CN106241763B - A kind of phosphor ammonium slurry filter device and its filter method - Google Patents

A kind of phosphor ammonium slurry filter device and its filter method Download PDF

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Publication number
CN106241763B
CN106241763B CN201610653162.4A CN201610653162A CN106241763B CN 106241763 B CN106241763 B CN 106241763B CN 201610653162 A CN201610653162 A CN 201610653162A CN 106241763 B CN106241763 B CN 106241763B
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Prior art keywords
filter
slurry
filtrate
phosphor ammonium
bag
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CN106241763A (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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    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Filtering Materials (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The present invention relates to phosphor ammonium slurry filtration arts, especially a kind of phosphor ammonium slurry filter device and its filter method, pass through the pH value of the phosphor ammonium slurry to entering filter device, temperature and phosphorus ammonium proportion, solid content is bound, after ensuring that phosphor ammonium slurry enters in filter device, liquid can rapid osmotic enter inside filter bag, so that filter bag support molding, in conjunction with aeration reverse osmosis filtration treatment, it can be effectively so that filtrate enters inside filter bag, and then impurity is remained in into filter bag outer surface, and in conjunction with the processing of falling bag and cleaning treatment, so that filter bag regeneration, and it is higher so that filtration difficulty to avoid filtrate viscosity, improve phosphorus ammonium purity in filtrate, the quality of phosphorus ammonium salt product is substantially ensured.

Description

A kind of phosphor ammonium slurry filter device and its filter method
Technical field
The present invention relates to phosphor ammonium slurry filtration art, especially a kind of phosphor ammonium slurry filter device and its filtering side Method.
Background technology
During wet phosphoric acid by dihydrate standing sedimentation, a large amount of solid precipitation slag will be precipitated, main component is phosphorus in slag Gypsum and (Fe, Al)3KH14(PO4)8·4H2O complex compounds, at the same also contain a large amount of soluble impurity, such as magnesium ion, calcium from Son, iron ion, aluminium ion, sulfate radical, fluosilicic acid root etc.;During phosphoric acid by wet process and ammonia neutralization reaction, these impurity will The compound for generating Various Complex, seriously affect the viscosity of phosphor ammonium slurry and the product form of phosphor ammonium slurry, physical characteristic and The dissolubility etc. of phosphorus pentoxide.Therefore, it when directly producing fine phosphorus ammonium salt product for phosphoric acid by wet process, needs to phosphor ammonium slurry It is filtered removal of impurities processing so that the quality for preparing phosphorus ammonium salt product is higher.
There are mainly three types of traditional phosphor ammonium slurry filter methods, gravitational settling, centrifugation, filter filtering;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 object is not easy rapid subsidence, in addition, because the reduction of slurry temperature will be brilliant with phosphorus ammonium salt in solid insoluble gravity settlement process Body is precipitated, and influences phosphor ammonium slurry utilization rate;Centrifugal separation equipment assembly is complicated, and inconvenient maintenance, investment and energy consumption are higher, and high viscous Property phosphor ammonium slurry easily block centrifugation rotatable parts;Filter plant currently be mainly plate and frame filter press and band filter etc., Filter is intermittent operation, and device switching is frequent, and filter cloth cleaning is inconvenient, for filtering the phosphorus ammonium material containing a certain amount of silica gel Slurry, equipment operation rate are extremely low.
It can be seen that there is numerous defects for phosphor ammonium slurry filter method in the prior art, all it is difficult to ensure that phosphorus ammonium The utilization rate of slurry is higher meanwhile, it is capable to improve the quality of phosphorus ammonium salt product, hinders phosphoric acid by wet process and directly prepares fine phosphorus The development of ammonium salt product.
Invention content
In order to solve the above technical problems existing in the prior art, the present invention provide a kind of phosphor ammonium slurry filter device and Its filter method.
It is achieved particular by following technical scheme:
A kind of phosphor ammonium slurry filter method, includes the following steps:
(1) at pH value it is 3-5, temperature 70-90 by the slurry preparation of phosphoric acid by wet process and ammonia neutralization reaction in filter pulp slot DEG C, solid content 1-2%, phosphorus ammonium proportion is the phosphor ammonium slurry of 1.1-1.3;
(2) by phosphor ammonium slurry be sent into filter device in, pass through be aerated reverse osmosis filtration treatment so that the filtrate of phosphor ammonium slurry into Entering in the filter bag of filter device, the filter residue of phosphor ammonium slurry stays in the outer surface of filter device filter bag and is deposited in filter device, It waits for that filter bag outer surface is blocked by slag blanket, and when filter bag internal filtrate amount is not further added by, starts the processing of falling bag so that filtrate enters Filtrate receiver;After the completion of bag, it is put into cleaning solution from cleaning liquid bath, rinses filter bag outer surface so that filter residue is cleaned to sinking Filter device, you can.
The step further includes after phosphor ammonium slurry is sent into filter device, and filtrate penetrates into the filter of filter device Bag is internal, and when filter residue deposits in filter device, lightweight filter residue enters the recoil of filter pulp slot from light slag slurry recoil hole and prepares phosphorus Ammonium slurry;Heavy slurry enters slurry slot from heavy slurry recoil hole, detects slurry concentration, if phosphorus pentoxide concentration is higher, And it is unsatisfactory for environmental emission standard, then returns to filter pulp slot and prepares phosphor ammonium slurry;If phosphorus pentoxide concentration is relatively low, and meets Environmental emission standard then discharges.
The step further includes after phosphor ammonium slurry is sent into filter device, and filtrate penetrates into the filter bag of filter device Interior, the supernatant liquor of filtrate constantly increases to the porous tube plate of filter device, and in the process, in filtrate concentration it is lower at Divide to sinking so that supernatant concentration is relatively low, and the low supernatant liquor of the concentration is entered filter pulp slot by filtrate refluxing opening Prepare phosphor ammonium slurry and/or by going cleaning solution notch to enter cleaning liquid bath.
The step is sent by phosphor ammonium slurry in filter device, uses pressure empty for the compression of 0.15-0.35MPa Gas is passed through filter device bottom and carries out Air Exposure, and the Air Exposure time is 1-2h.
The step is put into cleaning solution cleaning process from cleaning liquid bath in the after the completion of of falling bag, is used pressure The compressed air that power is 0.15-0.25MPa carries out Air Exposure, and aeration time is until filter bag outer surface slag blanket washes.
The step is put into from cleaning liquid bath in cleaning solution cleaning process, is first to be put into cleaning solution to impregnate 25- After 30min, then pressure is used to carry out Air Exposure for the compressed air of 0.15-0.25MPa.
The filter device, including cylinder, porous tube plate, filter bag, filtrate notch, phosphor ammonium slurry entrance, solarization air cap are removed, Wherein, inner barrel is provided with porous tube plate, the hole on porous tube plate is connected to the sack of filter bag, in cylinder close to the side at top It is provided with filtrate notch on wall, phosphor ammonium slurry entrance and solarization air cap are respectively arranged in bottom sidewall in cylinder;
The device further includes the filtrate refluxing opening being arranged on the side wall in cylinder close to top and removes cleaning solution notch With filter washing water inlet of the setting cylinder on the side wall of bottom;
The device further includes being arranged in the heavy slurry recoil hole of cylinder body bottom and being arranged in cylinder close to bottom Light slag slurry recoil hole on side wall.
The filter device, the longitudinal center line of solarization air cap are located at the bottom of filter bag.
The filter device further includes the supporting rod for being used to support the device;The supporting rod is at least 2.
The device, filter bag are polymeric membrane for separation, are provided with support element so that filter bag can be supported and be consolidated into Type, and the support element can be skidded off freely.
Compared with prior art, technique effect of the invention is embodied in:
It is bound by the pH value, temperature and phosphorus ammonium proportion, solid content of the phosphor ammonium slurry to entering filter device, really Protect after phosphor ammonium slurry enters in filter device, liquid can rapid osmotic enter inside filter bag so that filter bag support molding, in conjunction with It is aerated reverse osmosis filtration treatment, effectively filtrate can be entered inside filter bag, and then impurity is remained in filter bag outer surface, and And combine the processing of falling bag and cleaning treatment so that filter bag regenerates, and it is higher so that filtration difficulty, raising to avoid filtrate viscosity Phosphorus ammonium purity in filtrate, has substantially ensured the quality of phosphorus ammonium salt product.
The invention is the most outstanding to be, phosphor ammonium slurry filtering cost is relatively low, and low energy consumption, and equipment is simple, equipment cost Low, filter bag is easy to clean.
Description of the drawings
Fig. 1 is the phosphor ammonium slurry filtering technique flow diagram of the present invention.
A- filtrate receivers B- cleans liquid bath C- compressed gas D- filter device E- filter pulp slot F- slurry slots.
Fig. 2 is filter apparatus configuration schematic diagram.
1- filtrate refluxing openings 2- goes filtrate notch 3- that cleaning solution notch 4- porous tube plate 5- filter bag 6- cleaning solutions is gone to enter Mouth 7- solarization air cap 8- light slag slurries recoil hole 9- heavy slurries recoil hole 10- supporting rod 11- phosphor ammonium slurry entrances 12- Body.
Specific implementation mode
It is limited technical scheme of the present invention is further, but is required with specific embodiment below in conjunction with the accompanying drawings The range of protection describes made by being not only limited to.
Embodiment
The concrete principle and concrete operations mode of the present invention carries out in the following way, and those skilled in the art can be with The overall plan of the invention is understood according to the following contents:
A kind of phosphor ammonium slurry filter method, includes the following steps:
(1) at pH value it is 3-5, temperature 70- by the slurry preparation of phosphoric acid by wet process and ammonia neutralization reaction in filter pulp slot E 90 DEG C, solid content 1-2%, phosphorus ammonium proportion is the phosphor ammonium slurry of 1.1-1.3;
(2) phosphor ammonium slurry is sent into filter device D, by being aerated reverse osmosis filtration treatment so that the filtrate of phosphor ammonium slurry Into in the filter bag 5 of filter device D, the filter residue of phosphor ammonium slurry stays in the outer surface of filter device D filter bags 5 and in filter device D Middle deposition waits for that 5 outer surface of filter bag is blocked by slag blanket, and when 5 internal filtrate amount of filter bag is not further added by, and starts the processing of falling bag, makes It obtains filtrate and enters filtrate receiver A;After the completion of bag, it is put into cleaning solution from cleaning liquid bath B, rinses filter bag outer surface so that filter residue To sinking, and cleaning and filtrating equipment D, you can.Improve filtrate purity, it is ensured that the quality of phosphorus ammonium salt product, and realize Filtrate sedimentation was once dense.By being aerated reverse osmosis filtration treatment so that slag blanket remains in filter device, or passes through filter device Light slag slurry recoil hole or heavy slurry recoil hole exclude filter device so that phosphor ammonium slurry filtrate is purified, junction Reason process Air Exposure so that the rate that filter residue is adhered to filter bag outer surface slows down, and ensures to be adhered to filter bag outer surface Slag blanket is loose porous cellular, avoids filter bag regeneration difficult, reduces to filter bag cleaning of outer surface difficulty, realizes filtering dress The repeated reproducibility application set, reduces cost.
In certain embodiments, above-mentioned step further includes after phosphor ammonium slurry is sent into filter device D, and filtrate is oozed Thoroughly to filter device D filter bag 5 inside, when filter residue deposits in filter device D, lightweight filter residue from light slag slurry recoil hole 8 Phosphor ammonium slurry is prepared into the E recoils of filter pulp slot;Heavy slurry enters slurry slot 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 returns to filter pulp slot E and prepare phosphor ammonium slurry;If five It is relatively low to aoxidize two phosphorus concentrations, and meets environmental emission standard, then discharges.
In certain embodiments, above-mentioned step further includes the filtrate infiltration after phosphor ammonium slurry is sent into filter device D Into the filter bag 5 of filter device D, the supernatant liquor of filtrate constantly increases to the porous tube plate 4 of filter device D, and in this process In, the lower ingredient of concentration is to sinking in filtrate so that supernatant concentration is relatively low, and the low supernatant liquor of the concentration is passed through Filtrate refluxing opening 1 enters filter pulp slot E and prepares phosphor ammonium slurry and/or by going cleaning solution notch 3 to enter cleaning liquid bath B.
In certain embodiments, above-mentioned step is sent by phosphor ammonium slurry in filter device D, use pressure for The compressed air of 0.15MPa or 0.25MPa or 0.35MPa or 0.2MPa is passed through filter device bottom and carries out Air Exposure, aeration Processing time is 1h or 2h or 1.5h or 1.1h.Filter device load is reduced, cost and energy consumption are reduced.
In certain embodiments, above-mentioned step is put into cleaning solution cleaning in the after the completion of of falling bag from cleaning liquid bath B In the process, pressure is used to carry out Air Exposure, aeration time for the compressed air of 0.15MPa or 0.25MPa or 0.2MPa Until filter bag outer surface slag blanket washes.
In certain embodiments, above-mentioned step is put into from cleaning liquid bath in cleaning solution cleaning process, and being first will be clear After washing lotion is put into immersion 25min or 30min or 28min, then used pressure for 0.15MPa's or 0.25MPa or 0.2MPa Compressed air carries out Air Exposure.
In certain embodiments, above-mentioned filter device, including cylinder 12, porous tube plate 4, filter bag 5, go filtrate notch 2, Phosphor ammonium slurry entrance 11, solarization air cap 7, wherein cylinder 12 is internally provided with porous tube plate 4, the hole on porous tube plate 4 and filter bag 5 Sack connection, filtrate notch 2 is provided on side wall of the cylinder 12 close to top, in cylinder 12 in bottom sidewall point It is not provided with phosphor ammonium slurry entrance 11 and solarization air cap 7;
The device further includes the filtrate refluxing opening 1 being arranged on the side wall in cylinder 12 close to top and removes cleaning solution The filter washing water inlet 6 of notch 3 and setting cylinder 12 on the side wall of bottom;
The device, further include be arranged 12 bottom of cylinder heavy slurry recoil hole 9 and be arranged it is close in cylinder 12 Light slag slurry recoil hole 8 on the side wall of bottom.
In certain embodiments, above-mentioned filter device, the longitudinal center line of solarization air cap 7 are located at the bottom of filter bag 5.
In certain embodiments, above-mentioned filter device further includes the supporting rod 10 for being used to support the device;The branch Strut is 2,3.
In certain embodiments, above-mentioned device, filter bag 5 are polymeric membrane for separation, are provided with support element so that filter Bag 5 can support firm molding, and the support element can be skidded off freely.
In the invention, circular treatment is utilized so that the phosphorus ammonium ingredient 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 ingredient in filtrate, reduce phosphorus ammonium salt production Impurity content in product reduces phosphor ammonium slurry removal of impurities difficulty, reduces phosphor ammonium slurry removal of impurities cost.Processing step is simple, easily In industrialized production.

Claims (10)

1. a kind of phosphor ammonium slurry filter method, which is characterized in that include the following steps:
(1) at pH value it is 3-5 by the slurry preparation of phosphoric acid by wet process and ammonia neutralization reaction in filter pulp slot, 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 into filter device, by being aerated reverse osmosis filtration treatment so that the filtrate of phosphor ammonium slurry entered In the filter bag for filtering device, the filter residue of phosphor ammonium slurry stays in the outer surface of filter device filter bag and is deposited in filter device, 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 processing of falling bag so that filtrate enters filtrate Slot;After the completion of bag, it is put into cleaning solution from cleaning liquid bath, rinses filter bag outer surface so that filter residue cleans filtering to sinking Device, you can.
2. phosphor ammonium slurry filter method as described in claim 1, which is characterized in that the step further includes by phosphorus ammonium After slurry is sent into filter device, filtrate penetrates into inside the filter bag of filter device, light when filter residue deposits in filter device Matter filter residue enters the recoil of filter pulp slot from light slag slurry recoil hole and prepares phosphor ammonium slurry;Heavy slurry enters from heavy slurry recoil hole Slurry slot detects slurry concentration, if phosphorus pentoxide concentration is higher, and is unsatisfactory for environmental emission standard, then returns to filter pulp slot Prepare phosphor ammonium slurry;If phosphorus pentoxide concentration is relatively low, and meets environmental emission standard, then discharge.
3. phosphor ammonium slurry filter method as described in claim 1, which is characterized in that the step further includes by phosphorus ammonium After slurry is sent into filter device, filtrate penetrates into the filter bag of filter device, and the supernatant liquor of filtrate is constantly to filter device Porous tube plate increases, and in the process, and the higher ingredient of concentration is to sinking in filtrate so that and supernatant concentration is relatively low, and The low supernatant liquor of the concentration is entered into filter pulp slot by filtrate refluxing opening and prepares phosphor ammonium slurry and/or by removing cleaning solution notch Into cleaning liquid bath.
4. phosphor ammonium slurry filter method as described in claim 1, which is characterized in that the step is sent by phosphor ammonium slurry Enter in filter device, uses pressure to be passed through filter device bottom for the compressed air of 0.15-0.35MPa and carry out Air Exposure, expose The gas disposal time is 1-2h.
5. phosphor ammonium slurry filter method as described in claim 1, which is characterized in that the step, in the after the completion of of falling bag, It is put into cleaning solution cleaning process from cleaning liquid bath, pressure is used to be aerated for the compressed air of 0.15-0.25MPa Processing, aeration time is until filter bag outer surface slag blanket washes.
6. phosphor ammonium slurry filter method as claimed in claim 5, which is characterized in that the step, from cleaning liquid bath It is put into cleaning solution cleaning process, is after being first put into cleaning solution and impregnating 25-30min, then to be used pressure for 0.15- The compressed air of 0.25MPa carries out Air Exposure.
7. phosphor ammonium slurry filter method as claimed in any one of claims 1 to 6, which is characterized in that the filter device, packet It includes cylinder (12), porous tube plate (4), filter bag (5), remove filtrate notch (2), phosphor ammonium slurry entrance (11), solarization air cap (7), wherein Cylinder (12) is internally provided with porous tube plate (4), the hole on porous tube plate (4) is connected to the sack of filter bag (5), in cylinder (12) It is provided with filtrate notch (2) on the side wall at top, phosphorus ammonium material is respectively arranged in bottom sidewall in cylinder (12) Starch entrance (11) and solarization air cap (7);
The device further includes the filtrate refluxing opening (1) being arranged on the side wall in cylinder (12) close to top and removes cleaning solution The filter washing water inlet (6) of notch (3) and setting cylinder (12) on the side wall of bottom;
The device further includes that heavy slurry recoil hole (9) and setting of the setting in cylinder (12) bottom are leaned in cylinder (12) Light slag slurry recoil hole (8) on the side wall of nearly bottom.
8. phosphor ammonium slurry filter method as claimed in claim 7, which is characterized in that the filter device, solarization air cap (7) Longitudinal center line is located at the bottom of filter bag (5).
9. phosphor ammonium slurry filter method as claimed in claim 7, which is characterized in that the filter device further includes being used for Support the supporting rod (10) of the device;The supporting rod is at least 2.
10. phosphor ammonium slurry filter method as claimed in claim 7, which is characterized in that the device, filter bag (5) are high score Sub- seperation film, is provided with support element so that filter bag (5) can support firm molding, and the support element being capable of 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 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

Citations (5)

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Publication number Priority date Publication date Assignee Title
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
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)

* Cited by examiner, † Cited by third party
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
CN202740863U (en) * 2012-08-08 2013-02-20 安徽六国化工股份有限公司 Monoammonium phosphate slurry filter

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