CN106241763A - A kind of phosphor ammonium slurry defecator and filter method thereof - Google Patents

A kind of phosphor ammonium slurry defecator and filter method thereof Download PDF

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Publication number
CN106241763A
CN106241763A CN201610653162.4A CN201610653162A CN106241763A CN 106241763 A CN106241763 A CN 106241763A CN 201610653162 A CN201610653162 A CN 201610653162A CN 106241763 A CN106241763 A CN 106241763A
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CN
China
Prior art keywords
slurry
defecator
filter
filtrate
phosphor ammonium
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Granted
Application number
CN201610653162.4A
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Chinese (zh)
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CN106241763B (en
Inventor
项双龙
彭宝林
王先炜
潘礼富
徐圆
荷花
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Guiyang Kailin Chemical Co Ltd
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Guiyang Kailin Chemical Co Ltd
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Priority to CN201610653162.4A priority Critical patent/CN106241763B/en
Publication of CN106241763A publication Critical patent/CN106241763A/en
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Classifications

    • 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
    • C01B25/26Phosphates
    • C01B25/28Ammonium phosphates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D29/00Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/11Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with bag, cage, hose, tube, sleeve or like filtering elements
    • B01D29/13Supported filter elements
    • B01D29/15Supported filter elements arranged for inward flow filtration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D29/00Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/50Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition
    • B01D29/52Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with multiple filtering elements, characterised by their mutual disposition in parallel connection
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D29/00Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/62Regenerating the filter material in the filter
    • B01D29/66Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps

Abstract

The present invention relates to phosphor ammonium slurry filtration art, especially a kind of phosphor ammonium slurry defecator and filter method thereof, by the pH value to the phosphor ammonium slurry entering defecator, temperature and phosphorus ammonium proportion, solid content is bound, after guaranteeing that phosphor ammonium slurry enters in defecator, liquid can rapid osmotic enter inside filter bag, filter bag is made to support molding, in conjunction with aeration reverse osmosis filtration treatment, filtrate can be effectively made to enter inside filter bag, and then by impurities left at filter bag outer surface, and in conjunction with the process of falling bag and cleaning treatment, filter bag is regenerated, and avoid that filtrate viscosity is higher makes filtration difficulty, improve phosphorus ammonium purity in filtrate, substantially ensure that the quality of phosphorus ammonium salt product.

Description

A kind of phosphor ammonium slurry defecator and filter method thereof
Technical field
The present invention relates to phosphor ammonium slurry filtration art, especially a kind of phosphor ammonium slurry defecator and filtration side thereof Method.
Background technology
During wet phosphoric acid by dihydrate standing sedimentation, substantial amounts of solid precipitation slag will be separated out, slag will be mainly composed of phosphorus Gypsum Fibrosum and (Fe, Al)3KH14(PO4)8·4H2O complex, simultaneously possibly together with substantial amounts of soluble impurity, such as magnesium ion, calcium from Son, iron ion, aluminium ion, sulfate radical, hexafluosilicic acid root etc.;In phosphoric acid by wet process with ammonia and in course of reaction, these impurity will Generate the compound of Various Complex, have a strong impact on the product composition of the viscosity of phosphor ammonium slurry and phosphor ammonium slurry, physical characteristic and The dissolubility etc. of phosphorus pentoxide.Therefore, when fine phosphorus ammonium salt product is directly produced for phosphoric acid by wet process, need phosphor ammonium slurry Carry out filtering and impurity removing process so that the quality preparing phosphorus ammonium salt product is higher.
Traditional phosphor ammonium slurry filter method mainly has three kinds, and gravitational settling, centrifugation, filter filter;And gravity Sedimentation needs corollary apparatus huge, and investment and operation and maintenance cost are higher, and solid tiny in full-bodied phosphor ammonium slurry is not Molten thing is difficult to rapid subsidence, additionally, the reduction because of slurry temperature will be brilliant with phosphorus ammonium salt in solid insoluble gravity settlement process Body separates out, and affects phosphor ammonium slurry utilization rate;Centrifugal separation equipment assembling complexity, inconvenient maintenance, investment and energy consumption are higher, and high viscous The phosphor ammonium slurry of property easily blocks centrifugal rotatable parts;Filter plant is currently mainly filter press and band filter etc., Filter is intermittent operation, and frequently, filter cloth cleans inconvenience in device switching, for filtering the phosphorus ammonium material containing a certain amount of silica gel Slurry, equipment operation rate is extremely low.
As can be seen here, phosphor ammonium slurry filter method of the prior art also exists numerous defects, all it is difficult to ensure that phosphorus ammonium While the utilization rate of slip is higher, it is possible to improve the quality of phosphorus ammonium salt product, hinder phosphoric acid by wet process and directly prepare fine phosphorus The development of ammonium salt product.
Summary of the invention
In order to solve above-mentioned technical problem present in prior art, the present invention provide a kind of phosphor ammonium slurry defecator and Its filter method.
It is achieved particular by techniques below scheme:
A kind of phosphor ammonium slurry filter method, comprises the following steps:
(1) in filter pulp groove, by phosphoric acid by wet process with in ammonia and reaction slurry preparation become pH value to be 3-5, temperature is 70-90 DEG C, solid content is 1-2%, and phosphorus ammonium proportion is the phosphor ammonium slurry of 1.1-1.3;
(2) phosphor ammonium slurry is sent in defecator, by aeration reverse osmosis filtration treatment so that the filtrate of phosphor ammonium slurry is entered Entering in the filter bag of defecator, the filtering residue of phosphor ammonium slurry is stayed the outer surface of defecator filter bag and deposits in defecator, Treat that filter bag outer surface is blocked by slag blanket, and when filter bag internal filtrate amount is not further added by, start the process of falling bag so that filtrate enters Filtrate receiver;After the bag that falls completes, from cleaning, liquid bath is put into cleanout fluid, rinse filter bag outer surface so that filtering residue is to sinking, and cleans Defecator,.
Described step, is additionally included in after phosphor ammonium slurry is sent into defecator, and its filtrate penetrates into the filter of defecator Bag is internal, and when filtering residue deposits in defecator, its lightweight filtering residue enters filter pulp groove recoil preparation phosphorus from light slag slurry recoil hole Ammonium slip;Heavy slurry enters slurry groove from heavy slurry recoil hole, detects slurry concentration, if phosphorus pentoxide concentration is higher, And it is unsatisfactory for environmental emission standard, then returns filter pulp groove preparation phosphor ammonium slurry;If phosphorus pentoxide concentration is relatively low, and meets Environmental emission standard, then discharge.
Described step, is additionally included in after phosphor ammonium slurry is sent into defecator, and filtrate penetrates into the filter bag of defecator In, the supernatant of filtrate constantly increases to the porous tube plate of defecator, and in the process, the one-tenth that in filtrate, concentration is relatively low Divide to sinking so that supernatant concentration is relatively low, and the supernatant low for this concentration is entered filter pulp groove by filtrate refluxing opening Prepare phosphor ammonium slurry and/or clean liquid bath by going cleanout fluid notch to enter.
Described step, is sending in defecator by phosphor ammonium slurry, and the compression using pressure to be 0.15-0.35MPa is empty Gas is passed through bottom defecator and carries out Air Exposure, and the Air Exposure time is 1-2h.
Described step, after bag completes, it is put in cleanout fluid cleaning process from cleaning liquid bath, is used pressure Power is that the compressed air of 0.15-0.25MPa carries out Air Exposure, and aeration time is until filter bag outer surface slag blanket washes.
Described step, is putting in cleanout fluid cleaning process from cleaning liquid bath, is that cleanout fluid is first put into immersion 25- After 30min, then the compressed air being used pressure to be 0.15-0.25MPa carries out Air Exposure.
Described defecator, including cylinder, porous tube plate, filter bag, removes filtrate notch, phosphor ammonium slurry entrance, solarization air cap, Wherein, the hole that inner barrel is provided with on porous tube plate, porous tube plate connects with the bag mouth of filter bag, at cylinder near the side at top It is provided with filtrate notch on wall, on the sidewall of bottom, is respectively arranged with phosphor ammonium slurry entrance and solarization air cap at cylinder;
Described device, also includes being arranged on cylinder filtrate refluxing opening on the sidewall at top and removing cleanout fluid notch With cylinder filter washing water inlet on the sidewall of bottom is set;
Described device, also includes the heavy slurry recoil hole being arranged on cylinder body bottom and is arranged on cylinder near bottom Light slag slurry recoil hole on sidewall.
Described defecator, the longitudinal center line of solarization air cap is positioned at the bottom of filter bag.
Described defecator, also includes the support bar for supporting this device;Described support bar is at least 2.
Described device, filter bag is polymeric membrane for separation, is provided with support member so that filter bag can support and consolidate into Type, and this support member can freely skid off.
Compared with prior art, the technique effect of the present invention is embodied in:
By the entrance pH value of phosphor ammonium slurry of defecator, temperature and phosphorus ammonium proportion, solid content are bound, really After protecting in phosphor ammonium slurry entrance defecator, liquid can rapid osmotic enter inside filter bag so that filter bag supports molding, in conjunction with Aeration reverse osmosis filtration treatment, it is possible to effectively make filtrate enter inside filter bag, and then by impurities left at filter bag outer surface, and And combining the process of falling bag and cleaning treatment so that filter bag regenerates, and avoids the higher filtration difficulty that makes of filtrate viscosity, improves Phosphorus ammonium purity in filtrate, has substantially ensured that the quality of phosphorus ammonium salt product.
The invention is the most prominent, and phosphor ammonium slurry filtration cost is relatively low, and energy consumption is low, and equipment is simple, equipment cost Low, filter bag is easy to clean.
Accompanying drawing explanation
Fig. 1 is the phosphor ammonium slurry filtering technique schematic flow sheet of the present invention.
A-filtrate receiver B-cleans liquid bath C-compressed gas D-defecator E-filter pulp groove F-slurry groove.
Fig. 2 is filter apparatus configuration schematic diagram.
1-filtrate refluxing opening 2-goes filtrate notch 3-to go cleanout fluid notch 4-porous tube plate 5-filter bag 6-cleanout fluid to enter 9-heavy slurry recoil hole, mouth 7-solarization air cap 8-light slag slurry recoil hole 10-support bar 11-phosphor ammonium slurry entrance 12-cylinder Body.
Detailed description of the invention
With specific embodiment, technical scheme is further limited below in conjunction with the accompanying drawings, but requirement The scope of protection is not only limited to description.
Embodiment
Concrete principle and the concrete operations mode of the present invention are carried out in such a way, and those skilled in the art are permissible According to herein below, the overall plan of the invention is understood:
A kind of phosphor ammonium slurry filter method, comprises the following steps:
(1) in filter pulp groove E, by phosphoric acid by wet process with in ammonia and reaction slurry preparation become pH value to be 3-5, temperature is 70- 90 DEG C, solid content is 1-2%, and phosphorus ammonium proportion is the phosphor ammonium slurry of 1.1-1.3;
(2) phosphor ammonium slurry is sent in defecator D, by aeration reverse osmosis filtration treatment so that the filtrate of phosphor ammonium slurry Entering in the filter bag 5 of defecator D, the filtering residue of phosphor ammonium slurry stays the outer surface of defecator D filter bag 5 and at defecator D Middle deposition, treats that filter bag 5 outer surface is blocked by slag blanket, and when filter bag 5 internal filtrate amount is not further added by, starts the process of falling bag, make Obtain filtrate and enter filtrate receiver A;After the bag that falls completes, from cleaning, liquid bath B puts into cleanout fluid, rinse filter bag outer surface so that filtering residue To sinking, and cleaning and filtrating equipment D,.Improve filtrate purity, it is ensured that the quality of phosphorus ammonium salt product, and achieve Filtrate sedimentation is the denseest.By aeration reverse osmosis filtration treatment so that slag blanket remains in defecator, or by defecator Defecator is got rid of in light slag slurry recoil hole or heavy slurry recoil hole so that phosphor ammonium slurry filtrate obtains purification, junction Reason process Air Exposure so that filtering residue sticks to the speed of filter bag outer surface and slows down, and guarantee to stick to filter bag outer surface Slag blanket is loose porous cellular, it is to avoid filter bag regeneration difficulty, reduces filter bag cleaning of outer surface difficulty, it is achieved that filter dress That puts repeats regeneration application, reduces cost.
In certain embodiments, above-mentioned step, it is additionally included in after phosphor ammonium slurry is sent into defecator D, its filtrate is oozed Filter bag 5 to defecator D is internal thoroughly, and when filtering residue deposits in defecator D, its lightweight filtering residue is from light slag slurry recoil hole 8 Enter filter pulp groove E recoil preparation phosphor ammonium slurry;Heavy slurry enters slurry groove F from heavy slurry recoil hole 9, and detection slurry is dense Degree, if phosphorus pentoxide concentration is higher, and is unsatisfactory for environmental emission standard, then return filter pulp groove E and prepare phosphor ammonium slurry;If five Aoxidize two phosphorus concentrations relatively low, and meet environmental emission standard, then discharge.
In certain embodiments, above-mentioned step, it is additionally included in after phosphor ammonium slurry is sent into defecator D, filtrate is permeated In the filter bag 5 of defecator D, the supernatant of filtrate constantly increases to the porous tube plate 4 of defecator D, and in this process In, the composition that in filtrate, concentration is relatively low is to sinking so that supernatant concentration is relatively low, and the supernatant low for this concentration is passed through Filtrate refluxing opening 1 enters filter pulp groove E preparation phosphor ammonium slurry and/or cleans liquid bath B by going cleanout fluid notch 3 to enter.
In certain embodiments, above-mentioned step, phosphor ammonium slurry to be sent in defecator D, employing pressure is The compressed air of 0.15MPa or 0.25MPa or 0.35MPa or 0.2MPa is passed through bottom defecator and carries out Air Exposure, aeration The process time is 1h or 2h or 1.5h or 1.1h.Reduce defecator load, reduce cost and energy consumption.
In certain embodiments, above-mentioned step, after bag completes, it is put into cleanout fluid from cleaning liquid bath B and cleans During, the compressed air being used pressure to be 0.15MPa or 0.25MPa or 0.2MPa carries out Air Exposure, aeration time Until filter bag outer surface slag blanket washes.
In certain embodiments, above-mentioned step, putting in cleanout fluid cleaning process from cleaning liquid bath, be first will be clear After washing liquid puts into immersion 25min or 30min or 28min, then to be used pressure be 0.15MPa's or 0.25MPa or 0.2MPa Compressed air carries out Air Exposure.
In certain embodiments, above-mentioned defecator, including cylinder 12, porous tube plate 4, filter bag 5, go filtrate notch 2, Phosphor ammonium slurry entrance 11, solarization air cap 7, wherein, the hole that cylinder 12 is internally provided with on porous tube plate 4, porous tube plate 4 and filter bag 5 Bag mouth connection, on the sidewall at top, be provided with filtrate notch 2 at cylinder 12, at cylinder 12 on the sidewall of bottom point It is not provided with phosphor ammonium slurry entrance 11 and solarization air cap 7;
Described device, also includes being arranged on the cylinder 12 filtrate refluxing opening 1 on the sidewall at top and removing cleanout fluid The notch 3 and cylinder 12 filter washing water inlet 6 on the sidewall of bottom is set;
Described device, also includes being arranged on the recoil of the heavy slurry bottom cylinder 12 hole 9 and to be arranged on cylinder 12 close Light slag slurry recoil hole 8 on the sidewall of bottom.
In certain embodiments, above-mentioned defecator, the longitudinal center line of solarization air cap 7 is positioned at the bottom of filter bag 5.
In certain embodiments, above-mentioned defecator, also include the support bar 10 for supporting this device;Described props up Strut is 2,3.
In certain embodiments, above-mentioned device, filter bag 5 is polymeric membrane for separation, is provided with support member so that filter Bag 5 can support firm molding, and this support member can freely skid off.
In the invention, make use of circular treatment so that the phosphorus ammonium composition in heavy slurry, light slag slurry obtains fully Absorption and utilization, improve the utilization rate of phosphor ammonium slurry, improve the concentration of phosphorus ammonium composition in filtrate, reduce phosphorus ammonium salt produce Impurity content in product, reduces phosphor ammonium slurry remove impurity difficulty, reduces phosphor ammonium slurry remove impurity cost.Processing step is simple, easily In industrialized production.

Claims (10)

1. a phosphor ammonium slurry filter method, it is characterised in that comprise the following steps:
(1) in filter pulp groove, by phosphoric acid by wet process with in ammonia and reaction slurry preparation become pH value to be 3-5, temperature is 70-90 DEG C, Solid content is 1-2%, and phosphorus ammonium proportion is the phosphor ammonium slurry of 1.1-1.3;
(2) phosphor ammonium slurry is sent in defecator, by aeration reverse osmosis filtration treatment so that the filtrate of phosphor ammonium slurry entered In the filter bag of filter device, the filtering residue of phosphor ammonium slurry is stayed the outer surface of defecator filter bag and deposits in defecator, to be filtered Bag outer surface is blocked by slag blanket, and when filter bag internal filtrate amount is not further added by, starts the process of falling bag so that filtrate enters filtrate Groove;After the bag that falls completes, from cleaning, liquid bath is put into cleanout fluid, rinse filter bag outer surface so that filtering residue is to sinking, and cleans filtration Device,.
2. phosphor ammonium slurry filter method as claimed in claim 1, it is characterised in that described step, is additionally included in phosphorus ammonium After slip sends into defecator, its filtrate penetrates into inside the filter bag of defecator, and when filtering residue deposits in defecator, it is light Matter filtering residue enters filter pulp groove recoil preparation phosphor ammonium slurry from light slag slurry recoil hole;Heavy slurry enters from heavy slurry recoil hole Slurry groove, detects slurry concentration, if phosphorus pentoxide concentration is higher, and is unsatisfactory for environmental emission standard, then return filter pulp groove Preparation phosphor ammonium slurry;If phosphorus pentoxide concentration is relatively low, and meets environmental emission standard, then discharge.
3. phosphor ammonium slurry filter method as claimed in claim 1, it is characterised in that described step, is additionally included in phosphorus ammonium After slip sends into defecator, filtrate penetrates in the filter bag of defecator, and the supernatant of filtrate is constantly to defecator Porous tube plate increases, and in the process, the composition that in filtrate, concentration is relatively low is to sinking so that supernatant concentration is relatively low, and The supernatant low for this concentration is entered filter pulp groove preparation phosphor ammonium slurry and/or by removing cleanout fluid notch by filtrate refluxing opening Enter and clean liquid bath.
4. phosphor ammonium slurry filter method as claimed in claim 1, it is characterised in that described step, is sending phosphor ammonium slurry Entering in defecator, the compressed air using pressure to be 0.15-0.35MPa is passed through bottom defecator and carries out Air Exposure, exposes The gas disposal time is 1-2h.
5. phosphor ammonium slurry filter method as claimed in claim 1, it is characterised in that described step, after bag completes, its Putting in cleanout fluid cleaning process from cleaning liquid bath, the compressed air being used pressure to be 0.15-0.25MPa carries out aeration Processing, aeration time is until filter bag outer surface slag blanket washes.
6. phosphor ammonium slurry filter method as claimed in claim 5, it is characterised in that described step, from cleaning in liquid bath Put in cleanout fluid cleaning process, be first cleanout fluid is put into immersion 25-30min after, then to be used pressure be 0.15- The compressed air of 0.25MPa carries out Air Exposure.
7. the phosphor ammonium slurry filter method as described in any one of claim 1-6, it is characterised in that described defecator, bag Include cylinder (12), porous tube plate (4), filter bag (5), remove filtrate notch (2), phosphor ammonium slurry entrance (11), solarization air cap (7), wherein, The hole that cylinder (12) is internally provided with on porous tube plate (4), porous tube plate (4) connects with the bag mouth of filter bag (5), in cylinder (12) On the sidewall at top, it is provided with filtrate notch (2), on the sidewall of bottom, is respectively arranged with phosphorus ammonium material at cylinder (12) Slurry entrance (11) and solarization air cap (7);
Described device, also includes being arranged on the cylinder (12) filtrate refluxing opening (1) on the sidewall at top and removing cleanout fluid Notch (3) and the filter washing water inlet (6) arranged on the sidewall of the close bottom of cylinder (12);
Described device, also includes being arranged on heavy slurry recoil hole (9) of cylinder (12) bottom and being arranged on cylinder (12) leaning on Light slag slurry recoil hole (8) on the sidewall of nearly bottom.
8. phosphor ammonium slurry filter method as claimed in claim 7, it is characterised in that described defecator, solarization air cap (7) Longitudinal center line is positioned at the bottom of filter bag (5).
9. phosphor ammonium slurry filter method as claimed in claim 7, it is characterised in that described defecator, also include for Support the support bar (10) of this device;Described support bar is at least 2.
10. phosphor ammonium slurry filter method as claimed in claim 7, it is characterised in that described device, filter bag (5) is high score Son separates film, is provided with support member so that filter bag (5) can support firm molding, and this support member can free skating Go out.
CN201610653162.4A 2016-08-11 2016-08-11 A kind of phosphor ammonium slurry filter device and its filter method Active CN106241763B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112915639A (en) * 2021-01-28 2021-06-08 云南中正化学工业有限公司 Slurry filter-pressing separation device for solid fertilizer production

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CN102602904A (en) * 2012-04-16 2012-07-25 瓮福(集团)有限责任公司 Method for producing monoammonium phosphate from raffinate acid
CN202657964U (en) * 2012-06-05 2013-01-09 瓮福(集团)有限责任公司 Device for producing industrial monoammonium phosphate with raffinate
CN202740863U (en) * 2012-08-08 2013-02-20 安徽六国化工股份有限公司 Monoammonium phosphate slurry filter
CN102947229A (en) * 2010-05-18 2013-02-27 奥斯特拉营养康复技术有限公司 Treatment of phosphate-containing wastewater

Patent Citations (5)

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Publication number Priority date Publication date Assignee Title
CN102947229A (en) * 2010-05-18 2013-02-27 奥斯特拉营养康复技术有限公司 Treatment of phosphate-containing wastewater
CN202185197U (en) * 2011-07-05 2012-04-11 吴杰 Filter used for refined wet process phosphoric acid
CN102602904A (en) * 2012-04-16 2012-07-25 瓮福(集团)有限责任公司 Method for producing monoammonium phosphate from raffinate acid
CN202657964U (en) * 2012-06-05 2013-01-09 瓮福(集团)有限责任公司 Device for producing industrial monoammonium phosphate with raffinate
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112915639A (en) * 2021-01-28 2021-06-08 云南中正化学工业有限公司 Slurry filter-pressing separation device for solid fertilizer production

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