CN103641085B - Apparatus and method for purifying yellow phosphorus - Google Patents
Apparatus and method for purifying yellow phosphorus Download PDFInfo
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- CN103641085B CN103641085B CN201310572871.6A CN201310572871A CN103641085B CN 103641085 B CN103641085 B CN 103641085B CN 201310572871 A CN201310572871 A CN 201310572871A CN 103641085 B CN103641085 B CN 103641085B
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Abstract
The invention discloses an apparatus and a method for purifying yellow phosphorus. The method comprises: performing vacuum-pumping on a rectification device and filling with nitrogen, enabling industrial yellow phosphorus to be subjected to self-adsorption and go into a tower kettle, heating the tower kettle to perform reflux operation, so as to collect yellow phosphorus into a product collecting tank; enabling yellow phosphorus to go into a phosphorus melting tank, turning on a nitrogen generating device, fully replacing air in an oxidation tank, adding an oxidant, a catalyst and yellow phosphorus, reacting with stirring for 1-3 h, and standing for layering; sending yellow phosphorus into a washing tank for washing; enabling washed yellow phosphorus to go into zone melting equipment, wherein yellow phosphorus is melt in a divisional manner, gradually transfers to the two ends of a divisional-melting pool and respectively goes into a high-purity yellow phosphorus tank and a low-arsenic yellow phosphorus tank; and enabling yellow phosphorus coming from the high-purity yellow phosphorus tank to be pressed into a phosphorus pressing tank and go into a filter for filtering, so as to obtain a finished product. According to the technical scheme, yellow phosphorus is purified by employing rectification, oxidation, crystallization, washing, divisional melting and filtering, so that the purity of phosphorus is improved and the quality of yellow phosphorus is not influenced.
Description
Technical field
The present invention relates to a kind of yellow phosphorus purification devices, particularly a kind of high-purity yellow phosphorus process units.
Background technology
In industrial yellow phosphorus beyond arsenic removal, also containing mechanical admixture, inorganic impurity and organic matter.These impurity mainly contain:
Metallic element: Ca, Fe, Al, Mg, Sr, Mn, Na, K, Ti, V, Cr, Ni, Ga, Cd, Cu, Sb, Pb, Zn, Sn, U.
Semimetallic elements: Se, Si, C, B, As, Bi.
Organic matter: phenol, anthracene, tar and polyatom polycyclic aromatic hydrocarbon, more than about 30 kinds.
Owing to containing above-mentioned impurity in industrial yellow phosphorus, have a strong impact on its range of application, and the purposes of high purity phosphorus chemical products is very extensive, for high purity phosphorus, InP, GaP etc. are the important source material in electronics industry, are the adulterants of planar expitaxial transistor and integrated circuit; At petrochemical field, highly purified PCl3, P2O5 are advanced lubrication oil additives; In pharmaceuticals industry, high purity phosphorus is the raw material of the medicines such as production immunodepressant, vasodilator agent, nootropic agents; In addition, high purity phosphorus is also widely used in fields such as food industry, automobile making, military project, aviations.
Containing inorganic impurity, organic impurities and mechanical admixture in yellow phosphorus, have a strong impact on range of application and the economic value added of yellow phosphorus, for this reason Research Centers more both domestic and external in one's power colleges and universities all in the removal methods of research yellow phosphorus impurity.But because of the complexity of yellow phosphorus impurity, the chemical method making it report and the physical method arsenic removed in yellow phosphorus is all faced with that phosphorous recovery is low, refining effect is limited, etc. problem.
In prior art, the refining plant that patent discloses a kind of high-purity yellow phosphorus of publication number CN101912691A, this device mainly adopts the mode of rectifying to be separated yellow phosphorus, and the impurity component of industrial yellow phosphorus is very complicated, in order to reach more preferably, economic effect, inventor thinks and adopt the multiple method of purification to be coupled.
Summary of the invention
The object of the invention is to: one yellow phosphorus purification devices is safely and efficiently provided.To adapt to the needs of large-scale production, reach production operation controllability strong, the object that yellow phosphorus purification efficiency is high.
Technical scheme of the present invention: a kind of yellow phosphorus purification devices, comprises rectifier unit, oxidation unit, wash mill, district's fusing device and filter;
The raw material storage tank of described rectifier unit is connected with tower reactor, described tower reactor is provided with conduction oil expansion slot, the top of described tower reactor is rectifying column, one end of condenser is connected with the top of rectifying column, the other end of condenser connects return tank, described return tank also has pipeline to be connected to the tower top of rectifying column, and the outlet line of described return tank is connected with products pot A and products pot B respectively; The outlet line of described products pot A and products pot B is connected on the pipeline of raw material storage tank and tower reactor; The outlet line of described products pot B is connected to product-collecting groove; Described rectifier unit also comprises vavuum pump, and described vavuum pump connects raw material storage tank, condenser, return tank, products pot A and products pot B by surge tank; Described rectifier unit also comprises nitrogen pot, and described nitrogen pot connects raw material storage tank, condenser, return tank, products pot A and products pot B;
Described oxidation unit comprises phosphorus-melting groove and oxidation trough; Described phosphorus-melting groove top is provided with yellow phosphorus import, and be provided with yellow phosphorus outlet bottom phosphorus-melting groove, described phosphorus-melting groove skin is provided with insulation jacket, and the bottom of described insulation jacket is provided with the import of insulation liquid, is incubated liquid outlet being provided with upper lateral part of insulation jacket insulation liquid import; Described oxidation trough top arranges the import of oxidation trough yellow phosphorus, oxidant inlet, catalyst inlet, nitrogen inlet and offgas outlet respectively; The bottom of described oxidation trough is respectively equipped with the outlet of oxidation trough yellow phosphorus and waste liquid outlet; Described oxidation trough inside is provided with agitator;
Described wash mill is formed primarily of sink, and described sink top arranges the import of sink yellow phosphorus, nitrogen inlet, ultra-pure water import and offgas outlet respectively, and be provided with the outlet of sink yellow phosphorus bottom described sink, the downside of sink is provided with wastewater outlet; Described sink inside is provided with agitator;
Described district fusing device comprises dashpot, zone-melting equipment, high-purity yellow phosphorus groove and low-arsenic yellow phosphorus groove; Described dashpot top is provided with the import of dashpot yellow phosphorus and dashpot sealing water inlet; The outlet of dashpot yellow phosphorus is located at the bottom of dashpot; Described zone-melting equipment comprises molten bath, district, ring heater, annular cooler, drive unit, molten bath, district is arranged on bearing, ring heater and annular cooler are installed around molten bath, district, ring heater and annular cooler are formed by some groups respectively, along molten bath, district axially alternately, drive unit is connected with ring heater and annular cooler by connecting elements; Described high-purity yellow phosphorus groove top is provided with high-purity yellow phosphorus groove sealing water inlet and the import of high-purity yellow phosphorus groove yellow phosphorus; Bottom is provided with the outlet of high-purity yellow phosphorus groove yellow phosphorus; Described low-arsenic yellow phosphorus groove top is provided with low-arsenic yellow phosphorus groove sealing water inlet and the import of low-arsenic yellow phosphorus groove yellow phosphorus; Bottom is provided with the outlet of low-arsenic yellow phosphorus groove yellow phosphorus; Described dashpot yellow phosphorus outlet is connected to the zone-melting equipment yellow phosphorus import at zone-melting equipment top, the zone-melting equipment high-purity yellow phosphorus outlet of zone-melting device bottom is connected to the import of high-purity yellow phosphorus groove yellow phosphorus, and the zone-melting equipment low-arsenic yellow phosphorus outlet of zone-melting device bottom is connected to the import of low-arsenic yellow phosphorus groove yellow phosphorus;
Described filter comprises filter and pressure phosphorus tank; The top of described pressure phosphorus tank is respectively equipped with the tank yellow phosphorus import of pressure phosphorus and the outlet of pressure phosphorus tank yellow phosphorus, and the side surface upper part of pressure phosphorus tank is provided with phosphorous liquid flooding mouth; Described filter top is respectively equipped with the import of filter yellow phosphorus and cleaning solution import, and the bottom of described filter is provided with yellow phosphorus outlet, and the bottom of described filter is provided with sludge outlet;
Described phosphorus-melting groove yellow phosphorus inlet line is connected to product-collecting groove; Described phosphorus-melting groove yellow phosphorus outlet is connected to the import of oxidation trough yellow phosphorus by pipeline; Described oxidation trough yellow phosphorus outlet is connected to sink yellow phosphorus inlet line and is provided with yellow phosphorus pump; The outlet of sink yellow phosphorus is connected between the import of dashpot yellow phosphorus has pipeline to connect, and the outlet of high-purity yellow phosphorus groove yellow phosphorus is directly communicated to the import of pressure phosphorus tank yellow phosphorus; Described pressure phosphorus tank yellow phosphorus outlet is connected to the import of filter yellow phosphorus by pipeline.
The outside of described pressure phosphorus tank is provided with heat-insulation layer, and the bottom of heat-insulation layer is provided with the import of pressure phosphorus tank insulation liquid, is provided with the outlet of pressure phosphorus tank insulation liquid on the top of heat-insulation layer.
The outside of described filter is provided with heat-insulation layer, and the bottom of heat-insulation layer is provided with the import of filter insulation liquid, is provided with the outlet of filter insulation liquid at heat-insulation layer to upper lateral part.
Above-mentioned oxidation trough is also provided with insulation jacket, and insulation jacket is provided with oxidation trough insulation liquid import and the outlet of oxidation trough insulation liquid.
Above-mentioned sink is also provided with insulation jacket, and insulation jacket is provided with sink insulation liquid import and the outlet of sink insulation liquid.
The molten bath, district of described zone-melting equipment is the cylindrical shell of closed at both ends; The quantity of described ring heater is identical with the quantity of annular cooler.
The molten bath, district of described zone-melting equipment and horizontal angle are 10-15 degree.
The hot water inlet of the ring heater in described zone-melting equipment is above molten bath, district, and hot water outlet is in the below of molten bath, district opposite side; The cooling water inlet of annular cooler is above molten bath, district, and cooling water outlet is in the below of molten bath, district opposite side.
The filtering micropore size of the filter core of above-mentioned filter is at 2 ~ 5um.
A kind of production method utilizing above-mentioned yellow phosphorus purification devices, key step comprises: (1) first vacuumizes rectifier unit and is charged into nitrogen, industrial yellow phosphorus in raw material storage tank is through being certainly drawn onto in tower reactor, regulate the heating temperatures tower reactor of conduction oil expansion slot, carry out reflux operation, finally collect in product-collecting groove from the yellow phosphorus products pot B; Industrial yellow phosphorus is added phosphorus-melting groove, keeps insulation liquid in insulation jacket at 60 DEG C-80 DEG C, to ensure that yellow phosphorus is in liquid state; (2) yellow phosphorus is added phosphorus-melting groove, keep insulation liquid in insulation jacket at 60 DEG C-80 DEG C, to ensure that yellow phosphorus is in liquid state; (3) nitrogen gas generating device is started, nitrogen enters oxidation trough and enters exhaust treatment system from offgas outlet, after air in abundant substitutionary oxydation groove, oxidant and catalyst are added oxidation trough from oxidant inlet, catalyst inlet respectively, yellow phosphorus also sends into oxidation trough, start agitator, adjustment oxidation trough jacket water (J.W.) flow-control reaction temperature 70 DEG C-80 DEG C; After reaction 1-3h, stop stirring, leave standstill and make the abundant layering of the material in oxidation trough; In yellow phosphorus the impurity such as arsenic oxidized after enter waste liquid, be discharged to liquid waste treatment system from spent acid outlet; (4) add ultra-pure water from ultra-pure water import to sink, yellow phosphorus is added sink from oxidation trough, start agitator, adjustment sink jacket water (J.W.) flow-control wash temperature, after stirring certain hour, stop stirring, leave standstill and make the abundant layering of the material in sink; (5) yellow phosphorus is added district's bath of zone-melting equipment, ring heater and annular cooler is kept to be in conducting state, open drive unit, yellow phosphorus subregion melts the two ends transferring to molten bath, district gradually, and enters high-purity yellow phosphorus groove and low-arsenic yellow phosphorus groove respectively; (6) yellow phosphorus out obtained by high-purity yellow phosphorus groove enters pressure phosphorus tank; Regulate temperature of charge in pressure phosphorus tank chuck hot water flow adjustment pressure phosphorus tank, make yellow phosphorus be in liquid condition; Then enter filter, the yellow phosphorus after filtration enters final products stocking system; Filter residue then enters yellow phosphorus acid making system and fully utilizes; (7) low-arsenic yellow phosphorus groove yellow phosphorus is out sent into phosphoric acid system and prepare PHOSPHORIC ACID TECH.GRADE.
Advantage of the present invention: comprehensively have employed rectifying, oxidation, washing, Qu Rong, filtration method purifying is carried out to yellow phosphorus, can improve the purity of phosphorus, and the connecting of whole device unit is good, production operation serialization, not easily leak, can not to environment; And equipment of the present invention have employed the heat-insulation layer of jacket type, can be good at control temperature, decrease the waste of the energy, compared to existing external heat power supply device, not only reduce equipment cost, decrease the energy loss in heat trnasfer, and waste gas waste residue can not be produced, saving equipment takes up an area, and does not affect yellow phosphorus quality.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Fig. 2 is the structural representation of rectifier unit of the present invention;
Fig. 3 is the structural representation of oxidation unit of the present invention;
Fig. 4 is the structural representation of wash mill of the present invention;
The structural representation of Tu5Shi district of the present invention fusing device;
Fig. 6 is the structural representation of filter of the present invention;
In figure: 1-is incubated liquid import; The import of 2-yellow phosphorus; 3-oxidation trough; 4-sink; 5-is incubated liquid outlet; 6-yellow phosphorus exports; 7-phosphorus-melting groove; 8-presses the import of phosphorus tank yellow phosphorus; 9-presses the outlet of phosphorus tank insulation liquid; 10-presses the outlet of phosphorus tank yellow phosphorus; The phosphorous hydrorrhea head piece of 11-; 12-presses phosphorus tank; 13-presses the import of phosphorus tank insulation liquid; The import of 14-cleaning solution; 15-filter; The import of 16-filter insulation liquid; The import of 17-filter yellow phosphorus; The outlet of 18-filter insulation liquid; 19-filter yellow phosphorus exports; 20-sludge outlet; The import of 21-oxidation trough yellow phosphorus; 22-oxidant inlet; 23-catalyst inlet; 24-nitrogen inlet; 25-offgas outlet; The outlet of 26-oxidation trough insulation liquid; The import of 27-oxidation trough insulation liquid; 28 oxidation trough agitators; The import of 29-sink yellow phosphorus; The import of 30-sink insulation liquid; 31-sink nitrogen inlet; The import of 32-sink ultra-pure water; 33-sink offgas outlet; The outlet of 34-sink insulation liquid; 35-wastewater outlet; 36-sink agitator; 37-spent acid exports; 38-oxidation trough yellow phosphorus exports; The import of 40-high-purity yellow phosphorus groove yellow phosphorus; 41-high-purity yellow phosphorus groove sealing water inlet; 42-high-purity yellow phosphorus groove insulation water inlet; 43-high-purity yellow phosphorus groove sealing water overfall; 44-high-purity yellow phosphorus groove insulation water out; 45-high-purity yellow phosphorus groove yellow phosphorus exports; The import of 46-low-arsenic yellow phosphorus groove yellow phosphorus; 47-low-arsenic yellow phosphorus groove sealing water inlet; 48-low-arsenic yellow phosphorus groove sealing water overfall; 49-low-arsenic yellow phosphorus groove insulation water out; 50-low-arsenic yellow phosphorus groove insulation water inlet; ; 51-low-arsenic yellow phosphorus groove yellow phosphorus exports; 52-bearing; Molten bath, 53-district; The import of 54-zone-melting equipment yellow phosphorus; 55-dashpot yellow phosphorus exports; 56-dashpot insulation water inlet; 57-dashpot insulation water out; 58-dashpot sealing water overfall; The import of 59-dashpot yellow phosphorus; 60-hot water inlet; 61-hot water outlet; 62-cooling water inlet; 63-cooling water outlet; 64-zone-melting equipment high-purity yellow phosphorus exports; 65-zone-melting equipment low-arsenic yellow phosphorus exports; 71-raw material storage tank; 72-tower reactor; 73-rectifying column; 74-condenser; 75-reflux column; 76-products pot A; 77-products pot B; 78-surge tank; 79-vavuum pump; 80-nitrogen pot; 81-conduction oil expansion slot; 82-product-collecting groove; 101-rectifier unit; 102-oxidation unit; 103-wash mill; 104-district fusing device; 105-filter.
Detailed description of the invention
embodiment
A kind of yellow phosphorus purification devices, comprises rectifier unit 101, oxidation unit 102, wash mill 103, zone-melting device 104 and filter 105;
The raw material storage tank 71 of described rectifier unit is connected with tower reactor 72, described tower reactor 72 is provided with conduction oil expansion slot 81, the top of described tower reactor 72 is rectifying column 73, one end of condenser 74 is connected with the top of rectifying column 73, the other end of condenser 74 connects return tank 75, described return tank 75 also has pipeline to be connected to the tower top of rectifying column 73, and the outlet line of described return tank 75 is connected with products pot A76 and products pot B77 respectively; The outlet line of described products pot A76 and products pot B77 is connected to raw material storage tank 71 with on the pipeline of tower reactor 72; The outlet line of described products pot B77 is connected to product-collecting groove 32; Described rectifier unit also comprises vavuum pump 79, and described vavuum pump 79 connects raw material storage tank 71, condenser 74, return tank 25, products pot A26 and products pot B27 by surge tank 78; Described rectifier unit also comprises nitrogen pot 80, and described nitrogen pot 80 connects raw material storage tank 71, condenser 74, return tank 75, products pot A76 and products pot B77;
Described oxidation unit comprises phosphorus-melting groove 7 and oxidation trough 3; Described phosphorus-melting groove 7 top is provided with yellow phosphorus import 2, yellow phosphorus outlet 6 is provided with bottom phosphorus-melting groove 7, described phosphorus-melting groove 7 skin is provided with insulation jacket, and the bottom of described insulation jacket is provided with insulation liquid import 1, is incubated liquid outlet 5 being provided with upper lateral part of insulation jacket insulation liquid import; Described oxidation trough 3 top arranges oxidation trough yellow phosphorus import 21, oxidant inlet 22, catalyst inlet 23, nitrogen inlet 24 and offgas outlet 25 respectively; The bottom of described oxidation trough 3 is respectively equipped with oxidation trough yellow phosphorus outlet 38 and waste liquid outlet 37; Described oxidation trough 7 inside is provided with agitator 28;
Described wash mill is formed primarily of sink 4, described sink 4 top arranges sink yellow phosphorus import 29, nitrogen inlet 31, ultra-pure water import 32 and offgas outlet 33 respectively, be provided with the outlet of sink yellow phosphorus bottom described sink 4, the downside of sink 4 is provided with wastewater outlet 35; Described sink 4 inside is provided with agitator 36;
Described district fusing device comprises dashpot, zone-melting equipment, high-purity yellow phosphorus groove and low-arsenic yellow phosphorus groove; Described dashpot top is provided with dashpot yellow phosphorus import 59 and dashpot sealing water inlet 58; Dashpot yellow phosphorus outlet 55 is located at the bottom of dashpot; Described zone-melting equipment comprises molten bath, district 53, ring heater, annular cooler, drive unit, molten bath, district 53 is arranged on bearing 52, ring heater and annular cooler are installed around molten bath, district, ring heater and annular cooler are formed by some groups respectively, along molten bath, district axially alternately, drive unit is connected with ring heater and annular cooler by connecting elements; Described high-purity yellow phosphorus groove top is provided with high-purity yellow phosphorus groove sealing water inlet 41 and high-purity yellow phosphorus groove yellow phosphorus import 40; Bottom is provided with high-purity yellow phosphorus groove yellow phosphorus outlet 45; Described low-arsenic yellow phosphorus groove top is provided with low-arsenic yellow phosphorus groove sealing water inlet 47 and low-arsenic yellow phosphorus groove yellow phosphorus import 46; Bottom is provided with low-arsenic yellow phosphorus groove yellow phosphorus outlet 51; Described dashpot yellow phosphorus outlet 55 is connected to the zone-melting equipment yellow phosphorus import 54 at zone-melting equipment top, the zone-melting equipment high-purity yellow phosphorus outlet 64 of zone-melting device bottom is connected to high-purity yellow phosphorus groove yellow phosphorus import 40, and the zone-melting equipment low-arsenic yellow phosphorus outlet 65 of zone-melting device bottom is connected to low-arsenic yellow phosphorus groove yellow phosphorus import 46;
Described filter comprises filter 15 and pressure phosphorus tank 12; The top of described pressure phosphorus tank 12 is respectively equipped with pressure phosphorus tank yellow phosphorus import 8 and pressure phosphorus tank yellow phosphorus outlet 10, the side surface upper part of pressure phosphorus tank 8 is provided with phosphorous liquid flooding mouth 11, the outside of described pressure phosphorus tank 12 is provided with heat-insulation layer, the bottom of heat-insulation layer is provided with pressure phosphorus tank insulation liquid import 13, is provided with pressure phosphorus tank insulation liquid outlet 9 on the top of heat-insulation layer; Described filter 15 top is respectively equipped with filter yellow phosphorus import 17 and cleaning solution import 14, and the bottom of described filter 15 is provided with filter yellow phosphorus outlet 19, and the bottom of described filter 15 is provided with sludge outlet 20; The outside of described filter 15 is provided with heat-insulation layer, and the bottom of heat-insulation layer is provided with filter insulation liquid import 16, is provided with filter insulation liquid outlet 18 at heat-insulation layer to upper lateral part;
Described phosphorus-melting groove yellow phosphorus inlet line is connected to product-collecting groove 82; Described phosphorus-melting groove yellow phosphorus outlet 6 is connected to oxidation trough yellow phosphorus import 21 by pipeline; Described oxidation trough yellow phosphorus outlet 38 is connected to sink yellow phosphorus import 29 pipeline and is provided with yellow phosphorus pump; The outlet of sink yellow phosphorus is connected to has pipeline to connect between dashpot yellow phosphorus import 59, and high-purity yellow phosphorus groove yellow phosphorus outlet 64 is directly communicated to pressure phosphorus tank yellow phosphorus import 8; Described pressure phosphorus tank yellow phosphorus outlet 10 is connected to filter yellow phosphorus import 17 by pipeline.
Above-mentioned oxidation trough 3 is also provided with insulation jacket, and insulation jacket is provided with oxidation trough insulation liquid import 27 and oxidation trough insulation liquid outlet 26.
Above-mentioned sink 4 is also provided with insulation jacket, and insulation jacket is provided with sink insulation liquid import 30 and sink insulation liquid outlet 34.
The molten bath, district 53 of described zone-melting equipment is the cylindrical shell of closed at both ends; The quantity of described ring heater is identical with the quantity of annular cooler.
Molten bath, district 53 and the horizontal angle of described zone-melting equipment are 10-15 degree.
The hot water inlet 60 of the ring heater in described zone-melting equipment is above molten bath, district 53, and hot water outlet 61 is in the below of molten bath, district 53 opposite side; The cooling water inlet 62 of annular cooler is above molten bath, district 53, and cooling water outlet 63 is in the below of molten bath, district 53 opposite side.
The filtering micropore size of the filter core of above-mentioned filter 15 is at 2 ~ 5um.
A kind of production method utilizing above-mentioned yellow phosphorus purification devices, key step comprises: (1) first vacuumizes rectifier unit and is charged into nitrogen, industrial yellow phosphorus in raw material storage tank is through being certainly drawn onto in tower reactor, regulate the heating temperatures tower reactor of conduction oil expansion slot, carry out reflux operation, finally collect in product-collecting groove from the yellow phosphorus products pot B; Industrial yellow phosphorus is added phosphorus-melting groove, keeps insulation liquid in insulation jacket at 60 DEG C-80 DEG C, to ensure that yellow phosphorus is in liquid state; (2) yellow phosphorus is added phosphorus-melting groove, keep insulation liquid in insulation jacket at 60 DEG C-80 DEG C, to ensure that yellow phosphorus is in liquid state; (3) nitrogen gas generating device is started, nitrogen enters oxidation trough and enters exhaust treatment system from offgas outlet, after air in abundant substitutionary oxydation groove, oxidant and catalyst are added oxidation trough from oxidant inlet, catalyst inlet respectively, yellow phosphorus also sends into oxidation trough, start agitator, adjustment oxidation trough jacket water (J.W.) flow-control reaction temperature 70 DEG C-80 DEG C; After reaction 1-3h, stop stirring, leave standstill and make the abundant layering of the material in oxidation trough; In yellow phosphorus the impurity such as arsenic oxidized after enter waste liquid, be discharged to liquid waste treatment system from spent acid outlet; (4) add ultra-pure water from ultra-pure water import to sink, yellow phosphorus is added sink from oxidation trough, start agitator, adjustment sink jacket water (J.W.) flow-control wash temperature, after stirring certain hour, stop stirring, leave standstill and make the abundant layering of the material in sink; (5) yellow phosphorus is added district's bath of zone-melting equipment, ring heater and annular cooler is kept to be in conducting state, open drive unit, yellow phosphorus subregion melts the two ends transferring to molten bath, district gradually, and enters high-purity yellow phosphorus groove and low-arsenic yellow phosphorus groove respectively; (6) yellow phosphorus out obtained by high-purity yellow phosphorus groove enters pressure phosphorus tank; Regulate temperature of charge in pressure phosphorus tank chuck hot water flow adjustment pressure phosphorus tank, make yellow phosphorus be in liquid condition; Then enter filter, the yellow phosphorus after filtration enters final products stocking system; Filter residue then enters yellow phosphorus acid making system and fully utilizes; (7) low-arsenic yellow phosphorus groove yellow phosphorus is out sent into phosphoric acid system and prepare PHOSPHORIC ACID TECH.GRADE.
Claims (10)
1. a yellow phosphorus purification devices, is characterized in that this device comprises rectifier unit (101), oxidation unit (102), wash mill (103), zone-melting device (104) and filter (105);
The raw material storage tank (71) of described rectifier unit is connected with tower reactor (72), described tower reactor (72) is provided with conduction oil expansion slot (81), the top of described tower reactor (72) is rectifying column (73), one end of condenser (74) is connected with the top of rectifying column (73), the other end of condenser (74) connects return tank (75), described return tank (75) also has pipeline to be connected to the tower top of rectifying column (73), the outlet line of described return tank (75) respectively with products pot A(76) and products pot B(77) be connected; Described products pot A(76) and products pot B(77) outlet line be connected on the pipeline of raw material storage tank (71) and tower reactor (72); Described products pot B(77) outlet line be connected to product-collecting groove (32); Described rectifier unit also comprises vavuum pump (79), and described vavuum pump (79) connects raw material storage tank (71), condenser (74), return tank (25), products pot A(26 by surge tank (78)) and products pot B(27); Described rectifier unit also comprises nitrogen pot (80), and described nitrogen pot (80) connects raw material storage tank (71), condenser (74), return tank (75), products pot A(76) and products pot B(77);
Described oxidation unit comprises phosphorus-melting groove (7) and oxidation trough (3); Described phosphorus-melting groove (7) top is provided with yellow phosphorus import (2), phosphorus-melting groove (7) bottom is provided with yellow phosphorus outlet (6), described phosphorus-melting groove (7) skin is provided with insulation jacket, the bottom of described insulation jacket is provided with insulation liquid import (1), is incubated liquid outlet (5) being provided with upper lateral part of insulation jacket insulation liquid import; Described oxidation trough (3) top arranges oxidation trough yellow phosphorus import (21), oxidant inlet (22), catalyst inlet (23), nitrogen inlet (24) and offgas outlet (25) respectively; The bottom of described oxidation trough (3) is respectively equipped with the outlet of oxidation trough yellow phosphorus (38) and waste liquid outlet (37); Described oxidation trough (3) inside is provided with agitator (28);
Described wash mill is formed primarily of sink (4), described sink (4) top arranges sink yellow phosphorus import (29), nitrogen inlet (31), ultra-pure water import (32) and offgas outlet (33) respectively, described sink (4) bottom is provided with the outlet of sink yellow phosphorus, and the downside of sink (4) is provided with wastewater outlet (35); Described sink (4) inside is provided with agitator (36);
Described zone-melting device comprises dashpot, zone-melting equipment, high-purity yellow phosphorus groove and low-arsenic yellow phosphorus groove; Described dashpot top is provided with dashpot yellow phosphorus import (59) and dashpot sealing water inlet (58); Dashpot yellow phosphorus outlet (55) is located at the bottom of dashpot; Described zone-melting equipment comprises molten bath, district (53), ring heater, annular cooler, drive unit, molten bath, district (53) is arranged on bearing (52), ring heater and annular cooler are installed around molten bath, district, ring heater and annular cooler are formed by some groups respectively, along molten bath, district axially alternately, drive unit is connected with ring heater and annular cooler by connecting elements; Described high-purity yellow phosphorus groove top is provided with high-purity yellow phosphorus groove sealing water inlet (41) and high-purity yellow phosphorus groove yellow phosphorus import (40); Bottom is provided with high-purity yellow phosphorus groove yellow phosphorus outlet (45); Described low-arsenic yellow phosphorus groove top is provided with low-arsenic yellow phosphorus groove sealing water inlet (47) and low-arsenic yellow phosphorus groove yellow phosphorus import (46); Bottom is provided with low-arsenic yellow phosphorus groove yellow phosphorus outlet (51); Described dashpot yellow phosphorus outlet (55) is connected to zone-melting equipment yellow phosphorus import (54) at zone-melting equipment top, zone-melting equipment high-purity yellow phosphorus outlet (64) of zone-melting device bottom is connected to high-purity yellow phosphorus groove yellow phosphorus import (40), and zone-melting equipment low-arsenic yellow phosphorus outlet (65) of zone-melting device bottom is connected to low-arsenic yellow phosphorus groove yellow phosphorus import (46);
Described filter comprises filter (15) and pressure phosphorus tank (12); The top of described pressure phosphorus tank (12) is respectively equipped with pressure phosphorus tank yellow phosphorus import (8) and pressure phosphorus tank yellow phosphorus outlet (10), the side surface upper part of pressure phosphorus tank (12) is provided with phosphorous liquid flooding mouth (11), described filter (15) top is respectively equipped with filter yellow phosphorus import (17) and cleaning solution import (14), the bottom of described filter (15) is provided with filter yellow phosphorus outlet (19), and the bottom of described filter (15) is provided with sludge outlet (20);
Described phosphorus-melting groove yellow phosphorus inlet line is connected to product-collecting groove (82); Described phosphorus-melting groove yellow phosphorus outlet (6) is connected to oxidation trough yellow phosphorus import (21) by pipeline; Described oxidation trough yellow phosphorus outlet (38) is connected to sink yellow phosphorus import (29) pipeline and is provided with yellow phosphorus pump; The outlet of sink yellow phosphorus is connected to has pipeline to connect between dashpot yellow phosphorus import (59), and high-purity yellow phosphorus groove yellow phosphorus outlet (64) is directly communicated to pressure phosphorus tank yellow phosphorus import (8); Described pressure phosphorus tank yellow phosphorus outlet (10) is connected to filter yellow phosphorus import (17) by pipeline.
2. device as claimed in claim 1, is characterized in that described oxidation trough (3) is also provided with insulation jacket, and insulation jacket is provided with oxidation trough insulation liquid import (27) and oxidation trough insulation liquid outlet (26).
3. device as claimed in claim 1, is characterized in that described sink (4) is also provided with insulation jacket, and insulation jacket is provided with sink insulation liquid import (30) and sink insulation liquid outlet (34).
4. device as claimed in claim 1, is characterized in that the cylindrical shell that the molten bath, district (53) of described zone-melting equipment is closed at both ends; The quantity of described ring heater is identical with the quantity of annular cooler.
5. device as claimed in claim 1, is characterized in that the molten bath, district (53) of described zone-melting equipment and horizontal angle are 10-15 degree.
6. device as claimed in claim 1, it is characterized in that the hot water inlet (60) of the ring heater in described zone-melting equipment is in the top of molten bath, district (53), hot water outlet (61) is in the below of molten bath, district (53) opposite side; The cooling water inlet (62) of annular cooler is in the top of molten bath, district (53), and cooling water outlet (63) is in the below of molten bath, district (53) opposite side.
7. device as claimed in claim 1, it is characterized in that pressing the outside of phosphorus tank (12) to be provided with heat-insulation layer, the bottom of heat-insulation layer is provided with pressure phosphorus tank insulation liquid import (13), is provided with pressure phosphorus tank insulation liquid outlet (9) on the top of heat-insulation layer.
8. device as claimed in claim 1, it is characterized in that the outside of described filter (15) is provided with heat-insulation layer, the bottom of heat-insulation layer is provided with filter insulation liquid import (16), is provided with filter insulation liquid outlet (18) at heat-insulation layer to upper lateral part.
9. device as claimed in claim 1, is characterized in that the filtering micropore size of the filter core of described filter (15) is at 2 ~ 5um.
10. one kind utilizes the production method of yellow phosphorus purification devices described in above-mentioned any one of 1-9 claim, it is characterized in that key step comprises: (1) first vacuumizes rectifier unit and is charged into nitrogen, industrial yellow phosphorus in raw material storage tank is through being certainly drawn onto in tower reactor, regulate the heating temperatures tower reactor of conduction oil expansion slot, carry out reflux operation, finally collect in product-collecting groove from the yellow phosphorus products pot B; Industrial yellow phosphorus is added phosphorus-melting groove, keeps insulation liquid in insulation jacket at 60 DEG C-80 DEG C, to ensure that yellow phosphorus is in liquid state; (2) yellow phosphorus is added phosphorus-melting groove, keep insulation liquid in insulation jacket at 60 DEG C-80 DEG C, to ensure that yellow phosphorus is in liquid state; (3) nitrogen gas generating device is started, nitrogen enters oxidation trough and enters exhaust treatment system from offgas outlet, after air in abundant substitutionary oxydation groove, oxidant and catalyst are added oxidation trough from oxidant inlet, catalyst inlet respectively, yellow phosphorus also sends into oxidation trough, start agitator, adjustment oxidation trough jacket water (J.W.) flow-control reaction temperature 70 DEG C-80 DEG C; After reaction 1-3h, stop stirring, leave standstill and make the abundant layering of the material in oxidation trough; In yellow phosphorus arsenic impurities oxidized after enter waste liquid, from spent acid outlet be discharged to liquid waste treatment system; (4) add ultra-pure water from ultra-pure water import to sink, yellow phosphorus is added sink from oxidation trough, start agitator, adjustment sink jacket water (J.W.) flow-control wash temperature, after stirring certain hour, stop stirring, leave standstill and make the abundant layering of the material in sink; (5) yellow phosphorus is added district's bath of zone-melting equipment, ring heater and annular cooler is kept to be in conducting state, open drive unit, yellow phosphorus subregion melts the two ends transferring to molten bath, district gradually, and enters high-purity yellow phosphorus groove and low-arsenic yellow phosphorus groove respectively; (6) yellow phosphorus out obtained by high-purity yellow phosphorus groove enters pressure phosphorus tank; Regulate temperature of charge in pressure phosphorus tank chuck hot water flow adjustment pressure phosphorus tank, make yellow phosphorus be in liquid condition; Then enter filter, the yellow phosphorus after filtration enters final products stocking system; Filter residue then enters yellow phosphorus acid making system and fully utilizes; (7) low-arsenic yellow phosphorus groove yellow phosphorus is out sent into phosphoric acid system and prepare PHOSPHORIC ACID TECH.GRADE.
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