CN107720821A - A kind of constant pressure hydro-thermal method phase transfer process of bismuth oxide - Google Patents
A kind of constant pressure hydro-thermal method phase transfer process of bismuth oxide Download PDFInfo
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- CN107720821A CN107720821A CN201711197784.1A CN201711197784A CN107720821A CN 107720821 A CN107720821 A CN 107720821A CN 201711197784 A CN201711197784 A CN 201711197784A CN 107720821 A CN107720821 A CN 107720821A
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- bismuth oxide
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- C01G29/00—Compounds of bismuth
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Abstract
The invention discloses a kind of constant pressure hydro-thermal method phase transfer process of bismuth oxide, including following methods step, a, makes high-purity mangesium oxide bismuth；B, reacted with the bismuth oxide finished product and NH4VO3 solution machined at 60 DEG C or so in magnetic agitation container, obtain orange-yellow precipitation；C, take out orange-yellow sediment, after precipitation stands a period of time, it is filtered and distilled water, the washing of acetone, and be placed in after product is dried at 120 DEG C in corundum crucible, 3h is calcined at 550 DEG C, tube furnace is transferred to after cooling grinding, 15h is calcined at 650~700 DEG C, normal temperature is then cooled to 25 DEG C or so per hour of speed；D, phase inversion solution is configured, configuration phase inversion solution is then poured into reaction vessel, while add in step c the bismuth oxide processed, be sufficiently mixed, control time 3.5h；E, above-mentioned reacted mixture is taken out, drying temperature is controlled at 60 85 DEG C, produces product.Present invention process is simple and practical, very friendly to environment, and it is very high to obtain product purity.
Description
Technical field
The present invention relates to crystal processing technology of preparing field, the constant pressure hydro-thermal method phase transfer process of especially a kind of bismuth oxide.
Background technology
Bismuth oxide is also known as bismuth oxide, is the powder of yellow, not soluble in water, is dissolved in strong acid generation bismuth (III) salt.It is molten
824 °C of point, 1890 DEG C of boiling point.It is one of most important compound of bismuth, can is bismuth metal by hydrogen reducing.Although three oxidations two
Bismuth can be from natural bismite（A kind of mineral）Obtain, but accessory substance when its main source is typically copper metallurgy or lead, bismuth
Combustion Energy obtains bismuth oxide to powder in atmosphere.
Bismuth oxide sterling has α types and β types.α types bismuth oxide is yellow monoclinic system crystal, relative density 8.9, fusing point
825 °C, it is dissolved in acid, not soluble in water and alkali.β types bismuth oxide is glassy yellow to orange, tetragonal system, relative density 8.55, fusing point
860 °C, acid is dissolved in, it is not soluble in water, bismuth metal is easily reduced to by hydrogen, hydro carbons etc..From the limited public affairs of Hunan Jin Wang bismuth industry shares
Department takes the lead in preparing bismuth oxide for after industrialized production, α bismuth oxides to have new production technology by oxygen manufacture oxidation；I.e.：
It is beta-oxidation bismuth to be prepared into bismuth oxide by electric arc furnaces direct oxidation, and existing market demand is generally α bismuth oxides, traditional phase inversion
It is to be realized by chemical method, or high temperature calcining phase inversion.Described chemical method is that excessive nitric acid is dissolved in by bismuth ingot, then
By adding alkali to be converted into bismuth subnitrate, high temperature calcining is carried out by bismuth subnitrate solution and is prepared into α bismuth oxides；The technique auxiliary material disappears
Consumption is high, and cost is high, and environment is unfriendly, and technique productions long flow path, and energy consumption is also high, while cost can also improve.For the above
The problem of, herein it is proposed that a kind of constant pressure hydro-thermal method phase transfer process of bismuth oxide.
The content of the invention
The present invention is solves above-mentioned phenomenon, and using the technical scheme of following modification, a kind of constant pressure hydro-thermal method of bismuth oxide turns
Phase technique, including following methods step,
A, high-purity mangesium oxide bismuth is made, to bismuth nitrate solution, is controlled at 80~90 DEG C, not carbonated hydroxide is added dropwise
Sodium water solution, makes its mixing, and solution keeps alkalescence, generation white, the bismuth oxide hydrate Bi of volumetric expansion in precipitation process
(OH) 3 precipitation, this solution is heated, and short time mixing, which is just dehydrated, is changed into yellow bismuth oxide, through water decantate, is filtered, is done
It is dry, bismuth oxide finished product is made；
B, reacted in magnetic agitation container, controlled at 60 DEG C or so with the bismuth oxide finished product and NH4VO3 solution machined
PH value processed obtains orange-yellow precipitation in 9-10；
C, takes out orange-yellow sediment, after precipitation stands a period of time, it is filtered and distilled water, the washing of acetone, and
It is placed in after product is dried at 120 DEG C in corundum crucible, 3h is calcined at 550 DEG C, tube furnace is transferred to after cooling grinding, 650
15h is calcined at~700 DEG C, normal temperature is then cooled to 25 DEG C or so per hour of speed；
D, phase inversion solution is configured, configuration phase inversion solution is then poured into reaction vessel, while add in step c the oxidation processed
Bismuth, it is sufficiently mixed, control time 3.5h.
E, above-mentioned reacted mixture is taken out, mixture is put into inside centrifugation rotating machine and carries out centrifugation rotation, is centrifuged
15min is rotated, mixture then is put into filtering equipment carries out separation of solid and liquid, is dried after the completion of separation, drying temperature control
System produces product at 60-85 DEG C.
As present invention further optimization mode, the phase inversion solution includes dispersant, catalytic reaction agent and main solution,
The main solution entirety accounting is set to 85%, and the dispersant entirety accounting is set to 10, and the catalytic reaction agent entirety accounting is set to
5%。
As present invention further optimization mode, the dispersant weight percentage concentration is in 16-38%, selection
Na2CO3, K2CO3, NaHCO3, KHCO3 aqueous solution pass through according to 1:1.5:1.25:0.8 ratio is prepared by fully mixing.
As present invention further optimization mode, the corrosion-resistant agent is that sodium propionate selects 10-20 parts by weight, Ni
(N03) 30-45 parts by weight, organophosphorous ester are selected to select to mix the mixture of composition under 20-35 parts by weight normal temperature.
As present invention further optimization mode, the main solution is set to water and NaOH mixtures, NaOH concentration control
System is in 324g/ml.
As present invention further optimization mode, the main solution passes through chemical formula 2Na [Al (OH)4]+ 3H2=2Al
+ 2NaOH + 6H2O produces solution, and the main solution manufacturing process steps are as follows,
S1, the Na [Al (OH) for taking 100g4] deal；
S2, to raw material drying and broken, be dried first, then carry out raw material classification and is sent into pulverizer in batches, use 60-
100 eye mesh screens are crushed；
S3,200g pure water is configured as reaction dissolvent；
S4, by Na [Al (OH)4] pure water solution is poured into, it is sufficiently mixed after the completion of mixing, mixing liquid is poured into sealing container, leads to
Cross test tube and be intermittently injecting pure H2；
S5, after fully reflecting, sealed container interior liquid is filtered, aluminium block caused by filtering reaction, obtain main solution.
As present invention further optimization mode, in step e, the rotating speed of control centrifugation rotating machine, control rotating speed control 15-
45r/min, the temperature inside filtering equipment is controlled at 45-55 DEG C.
The present invention makes β type bismuth oxides be directly changed into α type bismuth oxides in aqueous phase, needs not move through high temperature calcining conversion,
The phase inversion of the present invention is using NaOH solution as medium, without using other any chemical assistants, while is carrying out transfer process
Middle addition dispersant, catalytic reaction agent, greatly improved the efficiency of reaction, are a kind of brand-new technique, simple production process, if
Standby simple, cost is cheap, and energy consumption is low, and phase inversion temperature is low, in the field of business to possess larger technological break-through.
Embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely retouched
State, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based on the present invention
In embodiment, the every other implementation that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to the scope of protection of the invention.
A kind of constant pressure hydro-thermal method phase transfer process of bismuth oxide, including following methods step,
A, high-purity mangesium oxide bismuth is made, to bismuth nitrate solution, is controlled at 80~90 DEG C, not carbonated hydroxide is added dropwise
Sodium water solution, makes its mixing, and solution keeps alkalescence, generation white, the bismuth oxide hydrate Bi of volumetric expansion in precipitation process
(OH) 3 precipitation, this solution is heated, and short time mixing, which is just dehydrated, is changed into yellow bismuth oxide, through water decantate, is filtered, is done
It is dry, bismuth oxide finished product is made；
B, reacted in magnetic agitation container, controlled at 60 DEG C or so with the bismuth oxide finished product and NH4VO3 solution machined
PH value processed obtains orange-yellow precipitation in 9-10；
C, takes out orange-yellow sediment, after precipitation stands a period of time, it is filtered and distilled water, the washing of acetone, and
It is placed in after product is dried at 120 DEG C in corundum crucible, 3h is calcined at 550 DEG C, tube furnace is transferred to after cooling grinding, 650
15h is calcined at~700 DEG C, normal temperature is then cooled to 25 DEG C or so per hour of speed；
D, phase inversion solution is configured, configuration phase inversion solution is then poured into reaction vessel, while add in step c the oxidation processed
Bismuth, it is sufficiently mixed, control time 3.5h.
E, above-mentioned reacted mixture is taken out, mixture is put into inside centrifugation rotating machine and carries out centrifugation rotation, is centrifuged
15min is rotated, mixture then is put into filtering equipment carries out separation of solid and liquid, is dried after the completion of separation, drying temperature control
System produces product at 60-85 DEG C.
The phase inversion solution includes dispersant, catalytic reaction agent and main solution, and the main solution entirety accounting is set to 85%,
The dispersant entirety accounting is set to 10, and the catalytic reaction agent entirety accounting is set to 5%.
The dispersant weight percentage concentration is in 16-38%, selection Na2CO3, K2CO3, NaHCO3, KHCO3 aqueous solution
By according to 1:1.5:1.25:0.8 ratio is prepared by fully mixing.
The corrosion-resistant agent is that sodium propionate selects 10-20 parts by weight, Ni (N03) to select 30-45 parts by weight, organic phosphoric acid
The mixture of composition is mixed under fat selection 20-35 parts by weight normal temperature.
The main solution is set to water and NaOH mixtures, and NaOH concentration is controlled in 324g/ml.
The main solution passes through chemical formula 2Na [Al (OH)4]+ 3H2=2Al + 2NaOH + 6H2O produces solution,
The main solution manufacturing process steps are as follows,
S1, the Na [Al (OH) for taking 100g4] deal；
S2, to raw material drying and broken, be dried first, then carry out raw material classification and is sent into pulverizer in batches, use 60-
100 eye mesh screens are crushed；
S3,200g pure water is configured as reaction dissolvent；
S4, by Na [Al (OH)4] pure water solution is poured into, it is sufficiently mixed after the completion of mixing, mixing liquid is poured into sealing container, leads to
Cross test tube and be intermittently injecting pure H2；
S5, after fully reflecting, sealed container interior liquid is filtered, aluminium block caused by filtering reaction, obtain main solution.
In step e, the rotating speed of control centrifugation rotating machine, control rotating speed control 15-45r/min, the temperature inside filtering equipment is controlled
Degree is at 45-55 DEG C.
Example one makes the main solution of 250g
The main solution passes through chemical formula 2Na [Al (OH)4]+ 3H2=2Al + 2NaOH + 6H2O produces solution, described
Main solution manufacturing process steps are as follows,
S1, the Na [Al (OH) for taking 100g4] deal；
S2, to raw material drying and broken, be dried first, then carry out raw material classification and is sent into pulverizer in batches, use 60-
100 eye mesh screens are crushed；
S3,200g pure water is configured as reaction dissolvent；
S4, by Na [Al (OH)4] pure water solution is poured into, it is sufficiently mixed after the completion of mixing, mixing liquid is poured into sealing container, leads to
Cross test tube and be intermittently injecting pure H2；
S5, after fully reflecting, sealed container interior liquid is filtered, aluminium block caused by filtering reaction, obtain main solution.
The main solution to complete is poured into reaction vessel, adds dispersant, catalytic reaction agent, weighs 120g high-purity
Bismuth oxide simultaneously pours into reaction vessel after being processed, and takes out above-mentioned reacted mixture, mixture is put into centrifugation rotating machine
Inside carries out centrifugation rotation, and centrifugation rotates 15min, and mixture then is put into filtering equipment carries out separation of solid and liquid, and separation is completed
After dried, drying temperature control at 60-85 DEG C, produce product, obtain 118.6g finished product.
Example two makes the main solution of 150g
The main solution passes through chemical formula 2Na [Al (OH)4]+ 3H2=2Al + 2NaOH + 6H2O produces solution, described
Main solution manufacturing process steps are as follows,
S1, the Na [Al (OH) for taking 75g4] deal；
S2, to raw material drying and broken, be dried first, then carry out raw material classification and is sent into pulverizer in batches, use 60-
100 eye mesh screens are crushed；
S3,100g pure water is configured as reaction dissolvent；
S4, by Na [Al (OH)4] pure water solution is poured into, it is sufficiently mixed after the completion of mixing, mixing liquid is poured into sealing container, leads to
Cross test tube and be intermittently injecting pure H2；
S5, after fully reflecting, sealed container interior liquid is filtered, aluminium block caused by filtering reaction, obtain main solution.
The main solution to complete is poured into reaction vessel, adds dispersant, catalytic reaction agent, weighs 80g high-purity
Bismuth oxide simultaneously pours into reaction vessel after being processed, and takes out above-mentioned reacted mixture, mixture is put into centrifugation rotating machine
Inside carries out centrifugation rotation, and centrifugation rotates 15min, and mixture then is put into filtering equipment carries out separation of solid and liquid, and separation is completed
After dried, drying temperature control at 60-85 DEG C, produce product, obtain 89.2g finished product.
To sum up, the present invention makes β type bismuth oxides be directly changed into α type bismuth oxides in aqueous phase, needs not move through high temperature calcining
Conversion, phase inversion of the invention is using NaOH solution as medium, without using other any chemical assistants, while is being changed
During add dispersant, catalytic reaction agent, the efficiency of reaction greatly improved, be a kind of brand-new technique, production technology letter
Single, equipment is simple, and cost is cheap, and energy consumption is low, and phase inversion temperature is low, in the field of business to possess larger technological break-through.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic.
Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., it should be included in the present invention's
Within protection domain.
Claims (7)
- A kind of 1. constant pressure hydro-thermal method phase transfer process of bismuth oxide, it is characterised in that：Including following methods step,A, high-purity mangesium oxide bismuth is made, to bismuth nitrate solution, is controlled at 80~90 DEG C, not carbonated hydroxide is added dropwise Sodium water solution, makes its mixing, and solution keeps alkalescence, generation white, the bismuth oxide hydrate Bi of volumetric expansion in precipitation process (OH) 3 precipitation, this solution is heated, and short time mixing, which is just dehydrated, is changed into yellow bismuth oxide, through water decantate, is filtered, is done It is dry, bismuth oxide finished product is made；B, reacted in magnetic agitation container, controlled at 60 DEG C or so with the bismuth oxide finished product and NH4VO3 solution machined PH value processed obtains orange-yellow precipitation in 9-10；C, takes out orange-yellow sediment, after precipitation stands a period of time, it is filtered and distilled water, the washing of acetone, and It is placed in after product is dried at 120 DEG C in corundum crucible, 3h is calcined at 550 DEG C, tube furnace is transferred to after cooling grinding, 650 15h is calcined at~700 DEG C, normal temperature is then cooled to 25 DEG C or so per hour of speed；D, phase inversion solution is configured, configuration phase inversion solution is then poured into reaction vessel, while add in step c the oxidation processed Bismuth, it is sufficiently mixed, control time 3.5h；E, above-mentioned reacted mixture is taken out, mixture is put into inside centrifugation rotating machine and carries out centrifugation rotation, centrifugation rotates 15min, mixture is then put into filtering equipment and carries out separation of solid and liquid, is dried after the completion of separation, drying temperature control exists 60-85 DEG C, produce product.
- 2. the constant pressure hydro-thermal method phase transfer process of a kind of bismuth oxide according to claim 1, it is characterised in that the phase inversion is molten Liquid includes dispersant, catalytic reaction agent and main solution, and the main solution entirety accounting is set to 85%, the dispersant entirety accounting 10 are set to, the catalytic reaction agent entirety accounting is set to 5%.
- A kind of 3. constant pressure hydro-thermal method phase transfer process of bismuth oxide according to claim 2, it is characterised in that the dispersant Concentration expressed in percentage by weight passes through according to 1 in 16-38%, selection Na2CO3, K2CO3, NaHCO3, KHCO3 aqueous solution:1.5:1.25: 0.8 ratio is prepared by fully mixing.
- 4. the constant pressure hydro-thermal method phase transfer process of a kind of bismuth oxide according to claim 2, it is characterised in that described corrosion-resistant Agent is that sodium propionate selects 10-20 parts by weight, Ni (N03) to select 30-45 parts by weight, organophosphorous ester to select 20-35 parts by weight normal The mixture that the lower mixing of temperature is formed.
- A kind of 5. constant pressure hydro-thermal method phase transfer process of bismuth oxide according to claim 2, it is characterised in that the main solution Water and NaOH mixtures are set to, NaOH concentration is controlled in 324g/ml.
- A kind of 6. constant pressure hydro-thermal method phase transfer process of bismuth oxide according to claim 5, it is characterised in that the main solution Pass through chemical formula 2Na [Al (OH)4]+ 3H2=2Al + 2NaOH + 6H2O produces solution, the main solution manufacture craft step It is rapid as follows,S1, the Na [Al (OH) for taking 100g4] deal；S2, to raw material drying and broken, be dried first, then carry out raw material classification and is sent into pulverizer in batches, use 60- 100 eye mesh screens are crushed；S3,200g pure water is configured as reaction dissolvent；S4, by Na [Al (OH)4] pure water solution is poured into, it is sufficiently mixed after the completion of mixing, mixing liquid is poured into sealing container, leads to Cross test tube and be intermittently injecting pure H2；S5, after fully reflecting, sealed container interior liquid is filtered, aluminium block caused by filtering reaction, obtain main solution.
- A kind of 7. constant pressure hydro-thermal method phase transfer process of bismuth oxide according to claim 1, it is characterised in that in step e, control The rotating speed of system centrifugation rotating machine, control rotating speed control 15-45r/min, controls the temperature inside filtering equipment at 45-55 DEG C.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320657A (en) * | 2011-08-04 | 2012-01-18 | 西南石油大学 | Method for preparing gamma-phase bismuth oxide |
| CN102923772A (en) * | 2012-11-12 | 2013-02-13 | 湖南金旺铋业股份有限公司 | Phase inversion method of bismuth oxide hydrothermal method |
| CN104030353A (en) * | 2014-06-20 | 2014-09-10 | 湖南金旺铋业股份有限公司 | Normal-pressure hydrothermal-method phase inversion process of bismuth oxide |
| CN104030352A (en) * | 2014-06-20 | 2014-09-10 | 湖南金旺铋业股份有限公司 | Normal-pressure hydrothermal-method phase inversion method of bismuth oxide |
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2017
- 2017-11-25 CN CN201711197784.1A patent/CN107720821A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320657A (en) * | 2011-08-04 | 2012-01-18 | 西南石油大学 | Method for preparing gamma-phase bismuth oxide |
| CN102923772A (en) * | 2012-11-12 | 2013-02-13 | 湖南金旺铋业股份有限公司 | Phase inversion method of bismuth oxide hydrothermal method |
| CN104030353A (en) * | 2014-06-20 | 2014-09-10 | 湖南金旺铋业股份有限公司 | Normal-pressure hydrothermal-method phase inversion process of bismuth oxide |
| CN104030352A (en) * | 2014-06-20 | 2014-09-10 | 湖南金旺铋业股份有限公司 | Normal-pressure hydrothermal-method phase inversion method of bismuth oxide |
Non-Patent Citations (1)
| Title |
|---|
| 余丹梅等: "《大学化学实验（第五版）》", 31 October 2004, 重庆大学出版社 * |
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