CN103771368A - Device for producing electronic grade phosphoric acid employing clapboard crystallization - Google Patents
Device for producing electronic grade phosphoric acid employing clapboard crystallization Download PDFInfo
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- CN103771368A CN103771368A CN201310745953.6A CN201310745953A CN103771368A CN 103771368 A CN103771368 A CN 103771368A CN 201310745953 A CN201310745953 A CN 201310745953A CN 103771368 A CN103771368 A CN 103771368A
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- acid
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- absorption tower
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- phosphoric acid
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 63
- 238000002425 crystallisation Methods 0.000 title claims abstract description 38
- 230000008025 crystallization Effects 0.000 title claims abstract description 36
- 239000002253 acid Substances 0.000 claims abstract description 169
- 238000010521 absorption reaction Methods 0.000 claims abstract description 59
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 claims abstract description 53
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 28
- 239000011574 phosphorus Substances 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 238000002485 combustion reaction Methods 0.000 claims abstract description 15
- 238000006477 desulfuration reaction Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000007872 degassing Methods 0.000 claims description 33
- 238000002309 gasification Methods 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000012717 electrostatic precipitator Substances 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 239000007921 spray Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 9
- 238000003860 storage Methods 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 238000012856 packing Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 230000008676 import Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 3
- 210000005056 cell body Anatomy 0.000 claims description 3
- 238000007791 dehumidification Methods 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- 238000005367 electrostatic precipitation Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 230000036571 hydration Effects 0.000 claims description 3
- 238000006703 hydration reaction Methods 0.000 claims description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 3
- 230000002093 peripheral effect Effects 0.000 claims description 3
- 230000002000 scavenging effect Effects 0.000 claims description 3
- 239000010865 sewage Substances 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 238000003466 welding Methods 0.000 claims description 3
- 229910052785 arsenic Inorganic materials 0.000 abstract description 5
- 230000023556 desulfurization Effects 0.000 abstract 2
- 230000003009 desulfurizing effect Effects 0.000 abstract 2
- 238000002156 mixing Methods 0.000 abstract 2
- 238000000034 method Methods 0.000 description 16
- 239000013078 crystal Substances 0.000 description 14
- 239000012535 impurity Substances 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 230000007423 decrease Effects 0.000 description 2
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000004973 liquid crystal related substance Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000035900 sweating Effects 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 230000036470 plasma concentration Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Abstract
The invention discloses a device for producing electronic grade phosphoric acid employing clapboard crystallization. The device is provided with a raw material purifying unit, a combustion absorption unit and a product purifying unit, wherein the raw material purifying unit comprises a yellow phosphorus rinsing tank, an air washing tower and a high-level phosphorus supply tank; the combustion absorption unit comprises a rectangular tube gasified yellow phosphorus combustion furnace, a primary absorption tower, a secondary absorption tower, a venturi tube, an electric demister and an induced draft fan; the product purifying unit comprises an acid adjusting tank, a de-arsenic reactor, a de-arsenic filter, a desulfurizing tower, a clapboard crystallizer, a desulfurization filter and a product blending tank; the yellow phosphorus rinsing tank, the high-level phosphorus supply tank, the rectangular tube gasified yellow phosphorus combustion furnace, the primary absorption tower, the secondary absorption tower, the acid adjusting tank, the de-arsenic reactor, the de-arsenic filter, the desulfurizing tower, the clapboard crystallizer, the desulfurization filter and the product blending tank are orderly connected; the rectangular tube gasified yellow phosphorus combustion furnace is connected with the air washing tower; the secondary absorption tower is also orderly connected with the venturi tube, the electric demister and the induced draft fan.
Description
Technical field
The invention belongs to technical field of chemical, relate to a kind of device of dividing plate crystallization production electron-level phosphoric acid.
Background technology
Electron-level phosphoric acid belongs to high-purity phosphoric acid, be widely used in large-scale integrated circuit, the microelectronics industry such as film liquid crystal display (TFT-LCD), be mainly used in cleaning and the etching of chip, its purity and the cleanliness factor yield rate to electronic devices and components, conductivity and reliability have a significant impact, the cleaning of what purity was lower be mainly used in liquid crystal panel parts, cleaning and the etching of electronic wafer production process that what purity was higher be mainly used in, due to insoluble solid particle or metal ion all may be between fine circuits On current, make it short circuit, so electron-level phosphoric acid has harsh requirement to insoluble solid particle and most metal ion content.
Owing to requiring in electron-level phosphoric acid, impurity metal ion content is few, and separating difficulty is larger, conventionally prepares electron-level phosphoric acid take the PHOSPHORIC ACID TECH.GRADE of food grade phosphoric acid or preliminary purification as raw material.At present, the purifying method of phosphoric acid generally has: solvent extration, ion exchange method, electroosmose process, crystallization process etc.Compared with other several method, crystallization process has that energy consumption is low, equipment is simple, running cost is little, pollute little advantage, and product purity is high simultaneously, and colourity is good, is used as primary study method prepared by electron-level phosphoric acid always.
Chinese patent CN2009l0094409.3, a kind ofly relate to phosphoric acid production method by the method that yellow phosphorus is directly produced electron-level phosphoric acid, to put into combustion tower through purifying pretreated industrial yellow phosphorus, through multilevel oil removal, removal of impurities, control wet air, industrial yellow phosphorus is fully burnt, then gas Vanadium Pentoxide in FLAKES burning being produced is sent into absorption tower, use the pure water absorption that circulates, absorbing the phosphoric acid concentration producing reaches after 85.0%-87.0%, send into phosphoric acid purification finishing apparatus, through the moon, positively charged ion removes, aeration, after multi-stage filtration purifying treatment, under ten thousand grades or thousand grades of purifying air environment, purify.This method complex manufacturing, production environment requires harsh, and quality product is difficult to control.
Chinese patent 200610013611.5 use preparing electronic-grade phosphoric acid via melting-crystallizations, at-45～-35 ℃, wall built-up produces crystal seed and is then warming up to-2～-10 ℃, circulation adds raw material to make it grow to when thickness reaches 2～4cm and start to heat up at plane of crystal, get rid of when liquid mass is 10～40% and stop, productive rate is 12～20%.This method service temperature is extremely low, and energy consumption is large, and need to carry out pre-treatment to raw material and remove arsenic, and the operating time is long, and production cost is high, and productive rate is low.
Chinese patent 201010100473.0 use preparing highly-pure phosphoric acid by flow chromatographic crystallization method, adopt additional sound field to go out crystalline substance, to raw materials used purity requirement high (major impurity ionic concn is all less than 1.7mg/L, and needs micro-pore-film filtration processing), application difficulty is larger, is not easy to industrialization.
Chinese patent 201010104321.8 adopts liquid membrane crystal legal system for electron-level phosphoric acid, on the wall of 10～20 ℃, add crystal seed to start cooling simultaneously, by sparger, raw material phosphor acid solution body is added on wall, raw material is liquid film state and flows through crystal seed, grow into epitaxial at wall, reach 5～10 ℃, terminal of cooling and start the sweating that heats up after mother liquor is fully got rid of,, stop when the sweating to 15～29 ℃.The method is a dynamic crystallization operation process, and crystalline mother solution is not discharged immediately.By disposable decrease temperature crystalline---constant temperature discharge opeing---intensification thermal treatment carrys out refined product.This method has been improved crystal seed producing method, and service temperature is brought up to easy to reach interval, twice crystallization yields 20～30%.But in the electron-level phosphoric acid preparing by the method, Na, Al, Mg, Cr plasma concentration higher (1.79mg/L, 0.94mg/L, 0.49mg/L, 0.37mg/L), can not meet the demand that user upgrades day by day, still needs further improvement.
Summary of the invention
The present invention, in order to overcome the deficiencies in the prior art, provides a kind of device simple, easily operation, and practical, product cost is lower, and the device of electron-level phosphoric acid is produced in the dividing plate crystallization of constant product quality.
Technical scheme of the present invention is as follows:
A device for electron-level phosphoric acid is produced in dividing plate crystallization, and purification of raw materials unit, burning absorptive unit and product purifier units are set; Purification of raw materials unit equipment comprises yellow phosphorus rinse tank, air scrubber and high-order phosphorus supply groove, burning absorptive unit equipment comprises rectangular pipe gasification yellow phosphorus burning stove, main absorption tower, secondary absorption tower, Venturi tube, electrostatic precipitator and induced draft fan, and product purifier units equipment comprises acid adjustment groove, dearsenification reactor, dearsenification filter, thionizer, dividing plate crystallization apparatus, plate-and-frame filter press and product preparing groove; Yellow phosphorus rinse tank, high-order phosphorus supply groove, rectangular pipe gasification yellow phosphorus burning stove, main absorption tower, secondary absorption tower, acid adjustment groove, dearsenification reactor, dearsenification filter, thionizer, dividing plate crystallization apparatus, plate-and-frame filter press are connected successively with product preparing groove, wherein rectangular pipe gasification yellow phosphorus burning stove being connected with air scrubber, secondary absorption tower is separately connected successively with Venturi tube, electrostatic precipitator and induced draft fan.
Above-described yellow phosphorus rinse tank is provided with washing recycle pump, and is provided with heating jacket and yellow phosphorus discharge port, and the water-in of heating jacket is connected with the water outlet of rectangular pipe gasification yellow phosphorus burning furnace roof portion, and yellow phosphorus discharge port is connected with the opening for feed at high-order phosphorus supply groove top.
The patent of invention " safe phosphorus supply device that thermal phosphoric acid is produced " that above-described high-order phosphorus supply groove is patent No. CN201010127143.0; This device is mainly provided with gauger, chuck, the molten phosphorus outlet of high-order phosphorus supply groove (5) adopts acid-proof pipe to be connected with variable valve, before and after gauger, adopt acid-proof pipe to be connected with variable valve, molten phosphorus import for rectangular pipe gasification yellow phosphorus burning stove hypomere adopts acid-proof pipe to be connected with variable valve, and the water-in of phosphorus-melting groove adopts attemperater to be connected with the water outlet of roasting kiln epimere.
Above-described air scrubber is the innovation and creation " with the device of phosphoric acid adsorption and dehumidification and dedusting air cleaning " of patent No. CN201120199684.4; This device comprises that scavenging tower, acid storage tank, acid circulating pump form, air washing top of tower arranges sprinkler head, and adopt acid-proof pipe to be connected with acid circulating pump, air washing hypomere adopts acid-proof pipe to be connected successively with acid storage tank and acid circulating pump, or be connected in thermal phosphoric acid production equipment, adopt acid-proof pipe to be connected for blower fan and air scrubber hypomere.
" a kind of rectangular pipe yellow phosphorus gasification combustion furnace " that above-described rectangular pipe gasification yellow phosphorus burning stove adopts our company to apply on the same day, this device comprises and in roasting kiln, is provided with rectangle vapor lamp, hook and bracing frame, one end of rectangle vapor lamp tiltedly extends downward in the middle of roasting kiln bottom from rectangular angular, and at rectangle vapor lamp tail end, nozzle is set, the sleeve pipe that the other end arranges by the stove chuck of roasting kiln is connected with phosphorus-melting groove.
He Fu absorption tower, above-described main absorption tower adopts conventional phosphoric acid hydration absorption tower, Countermeasure of Concentrated Acid Pump and concentrated acid groove have been set up in described main absorption tower, the acid inlet of described concentrated acid groove is connected with the acid mouth of rectangular pipe yellow phosphorus gasification combustion furnace epimere and the acid mouth of lower end, main absorption tower respectively, the acid inlet of described Countermeasure of Concentrated Acid Pump is connected with the acid mouth of concentrated acid groove, and the acid mouth of Countermeasure of Concentrated Acid Pump is connected with shower nozzle and Countermeasure of Concentrated Acid Pump acid mouth that top, main absorption tower arranges respectively; Thin acid pump and dilute acid bath have been set up in described secondary absorption tower, the acid inlet of described dilute acid bath is connected with acid mouth, the acid mouth of Venturi tube lower end and the acid mouth of electrostatic precipitator lower end on secondary absorption tower respectively, the acid inlet of described thin acid pump is connected with the acid mouth of dilute phosphoric acid groove, and the shower nozzle that the acid mouth of dilute phosphoric acid pump arranges with top, secondary absorption tower respectively, the shower nozzle that top, main absorption tower arranges and the acid inlet at acid adjustment groove top are connected.
Above-described electrostatic precipitator is the patent of invention " phosphoric acid tail gas electric demister " of patent No. CN201010127141.1; This device is provided with discharge chamber, cooling room, plenum chamber, inlet plenum, and its parts comprise: high voltage and constant current direct supply lead wire insulation case, without lead wire insulation case, top cover, housing, discharge chamber manhole, corona electrode device, card one, anode electrostatic precipitation pipe, water-in, card two, plenum chamber's manhole, gas distribution grid, inlet plenum manhole, inclined bottom plate, sewage draining exit, inlet mouth, water outlet, air outlet and flushing arrangement composition.
Above-described acid adjustment groove is provided with chuck and whipping appts, and the water-in of described chuck is connected with the water outlet of round tube gasification combustion furnace or the water outlet on main absorption tower.
Above-described dearsenification reactor mainly arranges pipe in dearsenification reactor, dearsenification recycle pump and dearsenification literary composition and also circulates and be connected successively; Described dearsenification reactor arranges opening for feed, P
2s
5dog-house and air outlet, in dearsenification literary composition, pipe arranges dearsenification reactor middle and lower part, the opening for feed of dearsenification recycle pump be located at dearsenification reactor bottom discharge port and be connected, dearsenification reactor top opening for feed is connected with acid adjustment groove and electrostatic precipitator respectively with air outlet.
Above-described thionizer is the patent of invention " a kind of food grade phosphoric acid removes the device of hydrogen sulfide " of patent No. CN201220735526.0; This device mainly arranges acid colleciton groove, desulfuration recycle pump and degassing tower, the connection that circulates successively of degassing tower, acid colleciton groove, desulfuration recycle pump; Described degassing tower is arranged at top, top, acid colleciton groove one end, and is communicated with the cell body welding of acid colleciton groove; Degassing tower arranges H
2s air outlet, spray header, packing layer; Described H
2s air outlet is arranged at degassing tower top, and is connected with the dearsenification reactor of peripheral hardware; Described spray header is arranged at the top of degassing tower, and is connected successively with valve V and desulfuration recycle pump with circulation tube; Packing layer and Stainless Steel Cloth are arranged at middle part and the bottom of degassing tower; The acid colleciton groove middle part side of being body, two ends is semicylinder; Acid colleciton groove arranges acid inlet, uncontaminated air air inlet port and valve VI, and acid inlet and manhole setting are positioned at acid colleciton groove near top, degassing tower one end, and acid inlet arranges cover plate and material inlet valve; Inlet mouth setting is positioned at acid colleciton groove away from top, degassing tower one end; The setting of valve III is positioned at acid colleciton groove away from bottom, degassing tower one end, and valve III is connected with desulphurization circulating pump inlet usage is blue; Desulphurization circulating pump discharge connecting tee pipe, wherein one first connects valve V, then is connected with the spray header of degassing tower tower top with circulation tube, and another connects valve IV and leads to dividing plate crystallization apparatus.
Than prior art, advantage of the present invention and positively effect are as follows:
1, the present invention adopts this enterprise security phosphorus supply device patented technology, burning fused raw material yellow phosphorus enters combustion chamber by the bottom of combustion tower, in low level phosphorus-melting groove with waterhead safe transport, avoid with high-pressure pump or pressurized air, the molten yellow phosphorus under high-risk status being transported to header tank in conventional production lines, and then through high pressure spraying this dangerous operation link that burns.
2, present method adopts ultrapure water to yellow phosphorus raw materials melt and rinsing removal of impurities pre-treatment, has effectively guaranteed the high purity of electronics acid starting material.
3, adopt phosphoric acid washing tower to purify dehumidifying, removal of impurities to the required air of yellow phosphorus burning, effectively avoid air to bring the yellow phosphorus burning effect that steam and dust cause into and pay no attention to the problem that product foreign matter content increases of thinking of.
4, by adopting dividing plate crystallizer to make phosphoric acid crystallization in separator face, increase unit crystallization area, improved crystalline rate.
5, in crystallizer, arrange and wash brilliant device, to the spray washing of crystal column surface and the remaining liquid phase of storage acid tank, avoided the situation of liquid phase that foreign matter content is higher and the miscible quality product decline causing of pure crystal.
6, utilize the thermal source of the self-produced hot water of phosphoric acid production enterprise as crystal melting, greatly reduce the production energy consumption of electron-level phosphoric acid, there is good economical efficiency.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that the device of electron-level phosphoric acid is produced in a kind of dividing plate crystallization of the present invention.
Accompanying drawing mark: 0-yellow phosphorus rinse tank, 1-washes recycle pump, 2-acid circulating pump, 3-air scrubber, 4-is for blower fan, 5 high-order phosphorus supply grooves, 6-rectangular pipe gasification yellow phosphorus burning stove, 7-concentrated acid groove, the main absorption tower of 8-, 9-Countermeasure of Concentrated Acid Pump, the secondary absorption tower of 10-, 11-dilute acid bath, 12-thin acid pump, 13-Venturi tube, 14-electrostatic precipitator, 15-induced draft fan, 16-acid adjustment groove, 17-dearsenification reactor, 18-dearsenification recycle pump, 19-dearsenification filter, 20-thionizer, 21-desulfuration recycle pump, 22-dividing plate crystallization apparatus, 23-water pump, 24-goes out acid/recycle pump, 25-plate-and-frame filter press, 26-storage tank, 27 product preparing grooves.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1:
A device for electron-level phosphoric acid is produced in dividing plate crystallization, and purification of raw materials unit, burning absorptive unit and product purifier units are set; Purification of raw materials unit equipment comprises yellow phosphorus rinse tank 0, air scrubber 3 and high-order phosphorus supply groove 5, burning absorptive unit equipment comprises rectangular pipe gasification yellow phosphorus burning stove 6, main absorption tower 8, secondary absorption tower 10, Venturi tube 13, electrostatic precipitator 14 and induced draft fan 15, and product purifier units equipment comprises acid adjustment groove 16, dearsenification reactor 17, dearsenification filter 19, thionizer 20, dividing plate crystallization apparatus 22, plate-and-frame filter press 25 and product preparing groove 27; Yellow phosphorus rinse tank 0, high-order phosphorus supply groove 5, rectangular pipe gasification yellow phosphorus burning stove 6, main absorption tower 8, secondary absorption tower 10, acid adjustment groove 16, dearsenification reactor 17, dearsenification filter 19, thionizer 20, dividing plate crystallization apparatus 22, plate-and-frame filter press 25 are connected successively with product preparing groove 27, its rectangular pipe gasification yellow phosphorus burning stove 6 is also connected with air scrubber 3, and secondary absorption tower 10 is separately connected successively with Venturi tube 13, electrostatic precipitator 14 and induced draft fan 15.
Above-described yellow phosphorus rinse tank 0 is provided with washing recycle pump 1, and be provided with heating jacket and yellow phosphorus discharge port, the water-in of heating jacket is connected with the water outlet at rectangular pipe gasification yellow phosphorus burning stove 6 tops, and yellow phosphorus discharge port is connected with the opening for feed at high-order phosphorus supply groove 5 tops.
The patent of invention " safe phosphorus supply device that thermal phosphoric acid is produced " that above-described high-order phosphorus supply groove 5 is patent No. CN201010127143.0; This device is mainly provided with gauger, chuck, the molten phosphorus outlet of high-order phosphorus supply groove 5 adopts acid-proof pipe to be connected with variable valve, before and after gauger, adopt acid-proof pipe to be connected with variable valve, molten phosphorus import for rectangular pipe gasification yellow phosphorus burning stove 6 hypomeres adopts acid-proof pipe to be connected with variable valve, and the water-in of phosphorus-melting groove adopts attemperater to be connected with the water outlet of roasting kiln epimere.
The patent of invention " with the device of phosphoric acid adsorption and dehumidification and dedusting air cleaning " that above-described air scrubber 3 is patent No. CN201120199684.4; This device comprises that scavenging tower, acid storage tank, acid circulating pump 2 form, air scrubber 3 tops arrange sprinkler head, and adopt acid-proof pipe to be connected with acid circulating pump 2, air washing 3 hypomeres adopt acid-proof pipe to be connected successively with acid storage tank and acid circulating pump 2, or be connected in thermal phosphoric acid production equipment, adopt acid-proof pipe to be connected for blower fan 4 with air scrubber 3 hypomeres.
" a kind of rectangle yellow phosphorus gasification combustion furnace " that above-described rectangular pipe gasification yellow phosphorus burning stove 6 adopts our company to apply on the same day, this device comprises and in roasting kiln, is provided with rectangle vapor lamp, hook and bracing frame, one end of rectangle vapor lamp tiltedly extends downward in the middle of roasting kiln bottom from rectangular angular, and at rectangle vapor lamp tail end, nozzle is set, the sleeve pipe that the other end arranges by the stove chuck of roasting kiln is connected with phosphorus-melting groove.
Above-described main absorption tower 8 and secondary absorption tower 10 adopt conventional phosphoric acid hydration absorption tower, Countermeasure of Concentrated Acid Pump 9 and concentrated acid groove 7 have been set up in described main absorption tower 8, the acid inlet of described concentrated acid groove 7 is connected with the acid mouth of rectangular pipe gasification yellow phosphorus burning stove 6 epimeres and the acid mouth of 8 lower ends, main absorption tower respectively, the acid inlet of described Countermeasure of Concentrated Acid Pump 9 is connected with the acid mouth of concentrated acid groove 7, and the acid mouth of Countermeasure of Concentrated Acid Pump 9 is connected with shower nozzle and Countermeasure of Concentrated Acid Pump 9 acid mouths that 8 tops, main absorption tower arrange respectively; Thin acid pump 12 and dilute acid bath 11 have been set up in described secondary absorption tower 10, the acid inlet of described dilute acid bath 11 is connected with acid mouth, the acid mouth of Venturi tube 13 lower ends and the acid mouth of electrostatic precipitator 14 lower ends on secondary absorption tower 10 respectively, the acid inlet of described thin acid pump 12 is connected with the acid mouth of dilute phosphoric acid groove 11, and the shower nozzle that the acid mouth of dilute phosphoric acid pump 12 arranges with 10 tops, secondary absorption tower respectively, the shower nozzle that 8 tops, main absorption tower arrange and the acid inlet at acid adjustment groove 16 tops are connected.
The patent of invention " phosphoric acid tail gas electric demister " that above-described electrostatic precipitator 14 is patent No. CN201010127141.1; This device is provided with discharge chamber, cooling room, plenum chamber, inlet plenum, and its parts comprise: high voltage and constant current direct supply lead wire insulation case, without lead wire insulation case, top cover, housing, discharge chamber manhole, corona electrode device, card one, anode electrostatic precipitation pipe, water-in, card two, plenum chamber's manhole, gas distribution grid, inlet plenum manhole, inclined bottom plate, sewage draining exit, inlet mouth, water outlet, air outlet and flushing arrangement composition.
Above-described acid adjustment groove is provided with chuck and whipping appts, and the water-in of described chuck is connected with the water outlet of round tube gasification combustion furnace or the water outlet on main absorption tower.
Above-described described dearsenification reactor mainly arranges pipe in dearsenification reactor 17, dearsenification recycle pump 18 and dearsenification literary composition and also circulates and be connected successively; Described dearsenification reactor 17 arranges opening for feed, P
2s
5dog-house and air outlet, in dearsenification literary composition, pipe arranges dearsenification reactor 17 middle and lower parts, the opening for feed of dearsenification recycle pump 18 be located at dearsenification reactor 17 bottom discharge mouths and be connected, dearsenification reactor 17 top opening for feeds are connected with acid adjustment groove 16 and electrostatic precipitator 14 respectively with air outlet.
The patent of invention " a kind of food grade phosphoric acid removes the device of hydrogen sulfide " that above-described thionizer 20 is patent No. CN201220735526.0; This device mainly arranges acid colleciton groove, desulfuration recycle pump 21 and degassing tower, the connection that circulates successively of degassing tower, acid colleciton groove, desulfuration recycle pump 21; Described degassing tower is arranged at top, top, acid colleciton groove one end, and is communicated with the cell body welding of acid colleciton groove; Degassing tower arranges H
2s air outlet, spray header, packing layer; Described H
2s air outlet is arranged at degassing tower top, and is connected with the dearsenification reactor of peripheral hardware; Described spray header is arranged at the top of degassing tower, and is connected successively with valve V and desulfuration recycle pump 21 with circulation tube; Packing layer and Stainless Steel Cloth are arranged at middle part and the bottom of degassing tower; The acid colleciton groove middle part side of being body, two ends is semicylinder; Acid colleciton groove arranges acid inlet, uncontaminated air air inlet port and valve VI, and acid inlet and manhole setting are positioned at acid colleciton groove near top, degassing tower one end, and acid inlet arranges cover plate and material inlet valve; Inlet mouth setting is positioned at acid colleciton groove away from top, degassing tower one end; The setting of valve III is positioned at acid colleciton groove away from bottom, degassing tower one end, and valve III is connected with desulphurization circulating pump inlet usage is blue; Desulfuration recycle pump 21 exports connecting tee pipe, and wherein one first connects valve V, then is connected with the spray header of degassing tower tower top with circulation tube, and another connects valve IV and leads to dividing plate crystallization apparatus 22; The material of described packing layer is the one in plastics Raschig ring, stainless steel Raschig ring and ceramic raschig rings.
Above-described dividing plate crystallization apparatus 22, comprise crystallizer, go out acid/recycle pump 24, described crystallizer includes crystallization case, dividing plate, wash brilliant device, crystallizer is also provided with and adds crystal seed mouth, acid mouth, cold and hot medium inlet and cold and hot media outlet, the acid mouth of crystallizer by valve with go out acid/recycle pump 24 and be connected, top and the top of acid-regulating tank are provided with opening for feed, water-in, venting port and recycle acid import, go out acid/recycle pump 24 and plate-and-frame filter press 25, storage tank 26 is connected successively with product preparing groove 27, the outlet of recycle acid import and recycle acid with acid-proof pipe by going out acid/recycle pump and recycle acid valve is connected, go out acid/recycle pump 24 also with wash brilliant device and be connected, described dividing plate is provided with more than four, the setting of reporting to the leadship after accomplishing a task of crystal lattice and cold and hot medium lattice, and described acid inlet is located at crystal lattice top, and acid mouth is located at crystal lattice bottom, described cold and hot medium inlet is connected with into cold medium tube, enters thermal medium pipe and drain tube, and cold medium inlet is connected to cold medium tank by water pump 23, cold and hot medium inlet connects heat extraction medium tube and cold medium back flow pipe, and described cold medium back flow pipe connects cold medium tank, the described brilliant device of washing comprises water inlet pipe and shower, and the parallel crystal lattice top that is located at of shower, is evenly provided with spray header on shower, wash brilliant device by valve with go out sour pump and be connected.
Claims (10)
1. a device for electron-level phosphoric acid is produced in dividing plate crystallization, and purification of raw materials unit, burning absorptive unit and product purifier units are set; Purification of raw materials unit equipment comprises yellow phosphorus rinse tank (0), air scrubber (3) and high-order phosphorus supply groove (5), burning absorptive unit equipment comprises rectangular pipe gasification yellow phosphorus burning stove (6), main absorption tower (8), secondary absorption tower (10), Venturi tube (13), electrostatic precipitator (14) and induced draft fan (15), and product purifier units equipment comprises acid adjustment groove (16), dearsenification reactor (17), dearsenification filter (19), thionizer (20), dividing plate crystallization apparatus (22), plate-and-frame filter press (25) and product preparing groove (27); Yellow phosphorus rinse tank (0), high-order phosphorus supply groove (5), rectangular pipe gasification yellow phosphorus burning stove (6), main absorption tower (8), secondary absorption tower (10), acid adjustment groove (16), dearsenification reactor (17), dearsenification filter (19), thionizer (20), dividing plate crystallization apparatus (22), plate-and-frame filter press (25) are connected successively with product preparing groove (27), wherein rectangular pipe gasification yellow phosphorus burning stove (6) being connected with air scrubber (3), secondary absorption tower (10) are separately connected successively with Venturi tube (13), electrostatic precipitator (14) and induced draft fan (15).
2. the device of electron-level phosphoric acid is produced in a kind of dividing plate crystallization according to claim 1, it is characterized in that: described yellow phosphorus rinse tank (0) is provided with washing recycle pump (1), and be provided with heating jacket and yellow phosphorus discharge port, the water-in of heating jacket is connected with the water outlet at rectangular pipe gasification yellow phosphorus burning stove (6) top, and yellow phosphorus discharge port is connected with the opening for feed at high-order phosphorus supply groove (5) top.
3. the device of electron-level phosphoric acid is produced in a kind of dividing plate crystallization according to claim 1, it is characterized in that: the patent of invention " safe phosphorus supply device that thermal phosphoric acid is produced " that described high-order phosphorus supply groove (5) is patent No. CN201010127143.0; This device is mainly provided with gauger, chuck, the molten phosphorus outlet of high-order phosphorus supply groove (5) adopts acid-proof pipe to be connected with variable valve, before and after gauger, adopt acid-proof pipe to be connected with variable valve, molten phosphorus import for rectangular pipe gasification yellow phosphorus burning stove (6) hypomere adopts acid-proof pipe to be connected with variable valve, and the water-in of phosphorus-melting groove adopts attemperater to be connected with the water outlet of roasting kiln epimere.
4. the device of electron-level phosphoric acid is produced in a kind of dividing plate crystallization according to claim 1, it is characterized in that: the patent of invention " with the device of phosphoric acid adsorption and dehumidification and dedusting air cleaning " that described air scrubber (3) is patent No. CN201120199684.4; This device comprises that scavenging tower, acid storage tank, acid circulating pump (2) form, air scrubber (3) top arranges sprinkler head, and adopt acid-proof pipe to be connected with acid circulating pump (2), air washing (3) hypomere adopts acid-proof pipe to be connected successively with acid storage tank and acid circulating pump (2), or be connected in thermal phosphoric acid production equipment, adopt acid-proof pipe to be connected for blower fan (4) and air scrubber (3) hypomere.
5. the device of electron-level phosphoric acid is produced in a kind of dividing plate crystallization according to claim 1, it is characterized in that: " a kind of rectangle yellow phosphorus gasification combustion furnace " that described rectangular pipe gasification yellow phosphorus burning stove (6) adopts our company to apply on the same day, this device comprises and in roasting kiln, is provided with rectangle vapor lamp, hook and bracing frame, one end of rectangle vapor lamp tiltedly extends downward in the middle of roasting kiln bottom from rectangular angular, and at rectangle vapor lamp tail end, nozzle is set, the sleeve pipe that the other end arranges by the stove chuck of roasting kiln is connected with phosphorus-melting groove.
6. the device of electron-level phosphoric acid is produced in a kind of dividing plate crystallization according to claim 1, it is characterized in that: described main absorption tower (8) and secondary absorption tower (10) adopt conventional phosphoric acid hydration absorption tower, Countermeasure of Concentrated Acid Pump (9) and concentrated acid groove (7) have been set up in described main absorption tower (8), the acid inlet of described concentrated acid groove (7) is connected with the acid mouth of rectangular pipe gasification yellow phosphorus burning stove (6) epimere and the acid mouth of lower end, main absorption tower (8) respectively, the acid inlet of described Countermeasure of Concentrated Acid Pump (9) is connected with the acid mouth of concentrated acid groove (7), the acid mouth of Countermeasure of Concentrated Acid Pump (9) is connected with shower nozzle and Countermeasure of Concentrated Acid Pump (9) acid mouth that top, main absorption tower (8) arranges respectively, thin acid pump (12) and dilute acid bath (11) have been set up in described secondary absorption tower (10), the acid inlet of described dilute acid bath (11) is connected with acid mouth, the acid mouth of Venturi tube (13) lower end and the acid mouth of electrostatic precipitator (14) lower end of secondary absorption tower (10) respectively, the acid inlet of described thin acid pump (12) is connected with the acid mouth of dilute phosphoric acid groove (11), and the shower nozzle that the acid mouth of dilute phosphoric acid pump (12) arranges with top, secondary absorption tower (10) respectively, the shower nozzle that top, main absorption tower (8) arranges and the acid inlet at acid adjustment groove (16) top are connected.
7. the device of electron-level phosphoric acid is produced in a kind of dividing plate crystallization according to claim 1, it is characterized in that: described electrostatic precipitator (14) is the patent of invention " phosphoric acid tail gas electric demister " of patent No. CN201010127141.1; This device is provided with discharge chamber, cooling room, plenum chamber, inlet plenum, and its parts comprise: high voltage and constant current direct supply lead wire insulation case, without lead wire insulation case, top cover, housing, discharge chamber manhole, corona electrode device, card one, anode electrostatic precipitation pipe, water-in, card two, plenum chamber's manhole, gas distribution grid, inlet plenum manhole, inclined bottom plate, sewage draining exit, inlet mouth, water outlet, air outlet and flushing arrangement composition.
8. the device of electron-level phosphoric acid is produced in a kind of dividing plate crystallization according to claim 1, it is characterized in that: described acid adjustment groove is provided with chuck and whipping appts, the water-in of described chuck is connected with the water outlet of round tube gasification combustion furnace or the water outlet on main absorption tower.
9. the device of electron-level phosphoric acid is produced in a kind of dividing plate crystallization according to claim 1, it is characterized in that: described dearsenification reactor mainly arranges dearsenification reactor (17), dearsenification recycle pump (18) and in dearsenification literary composition, manages and circulate and be connected successively; Described dearsenification reactor (17) arranges opening for feed, P
2s
5dog-house and air outlet, in dearsenification literary composition, pipe arranges dearsenification reactor (17) middle and lower part, the opening for feed of dearsenification recycle pump (18) be located at dearsenification reactor (17) bottom discharge mouth and be connected, dearsenification reactor (17) top opening for feed is connected with acid adjustment groove (16) and electrostatic precipitator (14) respectively with air outlet.
10. the device of electron-level phosphoric acid is produced in a kind of dividing plate crystallization according to claim 1, it is characterized in that: described thionizer (20) is the patent of invention " a kind of food grade phosphoric acid removes the device of hydrogen sulfide " of patent No. CN201220735526.0; This device mainly arranges acid colleciton groove, desulfuration recycle pump (21) and degassing tower, the connection that circulates successively of degassing tower, acid colleciton groove, desulfuration recycle pump (21); Described degassing tower is arranged at top, top, acid colleciton groove one end, and is communicated with the cell body welding of acid colleciton groove; Degassing tower arranges H
2s air outlet, spray header, packing layer; Described H
2s air outlet is arranged at degassing tower top, and is connected with the dearsenification reactor of peripheral hardware; Described spray header is arranged at the top of degassing tower, and is connected successively with valve V and desulfuration recycle pump (21) with circulation tube; Packing layer and Stainless Steel Cloth are arranged at middle part and the bottom of degassing tower; The acid colleciton groove middle part side of being body, two ends is semicylinder; Acid colleciton groove arranges acid inlet, uncontaminated air air inlet port and valve VI, and acid inlet and manhole setting are positioned at acid colleciton groove near top, degassing tower one end, and acid inlet arranges cover plate and material inlet valve; Inlet mouth setting is positioned at acid colleciton groove away from top, degassing tower one end; The setting of valve III is positioned at acid colleciton groove away from bottom, degassing tower one end, and valve III is connected with desulphurization circulating pump inlet usage is blue; Desulfuration recycle pump (21) outlet connecting tee pipe, wherein one first connects valve V, then is connected with the spray header of degassing tower tower top with circulation tube, and another connection valve IV is towards dividing plate crystallization apparatus (22).
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| CN201310745953.6A CN103771368B (en) | 2013-12-30 | 2013-12-30 | A kind of baffle crystallization produces the device of electron-level phosphoric acid |
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|---|---|---|---|
| CN201310745953.6A CN103771368B (en) | 2013-12-30 | 2013-12-30 | A kind of baffle crystallization produces the device of electron-level phosphoric acid |
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| CN103771368B CN103771368B (en) | 2016-03-02 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101804974A (en) * | 2010-03-18 | 2010-08-18 | 广西明利集团有限公司 | Method for directly preparing food-grade high-purity phosphoric acid from yellow phosphorus |
| CN101804975A (en) * | 2010-03-18 | 2010-08-18 | 广西明利集团有限公司 | Safe phosphorus supply device for thermal phosphoric acid production |
| CN101811093A (en) * | 2010-03-18 | 2010-08-25 | 广西明利集团有限公司 | Phosphoric acid tail gas electric demister |
| CN202146685U (en) * | 2011-06-15 | 2012-02-22 | 广西钦州桂金诺磷化工有限公司 | Device for absorbing and dehumidifying as well as dedusting and air purifying by using phosphorous acid |
| CN203079694U (en) * | 2012-12-27 | 2013-07-24 | 广西明利化工有限公司 | Device for removing hydrogen sulfide in food grade phosphoric acid |
-
2013
- 2013-12-30 CN CN201310745953.6A patent/CN103771368B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101804974A (en) * | 2010-03-18 | 2010-08-18 | 广西明利集团有限公司 | Method for directly preparing food-grade high-purity phosphoric acid from yellow phosphorus |
| CN101804975A (en) * | 2010-03-18 | 2010-08-18 | 广西明利集团有限公司 | Safe phosphorus supply device for thermal phosphoric acid production |
| CN101811093A (en) * | 2010-03-18 | 2010-08-25 | 广西明利集团有限公司 | Phosphoric acid tail gas electric demister |
| CN202146685U (en) * | 2011-06-15 | 2012-02-22 | 广西钦州桂金诺磷化工有限公司 | Device for absorbing and dehumidifying as well as dedusting and air purifying by using phosphorous acid |
| CN203079694U (en) * | 2012-12-27 | 2013-07-24 | 广西明利化工有限公司 | Device for removing hydrogen sulfide in food grade phosphoric acid |
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