CN109795996A - A kind of phosphoric acid by wet process vulcanization arsenic removal purification device and method - Google Patents

A kind of phosphoric acid by wet process vulcanization arsenic removal purification device and method Download PDF

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Publication number
CN109795996A
CN109795996A CN201910233474.3A CN201910233474A CN109795996A CN 109795996 A CN109795996 A CN 109795996A CN 201910233474 A CN201910233474 A CN 201910233474A CN 109795996 A CN109795996 A CN 109795996A
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phosphoric acid
vulcanizing agent
purification device
reactor tank
wet process
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CN201910233474.3A
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薛肖冲
田磊
董轩
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Shaanxi Yu Yu Technology Development Co Ltd
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Shaanxi Yu Yu Technology Development Co Ltd
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Priority to CN201910233474.3A priority Critical patent/CN109795996A/en
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Abstract

The invention discloses a kind of phosphoric acid by wet process vulcanization arsenic removal purification device and methods, including screw conveyor, vulcanizing agent feed bin, venturi mixer, reactor tank and equipment for separating liquid from solid;Vulcanizing agent enters vulcanizing agent feed bin, the vulcanizing agent import being arranged on vulcanizing agent bin outlet connection venturi mixer by screw conveyor;Venturi mixer outlet connection reactor tank import, reactor tank outlet connection equipment for separating liquid from solid;Phosphoric acid solution import is also set up on venturi mixer;Compressed air inlet is set on vulcanizing agent feed bin;Reactor tank is gas check.Tradition stirring is replaced by using venturi mixer, so that various materials uniformly mix in venturi mixer, occupation area of equipment is small, non-power consumption, saves the energy and cost.Meanwhile reactor tank is gas check and vulcanizing agent does not need to be individually configured to solution, effectively prevents the spilling of the hydrogen sulfide gas generated in reaction, improves execute-in-place safety and protection environment.

Description

A kind of phosphoric acid by wet process vulcanization arsenic removal purification device and method
Technical field
The invention belongs to phosphoric acid industry field, it is related to a kind of phosphoric acid by wet process vulcanization arsenic removal purification device and method.
Background technique
Phosphoric acid is widely used in the every field such as medicine, chemical industry, food as chemical industry base stock.But phosphoric acid by wet process Due to its impurity content height, the other field that can not be applied to other than chemical industry.Arsenic is mainly derived from phosphorus in phosphoric acid by wet process Ore, it is different according to the quality of rock phosphate in powder, slightly fluctuate.Though the content of arsenic is small, its presence often produces subsequent phosphate The quality of product produces bigger effect, and is one of the impurity of more difficult removal in phosphoric acid.The main method of phosphoric acid arsenic removal has chemistry heavy Shallow lake method, solvent extraction, ion-exchange etc..
Chemical precipitation method is one of the most widely used method in all multi-methods at present.Vulcanizing agent is added in phosphoric acid, So that arsenic ion and sulphion generate arsenones precipitating.The existing vulcanization arsenic removing apparatus that generally uses in phosphoric acid by wet process industry by Mixing channel and subsider composition, under usual production operation, vulcanizing agent and phosphoric acid are filled in mixing channel by mechanical stirring realization Divide reaction, hydrogen sulfide gas spilling is had during vulcanization reaction, influences execute-in-place safety and environment;Meanwhile whole device It is limited to the technique limitation of mechanical stirring and natural subsidence, occupied area is larger.
Summary of the invention
It is an object of the invention to overcome the above-mentioned prior art, a kind of phosphoric acid by wet process vulcanization arsenic removal purification dress is provided It sets and method.
In order to achieve the above objectives, the present invention is achieved by the following scheme:
A kind of phosphoric acid by wet process vulcanizes arsenic removal purification device, including screw conveyor, vulcanizing agent feed bin, venturi mixer, Reactor tank and equipment for separating liquid from solid;
Vulcanizing agent import is set on screw conveyor, and it is mixed that screw conveyor outlet is sequentially connected vulcanizing agent feed bin, venturi Clutch, reactor tank and equipment for separating liquid from solid;Phosphoric acid solution import is also set up on venturi mixer;Pressure is set on vulcanizing agent feed bin Contracting air intlet;Reactor tank is gas check.
A further improvement of the present invention lies in that:
Equipment for separating liquid from solid is subsider.
Equipment for separating liquid from solid includes slurry slot, liquid tank and exports sequentially connected filter liquid feeding pump and oneself with reactor tank Dynamic backwash surface filter;
Slurry slot and liquid tank are separately connected slurry outlet and the purified liquor outlet of automatic back-washing surface filter.
Filter liquid feeding pump is pneumatic diaphragm pump, the automatic back-washing surface filter, reactor tank, slurry slot and liquid tank It is all made of the production of acid-alkali-corrosive-resisting material.
Equipment for separating liquid from solid further includes ORP analyzer, and ORP analyzer is arranged in filter feed liquor pump discharge and automatic back-washing On pipeline between surface filter import;ORP analyzer is connect with screw conveyor.
Purification device further includes blender, and blender and reactor tank are tightly connected, for the mixed liquor in stirred tank.
Blender is ultrasonic stirrer.
Purification device further includes electromagnetic flowmeter, and the phosphoric acid solution inlet tube of venturi mixer is arranged in electromagnetic flowmeter On, for detecting the liquid inlet volume of phosphoric acid solution.
Aperture is set at the top of reactor tank, and aperture connects the gas feed being arranged on venturi mixer, pipeline by pipeline With aperture flanged joint.
The invention also discloses a kind of phosphoric acid by wet processes to vulcanize arsenic removal purification method, comprising the following steps:
Step 1: venturi mixer is added by electromagnetic flowmeter in phosphoric acid solution containing arsenic to be processed and measures additional amount; Meanwhile vulcanizing agent is added to vulcanizing agent feed bin by screw conveyor, vulcanizing agent enters venturi under Venturi effect and mixes Device is mixed with phosphoric acid solution containing arsenic to be processed, forms mixed solution A;The additional amount of vulcanizing agent can make ORP analyzer reading steady It is scheduled on preset value;
Step 2: mixed solution A gravity flow enters reactor tank and reacts, and forms sulfide precipitation and treated phosphoric acid solution;
Step 3: by the sulfide precipitation in step 2, phosphoric acid solution is delivered to automatic back-washing surface mistake jointly with treated Filter, by sulfide precipitation, phosphoric acid solution is separated with treated;
Step 4: sulfide precipitation being delivered to slurry slot, phosphoric acid solution is delivered to liquid tank by treated.
Compared with prior art, the invention has the following advantages:
Purification device of the present invention replaces tradition stirring by using venturi mixer, so that various materials are in venturi It is uniformly mixed in mixer, occupation area of equipment is small, non-power consumption, saves the energy and cost.Reactor tank is gas check, is had The spilling for preventing the hydrogen sulfide gas generated in reaction of effect improves execute-in-place safety and protection environment.Using spiral Conveyer, vulcanizing agent feed bin and compressed air are used cooperatively, and the addition rate of vulcanizing agent is controlled by screw conveyor, makes to react Object proportion is more reasonable;Meanwhile vulcanizing agent does not need to be individually configured to solution, avoids vulcanizing agent in configuration process and reacts with water Influence of the hydrogen sulfide gas of generation to system safety, improves the safety of device.
Further, use automatic back-washing surface filter as equipment for separating liquid from solid, principle is positive membrane filtration, accounts for Ground area is small, and filter cycle is short, and filtering accuracy is high, is able to achieve automatic discharge in the process of running, and bottom ash enters the progress of slurry slot Subsequent centralized processing, cleaning are convenient.
Further, chain using ORP analyzer and screw conveyor, reaction optimum state is determined by long-play It determines that ORP reading is oxidation-reduction potential afterwards, measurement information is sent to screw conveyor, is controlled and is conveyed by screw conveyor Calcium sulfide additional amount maintains ORP analyzer data stabilization, keeps the entire reaction process controllability stronger, reacts more abundant.
Further, catalysis reaction is carried out to mixed liquor from molecular level using ultrasonic stirrer, so that between material It is sufficiently mixed, reacts, accelerate reaction efficiency.
Further, it is equipped with aperture at the top of reactor tank, is connected to the gas feed being arranged on venturi mixer, venturi The hydrogen sulfide gas that the negative pressure that mixer generates generates reactor tank sucks, and is recycled into reactor tank, harmful hydrogen sulfide gas Can be used as vulcanizing agent, the reaction was continued, and safety is improved, and reaction is also more abundant.
Purification method of the present invention measures oxidation-reduction potential numerical value in chemical reaction process, first basis by ORP analyzer Longtime running situation combination assay determines that one has completely been reacted arsenic ion, while the ORP overflowed without hydrogen sulfide is surveyed Determine instrument reading, which is the preset value of ORP analyzer.When phosphoric acid solution flow or arsenic content fluctuate, ORP measurement Instrument reading changes, at this point, increasing or reducing the rate of screw conveyor conveying vulcanizing agent, until ORP analyzer is maintained to read Number is stablized in preset value, and the additional amount of control vulcanizing agent is passed through, it is ensured that arsenic ion reaches while effectively remove, and avoids vulcanizing agent The excessive danger for generating a large amount of hydrogen sulfide gas and generating is added, guarantees the safety of staff.
Detailed description of the invention
Fig. 1 is the structural diagram of the present invention;
Fig. 2 is the device of the invention process for using block diagram.
Wherein: 1- electromagnetic flowmeter;2- screw conveyor;3- vulcanizing agent feed bin;4- venturi mixer;5- blender; 6- reactor tank;7- filter liquid feeding pump;8-ORP analyzer;9- slurry slot;10- liquid tank;11- automatic back-washing surface filter.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, below in conjunction in the embodiment of the present invention Attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only The embodiment of a part of the invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people The model that the present invention protects all should belong in member's every other embodiment obtained without making creative work It encloses.
It should be noted that description and claims of this specification and term " first " in above-mentioned attached drawing, " Two " etc. be to be used to distinguish similar objects, without being used to describe a particular order or precedence order.It should be understood that using in this way Data be interchangeable under appropriate circumstances, so as to the embodiment of the present invention described herein can in addition to illustrating herein or Sequence other than those of description is implemented.In addition, term " includes " and " having " and their any deformation, it is intended that cover Cover it is non-exclusive include, for example, the process, method, system, product or equipment for containing a series of steps or units are not necessarily limited to Step or unit those of is clearly listed, but may include be not clearly listed or for these process, methods, product Or other step or units that equipment is intrinsic.
The invention will be described in further detail with reference to the accompanying drawing:
Referring to Fig. 1 and 2, a kind of phosphoric acid by wet process of the present invention vulcanizes arsenic removal purification device, including electromagnetic flowmeter 1, spiral transferring Send machine 2, vulcanizing agent feed bin 3, venturi mixer 4, ultrasonic stirrer 5, reactor tank 6, filter liquid feeding pump 7, ORP analyzer 8, slurry slot 9, liquid tank 10, automatic back-washing surface filter 11.
After phosphoric acid solution to be processed passes through phosphoric acid solution inlet tube, entered by 4 phosphoric acid solution import of venturi mixer Venturi mixer 4, and the electromagnetic flowmeter 1 by being arranged on phosphoric acid solution inlet tube detects phosphoric acid solution liquid inlet volume;Together When, quantitative vulcanizing agent is delivered to vulcanizing agent feed bin 3 by screw conveyor 2, is blown by compressed air into vulcanizing agent feed bin 3 Gas is sent vulcanizing agent to venturi mixer 4 by the vulcanizing agent import being arranged on venturi mixer 4.
Phosphoric acid solution is realized in venturi mixer 4 with vulcanization calcium powder to flow automatically into reactor tank 6, instead after solid-liquid mixes Answering tank 6 is gas check, effectively prevents the excessive of the hydrogen sulfide gas that reaction generates, while being equipped with blender 5, blender 5 can select ultrasonic stirrer, carry out catalysis reaction to mixed liquor from molecular level using ultrasonic wave agitating device, accelerate anti- Answer efficiency.Aperture is equipped at the top of reactor tank 6, aperture connects 4 feed inlet of venturi mixer, excessive hydrogen sulfide by pipeline Gas is recycled into reactor tank 6 as vulcanizing agent under the tiny structure effect of venturi mixer 4, and the reaction was continued.Aperture and pipeline It is attached by flange.
The outlet of reactor tank 6 connection filter liquid feeding pump 7, while in the outlet of filter liquid feeding pump 7 and automatic back-washing surface mistake ORP analyzer 8 is installed, ORP analyzer 8 and screw conveyor 2 are chain, and formation controls back on the pipeline between 11 import of filter Road;Helical feed 2, which is controlled, according to the measurement information of ORP analyzer 8 conveys calcium sulfide additional amount.It is determined by long-play anti- ORP reading, i.e. oxidation-reduction potential are determined after answering optimum state, and calcium sulfide additional amount is conveyed by control helical feed 2 to tie up Hold the data stabilization of ORP analyzer 8.Mixed solution enters automatic back-washing surface filter 11 under the action of the pump pressure of 0.2MPa Realize forced filtration, filter cake is periodically discharged into slurry slot 9 under the PLC program of automatic back-washing surface filter, and clear liquid enters clear liquid Slot 10.
Electromagnetic flowmeter 1 uses the product of resistance to phosphoric acid corrosion.It is molten into phosphoric acid that venturi mixer 4 designs a main inlet Liquid;Two branch mouths, respectively into vulcanization calcium powder and the excessive hydrogen sulfide gas of reactor tank.Filter liquid feeding pump 7 using pneumatically every Membrane pump, acid-alkali-corrosive-resisting.Automatic back-washing surface filter 11, reactor tank 6 are all made of 316L stainless steel material processing and fabricating.Slurry Slot 9 and liquid tank 10 are all made of 316L material processing and fabricating.It is all in this purification device to be all made of with phosphoric acid solution contact site Resistance to phosphoric acid corrosion material production.
Tradition stirring is replaced by using venturi mixer, so that various materials are uniformly mixed in venturi mixer It closes, occupation area of equipment is small, non-power consumption.It is used cooperatively using screw conveyor 2, vulcanizing agent feed bin 3 with compressed air, sulphur Agent does not need to be individually configured to solution, avoids vulcanizing agent in configuration process and reacts the hydrogen sulfide gas generated with water to system The influence of safety.Wherein, vulcanizing agent can select vulcanization calcium powder, using calcium sulfide as vulcanizing agent, send out during the reaction Raw following reaction:
As3++S2-=As2S3↓Ca2++PO4 3-=Ca3(PO4)2
The calcium ion introduced in the reaction as the calcium sulfide of vulcanizing agent is also precipitated as calcium phosphate, passes through automatic back-washing table After solid-liquid separation is filtered in face, other ions are not introduced in phosphoric acid arsenic removal.
It is equipped with bleeding point flange at the top of reactive tank 6, venturi mixer branch feed inlet is connected to, when phosphoric acid liquid passes through When, the hydrogen sulfide gas that the negative pressure that venturi mixer generates generates reactive tank sucks, and is recycled into reactive tank, harmful sulphur Change hydrogen can be used as vulcanizing agent, and the reaction was continued.
Use automatic back-washing surface filter 11 as equipment for separating liquid from solid, principle is positive membrane filtration, occupied area Small, filter cycle is short, and filtering accuracy is high, is able to achieve automatic discharge in the process of running, and bottom ash enters slurry slot 9 and carries out subsequent set Middle processing, cleaning are convenient.
The invention also discloses a kind of phosphoric acid by wet processes to vulcanize arsenic removal purification device, comprising the following steps:
Step 1: venturi mixer 4 is added by electromagnetic flowmeter 1 in phosphoric acid solution containing arsenic to be processed and measures addition Amount;Meanwhile vulcanizing agent is added to vulcanizing agent feed bin 3 by screw conveyor 2, in the present embodiment, vulcanizing agent selects vulcanization calcium powder End, because the negative pressure that Venturi effect is formed absorbs the vulcanization calcium powder in vulcanizing agent feed bin 3 in venturi mixer 4, Phosphoric acid solution to be processed and vulcanization calcium powder are sufficiently mixed in venturi mixer 4, form mixed solution A;Vulcanize calcium powder Additional amount can make 8 stable reading of ORP analyzer in preset value;According to longtime running situation combination assay, one is determined Arsenic ion is reacted completely, while the ORP analyzer 8 overflowed without hydrogen sulfide is read, which is the pre- of ORP analyzer 8 If value.
Step 2: mixed solution A gravity flow enter reactor tank 6 react, under the action of ultrasonic stirrer 5, calcium sulfide with to The arsenic ion reaction in phosphoric acid solution is handled, sulfide precipitation is formed and forms sulfide precipitation and treated phosphoric acid solution;And By the gas generated in reaction process being mixed with mixed solution A by being delivered to venturi mixer 4 by 6 top of reactor tank It closes.
Step 3: by the sulfide precipitation in step 2, phosphoric acid solution is delivered to automatic back-washing surface mistake jointly with treated Filter 11 is delivered to automatic back-washing surface filter, under pump pressure, forced filtration is realized, rapidly by sulfide precipitation and processing Phosphoric acid solution separation afterwards.
Step 4: sulfide precipitation being delivered to slurry slot 9, phosphoric acid solution is delivered to liquid tank 10 by treated.
Pass through the additional amount of control vulcanizing agent, it is ensured that arsenic ion reaches while effectively remove, and vulcanizing agent is avoided to be added Amount generates the danger that a large amount of hydrogen sulfide gas generate.The ORP interlock for devising a kind of control vulcanizing agent additional amount is installed at After reactor tank 6 on depot siding, ORP analyzer 8 can measure oxidation-reduction potential numerical value in chemical reaction process, first according to long-term Operating condition combination assay determines that one has completely been reacted arsenic ion, while without the ORP analyzer of hydrogen sulfide spilling 8 readings, the numerical value are the preset value of ORP analyzer 8.When phosphoric acid solution flow or arsenic content fluctuate, ORP analyzer 8 readings change, and increase or reduce the rate of screw conveyor conveying vulcanizing agent, until maintaining 8 stable reading of ORP analyzer Near preset value, resource utilization is improved, improves safety.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention Protection scope within.

Claims (10)

1. a kind of phosphoric acid by wet process vulcanizes arsenic removal purification device, which is characterized in that including screw conveyor (2), vulcanizing agent feed bin (3), venturi mixer (4), reactor tank (6) and equipment for separating liquid from solid;
Vulcanizing agent import is set on screw conveyor (2), and screw conveyor (2) outlet is sequentially connected vulcanizing agent feed bin (3), literary mound In mixer (4), reactor tank (6) and equipment for separating liquid from solid;Venturi mixer also sets up phosphoric acid solution import on (4);Vulcanization Compressed air inlet is arranged on (3) in agent feed bin;Reactor tank (6) is gas check.
2. phosphoric acid by wet process according to claim 1 vulcanizes arsenic removal purification device, which is characterized in that the equipment for separating liquid from solid For subsider.
3. phosphoric acid by wet process according to claim 1 vulcanizes arsenic removal purification device, which is characterized in that the equipment for separating liquid from solid Sequentially connected filter liquid feeding pump (7) and automatic back-washing are exported including slurry slot (9), liquid tank (10) and with reactor tank (6) Surface filter (11);
Slurry slot (9) and liquid tank (10) are separately connected slurry outlet and the purified liquor outlet of automatic back-washing surface filter (11).
4. phosphoric acid by wet process according to claim 3 vulcanizes arsenic removal purification device, which is characterized in that the filter liquid feeding pump It (7) is pneumatic diaphragm pump, the automatic back-washing surface filter (11), reactor tank (6), slurry slot (9) and liquid tank (10) are equal It is made of acid-alkali-corrosive-resisting material.
5. phosphoric acid by wet process according to claim 3 vulcanizes arsenic removal purification device, which is characterized in that the equipment for separating liquid from solid It further include ORP analyzer (8), ORP analyzer (8) setting is in filter liquid feeding pump (7) outlet and automatic back-washing surface filter (11) on the pipeline between import;ORP analyzer (8) is connect with screw conveyor (2).
6. phosphoric acid by wet process according to claim 1-5 vulcanizes arsenic removal purification device, which is characterized in that the purification Device further includes blender (5), and blender (5) and reactor tank (6) are tightly connected, for the mixed liquor in stirred tank.
7. phosphoric acid by wet process according to claim 6 vulcanizes arsenic removal purification device, which is characterized in that the blender (5) is Ultrasonic stirrer.
8. phosphoric acid by wet process according to claim 1-5 vulcanizes arsenic removal purification device, which is characterized in that the purification Device further includes electromagnetic flowmeter (1), and electromagnetic flowmeter (1) is arranged on the phosphoric acid solution inlet tube of venturi mixer, is used In the liquid inlet volume of detection phosphoric acid solution.
9. phosphoric acid by wet process according to claim 1-5 vulcanizes arsenic removal purification device, which is characterized in that the reaction Aperture is set at the top of tank (6), and aperture connects the gas feed being arranged on venturi mixer (4), pipeline and aperture by pipeline Flanged joint.
10. a kind of phosphoric acid by wet process based on claim 5 described device vulcanizes arsenic removal purification method, which is characterized in that including with Lower step:
Step 1: venturi mixer (4) are added by electromagnetic flowmeter (1) in phosphoric acid solution containing arsenic to be processed and measure addition Amount;Meanwhile vulcanizing agent is added to vulcanizing agent feed bin (3) by screw conveyor (2), vulcanizing agent enters text under Venturi effect Mixer (4) is mixed with phosphoric acid solution containing arsenic to be processed in mound, forms mixed solution A;The additional amount of vulcanizing agent can be such that ORP surveys Instrument (8) stable reading is determined in preset value;
Step 2: mixed solution A gravity flow enters reactor tank (6) and reacts, and forms sulfide precipitation and treated phosphoric acid solution;
Step 3: by the sulfide precipitation in step 2, phosphoric acid solution is delivered to automatic back-washing surface filter jointly with treated (11), by sulfide precipitation, phosphoric acid solution is separated with treated;
Step 4: sulfide precipitation being delivered to slurry slot (9), by treated, phosphoric acid solution is delivered to liquid tank (10).
CN201910233474.3A 2019-03-26 2019-03-26 A kind of phosphoric acid by wet process vulcanization arsenic removal purification device and method Pending CN109795996A (en)

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CN111282507A (en) * 2020-03-19 2020-06-16 江阴市恒中精工机械有限公司 Intelligent online glue metering, batching, dissolving and mixing device and method
CN115072682A (en) * 2022-06-07 2022-09-20 瓮福(集团)有限责任公司 Feed-grade wet-process phosphoric acid dearsenification method

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