
Description
Technical field
The present invention relates to the production fields of bismuth-series chemical product, more particularly to a kind of producer of five nitric hydrate bismuths
Method.
Background technique
Produce five nitric hydrate bismuth chemical products raw material it is general there are two types of.One is using refined bismuth as raw material, using essence
Bismuth prepares bismuth oxide, then bismuth nitrate is made, and the bismuth-series chemical products such as five water bismuth nitrates are finally made.Such as Chinese patent application
CN101628735A, it discloses a kind of preparation method of bismuth-series chemical product, this method requires height to raw materials for production refined bismuth,
Dissolving after bismuth nitrate solution is made does not have filter progress, and product purity does not ensure, while crystallisation by cooling temperature lower (10 ~ 30
DEG C), crystalline size is small, and industrialized production energy consumption is high.It is raw material that another kind, which is with thick bismuth oxide, such as Chinese patent application
CN107601560A, bismuth oxide obtain bismuth nitrate solution from a kind of electric arc furnaces expansion chamber material, bismuth oxide and dilute nitric acid reaction,
The concentrated rear concentrated nitric acid that is added crystallizes five water bismuth nitrates of precipitation, is packaged into product after filtering, drying；The method is to material purity requirement
It is relatively low, but the method, before concentration without filter progress, product purity does not ensure, while a large amount of dense nitre are added in crystallization stage
Acid (a quarter that liquid accumulates after concentration to 1/6th) causes system to be dissociated, and nitric acid content is high, and product size is small, and product exists
Still contain more free nitric acid after filtering, need to be dried, nitric acid easily decomposes generation nitrogen oxides in drying process, to setting
It is standby to require height, Environmental Inputs big, while impurity is readily incorporated in drying process.
Chemical reagent-grade reagent according to purity and impurity content number be divided into from high to low: guaranteed reagent, analysis are pure
Reagent, chemically pure reagent, experiment reagent.Five nitric hydrate bismuth characteristics of analytical reagents and chemically pure reagent please refer to
The production method of Fig. 1, five nitric hydrate bismuth of chemical reagent-grade have not been reported.
Therefore, in view of the above technical problems, the present invention is quasi- proposes a kind of especially chemical pure rank of chemical reagent-grade or more
Five nitric hydrate bismuths production method.
Summary of the invention
It is an object of the invention to propose a kind of five nitric hydrate bismuths of the especially chemical pure rank of chemical reagent-grade or more
Production method.
To realize foregoing purpose, the present invention adopts the following technical scheme: a kind of production method of five nitric hydrate bismuths, packet
Include following steps:
S1, bismuth oxide is added into a stainless steel kettle, the pure nitric acid of analysis that mass fraction is 63% ~ 68%, deionized water, oxidation
Bismuth, the mass ratio analyzed between pure nitric acid, deionized water are 1:1.45 ~ 1.7:1 ~ 1.8, dissolve and obtain under the conditions of 45 ~ 75 DEG C
Bismuth nitrate solution；
S2, clear bismuth nitrate solution is obtained after filtering the bismuth nitrate solution that S1 is obtained by two-stage filter, it will be clear
Bismuth nitrate solution is transferred to an evaporating kettle of resistance to nitric acid corrosion, is concentrated into bismuth nitrate solution under the conditions of normal pressure, 85 ~ 125 DEG C molten
Liquor ratio weight is 1.90 ~ 2.15, obtains concentrate；
S3, concentrate is then transferred to by a crystallization kettle with certain transfer rate, in certain holding temperature after transfer
Lower stirred crystallization simultaneously keeps the temperature a period of time, and material in crystallization kettle is then transferred to centrifuge, is centrifuged with certain centrifugation rate
Discharging after a period of time obtains five nitric hydrate bismuths.
As a further improvement of the present invention, bismuth oxide uses following steps to be prepared: using refined bismuth as raw material, melting
Heating melting in furnace, exhaust column collect bismuth vapour, rotary kiln secondary oxidation are entered after hot-air once oxidation, after crushing and screening
After obtain bismuth oxide.
As a further improvement of the present invention, holding temperature is 40 ~ 45 DEG C in S3.
As a further improvement of the present invention, soaking time is 0.5 ~ 2h in S3.
As a further improvement of the present invention, the transfer rate in S3 is 6 ~ 12L/min.
As a further improvement of the present invention, the first order of two-stage filter is bag filter, and filtering accuracy is 1 micro-
Rice.
As a further improvement of the present invention, the second level of two-stage filter is candle filter, and filtering accuracy is 0.5 micro-
Rice.
As a further improvement of the present invention, centrifugation rate is 2000 ~ 4000 RPM.
As a further improvement of the present invention, centrifugation time is 30 ~ 60min.
The production method of this five nitric hydrate bismuth removes insoluble matter by secondary filter, is obtained greatly using evaporation and crystallization mode
Sized crystals, be easy be separated by solid-liquid separation and residue of mother amount it is few, crystal by centrifugation after can be obtained chemical reagent-grade or more than it is pure
Five nitric hydrate bismuths of degree, purity is high, centrifugation is thoroughly not necessarily to drying, with short production cycle, is suitble to industrialization production.
Detailed description of the invention
Fig. 1 is five nitric hydrate bismuth characteristics of analytical reagents and chemically pure reagent.
Fig. 2 is the characteristics of the preparation-obtained five nitric hydrates bismuth of the present invention.
Specific embodiment
Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without making creative work
The every other embodiment obtained, shall fall within the protection scope of the present invention.
The present invention proposes a kind of production method of five nitric hydrate bismuths comprising following steps:
S1, bismuth oxide is added into a stainless steel kettle, the pure nitric acid of analysis that mass fraction is 63% ~ 68%, deionized water, oxidation
Bismuth, the mass ratio analyzed between pure nitric acid, deionized water are 1:1.45 ~ 1.7:1 ~ 1.8, dissolve and obtain under the conditions of 45 ~ 75 DEG C
Bismuth nitrate solution；
S2, clear bismuth nitrate solution is obtained after filtering the bismuth nitrate solution that S1 is obtained by two-stage filter, it will be clear
Bismuth nitrate solution is transferred to an evaporating kettle of resistance to nitric acid corrosion, is concentrated into bismuth nitrate solution under the conditions of normal pressure, 85 ~ 125 DEG C molten
Liquor ratio weight is 1.90 ~ 2.15, obtains concentrate；
S3, concentrate is then transferred to by a crystallization kettle with certain transfer rate, in certain holding temperature after transfer
Lower stirred crystallization simultaneously keeps the temperature a period of time, and material in crystallization kettle is then transferred to centrifuge, is centrifuged with certain centrifugation rate
Discharging after a period of time obtains five nitric hydrate bismuths.
In certain embodiments of the present invention, bismuth oxide uses following steps to be prepared: using refined bismuth as raw material, melting
Heating melting in furnace, exhaust column collect bismuth vapour, rotary kiln secondary oxidation are entered after hot-air once oxidation, after crushing and screening
After obtain bismuth oxide.After being heated to molten state due to bismuth, the sustainable induction subsequent melt of exothermic reaction, low energy consumption, production capacity is high.Together
When, which belongs to pyrogenic process reaction, has prevented the introducing of anionic impurity to greatest extent.
In certain embodiments of the present invention, holding temperature is 40 ~ 45 DEG C in S3.
In certain embodiments of the present invention, soaking time is 0.5 ~ 2h in S3.Preferably, in S3 soaking time be 1 ~
1.5 h。
In certain embodiments of the present invention, the transfer rate in S3 is 6 ~ 12L/min.Preferably, the transfer speed in S3
Rate is 8 ~ 10L/min.
In certain embodiments of the present invention, the first order of two-stage filter is bag filter, and filtering accuracy is 1 micro-
Rice.In certain embodiments of the present invention, the second level of two-stage filter is candle filter, and filtering accuracy is 0.5 micron.Two
Grade filter can thoroughly filter the impurity in bismuth nitrate solution, especially free nitric acid by secondary filter, control solution
Turbidity < 1.0NTU avoids the defect of the prior art.
In certain embodiments of the present invention, centrifugation rate is 2000 ~ 4000 RPM.Preferably, centrifugation rate be 3000 ~
3500 RPM.In certain embodiments of the present invention, centrifugation time is 30 ~ 60min.The crystal perfection that crystallization obtains in crystallization kettle
It is big to spend high size, purity is high can thoroughly be centrifuged under the centrifugation rate of 2000 ~ 4000 RPM, can directly make without drying
Five nitric hydrate bismuths needed for obtaining client also avoid the nitrogen oxides generated by dry bismuth nitrate, with short production cycle, are suitble to
Industrialized production.
Technical solution is clearly and completely described below in conjunction with the embodiment of the present invention, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.
Embodiment 1.
Using refined bismuth as raw material, the heating melting in melting furnace, exhaust column collects bismuth vapour, enters back after hot-air once oxidation
Rotary kiln secondary oxidation, obtains bismuth oxide afterwards after crushing and screening, and 100kg oxidation is added in the stainless steel interlayer kettle corroded to resistance to nitric acid
Bismuth, the pure nitric acid 150kg of analysis, the deionized water 180kg that Solute mass fraction is 63%, dissolution obtains nitric acid under the conditions of 45 DEG C
Bismuth solution, the interlayer of stainless steel interlayer kettle can lead to cooling water cooling or steam heating, bismuth nitrate solution passed through double-filtration
(the two-stage filter first order is bag filter to device, and filtering accuracy is 1 micron；The two-stage filter second level is candle filter,
Filtering accuracy be 0.5 micron) filtering after obtain clear bismuth nitrate solution, the turbidity of sample detection bismuth nitrate solution is
0.3NTU, Bi content are 22.1%, dissociate HNO3Content is 4.10%, and bismuth nitrate solution is qualified, and qualified bismuth nitrate solution is turned
The Ti evaporating kettle for entering resistance to nitric acid corrosion, it is 2.15 that solution, which is concentrated into gravity, under the conditions of normal pressure, 125 DEG C；By 50L containing crystalline substance
The slurry of body is transferred to the stainless steel kettle crystallization kettle of sandwich with the transfer rate of 6L/min, stirs after transfer in 45 DEG C of heat preservations
Crystallization 2h to be mixed, material in crystallization kettle is then transferred to centrifuge, centrifuge is centrifuged discharging after 30min with the rate of 3000RPM,
156.2kg product is obtained, sampling is analyzed according to Reagent grade nitric acid bismuth crystal, and product reaches analysis net product standard, specification
Parameter details are shown in Fig. 2.
Embodiment 2
Using refined bismuth as raw material, the heating melting in melting furnace, exhaust column collects bismuth vapour, enters back after hot-air once oxidation
Rotary kiln secondary oxidation, obtains bismuth oxide afterwards after crushing and screening, and 100kg oxidation is added in the stainless steel interlayer kettle corroded to resistance to nitric acid
Bismuth, the pure nitric acid 170kg of analysis, the deionized water 100kg that Solute mass fraction is 65%, dissolution obtains nitric acid under the conditions of 50 DEG C
Bismuth solution, the interlayer of stainless steel interlayer kettle can lead to cooling water cooling or steam heating, bismuth nitrate solution passed through double-filtration
(the two-stage filter first order is bag filter to device, and filtering accuracy is 1 micron；The two-stage filter second level is candle filter,
Filtering accuracy be 0.5 micron) filtering after obtain clear bismuth nitrate solution, the turbidity of sample detection bismuth nitrate solution is
0.9NTU, Bi content are 25.8%, dissociate HNO3Content is 8.80%, and bismuth nitrate solution is qualified, and qualified bismuth nitrate solution is turned
The Ti evaporating kettle for entering resistance to nitric acid corrosion, it is 2.05 that solution, which is concentrated into gravity, under the conditions of normal pressure, 85 DEG C；By 50L containing crystalline substance
The slurry of body is transferred to the stainless steel kettle crystallization kettle of sandwich with the transfer rate of 9L/min, stirs after transfer in 50 DEG C of heat preservations
Crystallization 1h to be mixed, material in crystallization kettle is then transferred to centrifuge, centrifuge is centrifuged discharging after 60min with the rate of 2000RPM,
145.6kg product is obtained, sampling is analyzed according to Reagent grade nitric acid bismuth crystal, and product reaches analysis net product standard, specification
Parameter details are shown in Fig. 2.
Embodiment 3.
Using refined bismuth as raw material, the heating melting in melting furnace, exhaust column collects bismuth vapour, enters back after hot-air once oxidation
Rotary kiln secondary oxidation, obtains bismuth oxide afterwards after crushing and screening, and 100kg oxidation is added in the stainless steel interlayer kettle corroded to resistance to nitric acid
Bismuth, the pure nitric acid 145kg of analysis, the deionized water 130kg that Solute mass fraction is 68%, dissolution obtains nitric acid under the conditions of 75 DEG C
Bismuth solution, the interlayer of stainless steel interlayer kettle can lead to cooling water cooling or steam heating, bismuth nitrate solution passed through double-filtration
(the two-stage filter first order is bag filter to device, and filtering accuracy is 1 micron；The two-stage filter second level is candle filter,
Filtering accuracy be 0.5 micron) filtering after obtain clear bismuth nitrate solution, the turbidity of sample detection bismuth nitrate solution is
0.5NTU, Bi content are 24.6%, dissociate HNO3Content is 5.60%, and bismuth nitrate solution is qualified, and qualified bismuth nitrate solution is turned
The Ti evaporating kettle for entering resistance to nitric acid corrosion, it is 1.90 that solution, which is concentrated into gravity, under the conditions of normal pressure, 105 DEG C；By 50L containing crystalline substance
The slurry of body is transferred to the stainless steel kettle crystallization kettle of sandwich with the transfer rate of 12L/min, keeps the temperature after transfer in 55 DEG C
Material in crystallization kettle is then transferred to centrifuge, after centrifuge is centrifuged 45min with the rate of 4000RPM by stirred crystallization 0.5h
Discharging obtains 140.5kg product, and sampling is analyzed according to Reagent grade nitric acid bismuth crystal, and product reaches analysis net product standard,
Specifications parameter details are shown in Fig. 2.
The production method of this five nitric hydrate bismuth removes insoluble matter by secondary filter, is obtained greatly using evaporation and crystallization mode
Sized crystals, be easy be separated by solid-liquid separation and residue of mother amount it is few, crystal by centrifugation after can be obtained chemical reagent-grade or more than it is pure
Five nitric hydrate bismuths of degree, purity is high, centrifugation is thoroughly not necessarily to drying, with short production cycle, is suitble to industrialization production.
Although for illustrative purposes, the preferred embodiment of the present invention is had been disclosed, but the ordinary skill people of this field
Member will realize without departing from the scope and spirit of the invention as disclosed by the appended claims, various to change
Into, increase and replace be possible.
Claims (9)
1. a kind of production method of five nitric hydrate bismuths, it is characterised in that: it includes the following steps:
S1, bismuth oxide is added into a stainless steel kettle, the pure nitric acid of analysis that mass fraction is 63% ~ 68%, deionized water, oxidation
Bismuth, the mass ratio analyzed between pure nitric acid, deionized water are 1:1.45 ~ 1.7:1 ~ 1.8, dissolve and obtain under the conditions of 45 ~ 75 DEG C
Bismuth nitrate solution；
S2, clear bismuth nitrate solution is obtained after filtering the bismuth nitrate solution that S1 is obtained by two-stage filter, it will be clear
Bismuth nitrate solution is transferred to an evaporating kettle of resistance to nitric acid corrosion, is concentrated into bismuth nitrate solution under the conditions of normal pressure, 85 ~ 125 DEG C molten
Liquor ratio weight is 1.90 ~ 2.15, obtains concentrate；
S3, concentrate is then transferred to by a crystallization kettle with certain transfer rate, in certain holding temperature after transfer
Lower stirred crystallization simultaneously keeps the temperature a period of time, and material in crystallization kettle is then transferred to centrifuge, is centrifuged with certain centrifugation rate
Discharging after a period of time obtains five nitric hydrate bismuths.
2. the production method of five nitric hydrates bismuth according to claim 1, it is characterised in that: bismuth oxide uses following steps
Be prepared: using refined bismuth as raw material, the heating melting in melting furnace, exhaust column collects bismuth vapour, after hot-air once oxidation
Into rotary kiln secondary oxidation, bismuth oxide is obtained afterwards after crushing and screening.
3. the production method of five nitric hydrates bismuth according to claim 1, it is characterised in that: in S3 holding temperature be 40 ~
45℃。
4. the production method of five nitric hydrates bismuth according to claim 1, it is characterised in that: in S3 soaking time be 0.5 ~
2h。
5. the production method of five nitric hydrates bismuth according to claim 1, it is characterised in that: transfer rate in S3 is 6 ~
12L/min。
6. the production method of five nitric hydrates bismuth according to claim 1, it is characterised in that: the first order of two-stage filter
For bag filter, filtering accuracy is 1 micron.
7. the production method of five nitric hydrates bismuth according to claim 1, it is characterised in that: the second level of two-stage filter
For candle filter, filtering accuracy is 0.5 micron.
8. the production method of five nitric hydrates bismuth according to claim 1, it is characterised in that: centrifugation rate be 2000 ~
4000 RPM。
9. the production method of five nitric hydrates bismuth according to claim 1, it is characterised in that: centrifugation time be 30 ~
60min。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114560499A (en) * | 2022-03-31 | 2022-05-31 | 广东先导稀材股份有限公司 | Production method of pentahydrate bismuth nitrate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4675171A (en) * | 1984-12-10 | 1987-06-23 | Sumitomo Metal Mining Company Limited | Production of finely-divided particulate bismuth oxide |
| CN101628735A (en) * | 2009-08-24 | 2010-01-20 | 中南大学 | Method for preparing bismuth-series chemical product |
| CN105016384A (en) * | 2015-07-01 | 2015-11-04 | 乐山沃耐稀电子材料有限公司 | Zirconium nitrate preparation method |
| CN206368039U (en) * | 2016-12-28 | 2017-08-01 | 广东先导稀材股份有限公司 | Bismuth oxide preparation facilities |
-
2019
- 2019-04-12 CN CN201910294160.4A patent/CN110015687A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4675171A (en) * | 1984-12-10 | 1987-06-23 | Sumitomo Metal Mining Company Limited | Production of finely-divided particulate bismuth oxide |
| CN101628735A (en) * | 2009-08-24 | 2010-01-20 | 中南大学 | Method for preparing bismuth-series chemical product |
| CN105016384A (en) * | 2015-07-01 | 2015-11-04 | 乐山沃耐稀电子材料有限公司 | Zirconium nitrate preparation method |
| CN206368039U (en) * | 2016-12-28 | 2017-08-01 | 广东先导稀材股份有限公司 | Bismuth oxide preparation facilities |
Non-Patent Citations (1)
| Title |
|---|
| 郭学益等: "《高纯金属材料》", 31 January 2010, 冶金工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114560499A (en) * | 2022-03-31 | 2022-05-31 | 广东先导稀材股份有限公司 | Production method of pentahydrate bismuth nitrate |
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Application publication date: 20190716 |