CN110510589A - A kind of Wet-process Phosphoric Acid Production method and production system - Google Patents

A kind of Wet-process Phosphoric Acid Production method and production system Download PDF

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Publication number
CN110510589A
CN110510589A CN201910851385.5A CN201910851385A CN110510589A CN 110510589 A CN110510589 A CN 110510589A CN 201910851385 A CN201910851385 A CN 201910851385A CN 110510589 A CN110510589 A CN 110510589A
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China
Prior art keywords
washing lotion
area
phosphoric acid
storage tank
pipeline
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CN201910851385.5A
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Chinese (zh)
Inventor
程来斌
章磊
吕景祥
刘光耀
胡挺
查炎华
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HUBEI XIANGYUN (GROUP) CHEMICAL CO Ltd
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HUBEI XIANGYUN (GROUP) CHEMICAL CO Ltd
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Priority to CN201910851385.5A priority Critical patent/CN110510589A/en
Publication of CN110510589A publication Critical patent/CN110510589A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/18Phosphoric acid
    • C01B25/22Preparation by reacting phosphate-containing material with an acid, e.g. wet process
    • C01B25/222Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a kind of Wet-process Phosphoric Acid Production method and production systems, belong to phosphoric acid production technical field.Area's slurry is washed as three using phosphoric acid return water, the filter cloth regeneration water using clean and high temperature condensed water as filter cloth regeneration area, by the way that the concentrated sulfuric acid is added in three washing lotion storage tanks;It one of is acted on: the substance of easy fouling can be settled down and be washed area three again and get express developed, the two of its effect are as follows: it is found by the applicant that can obviously reduce the structure risk of filter plate when sulfuric acid concentration is 5% or so, the three of effect can improve the acid concentration of subsequent washing lotion slightly to improve washing effect;Filter cloth washing water is cleaner and high temperature, the slurry that two washing lotion storage tanks of addition wash area as one can increase temperature, promote wash water dosage, dilute washing lotion impurity.By handle to phosphor-gypsum backwater and the blocking to spray head can be reduced using clean condensed water, extend the maintenance period of filter device.

Description

A kind of Wet-process Phosphoric Acid Production method and production system
Technical field
The invention belongs to phosphoric acid production technical field, in particular to a kind of Wet-process Phosphoric Acid Production method and production system.
Background technique
Phosphoric acid or orthophosphoric acid, chemical formula H3PO4, molecular weight 97.994 is a kind of common inorganic acid, is middle strong acid.Phosphorus Acid is mainly used for the industry such as pharmacy, food, fertilizer, including as antirust agent, food additives, dentistry and orthopaedic srugery, EDIC Corrosive agent, electrolyte, scaling powder, dispersing agent, industrial corrosion agent, the raw material and component household cleaning product of fertilizer.It also is used as Chemical reagent, phosphate are the nutrition of all life forms.In phosphorus ammonium and chemical fertilizer field, phosphoric acid generallys use wet process preparation.It is wet Method are as follows: the concentrated sulfuric acid reacts preparing phosphoric acid with calcium phosphate, rock phosphate in powder, filters off the calcium sulfate precipitation for being slightly soluble in water, and gained filtrate is exactly Phosphoric acid solution.
The production method for such as disclosing a kind of monoammonium phosphate application No. is the Chinese patent of CN201310111584.5 (only takes Phosphoric acid production part), including following process:
Process one: phosphorus ore ore matching weight ratio are as follows: P2O5%25.8-26.3%, MgO < 3%, K+Na < 1%.
Process two: it produces ore pulp: the phosphorus ore that process one obtains being broken using two-stage Hubei Province, level-one circular cone breaks and forms 15-25mm It after granularity, is sieved into vibrating screen, the thin Hubei Province of top coarse fodder return is broken, circular cone is broken, is crushed again, by under vibrating screen The granularity in portion enters ball mill in the fines of 15-20mm and produces ore pulp, and slurry fineness is made to reach 85-90%-100 mesh.
Process three: extraction: the ore pulp that process two is obtained, and from sulfuric acid library, to account for react whole dosages 1/5 The acid reflux of sulfuric acid and phosphoric acid subsider squeezes into pre-reactor, and three carries out pre-reaction, and reaction mass enters back into extraction tank, and is added The sulfuric acid for reacting whole dosages 4/5 is accounted for, further decompose ore pulp completely and forms slurry;The extraction tank of the process is six lattice square grooves Structure, four reaction areas, two digestion zones exchange circulating pump and import and export position, expand the slurry of four reaction chambers to four reaction chambers Overflow port, by phosphoric acid P2O5Concentration control is controlled in 17%-19%, extraction temperature to 83-87 DEG C, and vacuum cooled vacuum degree control arrives - 0.050 to -0.055MPa, it is installed additional on extraction tank automatically plus defoaming agent device, flash chamber outlet adds Despumation device.
Process four: filtering: squeezing into filter station for the slurry that process three obtains, by disk filter by phosphoric acid from slurry In separate, the phosphoric acid dephosphorization acid deposition slot separated further purifies, and upper clear supernate goes to neutralize concentration section, and lower part is thick Slurry returns to extraction tank as acid reflux;The gypsum separated refilters after washing, is finally sent to phosphogypsum slag by belt feeder It stacks field.
To phosphoric acid, (Jiangsu is new as shown in Figure 1, can use Turntable vacuum filter device in filtering for the preparation method of phosphoric acid The HDZP Series Filtration device of grand company) it is filtered.Wherein, filter device includes initial filter area, filtering area, a Xi Qu, two Xi Qu, three wash area, filter cloth regeneration area and ardealite hopper etc., and filtering area obtains phosphoric acid.Filter cloth regeneration area wash water (flushing water, 60 DEG C or more, while moisturizing as needed are heated in heating water tank) as slurry, three wash the wash water in area in the area Song Sanxi As slurry, two wash the area wash water Song Yixi in area as slurry in the area Song Erxi, and one washes the wash water in area and initial filter area Filtrate is as sour regurgitation.Area's slurry is washed (in filter cloth regeneration area as filter cloth regeneration water and three using process water in the prior art In the insufficient situation of the washing lotion of output), those skilled in the art both knows about, in Wet-process Phosphoric Acid Production, phosphor-gypsum backwater Measure larger, pH value 2-3, containing a small amount of titanium pigment (total phosphorus is less than 2%), can not direct emission, usually returned in the prior art It returns phosphoric acid production to be recycled as the filter cloth wash water and recycled water of filter, but phosphor-gypsum backwater impurity content is high (to be contained Not Soluble phosphorus and Leaching Properties of Soluble Phosphorus, acid and various metallic elements etc.), it is easy blocking phosphoric acid system, is particularly easy to make the filter plate of filter device Fouling.Our company 2016 and 2017 year is all made of slurry of the phosphor-gypsum backwater as filter device, it is found by the applicant that as follows Problem:
1. filter filter disc fouling, cleaning parking 24 hours, 50 people or more to clear up (filter plate and other structures) every time, annual stifled 1 to 2 time, filtering board is severely deformed after cleaning, and filter cloth regeneration effect is poor, and changes a filter plate and need 360,000.
2. the spray head on each scrubbing section and the distributor of renewing zone is also easy to fouling, periodic maintenance is needed.
3. filtration washing effect is poor since fouling causes lower acid unsmooth, water-soluble phosphorus loses at least 0.05%.
4. filter plate fouling can not reach design production capacity, while fouling also results in parking and repairs, and will affect production capacity.
Summary of the invention
The embodiment of the invention provides a kind of Wet-process Phosphoric Acid Production method and production system, which is made using phosphoric acid return water The slurry for washing area for three, the filter cloth regeneration water using clean and high temperature condensed water as filter cloth regeneration area, by three The concentrated sulfuric acid (sulfuric acid can be added in extraction tank to be reacted, impurity will not be introduced) is added in washing lotion storage tank;One of its effect: can The substance of easy fouling (metal salt etc. on phosphor-gypsum backwater and filter cloth) to settle down area washed three again get express developed, The two of its effect are as follows: it is found by the applicant that can obviously reduce the fouling risk of filter plate when sulfuric acid concentration is 5% or so, act on it Three can improve the acid concentration of subsequent washing lotion slightly to improve washing effect;Filter cloth washing water is cleaner and high temperature, and two washing lotions are added The slurry that storage tank washes area as one can increase flushing dose, increase wash temperature and have preferably washing effect.By to phosphorus Gypsum return water handle and can reduce the blocking to spray head using clean condensed water, extends the maintenance period of filter device. The technical solution is as follows:
On the one hand, the embodiment of the invention provides a kind of Wet-process Phosphoric Acid Production methods, which comprises ore pulp and carrys out inherent filtration The sour regurgitation of device is reacted, and is reacted again with the concentrated sulfuric acid after the reaction was completed, is filtered to obtain finally by filter device Phosphoric acid, sour regurgitation and ardealite, ardealite send phosphor-gypsum backwater processing system to handle to obtain phosphor-gypsum backwater;The filter device One washes the filtrate in the washing lotion in area 3 and initial filter area 1 as sour regurgitation;The heat exchange of the barometric condenser 20 of the phosphor-gypsum backwater and filter device Afterwards, it send the three of filter device to wash area 5 after neutralized reaction, sedimentation, filters pressing and heating and is used as three wash waters, the barometric condenser 20 The gas and condensation for collecting phosphoric acid separator 9, diafiltration liquid/gas separator 12, two washing lotion separators 14 and three washing lotion separators 17 obtain Condensed water, the condensed water send the filter cloth regeneration area 6 of filter device to be used as filter cloth regeneration water;Described three washing lotions for washing area 5 are added Sulfuric acid and adjust to h 2 so 4 concentration be 5.5-6.0% send the two of filter device wash area 4 be used as two wash waters;The filter cloth regeneration The washing lotion that the washing lotion in area 6 washes area 4 with two merges the area Hou Songyixi 3 and is used as a wash water.
Wherein, the neutralization reaction process in the embodiment of the present invention are as follows: limewash is added and adjusts the pH value of phosphor-gypsum backwater To 6.5-7.0;The infall process are as follows: organic polymer coargulator is added, the usage amount of the organic polymer coargulator is The 0.05-2% of phosphor-gypsum backwater quality, sedimentation time 0.5-6h;The pressure-filtering process are as follows: filters pressing is carried out using plate and frame filter press, Filter cloth aperture is 200-500 mesh;The heating process are as follows: three wash waters are heated to 60 DEG C or more.
Further, after the screenings that the infall process in the embodiment of the present invention generates merges with the filter residue that filter process generates Adjusting to density is 1.72-1.78g/cm3As ore pulp.
Further, the partial condensation Shui Song filter cloth regeneration area 6 in the embodiment of the present invention is used as filter cloth regeneration water, remaining cold Condensate with through filters pressing, treated that phosphor-gypsum backwater mixes, heats the area Hou Songsanxi 5 is used as three wash waters.
Wherein, the volume ratio of the ore pulp in the embodiment of the present invention, sour regurgitation and the concentrated sulfuric acid is 77-83:115-125:35-40, The density of the ore pulp is 1.72-1.78g/cm3, the phosphoric acid concentration of the sour regurgitation is 14-16%, and the concentration of the concentrated sulfuric acid is 90-99%。
Wherein, two in the embodiment of the present invention wash the washing lotion in area 4 after two washing lotion separators 14 carry out gas-liquid separation with filter The washing lotion of cloth renewing zone 6 mixes, then physics settles to obtain a wash water;Described three wash the washing lotion in area 5 through three washing lotion separators 17 into It is mixed with sulfuric acid after row gas-liquid separation, then physics sedimentation as two wash waters;Described one washes the filtrate of the washing lotion in area 3 and initial filter area 1 The phosphorus that filtering area 2 after diafiltration liquid/gas separator 12 carries out gas-liquid separation, then after physics sedimentation with or without filter device obtains Acid-mixed cooperation is sour regurgitation;The filtrate of the filtering area 2 is after phosphoric acid separator 9 carries out gas-liquid separation, then physics settles to obtain phosphorus Acid.
On the other hand, the embodiment of the invention also provides a kind of Wet-process Phosphoric Acid Production system, which includes pulp tank, pre- Reactive tank, phosphor-gypsum backwater processing system, phosphor-gypsum backwater storage tank, filter device, neutralization reaction storage tank 26, neutralizes extraction tank Reactive tank 27, subsider 28, filter press 29 and filtrate storage tank 31, the extraction tank are connect with sulfuric acid storage tank;The filter device Including rotary vacuum disk fiter 25, phosphoric acid storage tank 10, phosphoric acid separator 9, diafiltration liquid/gas separator 12, sour regurgitation slot 13, two washing lotions point From device 14, two washing lotion storage tanks 15, three washing lotion separators 17, three washing lotion storage tanks 18, heating water tank, barometric condenser 20, vacuum pump 23 and condensed water storage tank 21, the rotary vacuum disk fiter 25 includes that initial filter area 1, filtering area 2, one wash area 3, two and wash area 4, three and wash Area 6 and ardealite hopper 7 are washed by area 5, filter cloth regeneration;The pulp tank, anterior reactor, extraction tank and rotary vacuum disk fiter 25 Feed inlet is sequentially connected by pipeline, and the ardealite hopper 7, phosphor-gypsum backwater processing system and phosphor-gypsum backwater storage tank pass through Pipeline is sequentially connected, and the sour regurgitation slot 13 is connect by pipeline with anterior reactor, phosphoric acid storage tank 10 and diafiltration liquid/gas separator 12, institute It states diafiltration liquid/gas separator 12 to connect by pipeline with the washing lotion outlet that the filtrate (liquid in initial filter area 1 and one wash area 3, the phosphoric acid point It is connect by pipeline with the filtrate (liquid of filtering area 2 and phosphoric acid storage tank 10 from device 9;The described three washing lotion imports for washing area 5 pass through pipe Road is connect with heating water tank, and described three, which wash the washing lotion outlet in area 5, three washing lotion separators 17, three washing lotion storage tanks 18 and two, washes area 4 Washing lotion import is sequentially connected by pipeline, and described two wash the washing lotion outlet in area 4, two washing lotion separators 14, two washing lotion storage tanks, 15 and The one washing lotion import for washing area 3 is sequentially connected by pipeline;The air inlet of the barometric condenser 20 is separated by pipeline with phosphoric acid Device 9, diafiltration liquid/gas separator 12, two washing lotion separators 14 are connected with the gas vent of three washing lotion separators 17, condensation-water drain It is connect by pipeline with condensed water storage tank 21, exhaust outlet is connect with vacuum pump 23;The phosphor-gypsum backwater storage tank and big air cooling The cooling water inlet of condenser 20 by piping connection, the cooling water outlet of the barometric condenser 20, neutralization reaction storage tank 26, in It is sequentially connected with reactive tank 27, subsider 28, filter press 29, filtrate storage tank 31 and heating water tank by pipeline, the condensed water Storage tank 21 is connect by pipeline with the washing lotion import in filter cloth regeneration area 6 and hot water storage tank, the washing lotion outlet in the filter cloth regeneration area 6 It is connect by pipeline with two washing lotion storage tanks 15, the three washing lotions storage tank 18 is connect by pipeline with sulfuric acid storage tank.
Wherein, the phosphoric acid storage tank 10 in the embodiment of the present invention, sour regurgitation slot 13, two washing lotion storage tanks 15 and three washing lotion storage tanks 18 are equal Including sedimentation groove body and storage groove body, the sedimentation groove body and storage groove body are arranged side by side;The top of the sedimentation groove body is equipped with Feed inlet is simultaneously passed through its interior lower part, and upper part is equipped with overflow port and is connected to storage groove body top, and bottom is equipped with sewage draining exit;It is described It stores groove body bottom and is equipped with discharge port;Feed inlet on the sedimentation groove body of the three washing lotions storage tank 18 passes through pipeline and three washing lotions point Liquid outlet connection from device 17, storage groove body are equipped with thief hatch and blender and are connect by pipeline with sulfuric acid storage tank;Institute The feed inlet for stating the sedimentation groove body of two washing lotion storage tanks 15 passes through the washing lotion outlet and two washing lotion separators of pipeline and filter cloth regeneration area 6 14 liquid outlet connection.
Preferably, Wet-process Phosphoric Acid Production system provided in an embodiment of the present invention further includes screenings collecting tank 32 and stock tank again 33, the screenings collecting tank 32 is used to collect the filter residue of filter press 29 and it is connect by pipeline with stock tank 33 again, described to starch again Slot 33 is connect by pipeline with the outlet of the screenings of subsider 28 and pulp tank.
Wherein, phosphoric acid separator 9 provided in an embodiment of the present invention, diafiltration liquid/gas separator 12, two washing lotion separators 14 and three Washing lotion separator 17 is gas-liquid separator;The vacuum pump 23 is water ring vacuum pump;The hot water storage tank adds equipped with steam Hot coil and/or steam heating jacket;The neutralization reaction slot 26 is equipped with blender and steam(-)coil and/or steam heats Collet, the stock tank again 33 and screenings collecting tank 32 are equipped with blender.
Technical solution provided in an embodiment of the present invention has the benefit that the embodiment of the invention provides a kind of wet processes Phosphoric acid production method and production system can promote production capacity 4-5%, can increase 6-10 yuan/ton of profit, can extend the dimension of filter device The period is protected, maintenance cost can be reduced, 0.15% or more the yield of phosphorus pentoxide can be increased, the total phosphorus content of ardealite can be reduced 0.05% or more, water consumption and steam consumption, remarkable in economical benefits can be reduced.
Detailed description of the invention
Fig. 1 is the functional block diagram of existing Wet-process Phosphoric Acid Production system;
Fig. 2 is the functional block diagram of Wet-process Phosphoric Acid Production system provided in an embodiment of the present invention;
Fig. 3 is the functional block diagram of filter device provided in an embodiment of the present invention;
Fig. 4 is the structural schematic diagram of filter device provided in an embodiment of the present invention;
Fig. 5 is the distribution map of each functional areas of rotary vacuum disk fiter provided in an embodiment of the present invention.
Fig. 6 is the structural schematic diagram of neutralization reaction storage tank and neutralization reaction slot combination provided in this embodiment;
Fig. 7 is subsider provided in this embodiment, filter press, filtrate storage tank and the structural schematic diagram of stock tank combination again.
In figure: 1 initial filter area, 2 filtering areas, 3 wash area, 4 two wash area, 5 three wash area, 6 filter cloth regeneration areas, 7 gypsum hoppers, 8 Phosphoric acid discharge pump, 9 phosphoric acid separators, 10 phosphoric acid storage tanks, 11 sour regurgitations pump, 12 diafiltration liquid/gas separators, 13 sour regurgitation slots, 14 2 washing lotions point From device, 15 2 washing lotion storage tanks, 16 2 wash pump, 17 3 washing lotion separators, 18 3 washing lotion storage tanks, 19 3 wash pump, 20 barometric condensers, 21 condensed water storage tanks, 22 discharge air separators, 23 vacuum pumps, 25 rotary vacuum disk fiters, 26 neutralization reaction storage tanks, 27 neutralization reactions Slot, 28 subsiders, 29 filter presses, 30 filtrate collecting tanks, 31 filtrate storage tanks, 32 screenings collecting tanks, 33 again stock tank, a tail gas, b into Slurry, c sulfuric acid, d low-pressure steam, e phosphoric acid, f sour regurgitation, g sealing water, h condensed water, tri- wash water of i, j vacuum evacuation separation water, k phosphorus Gypsum and flushing water, l go two washing lotion storage tanks, m phosphor-gypsum backwater, n process water, o limewash, p go subsider, q go phosphoric acid geosyncline, R flocculant, s go pulp tank, t to remove heating water tank.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the present invention is made into one below in conjunction with attached drawing Step ground detailed description.
Embodiment 1
Referring to fig. 2-7, embodiment 1 provides a kind of Wet-process Phosphoric Acid Production system, which includes pulp tank, anterior reactor, extraction Take slot, phosphor-gypsum backwater processing system, phosphor-gypsum backwater storage tank, filter device, neutralization reaction storage tank 26, neutralization reaction slot 27, Subsider 28, filter press 29 and filtrate storage tank 31 etc., extraction tank is connect with sulfuric acid storage tank for sulfuric acid to be added.Filter device includes Rotary vacuum disk fiter 25, phosphoric acid storage tank 10, phosphoric acid separator 9, diafiltration liquid/gas separator 12, sour regurgitation slot 13, two washing lotion separators 14, two washing lotion storage tanks 15, three washing lotion separators 17, three washing lotion storage tanks 18, heating water tank, barometric condenser 20,23 and of vacuum pump Condensed water storage tank 21(seals simultaneously) etc..Rotary vacuum disk fiter 25 washes area 3, two including initial filter area 1, filtering area 2, one It washes that area 5 is washed in area 4, three, filter cloth regeneration washes area 6, ardealite hopper 7 and discharge auger structure etc., it is newly grand to be specifically as follows Jiangsu The HDZP series rotary vacuum disk fiter (HDZP-L160-00) of company.Pulp tank, anterior reactor, extraction tank and turntable vacuum mistake The feed inlet of filter 25 is sequentially connected by pipeline, and multiple-grooved side by side configuration (6 or 9 slot structures can be used in anterior reactor and extraction tank Deng), ardealite hopper 7, phosphor-gypsum backwater processing system (being specifically as follows ardealite storage yard) and phosphor-gypsum backwater storage tank pass through Pipeline is sequentially connected for by isolated phosphor-gypsum backwaters such as wet row or dry-extraction methods, sour regurgitation slot 13 to pass through pipeline and pre-reaction Slot, phosphoric acid storage tank 10(can overflow connections) and diafiltration liquid/gas separator 12 connect, diafiltration liquid/gas separator 12 passes through pipeline and initial filter area 1 Filtrate (liquid and one wash area 3 washing lotion outlet connection, phosphoric acid separator 9 passes through the filtrate (liquid and phosphorus of pipeline and filtering area 2 Acid storage tank 10 connects.The three washing lotion imports for washing area 5 are connect by pipeline with heating water tank, and three wash the washing lotion outlet in area 5, three washing lotions The washing lotion import that separator 17, three washing lotion storage tanks 18 and two wash area 4 is sequentially connected by pipeline, and two wash the washing lotion outlet in area 4, two The washing lotion import that washing lotion separator 14, two washing lotion storage tanks 15 and one wash area 3 is sequentially connected by pipeline.Barometric condenser 20 into Port by pipeline and phosphoric acid separator 9, diafiltration liquid/gas separator 12, two washing lotion separators 14 and three washing lotion separators 17 gas Outlet connection, condensation-water drain are connect by pipeline with condensed water storage tank 21, and exhaust outlet is connect with vacuum pump 23.Vacuum pump 23 can connect progress gas-liquid separation by pipeline with discharge air separator 22.Phosphor-gypsum backwater storage tank and barometric condenser 20(retain Cooling tower can specifically be connect with the circulating slot of cold water tower bottom) cooling water inlet by piping connection to carry out heat exchange promotion The temperature of phosphor-gypsum backwater, cooling water outlet, neutralization reaction storage tank 26, the neutralization reaction slot 27, subsider of barometric condenser 20 28, filter press 29, filtrate storage tank 31 and heating water tank are sequentially connected by pipeline to realize and handle to phosphor-gypsum backwater To subacidity and the low phosphor-gypsum backwater of solid content, condensed water storage tank 21 is (main by the washing lotion import in pipeline and filter cloth regeneration area 6 Consider the supply of hot water storage tank) and the connection (more than needed) of hot water storage tank, the washing lotion outlet in filter cloth regeneration area 6 washed by pipeline with two Liquid storage tank 15 connects, and three washing lotion storage tanks 18 are connect by pipeline with sulfuric acid storage tank.
Specifically, referring to fig. 4, the rotary vacuum disk fiter 25 in the present embodiment is compared with phosphoric acid separator 9, diafiltration liquid/gas separator 12, two washing lotion separators 14 and three washing lotion separators, 17 height are to form drop.Phosphoric acid separator 9(is 7-11m away from ground level) Can be set on ground compared with phosphoric acid storage tank 10() high (surface) with formed drop and between can be connected by vertical straight tube.Diafiltration liquid Separator 9(is 7-11m away from ground level) compared with sour regurgitation slot 13 high (surface) with formed drop and between can be by vertical straight tube Connection.Two washing lotion separator 14(are 7-11m away from ground level) compared with two washing lotion storage tank 15 high (surface) with formed drop and it Between can be connected by vertical straight tube.Three washing lotion separator 17(are 7-11m away from ground level) compared with the height of three washing lotion storage tank 18 (on just Side) with formed drop and between can be connected by vertical straight tube.Barometric condenser 20(is 7-11m away from ground level) compared with condensed water Storage tank 21 high (surface) with formed drop and between can be connected by vertical straight tube.Sour regurgitation slot 13 and extraction tank in the present invention Between pipeline be equipped with sour regurgitation pump 11, the pipeline that two washing lotion storage tanks 15 and one wash between the washing lotion import in area 3 is equipped with two and washes Pump 16, three washing lotion storage tanks 18 and two pipelines washed between the cleaning solution import in area 4 are equipped with three and wash pump 19, condensed water storage tank 21 with Pipeline between hot water storage tank is equipped with condensate pump, and phosphoric acid storage tank 10 is by phosphoric acid discharge pump 8 to sending phosphoric acid outside.
Wherein, referring to fig. 4, the phosphoric acid storage tank 10 in the embodiment of the present invention, sour regurgitation slot 13, two washing lotion storage tanks 15 and three washing lotions Storage tank 18 includes sedimentation groove body (round groove body, for making liquid sedimentation) and storage groove body (round groove body).Settle groove body and Groove body is stored to be arranged side by side.The top of sedimentation groove body is equipped with feed inlet and its interior lower part is connected and be passed through with corresponding separator, Top is equipped with overflow port (close to storage groove body side) and is connected to storage groove body top, and bottom is equipped with sewage draining exit and (passes through pipeline It is connect with phosphoric acid geosyncline).It stores groove body bottom and is equipped with discharge port.Feed inlet on the sedimentation groove body of three washing lotion storage tanks 18 passes through pipe The liquid outlet of Lu Yusan washing lotion separator 17 connects, and storage groove body (the settable sewage draining exit in its bottom) is equipped with thief hatch and stirs It mixes device and is connect by pipeline with sulfuric acid storage tank.The feed inlet of the sedimentation groove body of two washing lotion storage tanks 15 passes through pipeline and filter cloth regeneration The washing lotion outlet in area 6 is connected with the liquid outlet of two washing lotion separators 14, and the liquid outlet of storage groove body is washed by pipeline with one The washing lotion import in area 3 connects.
Preferably, referring to fig. 2 with 7, Wet-process Phosphoric Acid Production system provided in an embodiment of the present invention further includes screenings collecting tank 32 and stock tank 33 again, the filter residue that the screenings collecting tank 32 is used to collect filter press 29 (can be collected by slag bucket and pass through technique Water, phosphor-gypsum backwater are rinsed) and its connect with stock tank 33 again by pipeline, the stock tank again 33 passes through pipeline and subsider 28 screenings outlet is connected with pulp tank.
Specifically, referring to Fig. 6 and 7, the neutralization reaction storage tank 26 in the present embodiment and the pipe between neutralization reaction slot 27 Road is equipped with to back water pump, and neutralization reaction slot 27 is connected in series by 4 reactive tanks, the import of every order reaction slot and outlet difference position Lower part thereon, the outlet of upper level and the import of next stage are respectively positioned on top or are respectively positioned on lower part.By limewash storage tank come Lime stone water is stored and adds, limewash storage tank is connect by pipeline with first order reactive tank.It is equipped with and stirs in neutralization reaction slot 27 Mix device, which is provided with heating jacket (be set to reactive tank outside, connect with steam pipe network) and/or heating coil (in reactive tank, It is connect with steam pipe network) for realizing heating, size is specially 80 m3/h of φ 4500mm*h4500mm(water return amount or so), The specification of blender in it is φ 1800mm, revolving speed 50r/min or so.Pipeline between neutralization reaction slot 27 and subsider 28 It is equipped with reaction material stock pump (flow 200m3The flow of/h or so, subsequent pump are matched with this pump).The slurry outlet of subsider 28 Set on its bottom (taper), clarified solution outlet is set on its side wall, and top is equipped with flocculant adding mouth for flocculation to be added Agent is connect by pipeline with the import of filter press 29.Pipeline between subsider 28 and filter press 29 is fed equipped with filters pressing Pump.Screenings collecting tank 32(geosyncline) it is set to subsider 28 and again between stock tank 33;Screenings collecting tank 32 is located under subsider 28 Side, interior to be equipped with blender, feed inlet is connect by pipeline with the slurry outlet of subsider 28, and discharge port passes through band screenings The pipeline of pump and stock tank 33(geosyncline again) it connect.
Further, referring to Fig. 7, the production system in the embodiment of the present invention further includes that filtrate collecting tank 30(is stored up compared with filtrate Slot 31 is small, is arranged close to filter press 29 for collecting filtrate), filtrate collecting tank 30 is set to filtrate (liquid and the filtrate of filter press 29 Between storage tank 31.Stock tank 33 and filtrate collecting tank 30 are high more again for filter press 29.Pipeline and mine that stock tank 33 passes through band stock pump again again Stock tank connection.Filtrate collecting tank 30 is connect by the pipeline with filtrate pump with filtrate storage tank 31.
Wherein, phosphoric acid separator 9 provided in an embodiment of the present invention, diafiltration liquid/gas separator 12, two washing lotion separators 14 and three Washing lotion separator 17 is gas-liquid separator.Vacuum pump 23 is water ring vacuum pump.Hot water storage tank be equipped with steam(-)coil and/ Or steam heating jacket.Neutralization reaction slot 26 is equipped with blender and steam(-)coil and/or steam heating jacket, then stock tank 33 Blender is equipped with screenings collecting tank 32.Filter press is common plate and frame filter press, and filter cloth aperture is 200-500 mesh.
The structures such as pump, valve and/or flowmeter are set as needed on pipeline between aforementioned each structure.
Embodiment 2
Embodiment 2 provides a kind of Wet-process Phosphoric Acid Production method, the Wet-process Phosphoric Acid Production system provided using embodiment 1, the party Method includes: that ore pulp is reacted with the sour regurgitation from filter device (in anterior reactor), after the reaction was completed again with the concentrated sulfuric acid into Row reaction (in extraction tank), is filtered to obtain phosphoric acid, sour regurgitation and ardealite, ardealite and flushing finally by filter device Liquid send phosphor-gypsum backwater processing system to handle to obtain phosphor-gypsum backwater.The one of filter device washes the washing lotion in area 3 and the filter in initial filter area 1 Liquid (being added or be added without phosphoric acid according to concentration) merges into sour regurgitation.The heat exchange of the barometric condenser 20 of phosphor-gypsum backwater and filter device (water temperature is improved in order to subsequent neutralization reaction, retain cooling tower) afterwards, neutralized reaction (in neutralization reaction slot 27), sedimentation The three of filter device is sent to wash the work of area 5 after (in subsider 28), filters pressing (in filter press 29) and heating (in heating water tank) For three wash water (P2O50.2% or so, pH value 6 or so), barometric condenser 20 collects phosphoric acid separator 9, diafiltration liquid/gas separator 12, two The gas of washing lotion separator 14 and three washing lotion separators 17 and condensation obtain condensed water (temperature is higher and purer), and condensed water is sent The filter cloth regeneration area 6 of filter device is used as filter cloth regeneration water.Sulfuric acid (specific concentration is 90-99%) is added simultaneously in three washing lotions for washing area 5 Adjusting to h 2 so 4 concentration is that 5.5-6.0%(is slightly higher compared with 5%, and the sulfuric acid concentration to guarantee a washing lotion equally has 5% or so Have preferable washing effect, it is found by the applicant that sulfuric acid concentration can prevent filter plate fouling at 5% or so in washing lotion) send filter device Two wash area 4 as two wash waters (5% sulfuric acid concentration 5.5-6.0% of P <, the concentration of other acidic materials washed less than 0.3%) to two Area 4 carries out scale removal can promote wash temperature simultaneously.The washing lotion that the washing lotion in filter cloth regeneration area 6 washes area 4 with two merges the area Hou Songyixi 3 As a wash water (6% sulfuric acid concentration of P < is 5% or so, to guarantee the washing effect for washing area 3 to one), filter cloth regeneration area 6 is washed Liquid can slightly reduce sulfuric acid concentration, increase wash temperature, increase washing lotion dosage.
Wherein, the neutralization reaction process in the embodiment of the present invention are as follows: limewash is added and adjusts the pH value of phosphor-gypsum backwater To 6.5-7.0.Infall process are as follows: be added organic polymer coargulator (being specifically as follows polyacrylamide), organic polymer wadding The usage amount of solidifying agent is the 0.05-2%, sedimentation time 0.5-6h of phosphor-gypsum backwater quality.Pressure-filtering process are as follows: use plate compression Machine carries out filters pressing, and filter cloth aperture is 200-500 mesh, and filters pressing pressure is 0.2-0.5MPa;Heating process are as follows: be heated to three wash waters 60 DEG C or more.
Further, after the screenings that the infall process in the embodiment of the present invention generates merges with the filter residue that filter process generates Adjusting (filtrate or phosphor-gypsum backwater or process water can be added) to density is 1.72-1.78g/cm3As ore pulp.
Further, the partial condensation Shui Song filter cloth regeneration area 6 in the embodiment of the present invention is used as filter cloth regeneration water, remaining cold Condensate with through filters pressing, treated that phosphor-gypsum backwater mixes, heats the area Hou Songsanxi 5 can reduce heat energy as three wash waters and disappear Consumption, is diluted phosphor-gypsum backwater.
Wherein, the volume ratio of the ore pulp in the embodiment of the present invention, sour regurgitation and the concentrated sulfuric acid is 77-83:115-125:35-40, 80-95 DEG C of reaction temperature, the density of ore pulp is 1.72-1.78g/cm3, it is 1.48-1.52g/ that sour regurgitation, which is reacted with ore pulp to density, cm3Afterwards with strong sulfuric acid response, the phosphoric acid concentration (mass percent concentration, rear same) of sour regurgitation is 14-16%, and the concentration of the concentrated sulfuric acid is 90-99%。
Wherein, two in the embodiment of the present invention wash the washing lotion in area 4 after two washing lotion separators 14 carry out gas-liquid separation with filter The washing lotion of cloth renewing zone 6 mixes, then physics sedimentation (in sedimentation groove body) obtains a wash water.Three wash the washing lotion in area 5 through three washing lotions point Gas-liquid separation is carried out from device 17, then physics sedimentation (in sedimentation groove body) mixes afterwards with sulfuric acid as two wash waters.One washes the washing lotion in area 3 With the filtrate in initial filter area 1 after diafiltration liquid/gas separator 12 carries out gas-liquid separation, then physics sedimentation (in sedimentation groove body) afterwards with or not It is mixed with the phosphoric acid that the filtering area 2 of filter device obtains as sour regurgitation.The filtrate of filtering area 2 carries out gas-liquid through phosphoric acid separator 9 After separation, then physics settles to obtain phosphoric acid.
The phosphoric acid concentration of production is 21-24%, and content of magnesium 0.6-1.4%, solid content is less than 5%(in terms of 48% phosphoric acid), sulfuric acid Radical ion is less than 4%.Meet Wet Processes of Phosphoric Acid requirement.In March, 2018 in May, 2019 does not carry out large repairs cleaning still to filter plate Energy normal use, the maintenance period of spray head extended to 80-85 days by 45-55 days.
The economic benefit of the patent is (in terms of 300,000 tons of phosphoric acid yield, rough calculation):
Product cost is reduced to 3097 yuan/ton (43-50 yuan/ton of profits) by 3105 yuan/ton, increases by 2,400,000/year of profit;Specifically, Water consumption is reduced to 1.71 tons of water/ton acid by 2.12 tons of water/ton acid, consumes quantity of steam by the near 2.08t/ tons of phosphorus of 2.20t/ tons of phosphoric acid The total phosphorus content of acid, ardealite is reduced to 1.44% by 1.51%;In terms of phosphorus ore, the yield of phosphorus pentoxide is promoted to by 93.1% 93.3%.The maintenance and cleaning for saving rotary vacuum disk fiter takes ten thousand yuan/year of 30-55 (when computing staff's working hour based on 200 yuan/day). Ten thousand tons/year of yield 1.2-1.3 are promoted, additional increase profit about 560,000.It is annual to increase profit 3,500,000 or so.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of Wet-process Phosphoric Acid Production method, which comprises ore pulp is reacted with the sour regurgitation from filter device, reaction It is reacted again with the concentrated sulfuric acid after the completion, is filtered to obtain phosphoric acid, sour regurgitation and ardealite, ardealite finally by filter device Phosphor-gypsum backwater processing system is sent to handle to obtain phosphor-gypsum backwater;The one of the filter device washes washing lotion and the initial filter area in area (3) (1) filtrate is sour regurgitation;It is characterized in that, after the heat exchange of the barometric condenser (20) of the phosphor-gypsum backwater and filter device, warp The three of filter device is sent to wash area (5) as three wash waters, the barometric condenser (20) after neutralization reaction, sedimentation, filters pressing and heating Collect the gas of phosphoric acid separator (9), diafiltration liquid/gas separator (12), two washing lotion separators (14) and three washing lotion separators (17) simultaneously Condensation obtains condensed water, and the condensed water send the filter cloth regeneration area (6) of filter device as filter cloth regeneration water;Described three wash area (5) it is that 5.5-6.0% send the two of filter device to wash area (4) as two to wash that washing lotion, which is added sulfuric acid and adjusts to h 2 so 4 concentration, Water;The washing lotion that the washing lotion of the filter cloth regeneration area (6) washes area (4) with two merges the area Hou Songyixi (3) as a wash water.
2. Wet-process Phosphoric Acid Production method according to claim 1, which is characterized in that the neutralization reaction process are as follows: be added Limewash adjusts the pH value of phosphor-gypsum backwater to 6.5-7.0;The infall process are as follows: organic polymer coargulator, institute is added The usage amount for stating organic polymer coargulator is the 0.05-2%, sedimentation time 0.5-6h of phosphor-gypsum backwater quality;The filters pressing Journey are as follows: filters pressing is carried out using plate and frame filter press, filter cloth aperture is 200-500 mesh;The heating process are as follows: be heated to three wash waters 60 DEG C or more.
3. Wet-process Phosphoric Acid Production method according to claim 2, which is characterized in that the screenings and filtering that infall process generates It is 1.72-1.78g/cm that the filter residue that process generates, which is adjusted after merging to density,3As ore pulp.
4. Wet-process Phosphoric Acid Production method according to claim 1, which is characterized in that partial condensation Shui Song filter cloth regeneration area (6) be used as filter cloth regeneration water, remaining condensed water with through filters pressing, treated that phosphor-gypsum backwater mixes, heats the area Hou Songsanxi (5) As three wash waters.
5. Wet-process Phosphoric Acid Production method according to claim 1, which is characterized in that the ore pulp, sour regurgitation and the concentrated sulfuric acid Volume ratio is 77-83:115-125:35-40, and the density of the ore pulp is 1.72-1.78g/cm3, the phosphoric acid concentration of the sour regurgitation For 14-16%, the concentration of the concentrated sulfuric acid is 90-99%.
6. Wet-process Phosphoric Acid Production method according to claim 1, which is characterized in that described two wash the washing lotion in area (4) through two Washing lotion separator (14) mixes after carrying out gas-liquid separation with the washing lotion of filter cloth regeneration area (6), then physics settles to obtain a wash water;Institute The washing lotion in the area Shu Sanxi (5) is mixed with sulfuric acid after carrying out gas-liquid separation, then physics sedimentation through three washing lotion separators (17) as two Wash water;Described one washes the filtrate of the washing lotion in area (3) and initial filter area (1) after diafiltration liquid/gas separator (12) carry out gas-liquid separation, then The phosphoric acid mixing that filtering area (2) after physics sedimentation with or without filter device obtains is as sour regurgitation;The filter of the filtering area (2) Liquid is after phosphoric acid separator (9) carry out gas-liquid separation, then physics settles to obtain phosphoric acid.
7. a kind of Wet-process Phosphoric Acid Production system, including pulp tank, anterior reactor, extraction tank, phosphor-gypsum backwater processing system, phosphorus stone Cream return water storage tank and filter device, the extraction tank are connect with sulfuric acid storage tank;
The filter device includes rotary vacuum disk fiter (25), phosphoric acid storage tank (10), phosphoric acid separator (9), the separation of diafiltration liquid Device (12), sour regurgitation slot (13), two washing lotion separators (14), two washing lotion storage tanks (15), three washing lotion separators (17), three washing lotion storage tanks (18), heating water tank, barometric condenser (20), vacuum pump (23) and condensed water storage tank (21), the rotary vacuum disk fiter (25) include initial filter area (1), filtering area (2), one wash area (3), two wash area (4), three wash area (5), filter cloth regeneration washes area (6) and phosphorus Gypsum hopper (7);
The pulp tank, anterior reactor, extraction tank and rotary vacuum disk fiter (25) feed inlet be sequentially connected by pipeline, institute It states ardealite hopper (7), phosphor-gypsum backwater processing system and phosphor-gypsum backwater storage tank to be sequentially connected by pipeline, the sour regurgitation slot (13) it is connect by pipeline with anterior reactor, phosphoric acid storage tank (10) and diafiltration liquid/gas separator (12), the diafiltration liquid/gas separator (12) it is connect by pipeline with the washing lotion outlet that the filtrate (liquid of initial filter area (1) and one wash area (3), the phosphoric acid separator (9) It is connect by pipeline with the filtrate (liquid of filtering area (2) and phosphoric acid storage tank (10);
The described three washing lotion imports for washing area (5) are connect by pipeline with heating water tank, and described three wash the washing lotion outlet of area (5), three The washing lotion import of washing lotion separator (17), three washing lotion storage tank (18) areas He Erxi (4) is sequentially connected by pipeline, and described two wash area (4) washing lotion outlet, two washing lotion separators (14), two washing lotion storage tank (15) areas He Yixi (3) washing lotion import by pipeline according to Secondary connection;
The air inlet of the barometric condenser (20) passes through pipeline and phosphoric acid separator (9), diafiltration liquid/gas separator (12), two washing lotions Separator (14) is connected with the gas vent of three washing lotion separators (17), and condensation-water drain passes through pipeline and condensed water storage tank (21) it connects, exhaust outlet is connect with vacuum pump (23);It is characterized in that,
The Wet-process Phosphoric Acid Production system further includes neutralization reaction storage tank (26), neutralization reaction slot (27), subsider (28), filters pressing The cooling water inlet of machine (29) and filtrate storage tank (31), the phosphor-gypsum backwater storage tank and barometric condenser (20) is connected by pipeline Connect, the cooling water outlet of the barometric condenser (20), neutralization reaction storage tank (26), neutralization reaction slot (27), subsider (28), Filter press (29), filtrate storage tank (31) and heating water tank are sequentially connected by pipeline, and the condensed water storage tank (21) passes through pipeline Connect with the washing lotion import of filter cloth regeneration area (6) and hot water storage tank, the washing lotion outlet of the filter cloth regeneration area (6) by pipeline with The connection of two washing lotion storage tanks (15), the three washing lotions storage tank (18) are connect by pipeline with sulfuric acid storage tank.
8. Wet-process Phosphoric Acid Production system according to claim 7, which is characterized in that the phosphoric acid storage tank (10), sour regurgitation slot (13), two washing lotion storage tanks (15) and three washing lotion storage tanks (18) include sedimentation groove body and storage groove body, the sedimentation groove body with deposit Storage tank body is arranged side by side;The top of the sedimentation groove body is equipped with feed inlet and is passed through its interior lower part, upper part be equipped with overflow port with The connection of groove body top is stored, bottom is equipped with sewage draining exit;The storage groove body bottom is equipped with discharge port;The three washing lotions storage tank (18) the feed inlet on sedimentation groove body is connect by pipeline with the liquid outlet of three washing lotion separators (17), and storage groove body is set There are thief hatch and blender and is connect by pipeline with sulfuric acid storage tank;The feed inlet of the sedimentation groove body of the two washing lotions storage tank (15) It is connect by pipeline with the liquid outlet of the washing lotion outlet of filter cloth regeneration area (6) and two washing lotion separators (14).
9. Wet-process Phosphoric Acid Production system according to claim 7, which is characterized in that the Wet-process Phosphoric Acid Production system is also wrapped Screenings collecting tank (32) and again stock tank (33) are included, the screenings collecting tank (32) is used to collect the filter residue of filter press (29) and it is logical It crosses pipeline to connect with stock tank again (33), the stock tank again (33) is connected by pipeline and the screenings of subsider (28) outlet and pulp tank It connects.
10. Wet-process Phosphoric Acid Production system according to claim 9, which is characterized in that the phosphoric acid separator (9), diafiltration Liquid/gas separator (12), two washing lotion separators (14) and three washing lotion separators (17) are gas-liquid separator;The vacuum pump (23) For water ring vacuum pump;The hot water storage tank is equipped with steam(-)coil and/or steam heating jacket;The neutralization reaction slot (26) blender and steam(-)coil and/or steam heating jacket, the stock tank again (33) and screenings collecting tank (32) are equipped with Equipped with blender.
CN201910851385.5A 2019-09-10 2019-09-10 A kind of Wet-process Phosphoric Acid Production method and production system Pending CN110510589A (en)

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Application publication date: 20191129