CN109110738A - Yellow phosphorus deep-purifying method and system - Google Patents
Yellow phosphorus deep-purifying method and system Download PDFInfo
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- CN109110738A CN109110738A CN201810926763.7A CN201810926763A CN109110738A CN 109110738 A CN109110738 A CN 109110738A CN 201810926763 A CN201810926763 A CN 201810926763A CN 109110738 A CN109110738 A CN 109110738A
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- yellow phosphorus
- purifier
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- phosphorus
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/04—Purification of phosphorus
- C01B25/047—Purification of phosphorus of yellow phosphorus
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- Organic Chemistry (AREA)
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Abstract
The invention belongs to yellow phosphorus preparation field, specifically yellow phosphorus deep-purifying method and system, yellow phosphorus deep-purifying method, including following operating procedure: 1) carrying out heating evaporation for industrial yellow phosphorus, obtains yellow phosphorus steam；2) yellow phosphorus steam is filtered by powder sintered inorganic porous material filter membrane；3) yellow phosphorus steam is cooled down, inert gas is separated with liquefaction yellow phosphorus；4) liquefaction yellow phosphorus is collected, which is high-purity yellow phosphorus.Yellow phosphorus advanced purification system, comprising: yellow phosphorus purifier, nitrogen buffer tank, cooling collection device；Yellow phosphorus vapor filter is provided between yellow phosphorus purifier and cooling collection device.The present invention, which is used, is carrying out heating anoxybiotic evaporation, the yellow phosphorus steam of generation, by effectively being filtered to yellow phosphorus steam for yellow phosphorus evaporator section, remove the particulate contaminant in yellow phosphorus steam, available high-purity yellow phosphorus, without adding other chemicals, properties of product are easier to ensure.
Description
Technical field
The invention belongs to yellow phosphorus preparation fields, specifically yellow phosphorus deep-purifying method and system.
Background technique
Industrial yellow phosphorus purification is divided into two major class of chemical method and physical method.Chemical method is generally used for low-arsenic yellow phosphorus subtractive process,
Separating by extraction is high, but the foreign ion that more difficult removing reagent is brought into subtractive process.Physical method purified industrial yellow phosphorus, including area
Domain fusion method, electromagnetic purification method, the way of distillation and absorption method take its one or more, and gained, which refines yellow phosphorus purity, can reach 6N grades
(purity 99.9999%) or 7N (purity 99.99999%) grade.
The way of distillation be lower than 290 DEG C at a temperature of carry out multilevel vacuum distilling, arsenic enters gas phase in the form of arsenic hydride, pure
Net phosphorus is condensed water conservation, to obtain high purity phosphorus.
Vacuum distillation method is often used as post-processing means, first passes through chemicalpurification in advance and is converted to the impurity in phosphorus and is not easy
The substance of volatilization, or first fixed arsenic with reagent, then redistillation obtains high purity phosphorus.Vacuum distillation process can generate more miscellaneous
Matter evaporates excess, and phosphorus loss is larger, and the phosphrus reagent of vacuum distillation method is 60%~80% at present.
Summary of the invention
The purpose of the present invention is to provide a kind of better yellow phosphorus deep-purifying method and systems.
To achieve the goals above, as one aspect of the present invention, the present invention provides a kind of yellow phosphorus deep purifying sides
Method, including following operating procedure:
1) industrial yellow phosphorus is carried out in vacuum or in the yellow phosphorus purifier after inert gas replacement by yellow phosphorus purifier
Heating evaporation obtains yellow phosphorus steam；
2) pass through filter for the yellow phosphorus steam filtration；
3) filtered yellow phosphorus steam is cooled down by cooling tower, makes yellow phosphorus steam liquefied；
4) the liquefaction yellow phosphorus is collected to get high-purity yellow phosphorus.
This method belongs to physical method purified industrial yellow phosphorus, since high purity phosphorus has more the purification of trace solid granule foreign
High requirement, but there are currently no further technologies in the further deep purifying to high-purity yellow phosphorus.
The present invention, which is used, carries out heating evaporation in the evaporator section by yellow phosphorus in the yellow phosphorus purifier full of inert gas, generates
Yellow phosphorus steam and inert gas form high temperature gas mixture, by above-mentioned filter under the promotion of pressure difference, remove de-etiolation
Particulate contaminant in phosphorus steam, available high-purity yellow phosphorus.Compared to chemical method, this method is easy to operate, obtains product
Purity is reliable.
It is further that industrial yellow phosphorus is subjected to heating evaporation are as follows: inert gas is inputted in yellow phosphorus purifier, oxygen is replaced
Industrial yellow phosphorus is input in yellow phosphorus purifier by gas, then carries out heating evaporation, obtains the gaseous mixture of yellow phosphorus steam and inert gas
Body.
It is further to be cooled down to filtered mixed gas, when making yellow phosphorus steam liquefied, inert gas is back to
Yellow phosphorus purifier.
It is further industrial yellow phosphorus to be subjected to heating evaporation are as follows: yellow phosphorus purifier is vacuumized, industrial yellow phosphorus is inputted
Into yellow phosphorus purifier, heating evaporation is carried out, yellow phosphorus steam is obtained.
It is further to be purified by yellow phosphorus purifier by industrial yellow phosphorus in vacuum or by the yellow phosphorus after inert gas replacement
Heating evaporation is carried out in device to be heated at 290~320 DEG C.
At present in the way of distillation, phosphrus reagent controls temperature under 290 DEG C~320 DEG C environment only 60%~80%,
Heating evaporation is carried out to industrial yellow phosphorus, and is filtered, higher clean-up effect can be not only possessed, phosphrus reagent promotion is also allowed to be arrived
90%~95%.
As another aspect of the present invention, the present invention also provides a kind of yellow phosphorus advanced purification systems, for industry
Yellow phosphorus purification, comprising:
The entrance of yellow phosphorus purifier, the yellow phosphorus purifier is used for access industrial yellow phosphorus purification；
Nitrogen buffer tank is connect with yellow phosphorus purifier, for being filled with nitrogen to yellow phosphorus purifier；
Cooling collection device, connect with yellow phosphorus purifier, for the mixed gas to received yellow phosphorus steam and nitrogen into
Row condenses and collects high-purity yellow phosphorus；
It is provided with yellow phosphorus vapor filter between the yellow phosphorus purifier and cooling collection device, for leading to cooling tower
The mixed gas in particulate contaminant intercepted.
This yellow phosphorus advanced purification system carries out the purification (reaching 5N grades or more) of depth compared to chemical method, not only system knot
Structure is simple, and also without other chemicals are added, properties of product are easier to ensure.
It is further that the cooling collection device includes:
Cooling tower group, the gas feed of each cooling tower are connect with the mixed gas outlet of yellow phosphorus purifier, for pair
Received mixed gas is condensed to obtain liquefaction yellow phosphorus；
It by phosphorus slot, is connect with the yellow phosphorus discharge outlet of cooling tower group, for receiving liquefaction yellow phosphorus；
Transfer tank for collecting liquefaction yellow phosphorus, and separates yellow phosphorus with water as precipitation tank.
It is further that the nitrogen recycling pipeline is connect with the air inlet of yellow phosphorus purifier.
Directly isolated gas is recycled with facilitating in this way.
It is further that the yellow phosphorus vapor filter includes:
Filter container；
Card is set in filtering container, and filtering container is divided into net air cavity and Primordial Qi chamber；
Filter element is set on card, and Primordial Qi chamber is connected to by filter element with net air cavity.
It is further that the filter element of yellow phosphorus vapor filter is powder sintered inorganic porous material filter membrane, described
The aperture of filter element is 0.05~100 μm, and the porosity of the filter element is 25~75%.
It is further negative pressure ventilation mouth to be provided on the filtering container, for docking vaccum-pumping equipment.
It is further that the side wall of the filtering container prevents liquid for heat preservation sandwich layer to keep the temperature to yellow phosphorus steam
Change.
The present invention is described further with reference to the accompanying drawings and detailed description.The additional aspect of the present invention and excellent
Point will be set forth in part in the description, and partially will become apparent from the description below.Or practice through the invention
It solves.
Detailed description of the invention
The attached drawing for constituting a part of the invention is used to assist the understanding of the present invention, content provided in attached drawing and its
Related explanation can be used for explaining the present invention in the present invention, but not constitute an undue limitation on the present invention.In the accompanying drawings:
Fig. 1 is the yellow phosphorus advanced purification system schematic diagram for illustrating embodiment；
Fig. 2 is the yellow phosphorus vapor filter schematic diagram for illustrating embodiment；
In the figure, it is marked as 1- yellow phosphorus purifier, 2- nitrogen buffer tank, 3- yellow phosphorus vapor filter, 301- filtering container,
302- card, 303- filter element, 304- heat preservation sandwich layer, 4- cooling tower group, 5- are by phosphorus slot, 6- transfer tank, 7- nitrogen recycling pipe
Road.
Specific embodiment
Clear, complete explanation is carried out to the present invention with reference to the accompanying drawing.Those of ordinary skill in the art are being based on these
The present invention will be realized in the case where explanation.Before in conjunction with attached drawing, the present invention will be described, of particular note is that:
The technical solution provided in each section including following the description and technical characteristic in the present invention are not rushing
In the case where prominent, these technical solutions and technical characteristic be can be combined with each other.
In addition, the embodiment of the present invention being related in following the description is generally only the embodiment of a branch of the invention, and
The embodiment being not all of.Therefore, based on the embodiments of the present invention, those of ordinary skill in the art are not making creativeness
All other embodiment obtained, should fall within the scope of the present invention under the premise of labour.
About term in the present invention and unit.Term in description and claims of this specification and related part
" comprising " and its any deformation, it is intended that cover and non-exclusive include.
Such as Fig. 1, a kind of yellow phosphorus deep-purifying method, including following operating procedure:
1) industrial yellow phosphorus, inert gas input yellow phosphorus purifier are subjected to heating evaporation, obtain yellow phosphorus steam and indifferent gas
The mixed gas of body mixing；Heating evaporation is heated at 290~320 DEG C；
2) mixed gas is filtered by powder sintered inorganic porous material filter membrane；
3) filtered mixed gas is cooled down, makes yellow phosphorus steam liquefied, inert gas is separated with liquefaction yellow phosphorus；
4) the liquefaction yellow phosphorus is collected to get high-purity yellow phosphorus.
The present invention make the above-mentioned high temperature gas mixture after powder sintered inorganic porous material filter membrane filtration, purification into
It is cooling to enter cooler, yellow phosphorus steam becomes liquid (drop) from gas, carries out the separation of liquid gas using gas-liquid separation, isolates
Yellow phosphorus is collected as product, and gas then sends yellow phosphorus purifier recycling back to by the road.
Distillation process can generate more impurity and evaporate excess, the present invention use by yellow phosphorus in the yellow phosphorus for being full of inert gas
The evaporator section of purifier carries out heating evaporation, and the yellow phosphorus steam of generation is under the promotion of pressure difference by above-mentioned powder sintered inorganic
Porous material filter membrane removes the particulate contaminant in mixed gas, available high-purity yellow phosphorus.
Above-mentioned 1) it is also possible to by the way of being vacuumized to yellow phosphorus purifier, heating steaming is carried out to industrial yellow phosphorus
Hair.
Gas is obtained after the gas-liquid mixed material is carried out gas-liquid separation, by the gas backstreaming to yellow phosphorus purifier.
Embodiment: a kind of yellow phosphorus advanced purification system, for the industrial yellow phosphorus purification to 3N grades, comprising:
Yellow phosphorus purifier 1, the entrance of the yellow phosphorus purifier 1 are used to access 3N grades of industrial yellow phosphorus purification；
Nitrogen buffer tank 2 is connect with yellow phosphorus purifier 1, for being filled with nitrogen to yellow phosphorus purifier 1；
Cooling collection device, connect with yellow phosphorus purifier 1, for the mixed gas to received yellow phosphorus steam and nitrogen into
Row condenses and collects high-purity yellow phosphorus；
It is provided with yellow phosphorus vapor filter 3 between the yellow phosphorus purifier 1 and cooling collection device, for leading to cooling
Particulate contaminant in the mixed gas of tower is intercepted.The filter element 303 of yellow phosphorus vapor filter 3 is powder sintered
Inorganic porous material filter membrane.
By the way that above-mentioned yellow phosphorus vapor filter 3 is arranged, purified compared to chemical method, the side that the present invention is intercepted by physics
The mode that formula filters yellow phosphorus steam inlet keeps this yellow phosphorus advanced purification system system simpler, reliable, easy to maintain, makes
It can reach 5N~6N grades of high-purity yellow phosphorus to the purification of pure 3N grades of industrial yellow phosphorus.
The cooling collection device includes:
Cooling tower group 4, the gas feed of each cooling tower connect with the mixed gas outlet of yellow phosphorus purifier 1, are used for
Received mixed gas is condensed to obtain liquefaction yellow phosphorus, which is connected with nitrogen recycling pipeline 7；In this way with
It is convenient that directly isolated gas is recycled.
It by phosphorus slot 5, is connect with the yellow phosphorus discharge outlet of cooling tower group 4, for receiving liquefaction yellow phosphorus；
Transfer tank 6 for collecting liquefaction yellow phosphorus, and separates yellow phosphorus with water as precipitation tank.
I.e. after being filtered filtered mixed gas, the solid particle in yellow phosphorus steam is intercepted, cooling tower group 4
By yellow phosphorus steam liquefied, nitrogen is connected to the air inlet of Nitrogen source gases or yellow phosphorus purifier 1 by nitrogen recycling pipeline 7, in transfer
In slot, liquefy yellow phosphorus and water stratification, isolates high-purity yellow phosphorus product.
Such as Fig. 2, the yellow phosphorus vapor filter 3 includes:
Filter container 301；
Card 302 is set in filtering container 301, and filtering container 301 is divided into net air cavity and Primordial Qi chamber；
Filter element 303 is set on card 302, and Primordial Qi chamber is connected to by filter element 303 with net air cavity；
The aperture of the filter element 303 is 0.05~100 μm, and the porosity of the filter element 303 is 25~75%.
It is 0.05~100 μm by using aperture, the filter membrane that porosity is 25~75% makes this filter element 303 right
Yellow phosphorus steam filtration possesses higher reliability.
It is provided with negative pressure ventilation mouth on the filtering container 301, for docking vaccum-pumping equipment, is vacuumized with facilitating
Work, prevents yellow phosphorus steam from reacting with oxygen.
The side wall of the filtering container 301 is heat preservation sandwich layer 304, i.e. filtering container side wall is heat preservation sandwich layer, to yellow phosphorus
Steam is kept the temperature, and prevents from liquefying.
Use this yellow phosphorus advanced purification system below to carry out deep purifying experiment to 3N grades of industrial yellow phosphorus:
As seen from the above table, in yellow phosphorus purifier, heating and temperature control can bring higher phosphorus at 290 DEG C~320 DEG C
Yield.
Yellow phosphorus advanced purification system in the present embodiment has the advantage that
1, with high temperature purification technology and high temperature yellow phosphorus purification structure, overall structure is simple, equipment is arranged can be more flexible；
2, by the mixed gas of cooling yellow phosphorus steam and nitrogen, and cooling mode is carried out by nitrogen point to mixed gas
From reducing gas treatment difficulty, by nitrogen recycling pipeline 7, reduce gas consumption；
3, with high temperature purification technology and technique, without adding other chemicals, properties of product are easier to ensure.
Related content of the invention is illustrated above.Those of ordinary skill in the art are in the feelings illustrated based on these
The present invention will be realized under condition.Based on above content of the invention, those of ordinary skill in the art are not making creativeness
All other embodiment obtained, should fall within the scope of the present invention under the premise of labour.
Claims (10)
1. yellow phosphorus deep-purifying method, which is characterized in that including following operating procedure:
1) industrial yellow phosphorus is heated in vacuum or in the yellow phosphorus purifier after inert gas replacement by yellow phosphorus purifier
Evaporation, obtains yellow phosphorus steam；
2) pass through filter for the yellow phosphorus steam filtration；
3) filtered yellow phosphorus steam is cooled down by cooling tower, makes yellow phosphorus steam liquefied；
4) the liquefaction yellow phosphorus is collected to get high-purity yellow phosphorus.
2. yellow phosphorus deep-purifying method as described in claim 1, which is characterized in that industrial yellow phosphorus is carried out heating evaporation are as follows:
Inert gas is inputted in yellow phosphorus purifier, other gases is replaced, industrial yellow phosphorus is input in yellow phosphorus purifier, then is added
Thermal evaporation obtains the mixed gas of yellow phosphorus steam and inert gas.
3. yellow phosphorus deep-purifying method as claimed in claim 2, which is characterized in that carried out to filtered mixed gas cold
But, when making yellow phosphorus steam liquefied, inert gas is back to yellow phosphorus purifier.
4. yellow phosphorus deep-purifying method as described in claim 1, which is characterized in that industrial yellow phosphorus is carried out heating evaporation are as follows:
Yellow phosphorus purifier is vacuumized, industrial yellow phosphorus is input in yellow phosphorus purifier, heating evaporation is carried out, obtains yellow phosphorus steam.
5. yellow phosphorus deep-purifying method as described in claim 1, which is characterized in that industrial yellow phosphorus is existed by yellow phosphorus purifier
Vacuum by heating evaporation is carried out in the yellow phosphorus purifier after inert gas replacement is heated at 290 DEG C~320 DEG C.
6. yellow phosphorus advanced purification system, for being purified to industrial yellow phosphorus characterized by comprising
The entrance of yellow phosphorus purifier (1), the yellow phosphorus purifier (1) is used for access industrial yellow phosphorus purification；
Nitrogen buffer tank (2) is connect with yellow phosphorus purifier (1), for being filled with nitrogen to yellow phosphorus purifier (1)；
Cooling collection device, connect with yellow phosphorus purifier (1), carries out for the mixed gas to received yellow phosphorus steam and nitrogen
It condenses and collects high-purity yellow phosphorus；
Yellow phosphorus vapor filter (3) are provided between the yellow phosphorus purifier (1) and cooling collection device, for leading to cooling
Particulate contaminant in the mixed gas of tower is intercepted.
7. yellow phosphorus advanced purification system as claimed in claim 6, which is characterized in that the cooling collection device includes:
Cooling tower group (4), the gas feed of each cooling tower connect with the mixed gas outlet of yellow phosphorus purifier (1), are used for
Received mixed gas is condensed to obtain liquefaction yellow phosphorus, which is connected with nitrogen recycling pipeline (7)；
It by phosphorus slot (5), is connect with the yellow phosphorus discharge outlet of cooling tower group (4), for receiving liquefaction yellow phosphorus；
Transfer tank (6) for collecting liquefaction yellow phosphorus, and separates yellow phosphorus with water as precipitation tank.
8. yellow phosphorus advanced purification system as claimed in claim 7, which is characterized in that the nitrogen recycling pipeline (7) and yellow phosphorus
The air inlet of purifier (1) connects.
9. yellow phosphorus advanced purification system as claimed in claim 8, which is characterized in that the yellow phosphorus vapor filter (3) includes:
It filters container (301)；
Card (302) is set in filtering container (301), and filtering container (301) is divided into net air cavity and Primordial Qi chamber；
Filter element (303) is set on card (302), and Primordial Qi chamber is connected to by filter element (303) with net air cavity, yellow phosphorus
The filter element (303) of vapor filter (3) is powder sintered inorganic porous material filter membrane, the filter element (303)
Aperture is 0.05~100 μm, and the porosity of the filter element (303) is 25~75%.
10. yellow phosphorus advanced purification system as claimed in claim 9, which is characterized in that it is described filtering container (301) side wall be
Heat preservation sandwich layer (304).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810926763.7A CN109110738A (en) | 2018-08-15 | 2018-08-15 | Yellow phosphorus deep-purifying method and system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810926763.7A CN109110738A (en) | 2018-08-15 | 2018-08-15 | Yellow phosphorus deep-purifying method and system |
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| CN109110738A true CN109110738A (en) | 2019-01-01 |
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| CN201810926763.7A Pending CN109110738A (en) | 2018-08-15 | 2018-08-15 | Yellow phosphorus deep-purifying method and system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114192074A (en) * | 2021-11-26 | 2022-03-18 | 陈玖豪 | Yellow phosphorus raw material gasification calcining furnace |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105984860A (en) * | 2015-02-06 | 2016-10-05 | 云南天安化工有限公司 | Method for recovering and refining yellow phosphorus by phosphorus sludge |
| CN208916819U (en) * | 2018-08-15 | 2019-05-31 | 成都易态科技有限公司 | Yellow phosphorus advanced purification system |
-
2018
- 2018-08-15 CN CN201810926763.7A patent/CN109110738A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105984860A (en) * | 2015-02-06 | 2016-10-05 | 云南天安化工有限公司 | Method for recovering and refining yellow phosphorus by phosphorus sludge |
| CN208916819U (en) * | 2018-08-15 | 2019-05-31 | 成都易态科技有限公司 | Yellow phosphorus advanced purification system |
Non-Patent Citations (1)
| Title |
|---|
| 郭学益等: "《工业通风与除尘》", 冶金工业出版社, pages: 87 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114192074A (en) * | 2021-11-26 | 2022-03-18 | 陈玖豪 | Yellow phosphorus raw material gasification calcining furnace |
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