CN103964405B - A kind of production method of yellow phosphorus - Google Patents
A kind of production method of yellow phosphorus Download PDFInfo
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- CN103964405B CN103964405B CN201410182389.6A CN201410182389A CN103964405B CN 103964405 B CN103964405 B CN 103964405B CN 201410182389 A CN201410182389 A CN 201410182389A CN 103964405 B CN103964405 B CN 103964405B
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- yellow phosphorus
- phosphorus
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- hot water
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- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 76
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 72
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 71
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 65
- 239000011574 phosphorus Substances 0.000 claims abstract description 65
- 238000001914 filtration Methods 0.000 claims abstract description 55
- 239000007788 liquid Substances 0.000 claims abstract description 46
- 239000000843 powder Substances 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 238000007792 addition Methods 0.000 claims abstract description 13
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000002844 melting Methods 0.000 claims abstract description 7
- 210000002966 Serum Anatomy 0.000 claims abstract description 5
- 229910052799 carbon Inorganic materials 0.000 claims abstract 2
- 238000005192 partition Methods 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 239000012530 fluid Substances 0.000 claims description 9
- 239000002893 slag Substances 0.000 claims description 9
- 239000007791 liquid phase Substances 0.000 claims description 6
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000006073 displacement reaction Methods 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 238000007670 refining Methods 0.000 abstract description 3
- 238000009413 insulation Methods 0.000 description 7
- 239000002002 slurry Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 230000000712 assembly Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 239000000571 coke Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920002396 Polyurea Polymers 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000000903 blocking Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000000717 retained Effects 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Abstract
The invention discloses a kind of alternative current thick phosphorus process for refining, and the production method of the higher yellow phosphorus of purity can be produced, step includes: 1) thick phosphorus is sent into one with the reaction vessel of agitating device, make thick phosphorus enter to be passed through in advance in this reaction vessel and temperature remains in the hot water of 60-90 DEG C, then stir after all melting to yellow phosphorus add in the yellow phosphorus mixed serum with water again particle diameter be 80-500 μm, addition be the activated carbon powder that thick phosphorus adds weight 0.2-2%, make this activated carbon powder be sufficiently mixed with serosity by stirring；2) the above-mentioned serosity being mixed with activated carbon powder being sent into a solid-liquid filtration piece-rate system so that it is filtered by filter element under the temperature conditions of 60-90 DEG C, in the yellow phosphorus being filtered out, solid content controls at below 5mg/L；3) the above-mentioned yellow phosphorus filtered out feeding rinse-system is carried out at least three grades of rinsings；4) the quasi-yellow phosphorus product after rinsing is sent into product groove, by obtaining yellow phosphorus product after processing further.
Description
Technical field
The present invention relates to the production method of a kind of yellow phosphorus.
Background technology
Current phosphorus production flow process is phosphorus ore, coke and silica raw material to put into phosphor furnace reaction in proportion, then by spray
Drench device furnace gas is carried out spraying cooling and spray thrower bottom by phosphorus groove in obtain thick phosphorus, thicker phosphorus is imported in refinery pit
What carries out refine, finally give yellow phosphorus product.Above-mentioned thick phosphorus subtractive process can produce a large amount of mud phosphorus, the phosphorus content in mud phosphorus
Higher, it is currently and by multistage recovery process, the phosphorus in mud phosphorus is reclaimed, equipment, manpower, water and energy consumption all consume bigger；
Meanwhile, existing thick phosphorus process for refining is also difficult to produce high-purity yellow phosphorus (yellow phosphorus content >=99.99%), it is impossible to meet electric function
The requirement of the fine phosphorus chemical products such as material.
Summary of the invention
The technical problem to be solved is to provide a kind of alternative current thick phosphorus process for refining, and can produce purity
The production method of higher yellow phosphorus.
The production method of yellow phosphorus of the present invention, obtains, for carrying out thick phosphorus refined, the yellow phosphorus product that purity is higher, the method
Step includes: 1) sent into by thick phosphorus one with the reaction vessel of agitating device, make thick phosphorus enter be passed through this reaction vessel in advance in and
Temperature remains in the hot water of 60-90 DEG C, then stirs and adds in the mixed serum of yellow phosphorus and water after all melting to yellow phosphorus again
Particle diameter be 80-500 μm, addition be the activated carbon powder that thick phosphorus adds weight 0.2-2%, make this activated carbon powder and slurry by stirring
Liquid is sufficiently mixed；2) the above-mentioned serosity being mixed with activated carbon powder is sent into a solid-liquid filtration piece-rate system so that it is at 60-90 DEG C
Being filtered by filter element in this solid-liquid filtration piece-rate system under temperature conditions, in the yellow phosphorus being filtered out, solid content controls
Below 5mg/L；3) the above-mentioned yellow phosphorus filtered out feeding rinse-system is carried out at least three grades of rinsings, in every one-level rinse cycle first
A yellow phosphorus feeding one upper operation obtained, with the rinsing device of agitating device, makes yellow phosphorus enter and is passed through temperature in this rinsing device in advance
Remain in the hot water of 60-90 DEG C, protect with nitrogen above liquid phase in rinsing device, stand after being then sufficiently stirred for, after standing again
By hot water bottom but do not include that the yellow phosphorus bottom rinsing device enters subsequent processing；4) the quasi-yellow phosphorus product after rinsing is sent into product
Product groove, by obtaining yellow phosphorus product after processing further.
In above-mentioned phosphorus production method, its step 1) on the one hand to utilize activated carbon to have huge specific surface area, adsorptivity strong
Feature, is fully contacted reaction by activated carbon powder and liquid phosphor, reaches to adsorb in yellow phosphorus organic impurities and makes the tiny colloidal polyurea of part
The purpose of collection；On the other hand, the addition of activated carbon powder effectively improves the mobility of liquid phosphor, thus is follow-up solid-liquid mistake
Filter separation provides essential condition.Step 2) in define that in the yellow phosphorus being filtered out, solid content is at below 5mg/L, at this want
Ask lower filter element to reach the highest filtering accuracy, thus can either will adsorb in the activated carbon powder of organic impurities, yellow phosphorus
In colloidal substance, thick phosphorus, contained fine particle itself filters, and reaches to purify solid impurity and the purpose of colloid in removing yellow phosphorus.Step
Rapid 3) multistage rinsing process in, can reach and purify the purpose of impurity metal ion in removing yellow phosphorus.Pass through above-mentioned steps, it is possible to
Produce the yellow phosphorus product that purity is higher.
In said method, the particle diameter of activated carbon powder defines 80-500 μm；And the addition (weight) of activated carbon powder limits
Weight 0.2-2% is added for thick phosphorus.If the particle diameter of activated carbon powder is less than 80 μm, less activated carbon powder granule likely follow-up
Wear filter during filtration, reduce yellow phosphorus quality；And if the particle diameter of activated carbon powder is more than 500 μm easily in solid-liquid filtration piece-rate system
Pipeline, equipment adversely affect, and heavier activated carbon powder granule is not easy to be sufficiently mixed with yellow phosphorus, to ensureing yellow phosphorus stream
Dynamic property is unfavorable.The particle diameter of activated carbon powder can be preferably 100-500 μm on this basis, can more preferably 100-300 μm.
The addition of activated carbon powder can be more preferably the 0.3-0.5% that thick phosphorus adds weight.
As the further improvement to above-mentioned each technical scheme, described step 2) in specifically also comprise the steps: 1. will be mixed with
The serosity of activated carbon powder sends into a medial launder；2. the serosity in medial launder is pumped to a cross-flow filter and carries out cross flow filter；③
The yellow phosphorus that cross-flow filter filters out sends into rinse-system, and the serosity not carrying out in cross-flow filter filtering returns medial launder；4. return
Return step 2.；Wherein, the ground floor for receiving and transmit the hot water that temperature is 70-90 DEG C it is provided with in described cross-flow filter
Passage, for receive and transmit described serosity to be filtered second layer passage and for receive and transmit filtered the 3rd of yellow phosphorus
Layer passage, is separated via the first partition wall having by property between described ground floor passage and second layer passage, and the second layer leads to
Separated via the second partition wall doubling as filtering material between road and third layer passage, the fluid pressure in ground floor passage during filtration
The fluid pressure in fluid pressure ＞ third layer passage in power ＞ second layer passage, so that described hot water is through the first partition wall
Entering second layer passage, the mixture of hot water and described serosity to be filtered filters the second partition wall and enters third layer passage, and,
The liquid measure entering second layer passage through the first partition wall is to filter the 0.8-1.2 of the liquid measure that the second partition wall enters third layer passage
Times.Wherein, preferably the pressure differential between ground floor passage T1 and second layer passage T2 being controlled is 0.05-0.1MPa, second
Pressure differential between layer passage T2 and third layer passage T3 controls as 0.2-0.3MPa.
Temperature can be the heat of 70-90 DEG C in filter process by the cross-flow filter that above-mentioned solid-liquid filtration piece-rate system is used
Water mixes with serosity to be filtered, is both incubated yellow phosphorus, simultaneously because water mixes so that yellow phosphorus is subject to serosity to be filtered
To dilution, further increase the mobility of yellow phosphorus, effectively avoid in filtration yellow phosphorus to be filtered to be constantly concentrated and caused
Filter efficiency declines the problem even stagnated.Control to be 0.05 by the pressure differential between ground floor passage T1 and second layer passage T2
-0.1MPa, the pressure differential between second layer passage T2 and third layer passage T3 controls as 0.2-0.3MPa, it is possible to will pass
First partition wall enters the liquid measure of second layer passage and controls the most suitable with the liquid measure filtering the second partition wall entrance third layer passage
Level, it is ensured that stable filter.
On the premise of using above-mentioned solid-liquid filtration piece-rate system, can further the phosphorus mud of bottom phosphorus content≤3% of medial launder be arranged
Entering dehydration equipment and carry out processed, the dry slag after processed sends phosphor furnace back to, and Water Sproading utilizes.After processed
Dry slag sends phosphor furnace back to, just can utilize the activated carbon retained in dry slag, so that in the production method of yellow phosphorus of the present invention
The activated carbon put into is utilized effectively further.Described dehydration equipment can use the equipment such as pressure filter.
As the further improvement to above-mentioned each technical scheme, do not enter next by remaining in rinsing devices at different levels in described step 3
The yellow phosphorus loopback reaction vessel of operation.The most neither produce mud phosphorus, it is also possible to make yellow phosphorus be recycled as far as possible.
Above-mentioned each technical scheme preferably employs step 1) in mixed serum, add activated carbon powder and stir 30-120 and divide
Zhong Hou, with sending into solid-liquid filtration piece-rate system by this serosity.
Above-mentioned each technical scheme is preferably by described step 1) in hot water temperature in reaction vessel control at 70-80 DEG C；By described
Step 2) in serosity filter time temperature control at 70-80 DEG C；By step 3) in hot water temperature in rinsing device control
70-80 DEG C.
Below in conjunction with the accompanying drawings will be with the detailed description of the invention aspect that the present invention is described further, the present invention adds and advantage
Giving out in the middle part of explained below, part will become apparent from the description below, or is recognized by the practice of the present invention.
Accompanying drawing explanation
Fig. 1 is the process chart of the phosphorus production method of the specific embodiment of the invention.
Fig. 2 be the specific embodiment of the invention phosphorus production method in the structural representation of cross-flow filter.
Detailed description of the invention
As it is shown in figure 1, by be sequentially connected with after phosphorus groove 100 reactor 200, solid-liquid filtration piece-rate system 300, rinse-system 400,
Product groove 500, wherein, reactor 200 is provided with agitating device 210 and is provided with water inlet, solid-liquid filtration piece-rate system
300 include medial launder 310, cross-flow filter 320 and are connected between the circulation pipe between groove 310 and cross-flow filter 320
Road, circulation line is provided with circulating pump, and the outside of medial launder 310 and cross-flow filter 320 is equipped with steam insulation chuck,
The bottom of medial launder 310 connects a dehydration equipment 600 by blow-off line, and dehydration equipment 600 uses pressure filter；Rinse-system
400 include three grades of rinsing devices 410, respectively first order rinsing device 410a, second level rinsing device 410b, third level rinsing device 410c,
Agitating device 411, water inlet, yellow phosphorus entrance, yellow phosphorus outlet, nitrogen inlet and aerofluxus it is equipped with on three grades of rinsing devices 410
Mouthful, the outside of three grades of rinsing devices 410 is equipped with steam insulation chuck, and the bottom of three grades of rinsing devices 410 connects discharge duct, discharging
The outfan of pipe is connected with reactor 200 again, and discharge duct is provided with pump.Above-mentioned reactor 200 and solid-liquid filtration piece-rate system
Between 300, between solid-liquid filtration piece-rate system 300 and rinse-system 400 and solid-liquid filtration piece-rate system 300 inside and drift
Wash the pipeline within system 400 and all use utilidor.
When producing yellow phosphorus, phosphorus ore, coke and silica raw material are put in proportion phosphor furnace reaction, then by spray thrower to stove
Gas carry out spraying cooling and spray thrower bottom by phosphorus groove 100 in obtain thick phosphorus, the most according to the following steps to this thick phosphorus at
Reason: first, sends thick phosphorus into reactor 200, and this reactor is interior and temperature remains 60-90 DEG C to make the entrance of thick phosphorus be passed through in advance
Hot water in, then stirred by agitating device 210 in the mixed serum of yellow phosphorus and water, after all melting to yellow phosphorus, add grain again
Footpath be 80-500 μm, addition be the activated carbon powder that thick phosphorus adds weight 0.2-2%, be then stirred for 30-120 minute；Its
Secondary, send into medial launder 310 immediately after serosity stirring, the most again the serosity in medial launder 310 is pumped to cross-flow filter 320
Carry out cross flow filter, by outside steam insulation chuck, filtration temperature is maintained at 60-90 DEG C during cross flow filter, is filtered out
Yellow phosphorus in solid content be below 5mg/L, and cross-flow filter 320 does not carries out the serosity that filters and returns medial launder 310 then
Re-start filtration again；3) the above-mentioned yellow phosphorus filtered out feeding first order rinsing device 410a will be passed through the rinsing of this first order in advance
During temperature remains the hot water of 70-90 DEG C in device 410a, and make first by nitrogen injection in first order rinsing device 410a
It is full of the nitrogen for displaced air above liquid phase in level rinsing device 410a, then starts agitating device 411 and be stirred, stir
Mix rear sufficient standing, by hot water bottom but do not include that the yellow phosphorus bottom first order rinsing device 410a enters second level rinsing device the most again
410b, second level rinsing device 410b use the rinse method as first order rinsing device 410a to rinse, the most again by Huang
Phosphorus enters third level rinsing device 410c, third level rinsing device 410c and uses identical rinse method equally, rinses through the third level
Quasi-yellow phosphorus product after device 410c rinsing sends into product groove 500, by obtaining yellow phosphorus product after packaging.Above-mentioned three grades of rinsing devices 410
Interior remaining yellow phosphorus is by discharge duct loopback reactor 200, and the phosphorus mud of phosphorus content≤3% bottom medial launder 310 then enters pressure
Filter carries out processed, and after processed, dry slag sends phosphor furnace back to, and Water Sproading utilizes.
It addition, before the serosity being mixed with activated carbon powder is sent into solid-liquid filtration piece-rate system 300, the most first this solid-liquid filtration is divided
Carry out the pre-heat treatment from system 300, during the pre-heat treatment, the hot water that temperature is 70-90 DEG C is injected solid-liquid filtration piece-rate system and make it
Run until the temperature of solid-liquid filtration piece-rate system 300 reaches more than 50 DEG C by filter type.Secondly, solid-liquid filtration is used to separate
After the serosity being mixed with activated carbon powder is filtered by system 300, again the hot water that temperature is 70-90 DEG C can be injected this solid-liquid filtration
Piece-rate system 300 makes it run until yellow phosphorus in cross-flow filter 320 is fully cleaned displacement by filter type, and anti-locking system is residual
Blocking to pipe stage filter element after slag cooling.
Above-mentioned cross-flow filter 320 can use common cross-flow filter, but being gradually increased along with concentration of slurry, yellow phosphorus
Mobility is deteriorated, and filter efficiency is affected.In order to solve such problem, cross-flow filter 320 is improved to following structure:
As in figure 2 it is shown, improve cross-flow filter 320 in be provided with for receive and transmit the hot water that temperature is 70-90 DEG C first
Layer passage T1, for receive and transmit described serosity to be filtered second layer passage T2 and for receive and transmit filtered Huang
The third layer passage T3 of phosphorus, via the first partition wall having by property between described ground floor passage T1 and second layer passage T2
321 are separated, and are divided via the second partition wall 322 doubling as filtering material between second layer passage T2 and third layer passage T3
Every, during filtration in the fluid pressure ＞ third layer passage T3 in the fluid pressure ＞ second layer passage T2 in ground floor passage T1
Fluid pressure, so that described hot water enters second layer passage T2, hot water and described serosity to be filtered through the first partition wall 321
Mixture filter the second partition wall 322 and enter third layer passage T3, and, enter the second layer through the first partition wall 321 and lead to
The liquid measure of road T2 is filter the liquid measure that the second partition wall 322 enters third layer passage T3 0.8-1.2 times.
Specifically, as in figure 2 it is shown, the second partition wall 322 is by the inward flow filtration-type in being arranged on filter housing 323 through orifice plate
Chimney filter 325 is constituted, and this inward flow filtration-type chimney filter 325 uses sintered titanium Lu porous material to make, its two ends respectively with filter assemblies
The first port D1 and the second port D2 conducting, be third layer passage T3 between inward flow filtration-type chimney filter 325 and described shell 323,
Third layer passage T3 turns on the 3rd port D3 of filter；Described first partition wall 321 uses stainless porous material,
It is by being arranged on filter assemblies shell 323 through keeper and the core pipe 326 that is placed in inward flow filtration-type chimney filter 325 is constituted,
The top end of filter is provided with hot water and houses storehouse 327, and the upper end of core pipe 326 extends to this hot water matter and houses storehouse 327 and pass through hole
Plate communicates therewith, and the 4th port D4 is positioned at hot water and houses on storehouse 327, and the lower end of core pipe 326 terminates in entering of inward flow filtration-type chimney filter 325
Oral area is divided and is closed by plug, and the inner chamber of core pipe 326 is described ground floor passage T1, core pipe 326 and inward flow filtration-type chimney filter 325
Between be described second layer passage T2.In addition, filter assemblies shell 323 sidepiece is additionally provided with fifth port D5, for right
In hot water, backwash liquid is injected when inward flow filtration-type chimney filter 325 carries out backwash regeneration.It addition, be provided with insulation on filter housing specially
Set 324, described muff 324 is respectively equipped with thermal insulation medium input D6 and thermal insulation medium discharge end D7, thus preferably ties up
Hold the filtration temperature in assembly.Thermal insulation medium can use steam or other add thermal medium.
During filtration, the serosity in medial launder 310 is from the first port D1 input filter of filter, and then enters into filter
In inward flow filtration-type chimney filter 325, and from lower to upper to the second port D2 flowing；Now, by the pipeline facilities outside filter to
Two-port netwerk D4 injects the hot water of 70-90 DEG C, and the hot water entering filter moves from top to bottom from the inner chamber of core pipe 326；By
Pressure differential between one layer of passage T1 and second layer passage T2 controls as 0.05-0.1MPa, second layer passage T2 and third layer
Pressure differential between passage T3 controls as 0.2-0.3MPa, so that hot water enters second layer passage T2 through core pipe 326, heat
The mixture of water and serosity filters inward flow filtration-type chimney filter 325 and enters third layer passage T3, enters the second layer through the first partition wall 321
The liquid measure of passage T2 is to filter the second partition wall 322 to enter the liquid measure of third layer passage T3 substantially quite, enters third layer passage
The purer yellow phosphorus of T3 discharges assembly from the 3rd port D3, and the material not filtered flows out from the second port D2, returns middle
Groove 310.
Pass through said process, it can be seen that the technical scheme of above-mentioned embodiment can produce following effect: 1, by hot water by interior
Outwards give the direction motion outside inward flow filtration-type chimney filter 325 of one pressure of yellow phosphorus, beneficially yellow phosphorus, enhance yellow phosphorus cross flow filter mistake
Diffusion outside in journey, improves filtration separation efficiency；2, when yellow phosphorus moves in second layer passage T2 from lower to upper,
Along with the carrying out filtered, the concentration of yellow phosphorus is in the trend gradually risen；Meanwhile, when hot water in ground floor passage T1 from top to bottom
During motion, from large to small, therefore, the local hot water that the concentration of yellow phosphorus is the highest enters second layer passage T2 through core pipe 326 to pressure
Amount the biggest, the amount that local hot water that the concentration of yellow phosphorus is the lowest enters second layer passage T2 through core pipe 326 is the fewest,
Such that it is able to the concentration difference in balance second layer passage T2, improve the uniformity of concentration, can effectively avoid runner blockage problem,
And improve filtration stability and filter efficiency；3, by hot water, filter process is incubated, can preferably maintain filtration temperature
Degree, the filtration of the system that applicable temperature requirement is higher.
Embodiment 1
Thick phosphorus is sent into reactor 200, makes thick phosphorus enter and be passed through in advance in this reactor and temperature remains the hot water of 75 DEG C and (adopts
With pure water, lower same) in, then stirred by agitating device 210 after all melting to yellow phosphorus again to the mixing slurry of yellow phosphorus with water
Liquid adds particle diameter be 100-500 μm, addition be the activated carbon powder that thick phosphorus adds weight 0.2%, be then stirred for 30 minutes；
Secondly, send into medial launder 310 immediately after serosity stirring, the most again the serosity in medial launder 310 is pumped to cross-flow filter 320
Carrying out cross flow filter, filtration temperature during cross flow filter is maintained at 75 DEG C, between ground floor passage T1 and second layer passage T2
Pressure differential controls to be 0.05MPa, and the pressure differential between second layer passage T2 and third layer passage T3 controls as 0.2MPa, serosity
Flow velocity in second layer passage T2 is 2.5m/s, and in the yellow phosphorus being filtered out, solid content is 4.5mg/L, and cross-flow filter
The serosity not carrying out filtering in 320 returns medial launder 310 and re-starts filtration the most again；3) the above-mentioned yellow phosphorus filtered out is sent into
First order rinsing device 410a is passed through in advance in the hot water that temperature in this first order rinsing device 410a remains 75 DEG C, and by
Nitrogen injection in first order rinsing device 410a and be full of the nitrogen for displaced air above liquid phase in making first order rinsing device 410a
Gas, then start agitating device 411 stir 30 minutes, sufficient standing after stirring, the most again by hot water bottom but do not include first
Yellow phosphorus bottom level rinsing device 410a enters second level rinsing device 410b, second level rinsing device 410b and uses and first order rinsing device
Rinse method same for 410a rinses, and yellow phosphorus enters third level rinsing device 410c, third level rinsing device 410c the most again
The rinse method that same employing is identical, the quasi-yellow phosphorus product after third level rinsing device 410c rinses sends into product groove 500, logical
Obtaining yellow phosphorus product after crossing packaging, yellow phosphorus content reaches 99.97%.In above-mentioned three grades of rinsing devices 410, remaining yellow phosphorus passes through discharging
Pipe loopback reactor 200, the phosphorus mud of phosphorus content≤3% bottom medial launder 310 then enters pressure filter and carries out processed, de-
After water processes, dry slag sends phosphor furnace, Water circulation back to.
Embodiment 2
Thick phosphorus is sent into reactor 200, makes thick phosphorus enter and be passed through in advance in this reactor and temperature remains the hot water of 75 DEG C and (adopts
With pure water, lower same) in, then stirred by agitating device 210 after all melting to yellow phosphorus again to the mixing slurry of yellow phosphorus with water
Liquid adds particle diameter be 100-500 μm, addition be the activated carbon powder that thick phosphorus adds weight 0.3%, be then stirred for 60 minutes；
Secondly, send into medial launder 310 immediately after serosity stirring, the most again the serosity in medial launder 310 is pumped to cross-flow filter 320
Carrying out cross flow filter, filtration temperature during cross flow filter is maintained at 75 DEG C, between ground floor passage T1 and second layer passage T2
Pressure differential controls to be 0.075MPa, and the pressure differential between second layer passage T2 and third layer passage T3 controls as 0.25MPa, slurry
Liquid flow velocity in second layer passage T2 is 2.7m/s, and in the yellow phosphorus being filtered out, solid content is 4.6mg/L, and cross-flow filter
The serosity not carrying out filtering in 320 returns medial launder 310 and re-starts filtration the most again；3) the above-mentioned yellow phosphorus filtered out is sent into
First order rinsing device 410a is passed through in advance in the hot water that temperature in this first order rinsing device 410a remains 75 DEG C, and by
Nitrogen injection in first order rinsing device 410a and be full of the nitrogen for displaced air above liquid phase in making first order rinsing device 410a
Gas, then start agitating device 411 stir 25 minutes, sufficient standing after stirring, the most again by hot water bottom but do not include first
Yellow phosphorus bottom level rinsing device 410a enters second level rinsing device 410b, second level rinsing device 410b and uses and first order rinsing device
Rinse method same for 410a rinses, and yellow phosphorus enters third level rinsing device 410c, third level rinsing device 410c the most again
The rinse method that same employing is identical, the quasi-yellow phosphorus product after third level rinsing device 410c rinses sends into product groove 500, logical
Obtaining yellow phosphorus product after crossing packaging, yellow phosphorus content reaches more than 99.99%.In above-mentioned three grades of rinsing devices 410, remaining yellow phosphorus passes through
Discharge duct loopback reactor 200, the phosphorus mud of phosphorus content≤3% bottom medial launder 310 then enters pressure filter and carries out processed,
After processed, dry slag sends phosphor furnace back to, and Water Sproading utilizes.
Embodiment 3
Thick phosphorus is sent into reactor 200, makes thick phosphorus enter and be passed through in advance in this reactor and temperature remains the hot water of 75 DEG C and (adopts
With pure water, lower same) in, then stirred by agitating device 210 after all melting to yellow phosphorus again to the mixing slurry of yellow phosphorus with water
Liquid adds particle diameter be 100-500 μm, addition be the activated carbon powder that thick phosphorus adds weight 1.2%, be then stirred for 100 minutes；
Secondly, send into medial launder 310 immediately after serosity stirring, the most again the serosity in medial launder 310 is pumped to cross-flow filter 320
Carrying out cross flow filter, filtration temperature during cross flow filter is maintained at 75 DEG C, between ground floor passage T1 and second layer passage T2
Pressure differential controls to be 0.1MPa, and the pressure differential between second layer passage T2 and third layer passage T3 controls to be 0.3MPa, and serosity exists
Flow velocity in second layer passage T2 is 2.5m/s, and in the yellow phosphorus being filtered out, solid content is 4.5mg/L, and cross-flow filter 320
In do not carry out the serosity that filters and return medial launder 310 and re-start filtration the most again；3) the above-mentioned yellow phosphorus filtered out is sent into first
Level rinsing device 410a is passed through in the hot water that temperature in this first order rinsing device 410a remains 75 DEG C in advance, and by first
Nitrogen injection in level rinsing device 410a and make to be full of the nitrogen for displaced air above the liquid phase in first order rinsing device 410a,
Then start agitating device 411 to stir 40 minutes, sufficient standing after stirring, by hot water bottom but do not include that the first order is floated the most again
Wash the yellow phosphorus bottom device 410a and enter second level rinsing device 410b, second level rinsing device 410b employing and first order rinsing device 410a
Same rinse method rinses, and yellow phosphorus enters third level rinsing device 410c the most again, and rinsing device 410c is same for the third level
Using identical rinse method, the quasi-yellow phosphorus product after third level rinsing device 410c rinses sends into product groove 500, by bag
Obtaining yellow phosphorus product after dress, yellow phosphorus content reaches more than 99.99%.In above-mentioned three grades of rinsing devices 410, remaining yellow phosphorus passes through discharging
Pipe loopback reactor 200, the phosphorus mud of phosphorus content≤3% bottom medial launder 310 then enters pressure filter and carries out processed, de-
After water processes, dry slag sends phosphor furnace back to, and Water Sproading utilizes.
Claims (10)
1. a production method for yellow phosphorus, obtains, for carrying out thick phosphorus refined, the yellow phosphorus product that purity is higher, the method
Step includes: 1) by thick phosphorus feeding one with the reactor (200) of agitating device (210), makes thick phosphorus enter and is passed through this in advance
In reactor and temperature remains in the hot water of 60-90 DEG C, then stir after all melting to yellow phosphorus again to the mixing of yellow phosphorus Yu water
Serosity adds particle diameter be 80-500 μm, addition be the activated carbon powder that thick phosphorus adds weight 0.2-2%, make this work by stirring
Property powdered carbon is sufficiently mixed with serosity；2) the above-mentioned serosity being mixed with activated carbon powder is sent into a solid-liquid filtration piece-rate system (300), make
It by the filtration of filter element in this solid-liquid filtration piece-rate system (300), is filtered out under the temperature conditions of 60-90 DEG C
Yellow phosphorus in solid content control at below 5mg/L；3) the above-mentioned yellow phosphorus filtered out is sent into rinse-system (400) to carry out at least
Three grades of rinsings, the yellow phosphorus first a upper operation obtained in every one-level rinse cycle feeding one is with the rinsing device of agitating device (411)
(410), make yellow phosphorus enter and be passed through in advance in the hot water that this rinsing device (410) interior temperature remains 60-90 DEG C, rinsing device (410)
Protect with nitrogen above interior liquid phase, stand after being then sufficiently stirred for, after standing, by hot water bottom but do not include rinsing device (410) again
The yellow phosphorus of bottom enters subsequent processing；4) the quasi-yellow phosphorus product after rinsing is sent into product groove (500), by place further
Yellow phosphorus product is obtained after reason.
2. the production method of yellow phosphorus as claimed in claim 1, it is characterised in that: described step 2) in specifically include following step
Rapid: 1. the serosity being mixed with activated carbon powder is sent into a medial launder (310)；2. the serosity in medial launder (310) is pumped to one wrong
Flow filter (320) carries out cross flow filter；3. the yellow phosphorus that cross-flow filter (320) filters out sends into rinse-system (400),
The serosity not carrying out in cross-flow filter (320) filtering returns medial launder (310)；4. step is returned 2.；Wherein, described cross-flow
It is provided with the ground floor passage (T1) for receiving and transmit the hot water that temperature is 70-90 DEG C in filter (320), is used for connecing
Receive and transmit the second layer passage (T2) of serosity to be filtered and filtered the third layer passage (T3) of yellow phosphorus for reception transmission,
Separated via the first partition wall (321) having by property between described ground floor passage (T1) and second layer passage (T2),
Separated via the second partition wall (322) doubling as filtering material between second layer passage (T2) and third layer passage (T3),
Fluid pressure ＞ third layer passage (T3) in fluid pressure ＞ second layer passage (T2) in ground floor passage (T1) during filtration
In fluid pressure so that described hot water enters second layer passage (T2), hot water and described through the first partition wall (321)
The mixture of serosity to be filtered filters the second partition wall (322) and enters third layer passage (T3), and, through the first partition wall
(321) liquid measure entering second layer passage (T2) is to filter the second partition wall (322) to enter the liquid of third layer passage (T3)
0.8-1.2 times of amount.
3. the production method of yellow phosphorus as claimed in claim 2, it is characterised in that: ground floor passage (T1) is led to the second layer
Pressure differential between road (T2) controls to be 0.05-0.1MPa, between second layer passage (T2) and third layer passage (T3)
Pressure differential controls as 0.2-0.3MPa.
4. the production method of yellow phosphorus as claimed in claim 2, it is characterised in that: by medial launder (310) bottom phosphorus content≤
The phosphorus mud of 3% enters dehydration equipment (600) and carries out processed, and after processed, dry slag sends phosphor furnace back to, and Water Sproading utilizes.
5. the production method of yellow phosphorus as claimed in claim 2, it is characterised in that: the serosity being mixed with activated carbon powder is being sent into solid
It is front that liquid filters piece-rate system (300), first this solid-liquid filtration piece-rate system (300) is carried out the pre-heat treatment, will during the pre-heat treatment
Temperature is that the hot water of 70-90 DEG C injects solid-liquid filtration piece-rate system and makes it run until solid-liquid filtration piece-rate system by filter type
(300) temperature reaches more than 50 DEG C.
6. the production method of yellow phosphorus as claimed in claim 2, it is characterised in that: also include using solid-liquid filtration piece-rate system
(300) after the serosity being mixed with activated carbon powder being filtered, then the hot water that temperature is 70-90 DEG C is injected this solid-liquid filtration divide
It is made to run until yellow phosphorus in cross-flow filter (320) fully cleans the operation of displacement by filter type from system (300).
7. the production method of the yellow phosphorus as described in any one claim in claim 1-6, it is characterised in that: described step
Rapid 1) in, the addition of activated carbon powder is the 0.3-0.5% that thick phosphorus adds weight.
8. the production method of the yellow phosphorus as described in any one claim in claim 1-6, it is characterised in that: by described
Step 3) in remaining yellow phosphorus loopback reactor (200) not entering subsequent processing in rinsing devices at different levels (410).
9. the production method of the yellow phosphorus as described in any one claim in claim 1-6, it is characterised in that: described step
Rapid 1) after adding activated carbon powder in mixed serum and stirring 30-120 minute, with dividing by this serosity feeding solid-liquid filtration
From system (300).
10. the production method of yellow phosphorus as claimed in claim 1, it is characterised in that: by described step 1) in reactor (200)
Interior hot water temperature controls at 70-80 DEG C；By described step 2) in serosity filter time temperature control at 70-80 DEG C；Will
Step 3) in hot water temperature in rinsing device (410) control at 70-80 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410182389.6A CN103964405B (en) | 2014-04-30 | A kind of production method of yellow phosphorus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410182389.6A CN103964405B (en) | 2014-04-30 | A kind of production method of yellow phosphorus |
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| Publication Number | Publication Date |
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| CN103964405A CN103964405A (en) | 2014-08-06 |
| CN103964405B true CN103964405B (en) | 2016-11-30 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575090A (en) * | 2009-06-16 | 2009-11-11 | 云南马龙产业集团股份有限公司 | Phosphorus separation and purification method and equipment |
| CN103213958A (en) * | 2013-03-29 | 2013-07-24 | 成都易态科技有限公司 | Method for recovering simple-substance phosphorus from sludge phosphorus via terminal membrane microfiltration and application for same |
| CN103523762A (en) * | 2013-09-29 | 2014-01-22 | 成都易态科技有限公司 | Yellow phosphorus production method and equipment |
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575090A (en) * | 2009-06-16 | 2009-11-11 | 云南马龙产业集团股份有限公司 | Phosphorus separation and purification method and equipment |
| CN103213958A (en) * | 2013-03-29 | 2013-07-24 | 成都易态科技有限公司 | Method for recovering simple-substance phosphorus from sludge phosphorus via terminal membrane microfiltration and application for same |
| CN103523762A (en) * | 2013-09-29 | 2014-01-22 | 成都易态科技有限公司 | Yellow phosphorus production method and equipment |
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