CN109761209A - A kind of production technology and its production equipment of ferric phosphate - Google Patents

A kind of production technology and its production equipment of ferric phosphate Download PDF

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Publication number
CN109761209A
CN109761209A CN201910169493.4A CN201910169493A CN109761209A CN 109761209 A CN109761209 A CN 109761209A CN 201910169493 A CN201910169493 A CN 201910169493A CN 109761209 A CN109761209 A CN 109761209A
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China
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iron
ferric phosphate
kettle
phosphate
washing
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CN201910169493.4A
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江文革
方东东
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Bochuang Hongyuan new material Co.,Ltd.
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Shenzhen Haina Baichuan Technology Co Ltd
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Abstract

The invention discloses a kind of production technology of ferric phosphate and its production equipments.The production technology of the ferric phosphate is synthesized including 1) ferrous solution；2) ferric phosphate synthesizes；3) it washs；4) washing lotion recycles；5) dry and agglomerating plant；6) it is pulverized and mixed packaging.Device structure used in the present invention is simple and convenient to operate, raw material sources are extensive, simple and easy to get and at low cost, is offered convenience to industrialized production；The technique strong applicability that the present invention limits, can be adapted to the raw material such as a variety of sources of iron, phosphorus source, oxidant；Waste water that production technology of the present invention generates etc. can the recycling and reusing after conventional treatment, realize that water resource recycles, recycle salinity in waste water and be used as raw material, the outer pollution discharging environmental risk of reduction, while reducing the cost of raw material.

Description

A kind of production technology and its production equipment of ferric phosphate
Technical field
The invention belongs to lithium battery material manufacturing technology fields, and in particular to a kind of production technology and its production of ferric phosphate Equipment.
Background technique
Ferric phosphate is to prepare one of main raw material(s) of lithium cell anode material of lithium iron phosphate.Lithium iron phosphate positive material is made For the critical material of lithium ion battery, with high security, it is at low cost, the service life is long the advantages that.Common ferric phosphate produces work at present Skill and equipment, the degree of automation is low, and production process generates a large amount of waste water, does not handle that effect on environment is big, and cost of sewage disposal is high, Equipment applicability is low, can not be adapted to various type product techniques.
Summary of the invention
For the above-mentioned problems in the prior art, the purpose of the present invention is to provide a kind of production technologies of ferric phosphate And its production equipment.
The production technology of a kind of ferric phosphate, it is characterised in that include the following steps:
1) ferrous solution synthesizes
Source of iron, phosphorus source, acid and pure water are added in ferrous solution consersion unit by feed inlet, in the case where reaction temperature is 30-90 DEG C Acidolysis reaction is carried out, is filtered after reaction, except magnetic, obtains ferrous solution, the specific steps are as follows:
1.1) respectively from phosphoric acid feeder, water feeder and other sour feeders put into source of iron dissolution kettle phosphoric acid, water and its Its acid, while the agitating device for opening source of iron dissolution kettle is stirred, and is mixed to form uniform acid solution；
1.2) it is passed through hot fluid in the heat exchanging interlayer on the outside of from hot fluid inlet to source of iron dissolution kettle, passes through the first temperature detector Stablize with the temperature of solution in the first solenoid valve monitoring source of iron dissolution kettle at 50 ~ 90 DEG C, it is then molten from source of iron feeder to source of iron It solves and puts into source of iron in kettle, while lasting stirring, come into full contact with source of iron and acid solution and reacted, maintaining reaction temperature is stablized 50 ~ 90 DEG C, after 1 ~ 3 hour reaction time, obtain ferrous solution；
1.3) open ferrous solution discharging pump ferrous solution obtained by step 1.2) is delivered in condenser, at the same from cold fluid inlet to It is passed through cold fluid in condenser, the ferrous solution flowed out out of condenser is monitored by second temperature detector and third solenoid valve Temperature is stablized at 40 ~ 60 DEG C, after the ferrous solution flowed out out of condenser passes sequentially through the first filter plant and removes chinaware, into iron In solution pans, the ferrous solution in ferrous solution pans is delivered in the second filter plant by unlatching ferrous solution filter pump to be carried out Then the ferrous solution without residue is discharged in filtering out of second filter plant；
2) ferric phosphate synthesizes
The ferrous solution of step 1.3) is added in ferric phosphate consersion unit, oxidant is added through oxidant inlet, is 30- in temperature PH value tune is added from pH adjusting agent entrance until ferrous ion is all oxidized to ferric ion in 70 DEG C of progress oxidation reactions Agent is saved, until pH is 1.0-2.5, obtains yellow or flaxen phosphate dihydrate iron slurry, the ferric phosphate slurry is warming up to 90-99 DEG C, reaction 1-4h carries out ferric phosphate transformation of crystal, and unformed ferric phosphate is converted into phosphate dihydrate iron crystal form, after the completion of transformation of crystal Slurry by yellow or it is faint yellow be converted into white or white powder, obtain ferric phosphate slurry, specifically:
2.1) ferrous solution containing ferrous ion is put into stills for air blowing, while the agitating device for opening stills for air blowing is stirred, Then oxidant is slowly put into stills for air blowing, the charging time of oxidant is 30 ~ 90 minutes, controls the temperature of solution in stills for air blowing ≤ 70 DEG C, after solution is without ferrous ion in detection stills for air blowing are spent, the ferrous solution after being aoxidized；
2.2) ferrous solution after stills for air blowing internal oxidition is pumped out by stills for air blowing discharging pump and is delivered in stillpot, it is heavy to start simultaneously at The agitating device of shallow lake kettle is stirred, and pH adjusting agent is then slowly put into stillpot, and the pH for controlling solution in stillpot exists Between 1.0 ~ 2.5, the charging time of pH adjusting agent is 30 ~ 90 minutes；
2.3) after the completion of the pH adjusting agent in step 2.2) feeds intake, the temperature of solution in stillpot is warming up to 90 ~ 95 DEG C, is carried out Ferric phosphate transformation of crystal reaction, reaction 1 ~ 4 hour after, by stillpot discharging pump by stillpot react after ferric phosphate mashing pump Out；
3) it washs
The ferric phosphate slurries filtration that step 2.3) is obtained, ferric phosphate filter cake are added in washing facility, and pure water adds through pure water entrance Enter, with pure water 3-10 times, temperature controls 10-50 DEG C, obtains washing lotion and product ferric phosphate filter cake, specific washing process is such as Under:
3.1) corresponding cleaning solution is put into every grade of washing kettle in advance, then filters ferric phosphate reaction solution through pre-filtering equipment Mother liquor and ferric phosphate filter cake raw material are obtained, mother liquor is sent to washing lotion processing unit to recycle ferric phosphate residue therein, the phosphorus Sour iron filter cake raw material, which is put into level-one washing kettle, to be followed by stirring and washing；
3.2) in level-one washing kettle after the completion of washing, the slurry after washing be transported to by-pass filtration equipment be obtained by filtration a wash water and One filter wash cake, a filter wash cake are put into second level washing kettle, while the slurry in second level washing kettle is passed through secondary filtration equipment Two wash waters being obtained by filtration are transported in level-one washing kettle, washing process and so on；Wherein a wash water is sent to washing lotion processing Device is to recycle ferric phosphate residue therein；
3.3) after the completion of the washing of most rear class washing kettle, most rear class is obtained by filtration in grade filter plant to the slurry conveying after washing to the end Water and most rear class filter cake, while filling into pure water into most rear class washing kettle and will most rear class water be transported in previous stage washing kettle, Carry out the continuous washing of ferric phosphate；Filter ferric phosphate filter cake is to be processed；
4) washing lotion recycles
The wash pools that step 3) obtains are added mouth from neutralizer and neutralizer are added, by washing lotion pH tune into washing lotion recovery system Section to 6.0-9.0, neutralization reaction obtains sediment, after filtering filtrate be added washing lotion recovery system be concentrated, obtain pure water and Strong brine, high-purity quick lime or white lime are added into strong brine, and pH value is adjusted to 10-12, obtain byproduct calcium sulfate and Alkali, alkali is sent after alkali outlet recycling to pH adjusting agent entrance enters pure water for adjusting pH value, water after pure water outlet flows out Entrance or feed inlet reuse, specifically include as follows:
4.1) pH is adjusted: ferric phosphate production waste water is added in neutralization chamber, neutralizer, while turn on agitator are slow added into, It is uniformly mixed neutralizer and waste water, the pH of waste water is adjusted to 6.0-9.0；
4.2) it filters: after the completion of pH is adjusted, waste water being passed through into the first filter plant, removes the precipitating generated in pH adjustment process；
4.3) it is concentrated: waste water being squeezed into Waste water concentrating equipment, isolates pure water, while obtaining strong brine；
4.4) alkali collection is handled: strong brine is squeezed into alkali collection kettle, turn on agitator, while quick lime or white lime is added, it will PH is adjusted to 10-12, obtains alkali collection liquid；
4.5) product recycles: alkali collection liquid being passed through the second filter plant, respectively obtains calcium sulfate and corresponding neutralizer；
5) dry and agglomerating plant
The ferric phosphate filter cake of step 3.3) is added in drying equipment and is dehydrated at 100-300 DEG C, is removed in filter cake A large amount of Free water obtains phosphate dihydrate iron powder, phosphate dihydrate iron is delivered to high-temperature sintering apparatus, at 400-800 DEG C Sintering time 2-8h removes the crystallization water in phosphate dihydrate iron, while carrying out transformation of crystal, obtains product anhydrous iron phosphate, has Body includes the following steps:
5.1) drying and dehydrating
Drier is added by dry feed device in the ferric phosphate filter cake being prepared, it is dry in the case where temperature sets 100-300 DEG C The Free water in filter cake is removed, ferric phosphate filter cake becomes phosphate dihydrate iron crude product, and controls Free water in phosphate dihydrate iron and containing Within amount 1%, the tail gas for carrying a small amount of phosphate dihydrate iron laden dust secretly enters drying, dedusting equipment at the top of drier and is handled, and removes Tail gas after dirt is to be processed, and phosphate dihydrate iron crude product is recycled and post-processed from drying, dedusting device bottom；
5.2) high temperature sintering
Agglomerating plant is added through sintering feeder in the phosphate dihydrate iron crude product that step 5.1) is obtained, and warm area is divided into agglomerating plant Three sections, first segment is warming-up section, and temperature of charge rises to set temperature by room temperature, and second segment is soaking zone, and third section is temperature descending section, Material is down to 70 DEG C hereinafter, molecular water removes in phosphate dihydrate iron in agglomerating plant by set temperature, while transformation of crystal obtains To anhydrous phosphoric acid iron product, the tail gas that when sintering generates enters sintering dust equipment at the top of agglomerating plant, is entrained with by tail gas Anhydrous phosphoric acid iron laden dust recycled from sintering dust device bottom, the tail gas after dedusting is to be processed；
5.3) vent gas treatment
The tail gas of step 5.1) and step 5.2) is all collected and enters water absorption tower, is sprayed in water absorption tower by shower water Leaching absorbs remaining dust, SO in tail gas2And SO3Gas, water enter back into alkali adsorption tower after absorbing, by spraying sig water, into One step absorbs the sour gas in tail gas, air and vapor the gaseous mixture emptying that alkali adsorption tower is handled, water absorption tower and alkali The wastewater reuse approach of absorb the bottom of the tower；
6) it is pulverized and mixed packaging
Anhydrous iron phosphate after step 5) high temperature sintering is delivered to the pulverizer being pulverized and mixed in device to crush, is crushed to Granular size is D50 < 3 μm, and the ferric phosphate that multiple batches crush is added batch mixer and is mixed into 2-8h, and product is being packed after mixing It is packed in equipment by specification.
A kind of production technology of the ferric phosphate, it is characterised in that source of iron in step 1) be iron powder, iron filings, scrap iron, It is one or more of in ferrous sulfate, ferric sulfate, ferrous oxide, iron oxide, frerrous chloride or iron chloride；Phosphorus source is phosphoric acid；Acid is One or more of sulfuric acid, phosphoric acid, hydrochloric acid, formic acid, acetic acid, citric acid, tartaric acid；Phosphoric acid concentration is 0- in gained ferrous solution 2.0mol/L, acid provide H+Concentration is 0-3.0mol/L, ferrous ion and iron concentration and be 1.0-2.0mol/L.
The production technology of a kind of ferric phosphate, it is characterised in that the oxidant in step 2 is hydrogen peroxide, peroxide second The molar ratio of acid, nitric acid, ammonium persulfate, one or more of mixtures in hypochlorous acid, oxidant and ferrous ion is 0.5- 1.5:1；The detection method that ferrous ion reaction is completed is Phen indicator method or permanganimetric method.
The production technology of a kind of ferric phosphate, it is characterised in that the pH adjusting agent in step 2 is pH greater than 4 Ammonium hydroxide, aqueous slkali or salting liquid；Alkali is sodium hydroxide or potassium hydroxide；Salt is sodium carbonate, sodium bicarbonate, sodium phosphate, phosphoric acid hydrogen Disodium, sodium dihydrogen phosphate, potassium carbonate, saleratus, potassium phosphate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate, ammonium phosphate, phosphoric acid hydrogen two Ammonium, ammonium dihydrogen phosphate, ammonium carbonate or ammonium hydrogen carbonate.
The production technology of a kind of ferric phosphate, it is characterised in that the pure water dosage in step 3) is 7-15 times of ferric phosphate Siccative amount weight.
The production technology of a kind of ferric phosphate, it is characterised in that the neutralizer in step 4) is sodium hydroxide, hydrogen-oxygen Change potassium, sodium carbonate, potassium carbonate or ammonium hydroxide；
A kind of production technology of the ferric phosphate, it is characterised in that washing lotion recovery system in step 4) be amberplex or Evaporating waste water concentrator, the evaporating waste water concentrator are MVR, triple effect evaporator or multi-effect evaporator；High-purity life Lime purity > 95%, fineness > 200 mesh；High-purity white lime > 98%, fineness > 200 mesh.
A kind of production technology of the ferric phosphate, it is characterised in that drying equipment in step 5) be flash distillation dryer, Atomizing drier or fluidized bed type drier, the high-temperature sintering apparatus are rotary furnace, roller furnace or pusher furnace；It obtains Water content≤1% in phosphate dihydrate iron powder.
The production technology of a kind of ferric phosphate, it is characterised in that batch mixer in step 6) is ribbon batch mixer, double Bore mixing machine or V-type batch mixer；Pulverizer is airslide disintegrating mill, mechanical crusher or twin rollers.
The process units of the ferric phosphate, it is characterised in that including sequentially connected ferrous solution consersion unit, ferric phosphate Consersion unit, drying equipment, high-temperature sintering apparatus, is pulverized and mixed device and packaging facilities, the ferrous solution reaction at washing facility Source of iron, phosphorus source, acid and pure water feed mouth are set in equipment, and ferric phosphate consersion unit is equipped with pH adjusting agent entrance, and washing is set Standby top is equipped with pure water entrance, washing lotion recovery system, and washing lotion recovery system is equipped with pure water outlet and alkali exports, the pure water outlet The feed inlet of ferrous solution consersion unit is connected, alkali outlet is connected with pH adjusting agent entrance.
Specifically, the ferrous solution consersion unit includes the source of iron dissolution kettle for having agitating device, source of iron feeder, acid solution Feeding device, ferrous solution discharging pump, condenser, recycling precipitate device, the first temperature detection being set in source of iron dissolution kettle Device and the heat exchanging interlayer being socketed on the outside of source of iron dissolution kettle, the heat exchanging interlayer two sides respectively piping connection have hot fluid inlet and Hot fluid outlet ports, pipeline between hot fluid inlet and heat exchanging interlayer are equipped with the first solenoid valve, first solenoid valve and the The connection of one temperature detector signal is fed back and is controlled to detect the temperature of solution in source of iron dissolution kettle by the first temperature detector Make the opening size of the first solenoid valve；The source of iron feeder and acid solution feeding device respectively with source of iron dissolution kettle piping connection, Source of iron dissolution kettle bottom discharge port and ferrous solution discharging pump, condenser and recycling precipitate device successively piping connection；The iron It is additionally provided with blow-down pipe and first pressure measuring appliance at the top of the dissolution kettle of source, is additionally provided in the source of iron dissolution kettle for monitoring liquid level Liquid level measurer；The source of iron feeder includes source of iron feed bin and source of iron feeder, and source of iron feed bin passes through source of iron feeder and iron Source dissolution kettle piping connection；Acid solution feeding device includes feeding respectively with the phosphoric acid feeder of source of iron dissolution kettle piping connection, water Device and other sour feeders, the pipeline between the phosphoric acid feeder, water feeder and other sour feeders and source of iron dissolution kettle On be respectively arranged with volume control device system, the volume control device system includes flow detector and second solenoid valve, Flow detector is connect with second solenoid valve signal；The second temperature is provided on pipeline between condenser and recycling precipitate device Spend detector and second pressure measuring appliance；Piping connection has cold fluid inlet and cold fluid outlet respectively for the condenser two sides, Third solenoid valve is provided on pipeline between cold fluid inlet and condenser；The second temperature detector and third solenoid valve Signal connection feedbacks and controls third electricity with the temperature of the ferrous solution flowed out by the detection of second temperature detector from condenser The opening size of magnet valve；The recycling precipitate device include the first filter plant and with the first filter plant piping connection Except chinaware, first filter plant is plate frame filter, bag filter, centrifugal type filter or candle filter, institute State the first filter plant inlet and condenser liquid outlet piping connection；The recycling precipitate device further includes among ferrous solution Tank, ferrous solution filter pump and the second filter plant, second filter plant are plate frame filter, bag filter, centrifugation Formula filter or candle filter, at the top of ferrous solution pans inlet with remove chinaware liquid outlet piping connection, among ferrous solution Pot bottom liquid outlet passes through ferrous solution filter pump and the second filter plant piping connection.
The ferric phosphate consersion unit includes stills for air blowing, the stillpot with agitating device, iron with agitating device Solution feeding device, oxidant feed device, pH adjusting agent feeding device, stills for air blowing discharging pump and stillpot discharging pump, iron are molten Liquid feeding device and oxidant feed device connect with stills for air blowing piping connection, pH adjusting agent feeding device and stillpot pipeline respectively It connects；Stills for air blowing are equipped on the outside of the first temperature meter and the stills for air blowing and are socketed with the first heat exchanging interlayer, the first heat exchanging interlayer Piping connection has a hot fluid inlet and hot fluid outlet ports respectively for two sides, on the pipeline between hot fluid inlet and the first heat exchanging interlayer It is provided with the first solenoid valve, first solenoid valve is connect with the first temperature meter signal, to pass through the first temperature meter The temperature for detecting solution in stills for air blowing, feedbacks and controls the opening size of the first solenoid valve；Stills for air blowing bottom discharge port passes through oxygen Change kettle discharging pump and stillpot top feed mouth piping connection, stillpot bottom discharge port and stillpot discharging pump piping connection, The ferric phosphate suspension after reacting in stillpot to be pumped out；The first liquid level detector and the first pressure are additionally provided on the stills for air blowing Force detector, stillpot are equipped with the second liquid level detector and second pressure detector；The second temperature is additionally provided on the stillpot It is socketed with the second heat exchanging interlayer on the outside of degree measuring appliance and the stillpot, piping connection has heat source respectively for the second heat exchanging interlayer two sides Import and thermal source outlet are provided with second solenoid valve, second electricity on the pipeline between heat source import and the second heat exchanging interlayer Magnet valve is connect with second temperature measuring appliance signal, to detect the temperature of solution in stillpot, feedback by second temperature measuring appliance And the opening size of second solenoid valve is controlled, the ferrous solution feeding device, oxidant feed device and pH adjusting agent charging dress It sets and respectively includes ferrous solution feeder, oxidant feed device and pH adjusting agent feeder, ferrous solution feeder and oxidant feed Device respectively with stills for air blowing piping connection, pH adjusting agent feeder and stillpot piping connection；The ferrous solution feeder and oxidation Stream is provided on pipeline on pipeline between agent feeder and stills for air blowing and between pH adjusting agent feeder and stillpot Amount control device system, the volume control device system include flow detector and third solenoid valve, flow detector and Three solenoid signals connection, to feedback and control the opening size of third solenoid valve by flow detector detection flows.
Washing setting include the spaced washing kettle of several grades and filter plant further include washing lotion processing unit and Pre-filtering equipment, the washing kettle is identical with the series of filter plant, and from left to right starts, the grade of washing kettle and filter plant Number is sequentially increased, and the first liquid level measurer is provided on every grade of washing kettle, the bottom liquid outlet of every grade of washing kettle passes through The inlet piping connection of discharging pump and filter plant at the same level；The ferric phosphate that the filter cake import investment of level-one washing kettle needs to wash The filter cake import of filter cake, other washing kettles except level-one washing kettle is connected with the filtered solid outlet of previous stage filter plant； The filtrate import of most rear class washing kettle and pure water holding vessel are by piping connection, the filter of other washing kettles except most rear class washing kettle Liquid import is connect with the filtrate (liquid pipeline of rear stage filter plant；Wherein level-one is discharged in the filtrate (liquid of by-pass filtration equipment Wash filtered fluid, the phosphoric acid iron product that the filtered solid outlet discharge washing of most rear class filter plant is completed；Most rear class washing kettle with it is pure The filtrate import of other washing kettles on pipeline between water store tank and except most rear class washing kettle is set with rear stage filtering Be provided with the first solenoid valve on pipeline between standby filtrate (liquid, each first solenoid valve on corresponding washing kettle The connection of one liquid level measurer signal feedbacks and controls phase to detect the liquid level in washing kettle by the first liquid level measurer The opening size for answering the first solenoid valve is automatically maintained at the liquid level in washing kettle in setting range；The washing lotion processing Device includes the wash pools slot, washing lotion discharging pump and washing lotion filter of successively piping connection, the filter of the by-pass filtration equipment Liquid outlet and wash pools slot piping connection put into level-one washing filtered fluid in wash pools slot；The wash pools slot On be provided with the second liquid level measurer, second solenoid valve, institute are provided on the pipeline between washing lotion discharging pump and washing lotion filter It states second solenoid valve to connect with the second liquid level measurer signal, to detect the liquid in wash pools slot by the second liquid level measurer Position height, feedbacks and controls the opening size of second solenoid valve；The phosphorus that the inlet investment of the pre-filtering equipment needs to filter Sour iron reaction solution, the filtrate (liquid and wash pools slot piping connection of pre-filtering equipment, ferric phosphate reaction solution is set through pre-filtering The mother liquor obtained after standby filtering is collected into wash pools slot；The filter cake of the filtered solid outlet of pre-filtering equipment and level-one washing kettle into Mouth is connected, and the ferric phosphate filter cake that the needs being obtained by filtration through pre-filtering equipment wash is put into level-one washing kettle.
The washing lotion recovery system includes that from left to right successively the neutralization chamber of piping connection, the first filter plant, waste water are dense Contracting equipment, alkali collection kettle and the second filter plant；The Waste water concentrating equipment is that ion exchange film device and evaporating waste water are concentrated One of equipment or two kinds；Pipeline between the neutralization chamber and the first filter plant is equipped with neutralization chamber discharging pump, institute It states the pipeline between Waste water concentrating equipment and alkali collection kettle and is equipped with strong brine discharging pump, the alkali collection kettle is set with the second filtering Pipeline between standby is equipped with alkali collection kettle discharging pump；The neutralization chamber is equipped with neutralization chamber Liquid level instrument and neutralization chamber pH It is worth control instrument, the alkali collection kettle is equipped with alkali collection kettle liquid position control instrument and alkali collection kettle pH value control instrument.
The drying and sintering device, including drier, agglomerating plant, water absorption tower and alkali adsorption tower, it is characterised in that Drier is connect with dry feed device, and ferric phosphate filter cake enters drier by dry feed device, and the connection of drier top exit is dry Dry cleaner, outlet at bottom connect agglomerating plant by sintering feeder, and agglomerating plant top exit connection sintering dust is set Standby, the drying, dedusting device bottom is exported equipped with phosphate dihydrate iron laden dust, at the top of drying, dedusting equipment and sintering dust equipment Offgas outlet after being respectively equipped with dedusting, two offgas outlets are all connected with water absorb the bottom of the tower feed inlet, and water absorption tower top is set There is deionized water import, alkali adsorption tower top is equipped with 1.0-5.0w% sig water Inlet water, and gas outlet connection alkali is inhaled at the top of absorption tower Tower bottom feed inlet is received, water absorption tower and alkali adsorption tower bottom are equipped with waste water discharge opening.
By using above-mentioned technology, compared with prior art, beneficial effects of the present invention are as follows:
1) raw material sources of the present invention are extensive, simple and easy to get and at low cost, offer convenience to industrialized production；
2) the technique strong applicability that the present invention limits, can be adapted to the raw material such as a variety of sources of iron, phosphorus source, oxidant；The present invention is raw Waste water etc. that production. art generates can the recycling and reusing after conventional treatment, realize that water resource recycles, recycle salinity in waste water As raw material, outer pollution discharging environmental risk is reduced, while reducing the cost of raw material.
Detailed description of the invention
Fig. 1 is production technological process of the invention；
Fig. 2 is ferrous solution consersion unit structural schematic diagram of the invention；
Fig. 3 is the structural schematic diagram of ferric phosphate consersion unit of the invention；
Fig. 4 is the structural schematic diagram of ferric phosphate washing facility of the present invention；
Fig. 5 is the structural schematic diagram of drying and sintering equipment of the present invention；
Fig. 6 is the structural schematic diagram of washing lotion recovery system of the present invention.
In figure: 01- ferrous solution consersion unit, 02- ferric phosphate consersion unit, 03- washing facility, 04- drying and sintering device, 05- is pulverized and mixed device, 06- packaging facilities, 07- washing lotion recovery system, 08- pure water entrance, 09-pH value regulator entrance, The feed(raw material)inlet 010-, 011- oxidant inlet, the outlet of 012- alkali, 013- pure water outlet, 014- neutralizer entrance, 015- high temperature are burnt Tie equipment；
11- source of iron dissolution kettle, 12- condenser, the first filter plant of 13-, 14- remove chinaware, 15- ferrous solution pans, 16- second Filter plant, 17- ferrous solution discharging pump, 18- ferrous solution filter pump, 19- blow-down pipe, 110- source of iron feeder, 111- source of iron material Storehouse, 112- hot fluid inlet, 113- hot fluid outlet ports, 114- cold fluid inlet, 115- cold fluid outlet, the inspection of the first temperature of 116- Survey device, 117- fluid level measuring instrument, 118- first pressure measuring appliance, 119- second temperature detector, 120- second pressure measuring appliance, 121- Heat exchange jacekt, 122- flow detector, the first solenoid valve of 123-, 124- second solenoid valve, 125- third solenoid valve；
21- stills for air blowing, 22- stillpot, 23- stills for air blowing discharging pump, 24- stillpot discharging pump, 25- flow detector, 26- electromagnetism Valve III, the first temperature meter of 27-, 28- first pressure detector, the first liquid level detector of 29-, 210- solenoid valve II, 211- Second temperature measuring appliance, 212- second pressure detector, the second liquid level detector of 213-, 214- hot fluid inlet, 215- hot-fluid Body outlet, 216- heat source import, 217- thermal source outlet, the first heat exchanging interlayer of 218-, the second heat exchanging interlayer of 219-, 220- solenoid valve Ⅰ；
31- level-one washing kettle, 32- by-pass filtration equipment, 33- washing kettle discharging pump, the first liquid level measurer of 34-, 35- solenoid valve I, 36- wash pools slot, 37- washing lotion discharging pump, 38- washing lotion filter, 39- pre-filtering equipment, the second liquid level measurer of 310-, 311- solenoid valve II, n- most rear class washing kettle, N- most rear class filter plant；
41- drier；42- is sintered kettle；43- water absorption tower；44- alkali adsorption tower；45- dry feed device；46- drying, dedusting is set It is standby；47- is sintered feeder；48- sintering dust equipment；49- dries air-introduced machine；410- sintering wind fan；411- water absorption tower is followed Ring pump；412- alkali adsorption tower circulating pump；413- water absorbing tower liquid-level control instrument；414- alkali adsorption tower Liquid level instrument； 415- sintering temperature control instrument；
71- neutralization chamber, 72- Waste water concentrating equipment, 73- alkali collection kettle, the second filter of 74-, 75- neutralization chamber discharging pump, 76- are dense Salt water discharging pump, 77- alkali collection kettle discharging pump, 78- neutralization chamber Liquid level instrument, 79- alkali collection kettle liquid position control instrument, 710- neutralization chamber pH value control instrument, 711- alkali collection kettle pH value control instrument, 712- first filter.
Specific embodiment
Below in conjunction with Figure of description and embodiment, the invention will be further described, but protection scope of the present invention is simultaneously It is not limited only to this:
As shown in Figure 1, the process units of ferric phosphate of the invention, including sequentially connected ferrous solution consersion unit 01, ferric phosphate Consersion unit 02, drying and sintering device 04, high-temperature sintering apparatus 015, is pulverized and mixed device 05 and packaging facilities at washing facility 03 06, feed(raw material)inlet 010 of the setting for progress such as source of iron, phosphorus source, acid and pure water, ferric phosphate on the ferrous solution consersion unit 01 Consersion unit 02 is equipped with pH adjusting agent entrance 09, is equipped with pure water entrance 08, washing lotion recovery system 07 at the top of washing facility 03 Equipped with neutralizer entrance 014, pure water outlet 013 and alkali outlet 012, the pure water outlet 013 connects ferrous solution consersion unit 01 Feed(raw material)inlet 010 or the top of washing facility 03 pure water entrance 08,012 connection pH adjusting agent entrance 09 of alkali outlet.
The dehydration equipment is amberplex or evaporating waste water concentrator；High-purity quick lime purity > 95%, Fineness > 200 mesh；High-purity white lime > 98%, fineness > 200 mesh；Drying and sintering device 04 is flash distillation dryer, atomizing Drier or fluidized bed type drier, the high-temperature sintering apparatus are rotary furnace, roller furnace or pusher furnace；Two obtained water phosphorus Water content≤1% in sour iron powder；Batch mixer is ribbon batch mixer, double-cone mixer or V-type batch mixer；Pulverizer is air-flow powder Broken machine, mechanical crusher or twin rollers；
As shown in Fig. 2, ferrous solution consersion unit 01 of the invention includes that source of iron dissolution kettle 11, source of iron with agitating device are fed Device, ferrous solution discharging pump 17, condenser 12, recycling precipitate device, is set in source of iron dissolution kettle 11 acid solution feeding device First temperature detector 116 and the Heat exchange jacekt 121 for being set in 11 outside of source of iron dissolution kettle.It is equipped at the top of the source of iron dissolution kettle 11 Blow-down pipe 19 and first pressure measuring appliance 118(for monitoring 11 internal pressure of source of iron dissolution kettle work as the exceeded then alarm of pressure), Source of iron dissolution kettle 11 is equipped with the fluid level measuring instrument 117 for monitoring liquid level；Piping connection has respectively for 121 two sides of Heat exchange jacekt Hot fluid inlet 112 and hot fluid outlet ports 113, the pipeline between hot fluid inlet 112 and Heat exchange jacekt 121 are equipped with the first electromagnetism Valve 123, first solenoid valve 123 are connect with 116 signal of the first temperature detector, are detected by the first temperature detector 116 The temperature of solution in source of iron dissolution kettle 11 controls the opening size of the first solenoid valve 123 according to the detection temperature being timely fed back to； The source of iron feeder and acid solution feeding device respectively with 11 piping connection of source of iron dissolution kettle, 11 bottom discharge port of source of iron dissolution kettle With ferrous solution discharging pump 17, condenser 12 and recycling precipitate device successively piping connection.Condenser 2 and recycling precipitate device Between pipeline on be provided with second temperature detector 119 and second pressure measuring appliance 120；It manages respectively 12 two sides of condenser Road is connected with cold fluid inlet 114 and cold fluid outlet 115, is arranged on the pipeline between cold fluid inlet 114 and condenser 12 There is third solenoid valve 125；The second temperature detector 119 is connect with 125 signal of third solenoid valve, to be examined by second temperature The temperature that device 119 detects the ferrous solution flowed out from condenser 12 is surveyed, the opening size of third solenoid valve 125 is feedbacked and controlled.
The source of iron feeder includes source of iron feed bin 111 and source of iron feeder 110, and source of iron feed bin 111 is fed by source of iron Device 110 and 11 piping connection of source of iron dissolution kettle, put into the source of iron in source of iron feed bin 111 from there through source of iron feeder 110 In source of iron dissolution kettle 11 (when source of iron is solid, source of iron feeder 110 can select feed screw)；
Acid solution feeding device include respectively with the phosphoric acid feeder of 11 piping connection of source of iron dissolution kettle, water feeder and it is other acid into Glassware is respectively set on the pipeline between the phosphoric acid feeder, water feeder and other sour feeders and source of iron dissolution kettle 11 There is volume control device system, the volume control device system includes flow detector 122 and second solenoid valve 124, flow Detector 122 is connect with 124 signal of second solenoid valve, and flow detector 122 is monitored the flow of substance and feeds back to Two solenoid valves 124 control the opening size of second solenoid valve 124, thus can control respectively and put into original in source of iron dissolution kettle 11 The flow of material.
The recycling precipitate device includes the first filter plant 13 of successively piping connection, except chinaware 14, among solution Tank 15, ferrous solution filter pump 18 and the second filter plant 16, the inlet of the first filter plant 13 and the liquid outlet of condenser 12 Piping connection, the first filter plant 13 and the second filter plant 16 can be independently selected from plate frame filter, bag type filtering Device, centrifugal type filter or candle filter.
As shown in figure 3, ferric phosphate consersion unit 02 of the invention, including with agitating device stills for air blowing 21, with stirring Mix stillpot 22, ferrous solution feeding device, oxidant feed device, pH adjusting agent feeding device, the stills for air blowing discharging pump of device 23 and stillpot discharging pump 24, the first liquid level detector 29, first pressure detector 28 and the first temperature are additionally provided on stills for air blowing 21 Measuring appliance 27 is spent, stillpot 22 is equipped with the second liquid level detector 213, second pressure detector 212 and second temperature measuring appliance 211；
The first heat exchanging interlayer 218 is socketed on the outside of the stills for air blowing 21, piping connection has heat to 218 two sides of the first heat exchanging interlayer respectively Fluid inlet 214 and hot fluid outlet ports 215 are provided with electricity on the pipeline between hot fluid inlet 214 and the first heat exchanging interlayer 218 Magnet valve I 220, the solenoid valve I 220 are connect with 27 signal of the first temperature meter, to be detected by the first temperature meter 27 The temperature of solution in stills for air blowing 21, feedbacks and controls the opening size of solenoid valve I；21 bottom discharge port of stills for air blowing passes through stills for air blowing 22 top feed mouth piping connection of discharging pump 23 and stillpot, 22 bottom discharge port of stillpot and 24 pipeline of stillpot discharging pump connect It connects, the ferric phosphate suspension after reacting in stillpot 22 is pumped out；The second heat exchanging interlayer is socketed on the outside of the stillpot 22 219, piping connection has heat source import 216 and thermal source outlet 217, heat source import 216 and to 219 two sides of the second heat exchanging interlayer respectively Solenoid valve II 210, the solenoid valve II 210 and second temperature measuring appliance 211 are provided on pipeline between two heat exchanging interlayers 219 Signal connection feedbacks and controls solenoid valve II to detect the temperature of solution in stillpot 22 by second temperature measuring appliance 211 210 opening size.
Ferrous solution feeding device, oxidant feed device and pH adjusting agent feeding device respectively include ferrous solution feeder, Oxidant feed device and pH adjusting agent feeder, ferrous solution feeder and oxidant feed device connect with 21 pipeline of stills for air blowing respectively It connects, pH adjusting agent feeder and 22 piping connection of stillpot；The ferrous solution feeder and oxidant feed device and stills for air blowing 21 Between pipeline on and the pipeline between pH adjusting agent feeder and stillpot 22 on be provided with volume control device system, The volume control device system includes flow detector 25 and solenoid valve III 26, flow detector 25 and III 26 signal of solenoid valve Connection, to feedback and control the opening size of solenoid valve III 26 by 25 detection flows of flow detector.Ferrous solution feeder, Feed pump can be used in oxidant feed device and pH adjusting agent feeder.
As shown in figure 4, washing facility of the invention includes the spaced washing kettle of several grades and filter plant, further include Washing lotion processing unit and pre-filtering equipment 39, the washing kettle is identical with the series of filter plant, and from left to right starts, washing The series of kettle and filter plant is sequentially increased, and the first liquid level measurer 34, every grade of washing kettle are provided on every grade of washing kettle Bottom liquid outlet pass through the inlet piping connection of washing kettle discharging pump 33 and filter plant at the same level；Level-one washing kettle 31 Filter cake import puts into the ferric phosphate filter cake for needing to wash, and the filter cake import of other washing kettles except level-one washing kettle 31 is with before The filtered solid outlet of by-pass filtration equipment is connected；The filtrate import of most rear class washing kettle n and pure water holding vessel are by piping connection, most The filtrate import of other washing kettles except rear class washing kettle n is connect with the filtrate (liquid pipeline of rear stage filter plant；Its The filtrate (liquid discharge level-one of middle by-pass filtration equipment 32 washs filtered fluid, and the filtered solid outlet discharge of most rear class filter plant N is washed Wash the phosphoric acid iron product of completion；On pipeline between most rear class washing kettle n and pure water holding vessel and except most rear class washing kettle n The filtrate import of other washing kettles and the filtrate (liquid of rear stage filter plant between pipeline on be provided with solenoid valve I 35, each solenoid valve I 35 is connect with 34 signal of the first liquid level measurer on corresponding washing kettle, to pass through the first level gauging Device 34 detects the liquid level in washing kettle, feedbacks and controls the opening size of corresponding solenoid valve I 35, makes the liquid level in washing kettle Highly automated maintenance is within the set range；The washing lotion processing unit includes the wash pools slot 36 of successively piping connection, washing lotion Discharging pump 37 and washing lotion filter 38, the filtrate (liquid and 36 piping connection of wash pools slot of the by-pass filtration equipment 32 will Level-one washing filtered fluid is put into wash pools slot 36；The second liquid level measurer 310 is provided on the wash pools slot 36, Solenoid valve II 311, the solenoid valve II 311 and second are provided on pipeline between washing lotion discharging pump 37 and washing lotion filter 38 The connection of 310 signal of liquid level measurer, to detect the liquid level in wash pools slot 36 by the second liquid level measurer 310, instead Present and control the opening size of solenoid valve II 311；The ferric phosphate that the inlet investment of the pre-filtering equipment 39 needs to filter is anti- Answer liquid, the filtrate (liquid and 36 piping connection of wash pools slot of pre-filtering equipment 39, by ferric phosphate reaction solution through pre-filtering equipment The mother liquor obtained after 39 filterings is collected into wash pools slot 36；The filtered solid outlet of pre-filtering equipment 39 and level-one washing kettle 31 Filter cake import is connected, and the ferric phosphate filter cake that the needs being obtained by filtration through pre-filtering equipment 39 wash is put into level-one washing kettle In 31.
As shown in figure 5, drying and sintering device of the invention, including drier 41, sintering kettle 42, water absorption tower 43 and alkali are inhaled Tower 44 is received, drier 41 is connect with dry feed device 45, and ferric phosphate filter cake enters drier 41, drier by dry feed device 45 41 top exits connect drying, dedusting equipment 46, and outlet at bottom is pushed up by the sintering connection sintering kettle 42 of feeder 47, sintering kettle 42 Portion outlet connection sintering dust equipment 48,46 bottom of drying, dedusting equipment are exported equipped with phosphate dihydrate iron laden dust, and drying removes The offgas outlet after dedusting is equipped at the top of dirt equipment 46 and sintering dust equipment 48, two offgas outlets are all connected with water absorption tower 43 Bottom feed inlet, 43 top of water absorption tower be equipped with deionized water import, 44 top of alkali adsorption tower be equipped with 1.0-5.0w% sig water into Saliva, 43 top gas outlet of absorption tower connect 44 bottom feed inlet of alkali adsorption tower, and water absorption tower 43 and 44 bottom of alkali adsorption tower are equal Equipped with waste water discharge opening；
As shown, can smoothly enter into successor devices for the ease of tail gas, the present invention is in 46 top offgas outlet of drying, dedusting equipment It is equipped with dry air-introduced machine 49 between water absorption tower 43, is set between 48 top offgas outlet of sintering dust equipment and water absorption tower 43 There is sintering wind fan 410.
In order to improve tail gas absorption effect, the present invention is useless in the 43 top deionized water import of water absorption tower and its bottom By piping connection between water outlet, the circulatory system is constituted, circulatory system pipeline is equipped with water absorption tower circulating pump 411, leads to It crosses water absorption tower circulating pump 411 and circulation fluid is subjected to cyclic absorption, improve assimilation effect；44 top sig water import of alkali adsorption tower By piping connection between its bottom waste water discharge opening, the circulatory system is constituted, circulatory system pipeline is followed equipped with alkali adsorption tower Ring pump 412.
43 side of water absorption tower is equipped with water absorbing tower liquid-level control instrument 413, on the pipeline of bottom waste water discharge opening Equipped with solenoid valve, water absorbing tower liquid-level control instrument 413 is connected with corresponding solenoid valve；44 side of alkali adsorption tower is equipped with Alkali absorption Tower Liquid level instrument 414, the pipeline of bottom waste water discharge opening are equipped with solenoid valve, alkali adsorption tower Liquid level instrument 414 with Corresponding solenoid valve connection.
As shown in fig. 6, washing lotion recovery system 07 of the invention includes the from left to right successively neutralization chamber 71 of piping connection, the One filter 712, Waste water concentrating equipment 72, alkali collection kettle 73 and the second filter 74.Waste water concentrating equipment 72 is ion exchange One of film device and evaporating waste water concentrator or two kinds；Pipe between the neutralization chamber 71 and first filter 712 Road is equipped with neutralization chamber discharging pump 75, and the pipeline between Waste water concentrating equipment 72 and alkali collection kettle 73 is equipped with strong brine discharging pump 76, the pipeline between alkali collection kettle 73 and the second filter 74 is equipped with alkali collection kettle discharging pump 77.During neutralization chamber 71 is equipped with With tank liquor position control instrument 78 and neutralization chamber pH value control instrument 710, alkali collection kettle 73 is equipped with alkali collection kettle liquid level controller Table 79 and alkali collection kettle pH value control instrument 711；
The neutralization chamber 71 is for adding neutralizer, so as to adjust wastewater pH to 6.0-9.0.Waste water concentrating equipment 72 is for being concentrated Waste water, recovery section pure water.Alkali collection kettle 73 precipitates acid ion, generates lye for adding quick lime or white lime.Second Filter 74 recycles lye for filtering acid group sediment.
As shown in figures 1 to 6, the process units based on ferric phosphate of the invention, production technology include the following steps:
1) ferrous solution synthesizes
Source of iron, phosphorus source, acid and pure water are added in ferrous solution consersion unit 01 by feed(raw material)inlet 010, are 30- in reaction temperature Acidolysis reaction is carried out at 90 DEG C, is filtered and is removed magnetic after reaction, obtain ferrous solution, the specific steps are as follows:
1.1) respectively from phosphoric acid feeder, water feeder and other sour feeders put into source of iron dissolution kettle 11 phosphoric acid, water and Other acid, while the agitating device for opening source of iron dissolution kettle is stirred, are mixed to form uniform acid solution, other acid be sulfuric acid, One of phosphoric acid, hydrochloric acid, formic acid, acetic acid, citric acid, tartaric acid are several；In the acid solution that step 1) is mixed to form, phosphoric acid Concentration 0-2mol/L, the H+ concentration that other acid provide is in 0-3mol/L；
1.2) it is passed through hot fluid into the Heat exchange jacekt 121 in 11 outside of source of iron dissolution kettle from hot fluid inlet 112, passes through the first temperature The temperature of solution is stablized at 50 ~ 90 DEG C, then by source of iron in detector 116 and the first solenoid valve 123 monitoring source of iron dissolution kettle 11 Feeder 110 puts into source of iron, while lasting stirring into source of iron dissolution kettle 11, comes into full contact with source of iron and acid solution and is reacted, Maintaining reaction temperature is stablized after 50 ~ 90 DEG C, 1 ~ 3 hour reaction time, and ferrous solution is obtained；
1.3) open ferrous solution discharging pump 17 ferrous solution obtained by step 1.2) is delivered in condenser 12, at the same by cold fluid into Mouth 114 is passed through cold fluid into condenser 12, is monitored by second temperature detector 119 and third solenoid valve 125 from condenser The temperature of the ferrous solution flowed out in 12 is stablized at 40 ~ 60 DEG C, and the ferrous solution flowed out out of condenser 12 passes sequentially through the first filtering Equipment 13 and except after chinaware 14, into ferrous solution pans 15, opening ferrous solution filter pump 18 will be in ferrous solution pans 15 Ferrous solution be delivered in the second filter plant 16 and be filtered, it is molten that the iron without residue is then discharged out of second filter plant 16 Liquid；
2) ferric phosphate synthesizes
The ferrous solution of step 1.3) is added in ferric phosphate consersion unit 02, oxidant is added through oxidant inlet 011, in temperature PH is added from pH adjusting agent entrance 09 until ferrous ion is all oxidized to ferric ion in 30-70 DEG C of progress oxidation reaction It is worth regulator, control pH is 1.0-2.5, obtains yellow or flaxen phosphate dihydrate iron slurry, then by phosphate dihydrate iron slurry It is warming up to 90-99 DEG C, reaction 1-4h carries out ferric phosphate transformation of crystal, and unformed ferric phosphate is converted into phosphate dihydrate iron crystal form, brilliant Type conversion after the completion of slurry by yellow or it is faint yellow be converted into white or white powder, obtain ferric phosphate slurry, specifically:
2.1) ferrous solution containing ferrous ion is put into stills for air blowing 21, while the agitating device for opening stills for air blowing 21 is stirred It mixes, oxidant is then slowly put into stills for air blowing 21, the charging time of oxidant is 30 ~ 90 minutes, is controlled in stills for air blowing 21 Temperature≤70 DEG C of solution, detect stills for air blowing 21 in solution without ferrous ion after, the ferrous solution after being aoxidized；
2.2) ferrous solution after 21 internal oxidition of stills for air blowing is pumped out by stills for air blowing discharging pump 23 and is delivered in stillpot 22, simultaneously The agitating device for starting stillpot 22 is stirred, and pH adjusting agent is then slowly put into stillpot 22, controls stillpot 22 For the pH of interior solution between 1.0 ~ 2.5, the charging time of pH adjusting agent is 30 ~ 90 minutes；
2.3) after the completion of the pH adjusting agent in step 2.2) feeds intake, the temperature of solution in stillpot 22 is warming up to 90 ~ 95 DEG C, into The reaction of row ferric phosphate transformation of crystal after reaction 1 ~ 4 hour, is starched the ferric phosphate after reacting in stillpot by stillpot discharging pump 24 Material pumps out；
3) it washs
The ferric phosphate slurries filtration that step 2 is obtained, ferric phosphate filter cake are added in washing facility 03, and pure water is through pure water entrance 08 It is added, with pure water 3-10 times, each dosage of pure water dosage is 7-15 times of phosphoric acid iron drier filter cake, and temperature controls 10- 50 DEG C, washing lotion and product ferric phosphate filter cake are obtained, specific washing process is as follows:
3.1) corresponding cleaning solution is put into every grade of washing kettle in advance, then filters ferric phosphate slurry through pre-filtering equipment 39 Mother liquor and ferric phosphate filter cake raw material are obtained, mother liquor is sent to washing lotion processing unit to recycle ferric phosphate residue therein, the phosphorus Sour iron filter cake raw material, which is put into level-one washing kettle 31, to be followed by stirring and washing；
3.2) in level-one washing kettle 31 after the completion of washing, the slurry after washing, which is transported to by-pass filtration equipment 32 and is obtained by filtration one, to be washed Water and a filter wash cake, a filter wash cake is put into second level washing kettle, while the slurry in second level washing kettle is passed through secondary filtration Two wash waters that equipment is obtained by filtration are transported in level-one washing kettle, washing process and so on；Wherein a wash water is sent to washing lotion Processing unit is to recycle ferric phosphate residue therein；
3.3) after the completion of most rear class washing kettle n washing, grade filter plant N is obtained by filtration finally the slurry conveying after washing to the end Grade water and most rear class filter cake, while filling into pure water into most rear class washing kettle n and most will be transported to previous stage washing kettle by rear class water In 31, the continuous washing of ferric phosphate is carried out；Filter ferric phosphate filter cake is to be processed；
4) washing lotion recycles
Neutralizer is added into washing lotion recovery system 07, from neutralizer entrance 14 in the wash pools of step 3), and washing lotion pH is adjusted To 6.0-9.0, neutralization reaction obtains sediment, after filtering filtrate be added washing lotion recovery system 07 be concentrated, obtain pure water and Strong brine, high-purity quick lime or white lime are added into strong brine, and pH value is adjusted to 10-12, obtain byproduct calcium sulfate and The alkali of alkali, recycling discharges from alkali outlet 012 and send to pH adjusting agent entrance 09 for adjusting pH value, and water is through pure water outlet 013 Enter 010 reuse of pure water entrance 08 or feed(raw material)inlet after outflow, specifically include as follows:
4.1) pH is adjusted: ferric phosphate production waste water being added in neutralization chamber 71, is slow added into neutralizer, while opening stirring Device is uniformly mixed neutralizer and waste water, the pH of waste water is adjusted to 6.0-9.0；
4.2) it filters: after the completion of pH is adjusted, waste water being passed through into the first filter plant 712, what is generated in removing pH adjustment process is heavy It forms sediment；
4.3) it is concentrated: waste water being squeezed into Waste water concentrating equipment 72, isolates pure water, while obtaining strong brine；
4.4) alkali collection is handled: strong brine being squeezed into alkali collection kettle 73, turn on agitator, while quick lime is added, can also be added Enter white lime, pH is adjusted to 10-12, obtains alkali collection liquid；
4.5) product recycles: alkali collection liquid being passed through the second filter plant 74, respectively obtains calcium sulfate and corresponding neutralizer；
5) drying and sintering equipment
The ferric phosphate filter cake of step 3) is added in drying and sintering device 04 and is dehydrated at 100-300 DEG C, filter is removed A large amount of Free water in cake, obtains phosphate dihydrate iron powder, phosphate dihydrate iron is delivered to high-temperature sintering apparatus 015, in 400- Sintering time 2-8h at 800 DEG C removes the crystallization water in phosphate dihydrate iron, while carrying out transformation of crystal, obtains the anhydrous phosphorus of product Sour iron, specifically comprises the following steps:
5.1) drying and dehydrating
Drier 41 is added by dry feed device 45 in the ferric phosphate filter cake being prepared, is set at 100-300 DEG C in temperature The Free water in filter cake is dried and removed, ferric phosphate filter cake becomes phosphate dihydrate iron crude product, and controls Free water in phosphate dihydrate iron Within content 1%, the tail gas for carrying a small amount of phosphate dihydrate iron laden dust secretly enters drying, dedusting equipment 46 at the top of drier 41 to be carried out Processing, the tail gas after dedusting is to be processed, and phosphate dihydrate iron crude product is recycled and post-processed from 46 bottom of drying, dedusting equipment；
5.2) high temperature sintering
Sintering kettle 42 is added through sintering feeder 47 in the phosphate dihydrate iron crude product that step 5.1) is obtained, and is sintered warm area point in kettle 42 It is three sections, first segment is warming-up section, and temperature of charge rises to set temperature by room temperature, and second segment is soaking zone, and third section is cooling Section, material is down to 70 DEG C hereinafter, molecular water removes in phosphate dihydrate iron in sintering kettle 42 by set temperature, while crystal form turns Change, obtain anhydrous phosphoric acid iron product, the tail gas that when sintering generates enters sintering dust equipment 48 at the top of sintering kettle 42, by tail gas The anhydrous phosphoric acid iron laden dust being entrained with is recycled from 48 bottom of sintering dust equipment, and the tail gas after dedusting is to be processed；
5.3) vent gas treatment
The tail gas of step 5.1) and step 5.2) is all collected and enters water absorption tower 43, passes through shower water in water absorption tower 43 Spray absorbs remaining dust, SO in tail gas2And SO3Gas, water enter back into alkali adsorption tower 44 after absorbing, by spraying diluted alkaline Liquid further absorbs the sour gas in tail gas, and air and vapor the gaseous mixture emptying that alkali adsorption tower 44 is handled, water absorb The wastewater reuse approach of tower and alkali adsorption tower bottom；
6) it is pulverized and mixed packaging
Anhydrous iron phosphate after the step 5) high temperature sintering of different batches is delivered to the pulverizer that is pulverized and mixed in device 05 into Row crushes, and being crushed to granular size is D50 < 3 μm, and the ferric phosphate crushed is added batch mixer and is mixed into 2-8h, product after mixing It is packed in packaging facilities 06 by specification, batch mixer load is 80%, incorporation time 2-8h；Make-up room control air humidity < 30% hereinafter, temperature < 30 DEG C.
The source of iron is iron powder, iron filings, scrap iron, ferrous sulfate, ferric sulfate, ferrous oxide, iron oxide, frerrous chloride or chlorine Change one or more of in iron；Phosphorus source is phosphoric acid；Sour one in sulfuric acid, phosphoric acid, hydrochloric acid, formic acid, acetic acid, citric acid, tartaric acid Kind is several；For 0-2.0mol/L, any situation is that 0, acid provides H to phosphoric acid concentration in gained ferrous solution+Concentration is 0-3.0mol/ L, it includes 2+ valence and 3+ valence that iron concentration, which is 1.0-2.0mol/L().
The oxidant is hydrogen peroxide, Peracetic acid, nitric acid, ammonium persulfate, one or more of mixtures in hypochlorous acid, oxygen The molar ratio of agent and ferrous ion is 0.5-1.5:1；The detection method that ferrous ion reaction is completed is Phen Indicator method or permanganimetric method.
The pH adjusting agent is ammonium hydroxide, aqueous slkali or the salting liquid that pH is greater than 4；Alkali is sodium hydroxide or potassium hydroxide； Salt is sodium carbonate, sodium bicarbonate, sodium phosphate, disodium hydrogen phosphate, sodium dihydrogen phosphate, potassium carbonate, saleratus, potassium phosphate, phosphoric acid Hydrogen dipotassium, potassium dihydrogen phosphate, ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium carbonate or ammonium hydrogen carbonate.
The neutralizer is sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or ammonium hydroxide；
Embodiment 1
Ferrous solution synthesis: 98.5% iron powder of 682kg, 85% phosphoric acid of 1425kg, 98% sulfuric acid of 1200kg and 7693kg pure water are utilized Acidolysis reaction is carried out, ferrous solution is prepared.Phosphoric acid concentration is 1.236mol/L in ferrous solution after preparation, sulfuric acid provides H+ concentration and is 2.4mol/L, iron concentration 1.2mol/L, 85 DEG C of reaction temperature.Magnetic is filtered and removed after having reacted, and obtains finally obtaining To 11000kg ferrous solution.
Ferric phosphate synthesis: after ferrous solution enters ferric phosphate synthesis device, 890kg hydrogen peroxide, oxidizing temperature are firstly added 30-70℃.It is fully oxidized, until detecting redfree with Phen.8% ammonium hydroxide of 3570kg is added after the completion of oxidation, controls pH 1.5, iron ion and phosphate anion is made to combine precipitating.Above-mentioned ferric phosphate slurry is warming up to 95 DEG C, carries out ferric phosphate crystal form Unformed ferric phosphate is converted phosphate dihydrate iron crystal form by conversion, reaction time 2h, after the completion of transformation of crystal slurry by yellow or It is faint yellow to be converted into white or white powder.
Washing facility: by ferric phosphate slurries filtration after reaction, ferric phosphate filter cake uses 1800kg pure water 4 again after filtering It is secondary.Temperature of washing water controls 30 DEG C.
Washing lotion reclaimer: 25% ammonium hydroxide of 490kg is added into washing lotion, washing lotion pH is adjusted to 6.0-9.0.Mistake after neutralization Sediment is filtered, by 13% ammonium sulfate salt water of washing lotion 12080kg after filtering, amberplex is added and is concentrated, 574kg is isolated Pure water reuse, while obtaining 25% ammonium sulfate strong brine of 633kg.
90% quick lime of 747kg is added into strong brine, pH value is adjusted to 10-12, recycling 408kg ammonia is used for ferrophosphorus PH when synthesis is adjusted, and so that raw material is recycled, while obtaining 3264kg byproduct calcium sulfate.
Dry and agglomerating plant: by ferric phosphate filter cake after washing according to 300kg/h be added in flash dryer 200 DEG C into Row dehydration, removes a large amount of Free water in filter cake, obtains 187kg/h phosphate dihydrate iron powder, water content≤1% in powder.
Phosphate dihydrate iron is delivered to rotary furnace, temperature is set as 500 DEG C, and sintering time sets 6h, removes phosphate dihydrate The crystallization water in iron, while transformation of crystal is carried out, obtain 150kg/h anhydrous iron phosphate.
It is pulverized and mixed packaging facilities: the anhydrous iron phosphate after high temperature sintering being delivered in airslide disintegrating mill, is crushed, Being crushed to granular size is D50 < 3 μm.The ferric phosphate that will be crushed, is added ribbon batch mixer, and additional amount is batch mixer load 80%, incorporation time 5h are sufficiently mixed material, guarantee the consistency and uniformity of product.By product in make-up room, pass through Dehumidifier and air-conditioning equipment, control air humidity < 30% is hereinafter, temperature < 30 DEG C, according to 25kg/ packet or 500kg/ packet equal-specification Packaging.
Embodiment 2
Ferrous solution synthesis: it is anti-that acidolysis is carried out using 99% ferrous sulfate of 2808kg, 85% phosphoric acid of 1188kg and 7000kg pure water It answers, prepares ferrous solution.After preparation in ferrous solution phosphoric acid concentration be 1.03mol/L, iron concentration 1mol/L, reaction temperature 50 ℃.Magnetic is filtered and removed after having reacted, and obtains final ferrous solution.
Ferric phosphate synthesis: after ferrous solution enters ferric phosphate synthesis device, 742kg hydrogen peroxide, oxidizing temperature are firstly added 30-70 DEG C, until detecting redfree with Phen.12% sodium hydroxide solution of 6000kg is added after the completion of oxidation, controls pH 1.8, iron ion and phosphate anion is made to combine precipitating.Above-mentioned ferric phosphate slurry is warming up to 98 DEG C, carries out ferric phosphate crystal form Unformed ferric phosphate is converted phosphate dihydrate iron crystal form by conversion, reaction time 4h, after the completion of transformation of crystal slurry by yellow or It is faint yellow to be converted into white or white powder.
Washing facility: by ferric phosphate slurries filtration after reaction, ferric phosphate filter cake uses 1200kg pure water 6 again after filtering It is secondary.Temperature of washing water controls 30 DEG C.
Washing lotion reclaimer: 250kg sodium hydroxide is added into washing lotion, washing lotion pH is adjusted to 6.0-9.0.After neutralization 10.5% sodium sulphate salt water of washing lotion 16178kg after filtering is added evaporating waste water concentrator and is concentrated by filtering precipitate, point 765kg pure water reuse is separated out, while obtaining 20% sodium sulphate strong brine of 852kg.The raw stone of 747kg 90% is added into strong brine PH value is adjusted to 10-12 by ash, and PH when recycling liquid alkaline is synthesized for ferrophosphorus is adjusted, and so that raw material is recycled, simultaneously Obtain 3264kg byproduct calcium sulfate.
Dry and agglomerating plant: by ferric phosphate filter cake after washing according to 200kg/h be added in flash dryer 150 DEG C into Row dehydration, removes a large amount of Free water in filter cake, obtains 125kg/h phosphate dihydrate iron powder, water content≤1% in powder.
Phosphate dihydrate iron is delivered to rotary furnace, temperature is set as 600 DEG C, and sintering time sets 5h, removes phosphate dihydrate The crystallization water in iron, while transformation of crystal is carried out, obtain 100kg/h pure phase anhydrous iron phosphate.
It is pulverized and mixed packaging facilities: the anhydrous iron phosphate after high temperature sintering being delivered in airslide disintegrating mill, is crushed, Being crushed to granular size is D50 < 3 μm.The ferric phosphate that will be crushed, is added ribbon batch mixer, and additional amount is batch mixer load 80%, incorporation time 6h are sufficiently mixed material, guarantee the consistency and uniformity of product.By product in make-up room, pass through Dehumidifier and air-conditioning equipment, control air humidity < 30% is hereinafter, temperature < 30 DEG C, according to 25kg/ packet or 500kg/ packet equal-specification Packaging.
Unless otherwise specified, consersion unit and device involved in the present invention, are commonly used equipment to the present invention.

Claims (10)

1. a kind of production technology of ferric phosphate, it is characterised in that include the following steps:
1) ferrous solution synthesizes
Source of iron, phosphorus source, acid and pure water are added in ferrous solution consersion unit (01) by feed inlet (010), are in reaction temperature Acidolysis reaction is carried out at 30-90 DEG C, is filtered after reaction, is removed magnetic, obtains ferrous solution；
2) ferric phosphate synthesizes
The ferrous solution of step 1) is added in ferric phosphate consersion unit (02), while oxidant is added through oxidant inlet (011), It is 30-70 DEG C of progress oxidation reaction in temperature, until ferrous ion is all oxidized to ferric ion, from pH adjusting agent entrance (09) pH adjusting agent is added, until pH is 1.0-2.5, obtains yellow or faint yellow phosphate dihydrate iron slurry, the phosphate dihydrate Iron slurry is warming up to 90-99 DEG C of reaction 1-4h, and unformed ferric phosphate is converted into phosphate dihydrate iron crystal form, starches after the completion of transformation of crystal Material by yellow or it is faint yellow be converted into white or white powder, obtain ferric phosphate slurry；
3) it washs
The ferric phosphate slurries filtration that step 2 is obtained, ferric phosphate filter cake is added in washing facility (03), through pure water entrance (08) Pure water is added, with pure water 3-10 times, temperature controls 10-50 DEG C, obtains washing lotion and product ferric phosphate filter cake；
4) washing lotion recycles
The wash pools of step 3) are added mouth (014) from neutralizer and neutralizer are added, by washing lotion into washing lotion recovery system (07) PH is adjusted to 6.0-9.0, and neutralization reaction obtains sediment, and filtrate is concentrated in washing lotion recovery system (07) after filtering, obtains Pure water and strong brine, high-purity quick lime or white lime are added into strong brine, and pH value is adjusted to 10-12, obtain byproduct sulphur Sour calcium and alkali, alkali are sent to pH adjusting agent entrance (09) from alkali outlet (012) recycling for adjusting pH value, and water is through pure water outlet (013) enter pure water entrance (08) or feed inlet (10) reuse after flowing out；
5) dry and agglomerating plant
The ferric phosphate filter cake of step 3) is added in drying and sintering device (04) and is dehydrated at 100-300 DEG C, is removed A large amount of Free water in ferric phosphate filter cake, obtains phosphate dihydrate iron powder, and phosphate dihydrate iron powder is delivered to high temperature sintering and is set Standby (015), the sintering time 2-8h at 400-800 DEG C remove the crystallization water in phosphate dihydrate iron, while carrying out transformation of crystal, Obtain product anhydrous iron phosphate；
6) it is pulverized and mixed packaging
Anhydrous iron phosphate after step 5) high temperature sintering is delivered to the pulverizer being pulverized and mixed in device (05) to crush, powder Being broken to granular size is D50 < 3 μm, and batch mixer mixing 2-8h is added in the ferric phosphate that multiple batches crush, and product is wrapping after mixing It installs in standby (06) and is packed by specification.
2. a kind of production technology of ferric phosphate according to claim 1, it is characterised in that source of iron in step 1) be iron powder, It is one or more of in iron filings, scrap iron, ferrous sulfate, ferric sulfate, ferrous oxide, iron oxide, frerrous chloride or iron chloride；Phosphorus source is Phosphoric acid；Acid is one or more of sulfuric acid, phosphoric acid, hydrochloric acid, formic acid, acetic acid, citric acid, tartaric acid；Phosphorus in gained ferrous solution Acid concentration is 0-2.0mol/L, acid provides H+Concentration is 0-3.0mol/L, ferrous ion and iron concentration and be 1.0- 2.0mol/L。
3. a kind of production technology of ferric phosphate according to claim 1, it is characterised in that the oxidant in step 2 is double Oxygen water, Peracetic acid, nitric acid, ammonium persulfate, one or more of mixtures in hypochlorous acid, oxidant and feeding intake for ferrous ion are rubbed You are than being 0.5-1.5:1；The detection method that ferrous ion reaction is completed is Phen indicator method or permanganate titration Method.
4. a kind of production technology of ferric phosphate according to claim 1, it is characterised in that the pH adjusting agent in step 2 It is greater than 4 ammonium hydroxide, aqueous slkali or salting liquid for pH；Alkali is sodium hydroxide or potassium hydroxide；Salt is sodium carbonate, sodium bicarbonate, phosphorus Sour sodium, disodium hydrogen phosphate, sodium dihydrogen phosphate, potassium carbonate, saleratus, potassium phosphate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate, phosphoric acid Ammonium, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, ammonium carbonate or ammonium hydrogen carbonate.
5. a kind of production technology of ferric phosphate according to claim 1, it is characterised in that the pure water dosage in step 3) is 7-15 times of phosphoric acid iron drier amount weight.
6. a kind of production technology of ferric phosphate according to claim 1, it is characterised in that the neutralizer in step 4) is hydrogen Sodium oxide molybdena, potassium hydroxide, sodium carbonate, potassium carbonate or ammonium hydroxide.
7. a kind of production technology of ferric phosphate according to claim 1, it is characterised in that the washing lotion in step 4) recycles system (07) is united as amberplex or evaporating waste water concentrator, the evaporating waste water concentrator is MVR, triple effect evaporator or more Imitate evaporator；High-purity quick lime purity > 95%, fineness > 200 mesh；High-purity white lime > 98%, fineness > 200 mesh.
8. a kind of production technology of ferric phosphate according to claim 1, it is characterised in that the drying and sintering dress in step 5) Setting (04) is flash distillation dryer, atomizing drier or fluidized bed type drier, and the high-temperature sintering apparatus (015) is revolution Furnace, roller furnace or pusher furnace；Water content≤1% in obtained phosphate dihydrate iron powder.
9. a kind of production technology of ferric phosphate according to claim 1, it is characterised in that the batch mixer in step 6) is spiral shell Band batch mixer, double-cone mixer or V-type batch mixer；Pulverizer is airslide disintegrating mill, mechanical crusher or twin rollers.
10. a kind of process units of ferric phosphate according to claim 1, it is characterised in that including sequentially connected ferrous solution Consersion unit (01), ferric phosphate consersion unit (02), washing facility (03), drying and sintering device (04), high-temperature sintering apparatus (015), it is pulverized and mixed device (05) and packaging facilities (06), setting is used for source of iron, phosphorus on the ferrous solution consersion unit (01) The feed(raw material)inlet (010) in source, acid and pure water feed, ferric phosphate consersion unit (02) are equipped with pH adjusting agent entrance (09), wash It washs and is equipped with pure water entrance (08) at the top of equipment (03), bottom connects washing lotion recovery system (07), and washing lotion recovery system is set on (07) There are pure water outlet (013) and alkali outlet (012), the raw material of pure water outlet (013) connection ferrous solution consersion unit (01) enters Mouth (010) or pure water entrance (08), alkali outlet (012) are connected with pH adjusting agent entrance (09)；
The ferrous solution consersion unit (01) include with the source of iron dissolution kettle (11) of agitating device, source of iron feeder, acid solution into Material device, ferrous solution discharging pump (17), condenser (12), recycling precipitate device, be set on source of iron dissolution kettle (11) the One temperature detector (116) and the Heat exchange jacekt (121) being set on the outside of source of iron dissolution kettle (11), source of iron dissolution kettle (11) top Portion is equipped with blow-down pipe (19) and the first pressure measuring appliance (118) for monitoring source of iron dissolution kettle (11) internal pressure, and source of iron is molten Kettle (11) are solved equipped with the fluid level measuring instrument (117) for monitoring liquid level；The Heat exchange jacekt (121) is equipped with hot fluid inlet (112) and hot fluid outlet ports (113)；The source of iron feeder and acid solution feeding device connect with source of iron dissolution kettle (11) pipeline respectively It connects, source of iron dissolution kettle (11) bottom discharge port and ferrous solution discharging pump (17), condenser (12) and recycling precipitate device are successively Piping connection；
The ferric phosphate consersion unit (02) includes stills for air blowing (21), the stillpot with agitating device with agitating device (22), ferrous solution feeding device, oxidant feed device, pH adjusting agent feeding device, stills for air blowing discharging pump (23) and stillpot Discharging pump (24) is additionally provided with the first liquid level detector (29), first pressure detector (28) and the first temperature on stills for air blowing (21) Measuring appliance (27), stillpot (22) are equipped with the second liquid level detector (213), second pressure detector (212) and second temperature Measuring appliance (211)；
The washing facility (03) includes the spaced washing kettle of several grades and filter plant, further include washing lotion processing unit and Pre-filtering equipment (39), the washing kettle is identical with the series of filter plant, and from left to right starts, washing kettle and filter plant Series be sequentially increased, the first liquid level measurer (34) are provided on every grade of washing kettle, the bottom of every grade of washing kettle goes out liquid Mouth passes through the inlet piping connection of washing kettle discharging pump (33) and filter plant at the same level；
The drying and sintering device (04) includes drier (41), is sintered kettle (42), water absorption tower (43) and alkali adsorption tower (44), Drier (41) is connect with dry feed device (45), and ferric phosphate filter cake enters drier (41) by dry feed device (45), dry Device (41) top exit connects drying, dedusting equipment (46), and outlet at bottom is sintered kettle (42) by sintering feeder (47) connection, It is sintered kettle (42) top exit connection sintering dust equipment (48)；
The washing lotion recovery system (07) include the neutralization chamber (71) of from left to right successively piping connection, first filter (712), Waste water concentrating equipment (72), alkali collection kettle (73) and the second filter (74)；The neutralization chamber (71) and first filter (712) Between pipeline be equipped with neutralization chamber discharging pump (75), set on the pipeline between Waste water concentrating equipment (72) and alkali collection kettle (73) Have strong brine discharging pump (76), the pipeline between alkali collection kettle (73) and the second filter (74) is equipped with alkali collection kettle discharging pump (77).
CN201910169493.4A 2019-03-06 2019-03-06 A kind of production technology and its production equipment of ferric phosphate Pending CN109761209A (en)

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