CN110255518A - A kind of yellow phosphorus preparation method - Google Patents
A kind of yellow phosphorus preparation method Download PDFInfo
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- CN110255518A CN110255518A CN201910576988.9A CN201910576988A CN110255518A CN 110255518 A CN110255518 A CN 110255518A CN 201910576988 A CN201910576988 A CN 201910576988A CN 110255518 A CN110255518 A CN 110255518A
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- refining kettle
- 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
- C01B25/02—Preparation of phosphorus
- C01B25/027—Preparation of phosphorus of yellow 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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- Mixers Of The Rotary Stirring Type (AREA)
Abstract
The present invention relates to phosphorus production manufacture field, specifically a kind of yellow phosphorus preparation method, the preparation facilities that this method uses, including refining kettle, stirring structure, closing structure, anti-sediment structure and sealing structure；When injecting the steam thick phosphorus of heating into refining kettle, stirring structure is able to drive while steam injection, and sufficient agitating and heating is carried out to the thick phosphorus solution in refining kettle, it can make being uniformly heated for thick phosphorus, so as to increase the purification efficiency of thick phosphorus, while stirring structure work, anti- sediment structure is able to drive to work, pass through the work of anti-sediment structure, the thick phosphorus being deposited in refining kettle can timely be blown afloat, it can prevent thick phosphorus from precipitating, stirring structure can also be reacted on, keep the work of stirring structure more thorough, to further increase the purification efficiency of thick phosphorus.
Description
Technical field
The present invention relates to phosphorus production manufacture field, specifically a kind of yellow phosphorus preparation method.
Background technique
Yellow phosphorus refers generally to white phosphorus, and white phosphorus is white or light yellow translucence solid.Matter is soft, and property is crisp when cold, light-exposed discoloration
It is deep.Green phosphorescent and white cigarette are generated in exposure air in the dark.About 40 DEG C of kindlings in humid air, in dry air then slightly
It is high.Relative density 1.83 (α type), 1.88 (β types).44.1 DEG C of fusing point (β type).White phosphorus can be acted as directly with halogen, sulphur, metal etc.
With generating phosphoric acid with nitric acid, generate hydrogen phosphide and sodium hypophosphite with sodium hydroxide or potassium hydroxide.In the preparation process of yellow phosphorus
In, the raw material for producing yellow phosphorus are rock phosphate in powder, coke (anthracite), silica, and coke (anthracite) is both in producing yellow Phosphorus by electric oven
Reducing agent is electric conductor again；Silica is cosolvent, can reduce slag melting, convenient for slagging tap.It refines by rock phosphate in powder to thick phosphorus
Afterwards, it is also necessary to carry out heating and refine smart phosphorus.
Due to the characteristic of phosphorus, steam heating is generally used when thick phosphorus is purified to smart phosphorus, but thick phosphorus solution is falling
It will appear precipitation status after entering in refining kettle, to the purity refined can be made to be affected, and due to being to be passed through height in refining kettle
Press steam, it is thus possible to will cause that pressure is uncontrollable to make thick phosphorus purification be affected.
Summary of the invention
For the problems of the prior art, the present invention provides a kind of yellow phosphorus preparation methods.
The technical solution adopted by the present invention to solve the technical problems is: a kind of yellow phosphorus preparation method, this method include with
Lower step:
S1: washing, drying: rock phosphate in powder, anthracite and silicon ore are respectively fed to washup system and carry out washing, removes dephosphorization
Dust in ore, anthracite and silicon ore makes the control of its dustiness in 1-2%, then by rock phosphate in powder, anthracite and silicon mine
Stone is respectively fed in dryer, dries 10-15min using 400~450 DEG C of temperature；
S2: hybrid reaction: by the fine powder of rock phosphate in powder, anthracite and silicon ore according to 1:(0.25~0.35): (0.15~
0.2) mass ratio is sent into furnace and is mixed, and controlled at 1400~1500 DEG C, the reaction time is 1~2h, obtains furnace
Gas and clinker；
S3: cooling: furnace gas being sent into cooling tower, after cooling under the action of shower water, obtains slurry, wherein furnace gas
Volume ratio with shower water is (0.6~0.8): 1；
S4: sedimentation: slurry is sent into preparation facilities, it is ensured that the volume of slurry and space in preparation facilities in preparation facilities
Than for (60~80): 100, so that slurry is settled 40~50min in preparation facilities；Simultaneously in refining kettle, it is ensured that in refining kettle
The volume ratio in space is (60~80) in slurry and refining kettle: 100, and slurry is made to settle 50~60min in refining kettle, then
It is heated, and is stirred continuously with 200~220 DEG C of steam in refining kettle, after then clarifying, pure phosphorus is deposited in the bottom of a pan, by pure phosphorus
Yellow phosphorus product is obtained after cooling and shaping；The slurry after pure phosphorus will be isolated to be sent into sludge phosphorus pool, it is ensured that slurry and mud phosphorus in sludge phosphorus pool
The volume ratio in space is (60~80) in pond: 100, the sedimentation time is 65~75min, then obtains yellow phosphorus after carrying out solid-liquor separation；
The preparation facilities that the present invention uses includes refining kettle, stirring structure, closing structure, anti-sediment structure and sealing knot
Structure, the refining kettle that smart phosphorus place is purified to for providing thick phosphorus are internally connected with for will be thick inside the refining kettle
The stirring structure that phosphorus is stirred；The top of the refining kettle is connected with for close described in on-off to heating steam
Close structure, the anti-precipitating knot for being internally connected with the blister copper for precipitating the refining kettle bottom end and blowing afloat of the refining kettle
Structure；The sealing structure of the closing structure being internally connected with for being sealed to the closing structure.
Specifically, the stirring structure includes steam pipe, protective jacket, shaft, impeller, stirring rod, fixed link and stirs ring,
The protective jacket is welded in the top dead center position of the refining kettle, and the outside weldings of the protective jacket have the steam pipe, institute
The inner rotation for stating refining kettle is connected with the shaft, and the shaft and the protective jacket are rotatablely connected, the protective jacket
External circular array is fixed with multiple impellers, and the outside of the shaft is fixed with three groups of L-shaped stirring rods,
Stirring rod described in three groups is equidistantly fixed on the outside of the shaft, and stirring rod described in one group is set there are three the stirring rod, and three
A stirring rod circular array distribution, the outside of the stirring rod are fixed with multiple fixed links in serpentine structure,
The stirring rod is fixed with the stirring ring of ring structure away from one end of the shaft.
Specifically, the anti-sediment structure includes fixed column, pressing plate, air bag, air flue, venthole and second spring, it is described
The perpendicular relationship of fixed column is fixed on the outside of the shaft, and the fixed column and the refining kettle are rotatablely connected, the essence
The internal slide of pot processed is connected with the pressing plate, and the pressing plate is arcuate structure, the pressing plate close to one end of the shaft
It is clamped with the air bag between the refining kettle, second bullet is fixedly connected between the pressing plate and the refining kettle
Spring, the inside of the refining kettle is equipped with the air flue that section is " recessed " shape structure, and the air flue is communicated with the air bag, institute
The inner bottom for stating refining kettle is equipped with multiple ventholes, and multiple ventholes distribute as net shape, it is multiple it is described go out
Stomata is " Z " character form structure, and multiple ventholes are communicated with the air flue.
Specifically, the closing structure includes stall, slide plate, air drain, the first spring, air inlet, steam channel and cunning
The stall of slot, rectangular parallelepiped structure and boring is fixed on the top of the refining kettle, and the steam pipe with it is described
Stall is fixedly connected, and the inside of the stall is equipped with the steam channel identical with the steam pipe inside diameter, institute
The inside for stating stall is equipped with the air drain, and the air drain is communicated by the air inlet with the inside of the refining kettle, institute
The internal slide for stating stall is connected with the slide plate, and the diameter of slide plate arc one end is greater than the straight of the steam channel
Diameter, is fixedly connected with first spring between the slide plate and the stall, the inside of the stall is equipped with the cunning
Slot.
Specifically, the sealing structure includes rubber ring, the first venthole and the second venthole, the annular rubber ring
It is fixed on one end of the slide plate, first venthole is set to the slide plate, and first venthole and the rubber ring
Inside communicate, the inside of the stall is equipped with second venthole, and the angle of first venthole and the slide plate
Degree and second venthole are identical as the angle of the stall, and first venthole can phase with second venthole
It is logical.
Beneficial effects of the present invention:
(1) a kind of yellow phosphorus preparation method of the present invention, when injecting the steam thick phosphorus of heating into refining kettle, in steam
It is able to drive stirring structure while injection, sufficient agitating and heating is carried out to the thick phosphorus solution in refining kettle, thick phosphorus can be made
It is uniformly heated, so as to increase the purification efficiency of thick phosphorus, while stirring structure work, is able to drive anti-precipitating knot
Structure works, and by the work of anti-sediment structure, can timely blow afloat the thick phosphorus being deposited in refining kettle, can prevent
Only thick phosphorus precipitating, additionally it is possible to react on stirring structure, keep the work of stirring structure more thorough, to further increase thick phosphorus
Purification efficiency.
(2) a kind of yellow phosphorus preparation method of the present invention, heating steam enter the inside of refining kettle by stirring structure,
When heating steam is after the inside of refining kettle reaches abundance, the air pressure inside refining kettle will be increased constantly, at this time in refining kettle
The air pressure in portion will squeeze closing structure, and heating steam inlet can be closed by closing structure work, so as to
Heating steam is enough prevented to be further continued for the inside into refining kettle, so as to prevent heating steam from purification excessively being caused to fail,
Closing structure can be such that sealing structure communicates with the inside of refining kettle while work, so as to steam the heating in refining kettle
Vapour enters sealing structure, can react on closing structure again by the work of sealing structure, make the closure of closing structure more
With leakproofness, so as to guarantee to heat steam not further into the inside of refining kettle.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is flow chart of the method for the present invention；
Fig. 2 is the preparation facilities overall structure diagram that yellow phosphorus preparation method of the present invention uses；
Fig. 3 is the attachment structure schematic diagram of stirring structure shown in Fig. 2 and anti-sediment structure；
Fig. 4 is the attachment structure schematic diagram of refining kettle shown in Fig. 2 and anti-sediment structure；
Fig. 5 is the attachment structure schematic diagram of closing structure shown in Fig. 2 and sealing structure.
In figure: 1, refining kettle, 2, stirring structure, 21, steam pipe, 22, protective jacket, 23, shaft, 24, impeller, 25, stirring
Bar, 26, fixed link, 27, stirring ring, 3, closing structure, 31, stall, 32, slide plate, 33, air drain, the 34, first spring, 35, into
Stomata, 36, steam channel, 37, sliding slot, 4, anti-sediment structure, 41, fixed column, 42, pressing plate, 43, air bag, 44, air flue, 45, go out
Stomata, 46, second spring, 5, sealing structure, 51, rubber ring, the 52, first venthole, the 53, second venthole.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained.
As Figure 1-Figure 5, a kind of yellow phosphorus preparation method of the present invention, method includes the following steps:
S1: washing, drying: rock phosphate in powder, anthracite and silicon ore are respectively fed to washup system and carry out washing, removes dephosphorization
Dust in ore, anthracite and silicon ore makes the control of its dustiness in 1-2%, then by rock phosphate in powder, anthracite and silicon mine
Stone is respectively fed in dryer, dries 10-15min using 400~450 DEG C of temperature；
S2: hybrid reaction: by the fine powder of rock phosphate in powder, anthracite and silicon ore according to 1:(0.25~0.35): (0.15~
0.2) mass ratio is sent into furnace and is mixed, and controlled at 1400~1500 DEG C, the reaction time is 1~2h, obtains furnace
Gas and clinker；
S3: cooling: furnace gas being sent into cooling tower, after cooling under the action of shower water, obtains slurry, wherein furnace gas
Volume ratio with shower water is (0.6~0.8): 1；
S4: sedimentation: slurry is sent into preparation facilities, it is ensured that the volume of slurry and space in preparation facilities in preparation facilities
Than for (60~80): 100, so that slurry is settled 40~50min in preparation facilities；Simultaneously in refining kettle, it is ensured that in refining kettle
The volume ratio in space is (60~80) in slurry and refining kettle: 100, and slurry is made to settle 50~60min in refining kettle, then
It is heated, and is stirred continuously with 200~220 DEG C of steam in refining kettle, after then clarifying, pure phosphorus is deposited in the bottom of a pan, by pure phosphorus
Yellow phosphorus product is obtained after cooling and shaping；The slurry after pure phosphorus will be isolated to be sent into sludge phosphorus pool, it is ensured that slurry and mud phosphorus in sludge phosphorus pool
The volume ratio in space is (60~80) in pond: 100, the sedimentation time is 65~75min, then obtains yellow phosphorus after carrying out solid-liquor separation；
The preparation facilities that the present invention uses includes refining kettle 1, stirring structure 2, closing structure 3, anti-sediment structure 4 and sealing
Structure 5, the refining kettle 1 that smart phosphorus place is purified to for providing thick phosphorus are internally connected with for will be in the refining kettle 1
The stirring structure 2 that the thick phosphorus in portion is stirred；The top of the refining kettle 1 is connected with for carrying out on-off to heating steam
The closing structure 3, the refining kettle 1 is internally connected with what the blister copper for precipitating 1 bottom end of refining kettle was blown afloat
The anti-sediment structure 4；Being internally connected with for the closing structure 3 is described close for being sealed to the closing structure 3
Seal structure 5.
Specifically, the stirring structure 2 includes steam pipe 21, protective jacket 22, shaft 23, impeller 24, stirring rod 25, fixes
Bar 26 and stirring ring 27, the protective jacket 22 are welded in the top dead center position of the refining kettle 1, the outside of the protective jacket 22
It is welded with the steam pipe 21, the inner rotation of the refining kettle 1 is connected with the shaft 23, and the shaft 23 is prevented with described
Sheath 22 is rotatablely connected, and the external circular array of the protective jacket 22 is fixed with multiple impellers 24, the shaft 23
Outside is fixed with three groups of L-shaped stirring rods 25, and stirring rod 25 described in three groups is equidistantly fixed on the outer of the shaft 23
Portion, stirring rod 25 described in one group is set there are three the stirring rod 25, and three 25 circular array of stirring rod distributions, described
The outside of stirring rod 25 is fixed with multiple fixed links 26 in serpentine structure, and the stirring rod 25 deviates from the shaft 23
One end be fixed with the stirring ring 27 of ring structure, when in use, the steam pipe 21 is inputted with external steam first
Pipe is attached, and is made to heat steam and is able to enter the inside of the refining kettle 1 and carries out heating Purification to thick phosphorus solution, when adding
Hot steam, by the flowing pressure of steam, can make the leaf behind the inside that the steam pipe 21 enters the protective jacket 22
Wheel 24 is rotated, and the impeller 24 is just able to drive the shaft 23 in the course of rotation and is rotated, the shaft 23
In rotation, it will be able to which stirring rod 25 described in driving three groups be fixed on outside the shaft 23 is rotated, and is stirred described in three groups
It mixes bar 25 to be equally spaced in the shaft 23, and stirring rod 25 described in every group is set there are three the stirring rod 25, described in three
The distribution of 25 circular array of stirring rod, and the stirring rod 25 is L shape structure, by the setting of multiple stirring rods 25,
Thick phosphorus solution in the refining kettle 1 can be made heated more and, so as to guarantee the efficiency of thick phosphorus purification, and in institute
Stirring rod 25 is stated equipped with multiple fixed links 26 in serpentine, by the setting of the fixed link 26, can be increased described
The stirring efficiency of stirring rod 25 is equipped with the stirring ring 27 of annular in the stirring rod 25 away from one end of the shaft 23,
By the setting of the stirring ring 27, it can make to stir more uniform, to make being uniformly heated for thick phosphorus, can achieve
Accelerate the effect of purification.
Specifically, the anti-sediment structure 4 includes fixed column 41, pressing plate 42, air bag 43, air flue 44, venthole 45 and the
Two springs 46, the perpendicular relationship of the fixed column 41 are fixed on the outside of the shaft 23, and the fixed column 41 and the essence
Pot 1 processed is rotatablely connected, and the internal slide of the refining kettle 1 is connected with the pressing plate 42, and the pressing plate 42 is close to the shaft
23 one end is arcuate structure, and the air bag 43, the pressing plate 42 and institute are clamped between the pressing plate 42 and the refining kettle 1
It states and is fixedly connected with the second spring 46 between refining kettle 1, it is " recessed " shape structure that the inside of the refining kettle 1, which is equipped with section,
The air flue 44, and the air flue 44 is communicated with the air bag 43, the inner bottom of the refining kettle 1 is equipped with multiple outlets
Hole 45, and multiple ventholes 45 distribute as net shape, multiple ventholes 45 are " Z " character form structure, and multiple institutes
Venthole 45 is stated to communicate with the air flue 44, when the shaft 23 drives the stirring rod 25 while being stirred, Gu
The fixed column 41 being scheduled in the shaft 23 can also be rotated with the shaft 23, and the fixed column 41 is in rotation
Meanwhile, it is capable to constantly squeeze the pressing plate 42, the pressing plate 42 is in the continuous extruding of the fixed column 41 and second bullet
It can be realized as bilateral reciprocation under the elastic force effect of spring 46, the institute being clamped between the pressing plate 42 and the protective jacket 22
Stating air bag 43 will constantly be squeezed, and the air bag 43 will be inflated work, the air bag under continuous squeeze
Gas inside 43 runs past the air flue 44 that section is " recessed " shape structure and enters the venthole 45, then from the outlet
Hole 45 is discharged into the inside of the refining kettle 1, is equipped in venthole 45 described in Z-shaped configuration multiple, and multiple ventholes 45 are in
Distributed in grid can be blown again the thick phosphorus for being deposited in 1 bottom end of refining kettle by the setting of multiple ventholes 45
It rises, the bottom end so as to prevent unpurified thick phosphorus to be deposited in the refining kettle 1 cannot complete to purify.
Specifically, the closing structure 3 includes stall 31, slide plate 32, air drain 33, the first spring 34, air inlet 35, steams
The stall 31 of vapour channel 36 and sliding slot 37, rectangular parallelepiped structure and boring is fixed on the top of the refining kettle 1, and
The steam pipe 21 is fixedly connected with the stall 31, and the inside of the stall 31 is equipped with straight with 21 inside of steam pipe
The identical steam channel 36 of diameter, the inside of the stall 31 is equipped with the air drain 33, and the air drain 33 is described in
Air inlet 35 is communicated with the inside of the refining kettle 1, and the internal slide of the stall 31 is connected with the slide plate 32, and described
The diameter of 32 arc one end of slide plate is greater than the diameter of the steam channel 36, fixed between the slide plate 32 and the stall 31
It is connected with first spring 34, the inside of the stall 31 is equipped with the sliding slot 37, when the steam inside of the refining kettle 1
When air pressure reaches enough, it will be able to the inside for entering the air drain 33 from the air inlet 35, into inside the air drain 33
Steam can squeeze the slide plate 32, and the slide plate 32 can be to the inside of the sliding slot 37 under the squeezing action of steam
It is slided, when the slide plate 32, which slides into, to fit like a glove with the sliding slot 37, the slide plate 32 can will be steamed for heating
The steam channel 36 that vapour passes through is stopped, so as to cut off the inside that heating steam enters the refining kettle 1, effectively
It prevents from continuously causing the vapor pressure in the refining kettle 1 excessive for heating steam, influences refining effect.
Specifically, the sealing structure 5 includes rubber ring 51, the first venthole 52 and the second venthole 53, annular institute
One end that rubber ring 51 is fixed on the slide plate 32 is stated, first venthole 52 is set to the slide plate 32, and described first is logical
Stomata 52 is communicated with the inside of the rubber ring 51, and the inside of the stall 31 is equipped with second venthole 53, and described
The angle and second venthole 53 of first venthole 52 and the slide plate 32 are identical as the angle of the stall 31, and institute
Stating the first venthole 52 can communicate with second venthole 53, coincide when the slide plate 32 slides into completely with the sliding slot 37
When, first venthole 52 on the slide plate 32 is connected to second venthole 53 on the stall 31, at this time
High steam in the refining kettle 1 runs past first venthole 52 and second ventilation 53 enters the rubber ring
51 inside will be inflated the inside of the rubber ring 51, described so as to expand the rubber ring 51
Rubber ring 51 expands the better tightness that can make between the slide plate 32 and the stall 31.
When in use, steam pipe 21 and external steam input pipe are attached first, heating steam is made to be able to enter essence
The inside of pot 1 processed carries out heating Purification to thick phosphorus solution, when inside of the heating steam from steam pipe 21 into protective jacket 22
Afterwards, by the flowing pressure of steam, impeller 24 can be made to be rotated, impeller 24 is just able to drive shaft in the course of rotation
23 are rotated, and shaft 23 is in rotation, it will be able to and drive three groups of stirring rods 25 being fixed on outside shaft 23 to be rotated, three
Group stirring rod 25 is equally spaced in shaft 23, and every group of stirring rod 25 is set there are three stirring rod 25, and three stirring rods 25 are in ring
Shape array distribution, and stirring rod 25 can make the thick phosphorus in refining kettle 1 by the setting of multiple stirring rods 25 for L shape structure
Solution it is heated more with so as to guarantee the efficiency of thick phosphorus purification, and be equipped on stirring rod 25 multiple in serpentine
Fixed link 26 can increase the stirring efficiency of stirring rod 25 by the setting of fixed link 26, in stirring rod 25 away from shaft 23
One end be equipped with annular stirring ring 27, by stir ring 27 setting, can make to stir more uniform, thus make thick phosphorus by
Heat is more uniform, can achieve the effect for accelerating purification；When shaft 23 drive stirring rod 25 while being stirred, be fixed on
Fixed column 41 in shaft 23 can also be rotated with shaft 23, and fixed column 41 can be squeezed constantly while rotation
Pressing plate 42, pressing plate 42 can be realized as left and right under the constantly elastic force of extruding and second spring 46 effect of fixed column 41 and back and forth transport
Dynamic, the air bag 43 being clamped between pressing plate 42 and protective jacket 22 will be constantly squeezed, and air bag 43 is under continuous squeeze
It will be inflated work, the gas inside air bag 43 runs past the air flue 44 that section is " recessed " shape structure and enters venthole
45, then be discharged into from venthole 45 inside of refining kettle 1, it is equipped in Z-shaped configuration venthole 45 multiple, multiple ventholes 45 are in net
Trellis distribution, by the setting of multiple ventholes 45, can blow afloat again the thick phosphorus for being deposited in 1 bottom end of refining kettle, so as to
The bottom end for enough preventing unpurified thick phosphorus to be deposited in refining kettle 1 cannot complete to purify；When the steam inside air pressure of refining kettle 1 reaches
When enough, it will be able to the inside for entering air drain 33 from air inlet 35 can squeeze slide plate 32 into the steam inside air drain 33,
Slide plate 32 can be slided under the squeezing action of steam to the inside of sliding slot 37, when slide plate 32 slide into it is complete with sliding slot 37
When complete identical, slide plate 32 can stop the steam channel 36 passed through for heating steam, steam so as to cut off heating
Vapour enters the inside of refining kettle 1, effectively prevent continuously causing the vapor pressure in refining kettle 1 excessive for heating steam, influences to mention
Pure effect；When slide plate 32 slides into completely to coincide with sliding slot 37, on the first venthole 52 and stall 31 on slide plate 32
The connection of second venthole 53, the high steam in refining kettle 1 runs past the first venthole 52 at this time and the second ventilation 53 enters
The inside of rubber ring 51 will be inflated the inside of rubber ring 51, so as to expand rubber ring 51, rubber ring
51 expansions can make the better tightness between slide plate 32 and stall 31.
The basic principles, main features and advantages of the invention have been shown and described above.The technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the description in above embodiment and specification only illustrates the present invention
Principle, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these variation and
Improvement is both fallen in the scope of protection of present invention.The claimed scope of the invention is by appended claims and its equivalent
Object defines.
Claims (5)
1. a kind of yellow phosphorus preparation method, it is characterised in that: method includes the following steps:
S1: washing, drying: rock phosphate in powder, anthracite and silicon ore are respectively fed to washup system and carry out washing, removes phosphorus ore
Dust in stone, anthracite and silicon ore makes the control of its dustiness in 1-2%, then by rock phosphate in powder, anthracite and silicon ore
It is respectively fed in dryer, dries 10-15min using 400~450 DEG C of temperature；
S2: hybrid reaction: by the fine powder of rock phosphate in powder, anthracite and silicon ore according to 1:(0.25~0.35): (0.15~0.2)
Mass ratio is sent into furnace and is mixed, and controlled at 1400~1500 DEG C, the reaction time is 1~2h, obtains furnace gas and furnace
Slag；
S3: cooling: furnace gas being sent into cooling tower, after cooling under the action of shower water, obtains slurry, wherein furnace gas and spray
The volume ratio of water drenching is (0.6~0.8): 1；
S4: sedimentation: slurry is sent into preparation facilities, it is ensured that slurry and the volume ratio in space in preparation facilities are in preparation facilities
(60~80): 100, so that slurry is settled 40~50min in preparation facilities；Simultaneously in refining kettle, it is ensured that slurry in refining kettle
Volume ratio with space in refining kettle is (60~80): 100, and slurry is made to settle 50~60min in refining kettle, then in essence
It is heated, and is stirred continuously with 200~220 DEG C of steam in pot processed, after then clarifying, deposit pure phosphorus in the bottom of a pan, pure phosphorus is cooling
Yellow phosphorus product is obtained after molding；The slurry after pure phosphorus will be isolated to be sent into sludge phosphorus pool, it is ensured that in sludge phosphorus pool in slurry and sludge phosphorus pool
The volume ratio in space is (60~80): 100, the sedimentation time is 65~75min, then obtains yellow phosphorus after carrying out solid-liquor separation；
The preparation facilities that the present invention uses include refining kettle (1), stirring structure (2), closing structure (3), anti-sediment structure (4) and
Sealing structure (5), the refining kettle (1) that smart phosphorus place is purified to for providing thick phosphorus are internally connected with for by the essence
The stirring structure (2) that the internal thick phosphorus of pot (1) processed is stirred；The top of the refining kettle (1) is connected with for adding
Hot steam carries out the closing structure (3) of on-off, and the refining kettle (1) is internally connected with for by the refining kettle (1)
The anti-sediment structure (4) that the blister copper of bottom end precipitating is blown afloat；The closing structure (3) is internally connected with for closing to described
Close the sealing structure (5) that structure (3) are sealed.
2. a kind of yellow phosphorus preparation method according to claim 1, it is characterised in that: the stirring structure (2) includes steam
(21), protective jacket (22), shaft (23), impeller (24), stirring rod (25), fixed link (26) and stirring ring (27) are managed, it is described anti-
Sheath (22) is welded in the top dead center position of the refining kettle (1), and the outside weldings of the protective jacket (22) have the steam
It manages (21), the inner rotation of the refining kettle (1) is connected with the shaft (23), and the shaft (23) and the protective jacket
(22) it is rotatablely connected, the external circular array of the protective jacket (22) is fixed with multiple impellers (24), the shaft
(23) outside is fixed with three groups of L-shaped stirring rods (25), and stirring rod described in three groups (25) is equidistantly fixed on described
The outside of shaft (23), stirring rod described in one group (25) is set there are three the stirring rod (25), and three stirring rods (25)
Circular array distribution, the outside of the stirring rod (25) is fixed with multiple fixed links (26) in serpentine structure, described
Stirring rod (25) is fixed with the stirring ring (27) of ring structure away from the one end of the shaft (23).
3. a kind of yellow phosphorus preparation method according to claim 2, it is characterised in that: the anti-sediment structure (4) includes solid
Fixed column (41), pressing plate (42), air bag (43), air flue (44), venthole (45) and second spring (46), the fixed column (41) are in
Vertical relation is fixed on the outside of the shaft (23), and the fixed column (41) and the refining kettle (1) are rotatablely connected, described
The internal slide of refining kettle (1) is connected with the pressing plate (42), and the pressing plate (42) is close to the one end of the shaft (23)
Arcuate structure is clamped with the air bag (43) between the pressing plate (42) and the refining kettle (1), the pressing plate (42) and described
It is fixedly connected between refining kettle (1) second spring (46), it is " recessed " shape knot that the inside of the refining kettle (1), which is equipped with section,
The air flue (44) of structure, and the air flue (44) is communicated with the air bag (43), the inner bottom of the refining kettle (1) is equipped with
Multiple ventholes (45), and multiple ventholes (45) distribute as net shape, multiple ventholes (45) are " Z "
Character form structure, and multiple ventholes (45) are communicated with the air flue (44).
4. a kind of yellow phosphorus preparation method according to claim 1, it is characterised in that: the closing structure (3) includes closure
(31), slide plate (32), air drain (33), the first spring (34), air inlet (35), steam channel (36) and sliding slot (37) are covered, it is rectangular
The stall (31) of body structure and boring is fixed on the top of the refining kettle (1), and the steam pipe (21) with
The stall (31) is fixedly connected, and the inside of the stall (31) is equipped with identical with the steam pipe (21) inside diameter
The inside of the steam channel (36), the stall (31) is equipped with the air drain (33), and the air drain (33) is described in
Air inlet (35) is communicated with the inside of the refining kettle (1), and the internal slide of the stall (31) is connected with the slide plate
(32), and the diameter of the slide plate (32) arc one end is greater than the diameter of the steam channel (36), the slide plate (32) and institute
It states and is fixedly connected with first spring (34) between stall (31), the inside of the stall (31) is equipped with the sliding slot
(37)。
5. a kind of yellow phosphorus preparation method according to claim 4, it is characterised in that: the sealing structure (5) includes rubber
Circle (51), the first venthole (52) and the second venthole (53), the annular rubber ring (51) are fixed on the slide plate (32)
One end, first venthole (52) is set to the slide plate (32), and first venthole (52) and the rubber ring
(51) inside communicates, and the inside of the stall (31) is equipped with second venthole (53), and first venthole
(52) and the angle of the slide plate (32) and second venthole (53) and the angle of the stall (31) it is identical and described
First venthole (52) can be communicated with second venthole (53).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910576988.9A CN110255518A (en) | 2019-06-28 | 2019-06-28 | A kind of yellow phosphorus preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910576988.9A CN110255518A (en) | 2019-06-28 | 2019-06-28 | A kind of yellow phosphorus preparation method |
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| Publication Number | Publication Date |
|---|---|
| CN110255518A true CN110255518A (en) | 2019-09-20 |
Family
ID=67923020
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910576988.9A Withdrawn CN110255518A (en) | 2019-06-28 | 2019-06-28 | A kind of yellow phosphorus preparation method |
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| Country | Link |
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| CN (1) | CN110255518A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110813216A (en) * | 2019-11-04 | 2020-02-21 | 金博 | Anti-reation kettle feeding filter equipment who rocks |
| CN112048722A (en) * | 2020-09-01 | 2020-12-08 | 武汉思越化学技术有限公司 | Preparation method and preparation system of special corrosion inhibitor for metal equipment |
| CN114560545A (en) * | 2022-03-08 | 2022-05-31 | 贵州开阳青利天盟化工有限公司 | A waste water cyclic utilization system for in yellow phosphorus storage |
-
2019
- 2019-06-28 CN CN201910576988.9A patent/CN110255518A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110813216A (en) * | 2019-11-04 | 2020-02-21 | 金博 | Anti-reation kettle feeding filter equipment who rocks |
| CN112048722A (en) * | 2020-09-01 | 2020-12-08 | 武汉思越化学技术有限公司 | Preparation method and preparation system of special corrosion inhibitor for metal equipment |
| CN114560545A (en) * | 2022-03-08 | 2022-05-31 | 贵州开阳青利天盟化工有限公司 | A waste water cyclic utilization system for in yellow phosphorus storage |
| CN114560545B (en) * | 2022-03-08 | 2023-10-03 | 贵州开阳青利天盟化工有限公司 | Wastewater recycling system for yellow phosphorus storage |
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