CN203582491U - Yellow phosphorus purifying device - Google Patents

Yellow phosphorus purifying device Download PDF

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Publication number
CN203582491U
CN203582491U CN201320727082.0U CN201320727082U CN203582491U CN 203582491 U CN203582491 U CN 203582491U CN 201320727082 U CN201320727082 U CN 201320727082U CN 203582491 U CN203582491 U CN 203582491U
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China
Prior art keywords
yellow phosphorus
outlet
import
groove
phosphorus
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Expired - Lifetime
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CN201320727082.0U
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Chinese (zh)
Inventor
王邵东
李红林
段仕东
杨光明
吴邦文
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Wengfu Group Co Ltd
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Wengfu Group Co Ltd
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Abstract

The utility model discloses a yellow phosphorus purifying device which comprises an oxidation device, a washing device and a zone melting device, wherein a phosphorus melting tank yellow phosphorus outlet (6) is connected with an oxidation tank yellow phosphorus inlet (21) through a pipeline; a pipeline connecting an oxidation tank yellow phosphorus outlet (38) with a washing tank yellow phosphorus inlet (29) is provided with a yellow phosphorus pump; a washing tank yellow phosphorus outlet is connected with a buffer tank yellow phosphorus inlet (59) through a pipeline. The device disclosed by the utility model purifies yellow phosphorus by combining oxidation, washing and zone melting processes, and can improve the purity of phosphorus while the effect is relatively good.

Description

Yellow phosphorus purification devices
Technical field
The utility model relates to a kind of yellow phosphorus purification devices, particularly a kind of high-purity yellow phosphorus production equipment.
Background technology
In industrial yellow phosphorus, beyond arsenic removal, also contain mechanical impurity, 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.
Organism: phenol, anthracene, tar and polyatom polycyclic aromatic hydrocarbons, more than approximately 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 Chemicals is very extensive, take high purity phosphorus as example, InP, GaP etc. is the important source material in electronic industry, is the doping agent of planar expitaxial transistor and unicircuit; At petrochemical field, highly purified PCl3, P2O5 are advanced lubrication oil additivess; In pharmaceutical industries, high purity phosphorus is the raw material of the medicines such as production immunosuppressor, vasodilator, nootropic agents; In addition, high purity phosphorus is also widely used in fields such as foodstuffs industry, automobile making, military project, aviations.
In yellow phosphorus, contain inorganic impurity, organic impurity and mechanical impurity, 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 research yellow phosphorus impurity removal methods.But because of the complicacy of yellow phosphorus impurity, make its chemical method of having reported and physical method remove arsenic in yellow phosphorus be all faced with that phosphorous recovery is low, refining effect is limited, etc. problem.
The impurity component of industrial yellow phosphorus is very complicated, adopt a kind of single method method, is difficult to reach effect desirable, economy, therefore must adopt multiple method of purification coupling.
Summary of the invention
The purpose of this utility model is: one yellow phosphorus purification devices is safely and efficiently provided, to adapt to the needs of large-scale production, reaches production operation controllability strong, the object that yellow phosphorus purification efficiency is high.
The technical solution of the utility model: a kind of yellow phosphorus purification devices, comprises oxidation unit, washing device and district's fusing device;
Described oxidation unit comprises phosphorus-melting groove and oxidation trough; Described phosphorus-melting groove top is provided with yellow phosphorus import, and phosphorus-melting groove bottom is provided with yellow phosphorus outlet, and 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, upper lateral part is provided with and is incubated liquid outlet in the import of insulation jacket insulation liquid; Described oxidation trough top arranges respectively the import of oxidation trough yellow phosphorus, oxidant inlet, catalyst inlet, nitrogen inlet and tail gas outlet; 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 washing device mainly consists of rinse bath, and described rinse bath top arranges respectively the import of rinse bath yellow phosphorus, nitrogen inlet, ultrapure water import and tail gas outlet, and described rinse bath bottom is provided with the outlet of rinse bath yellow phosphorus, and the downside of rinse bath is provided with wastewater outlet; Described rinse bath 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 water cooler, drive unit, molten bath, district is arranged on bearing, ring heater and annular water cooler are installed around molten bath, district, ring heater and annular water cooler form by some groups respectively, along molten bath, district axially alternately, drive unit is connected with ring heater and annular water cooler by transom; 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 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 rinse bath yellow phosphorus inlet line and is provided with yellow phosphorus pump; The outlet of rinse bath yellow phosphorus is connected between the import of dashpot yellow phosphorus has pipeline to connect.
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 rinse bath is also provided with insulation jacket, and insulation jacket is provided with rinse bath insulation liquid import and the outlet of rinse bath insulation liquid.
The cylindrical shell that the molten bath, district of described zone melting equipment is closed at both ends; The quantity of described ring heater is identical with the quantity of annular water 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 below the opposite side of molten bath, district; The cooling water inlet of annular water cooler is above molten bath, district, and cooling water outlet is below the opposite side of molten bath, district.
The filtering micropore size of the filter core of above-mentioned strainer is at 2~5um.
During the utility model work, industrial yellow phosphorus enters phosphorus-melting groove from yellow phosphorus import, hot water in device enters insulation jacket from the import of insulation liquid, from the outlet of insulation liquid, flow out insulation jacket again, to guarantee that yellow phosphorus is in liquid state, nitrogen enters oxidation trough from nitrogen gas generating device from nitrogen inlet, from tail gas outlet, enter exhaust treatment system again, fully replaced after the air in oxidation trough, oxygenant and catalyzer are respectively from oxidant inlet, catalyst inlet, enter oxidation trough, yellow phosphorus enters oxidation trough through yellow phosphorus pipeline from the import of oxidation trough yellow phosphorus from the yellow phosphorus outlet of phosphorus-melting groove bottom, start agitator, adjust reactive tank jacket water (J.W.) flow control temperature of reaction, reach after the reaction times, stop stirring, the standing abundant layering of material making in oxidation trough, from ultrapure water import, to rinse bath, add ultrapure water, nitrogen enters from tail gas outlet and draws from nitrogen inlet, yellow phosphorus enters rinse bath through pipeline from the import of rinse bath yellow phosphorus from the outlet of oxidation trough yellow phosphorus, in yellow phosphorus, the impurity such as arsenic enters waste liquid after oxidized, from spent acid outlet, is discharged to liquid waste treatment system, starts agitator, adjust rinse bath jacket water (J.W.) flow control wash temperature, stir after certain hour, stop stirring the standing abundant layering of material making in rinse bath, yellow phosphorus after washing enters dashpot buffering, then by the import of zone melting equipment yellow phosphorus, enter molten bath, district, keep ring heater and annular water cooler in conducting state, open drive unit, yellow phosphorus subregion melts the two ends of transferring to gradually molten bath, district, by the outlet of zone melting equipment high-purity yellow phosphorus and the outlet of zone melting equipment low-arsenic yellow phosphorus, enters respectively high-purity yellow phosphorus groove and low-arsenic yellow phosphorus groove, what by high-purity yellow phosphorus groove, out obtained is high-purity yellow phosphorus, by low-arsenic yellow phosphorus groove low-arsenic yellow phosphorus out, enter phosphoric acid system and prepare PHOSPHORIC ACID TECH.GRADE.
Advantage of the present utility model: comprehensively adopted oxidation, washing, the molten method in district to carry out purifying to yellow phosphorus, can improve the purity of phosphorus, and the connecting of whole device unit has been good, production operation serialization, is difficult for leaking, can be to environment; And equipment of the present utility model has adopted the thermal insulation layer of jacketed type, can be good at controlling temperature, reduced the waste of the energy, than existing external heat power supply device, not only reduce equipment cost, reduced the energy waste in hot transmission, and can not produce waste gas waste residue, saving equipment takes up an area, and does not affect yellow phosphorus quality.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model;
The import of 1-insulation liquid; The import of 2-yellow phosphorus; 3-oxidation trough; 4-rinse bath; The outlet of 5-insulation liquid; The outlet of 6-yellow phosphorus; 7-phosphorus-melting groove; The import of 21-oxidation trough yellow phosphorus; 22-oxidant inlet; 23-catalyst inlet; 24-nitrogen inlet; The outlet of 25-tail gas; The outlet of 26-oxidation trough insulation liquid; The import of 27-oxidation trough insulation liquid; 28 oxidation trough agitators; The import of 29-rinse bath yellow phosphorus; The import of 30-rinse bath insulation liquid; 31-rinse bath nitrogen inlet; The import of 32-rinse bath ultrapure water; The outlet of 33-rinse bath tail gas; The outlet of 34-rinse bath insulation liquid; 35-wastewater outlet; 36-rinse bath agitator; The outlet of 37-spent acid; The outlet of 38-oxidation trough yellow phosphorus; 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 overflow port; 44-high-purity yellow phosphorus groove insulation water out; The outlet of 45-high-purity yellow phosphorus groove yellow phosphorus; 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 overflow port; 49-low-arsenic yellow phosphorus groove insulation water out; 50-low-arsenic yellow phosphorus groove insulation water inlet; ; The outlet of 51-low-arsenic yellow phosphorus groove yellow phosphorus; 52-bearing; Molten bath, 53-district; The import of 54-zone melting equipment yellow phosphorus; The outlet of 55-dashpot yellow phosphorus; 56-dashpot insulation water inlet; 57-dashpot insulation water out; 58-dashpot sealing water overflow port; The import of 59-dashpot yellow phosphorus; 60-hot water inlet; 61-hot water outlet; 62-cooling water inlet; 63-cooling water outlet; The outlet of 64-zone melting equipment high-purity yellow phosphorus; The outlet of 65-zone melting equipment low-arsenic yellow phosphorus.
Embodiment
embodiment
A kind of yellow phosphorus purification devices, comprises oxidation unit, washing device and district's fusing device;
Described oxidation unit comprises phosphorus-melting groove 7 and oxidation trough 3; Described phosphorus-melting groove 7 tops are provided with yellow phosphorus import 2, phosphorus-melting groove 7 bottoms are provided with yellow phosphorus outlet 6, described phosphorus-melting groove 7 skins are provided with insulation jacket, and the bottom of described insulation jacket is provided with insulation liquid import 1, upper lateral part is provided with and is incubated liquid outlet 5 in the import of insulation jacket insulation liquid; Described oxidation trough 3 tops arrange respectively oxidation trough yellow phosphorus import 21, oxidant inlet 22, catalyst inlet 23, nitrogen inlet 24 and tail gas outlet 25; The bottom of described oxidation trough 3 is respectively equipped with the outlet 38 of oxidation trough yellow phosphorus and waste liquid outlet 37; Described oxidation trough 7 inside are provided with agitator 28;
Described washing device mainly consists of rinse bath 4, described rinse bath 4 tops arrange respectively rinse bath yellow phosphorus import 29, nitrogen inlet 31, ultrapure water import 32 and tail gas outlet 33, described rinse bath 4 bottoms are provided with the outlet of rinse bath yellow phosphorus, and the downside of rinse bath 4 is provided with wastewater outlet 35; Described rinse bath 4 inside are 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 the import 59 of dashpot yellow phosphorus 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 water cooler, drive unit, molten bath, district 53 is arranged on bearing 52, ring heater and annular water cooler are installed around molten bath, district, ring heater and annular water cooler form by some groups respectively, along molten bath, district axially alternately, drive unit is connected with ring heater and annular water cooler by transom; 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 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 rinse bath yellow phosphorus import 29 pipelines and is provided with yellow phosphorus pump; The outlet of rinse bath yellow phosphorus is connected between dashpot yellow phosphorus import 59 has pipeline to connect.
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 rinse bath 4 is also provided with insulation jacket, and insulation jacket is provided with rinse bath insulation liquid import 30 and rinse bath insulation liquid outlet 34.
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 water cooler.
Molten bath, district 53 and the horizontal angle of described zone melting equipment are 10-15 degree.
The top in the molten bath, hot water inlet 60 district 53 of the ring heater in described zone melting equipment, the below of molten bath, hot water outlet 61 district 53 opposite sides; The top in the molten bath, cooling water inlet 62 district 53 of annular water cooler, the below of molten bath, cooling water outlet 63 district 53 opposite sides.
The filtering micropore size of the filter core of above-mentioned strainer 15 is at 2~5um.

Claims (6)

1. a yellow phosphorus purification devices, is characterized in that this device comprises oxidation unit, washing device and district's fusing device;
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), upper lateral part is provided with and is incubated liquid outlet (5) in the import of insulation jacket insulation liquid; Described oxidation trough (3) top arranges respectively oxidation trough yellow phosphorus import (21), oxidant inlet (22), catalyst inlet (23), nitrogen inlet (24) and tail gas outlet (25); 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 (7) inside is provided with agitator (28);
Described washing device mainly consists of rinse bath (4), described rinse bath (4) top arranges respectively rinse bath yellow phosphorus import (29), nitrogen inlet (31), ultrapure water import (32) and tail gas outlet (33), described rinse bath (4) bottom is provided with the outlet of rinse bath yellow phosphorus, and the downside of rinse bath (4) is provided with wastewater outlet (35); Described rinse bath (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 water cooler, drive unit, molten bath, district (53) is arranged on bearing (52), ring heater and annular water cooler are installed around molten bath, district, ring heater and annular water cooler form by some groups respectively, along molten bath, district axially alternately, drive unit is connected with ring heater and annular water cooler by transom; 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 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 rinse bath yellow phosphorus import (29) pipeline and is provided with yellow phosphorus pump; The outlet of rinse bath yellow phosphorus is connected between dashpot yellow phosphorus import (59) has pipeline to connect.
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 rinse bath (4) is also provided with insulation jacket, and insulation jacket is provided with rinse bath insulation liquid import (30) and rinse bath insulation liquid outlet (34).
4. device as claimed in claim 1, is characterized in that the molten bath, district (53) of described zone melting equipment is for the cylindrical shell of closed at both ends; The quantity of described ring heater is identical with the quantity of annular water 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, 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), and hot water outlet (61) is in the below of molten bath, district (53) opposite side; The cooling water inlet (62) of annular water 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.
CN201320727082.0U 2013-11-18 2013-11-18 Yellow phosphorus purifying device Expired - Lifetime CN203582491U (en)

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Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112813503A (en) * 2021-01-13 2021-05-18 贵州威顿晶磷电子材料股份有限公司 Device and method for removing S impurities in yellow phosphorus through all-melting directional solidification

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112813503A (en) * 2021-01-13 2021-05-18 贵州威顿晶磷电子材料股份有限公司 Device and method for removing S impurities in yellow phosphorus through all-melting directional solidification
CN112813503B (en) * 2021-01-13 2021-11-23 贵州威顿晶磷电子材料股份有限公司 Device and method for removing S impurities in yellow phosphorus through all-melting directional solidification

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