CN107161966B - The method and device of Wet-process Phosphoric Acid Production Diammonium phosphate (DAP) - Google Patents
The method and device of Wet-process Phosphoric Acid Production Diammonium phosphate (DAP) Download PDFInfo
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- CN107161966B CN107161966B CN201710509627.3A CN201710509627A CN107161966B CN 107161966 B CN107161966 B CN 107161966B CN 201710509627 A CN201710509627 A CN 201710509627A CN 107161966 B CN107161966 B CN 107161966B
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/28—Ammonium phosphates
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Abstract
The invention discloses a kind of method and device of Wet-process Phosphoric Acid Production Diammonium phosphate (DAP), processes are as follows: preparing phosphoric acid by wet process；Phosphoric acid by wet process pretreatment；It is primary to neutralize；Belt feeder filtering；Secondary neutralization；Secondary filter press filtering；Index is adjusted；Condensing crystallizing；Separation drying.The beneficial effects of the present invention are: replacing thermal phosphoric acid to prepare PHOSPHORIC ACID TECH.GRADE potassium dihydrogen using liquid extraction phosphoric acid, achievees the purpose that reduce production cost, promoted product competitiveness in the market.This technique takes Recycling Mother Solution processing to carry out deep impurity-removing matter, can be good at solving the contaminant problem in phosphoric acid by wet process, meets the production requirement of PHOSPHORIC ACID TECH.GRADE potassium dihydrogen, and makes to produce continuous and steady operation.To reach reduction production cost, the effect of product competitiveness in the market is promoted.
Description
Technical field
The present invention relates to a kind of methods of industrial production Diammonium phosphate (DAP), more particularly to a kind of Wet-process Phosphoric Acid Production di(2-ethylhexyl)phosphate
The method and device of ammonium.
Background technique
Diammonium phosphate (DAP) is a kind of high-concentration compound fertilizer, because of its nutrient height, is widely used in the fertilising of all kinds of plants.It passes
Almost all is raw material production using thermal phosphoric acid in technique of uniting, since 2003, since China Power commercialization paces are accelerated
And power shortages, leading to thermal phosphoric acid rise in price, many ammonium phosphate production producers have to stop production because cost is excessively high,
It is in great shortage so as to cause the market source of goods, so that the spurt in prices of PHOSPHORIC ACID TECH.GRADE ammonium, domestic many R&D institutions and phosphate production
Producer all actively develops research of technique.Wet production is to use inorganic acid decomposing rock phosphate with hydrogen, isolates raw phosphoric acid, then purified rear system
Obtain phosphoric acid product.Phosphoric acid by wet process method of specific heat phosphoric acid 20%-30% at low cost, and it is more energy saving, and Wet Processes of Phosphoric Acid has been located at present
In the leading position of phosphoric acid production.
It is the main technique that raw material produces PHOSPHORIC ACID TECH.GRADE diammonium using phosphoric acid by wet process are as follows: phosphoric acid by wet process desulfurization defluorinate → mono-
It is secondary to neutralize → once filtering → secondary neutralization → secondary filter → vacuum concentration → crystallisation by cooling → fluidized drying.Liquid extraction phosphorus
Containing the cations such as a large amount of iron, aluminium, magnesium, silicon in acid, content 3-5%, while fluorine in phosphoric acid by wet process containing 1-3% and sulfate radical etc.
Anion.Purity can only be produced mostly with phosphoric acid by wet process at present as the product of 96% or 98% rank, and water-insoluble therein
It is highest to reach 0.5% in O.1% left and right.
In addition, domestic industry features of DAP production producer, filter progress are all made of filter press and filter at present, same production capacity,
Required matched filter press number of units is more, and labor intensity of workers is big, and filter cloth unpicks and washes difficulty, and production auxiliary material consumption is big, continuous production
Difference.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of methods of Wet-process Phosphoric Acid Production Diammonium phosphate (DAP)
And device, thermal phosphoric acid is replaced using liquid extraction phosphoric acid, reaches reduction production cost, promotes the mesh of product competitiveness in the market
's；It takes Recycling Mother Solution processing to carry out the work of deep impurity-removing matter, can solve the contaminant problem in phosphoric acid by wet process.
The purpose of the present invention is achieved through the following technical solutions: the method for Wet-process Phosphoric Acid Production Diammonium phosphate (DAP), packet
Include following steps:
S1: phosphoric acid by wet process preparing phosphoric acid by wet process: is made with sulfuric acid decomposition phosphorus ore；
S2: phosphoric acid by wet process pretreatment: carrying out engaging sulphate to phosphoric acid by wet process and defluorinate handled, and then adds complexing agent to wet
Cation impurity in method phosphoric acid is handled；
S3: primary to neutralize: deep purifying agent to be added into pretreated phosphoric acid by wet process, while using in gas ammonia progress
With curing；It is passed through gas ammonia while stirring, when the molar ratio of gas ammonia and phosphoric acid wait be passed through is 0.4-0.8, continues to stir 20-
25min, and heating treatment is carried out, heating rate is 0.4-0.6 DEG C/min, and adjustment degree of neutralization to 0.6-0.8 stops heating, obtains
Obtain solidliquid mixture；
S4: belt feeder filtering: it will once neutralize obtained solidliquid mixture slurry and import belt feeder progress solid-liquid point
From liquid enters next process；
S5: secondary neutralization secondary neutralization: is carried out to the liquid being once obtained by filtration using gas ammonia；It is passed through gas while stirring
Ammonia, when the molar ratio of gas ammonia and phosphoric acid wait be passed through is 1.4-1.6, adjustment solution ph is 5.3-5.6, obtains Diammonium phosphate (DAP) material
Slurry；
S6: secondary filter press filtering: importing filter press progress secondary filter for the secondary obtained slurry that neutralizes, isolated
Solid drying after be made the white fertilizer of accessory substance, isolated liquid be Diammonium phosphate (DAP) clear liquid；
S7: index is adjusted: regulator is added in isolated Diammonium phosphate (DAP) clear liquid and carries out index accurate adjustment；
S8: crystallization: qualified Diammonium phosphate (DAP) solution is adjusted to index and is concentrated, and crystallizer is added and is crystallized；
S9: separation drying: centrifuge is added in the Diammonium phosphate (DAP) after crystallization and is separated by solid-liquid separation, it is dry that solid is sent into fluidized bed
Dry device is dried, and finished industrial grade Diammonium phosphate (DAP) is obtained, and Recycling Mother Solution uses.
In the phosphoric acid by wet process pre-treatment step, further includes a supernatant purifying step before desulfurization defluorinate processing, sink
Precipitation goes out the dissolubility impurity in phosphoric acid by wet process.
The deep purifying agent is polyacrylamide, and the regulator is PHOSPHORIC ACID TECH.GRADE.
The step of Recycling Mother Solution uses in step S9 are as follows: the mother liquor for separating centrifuge continues sedimentation separation,
Feeding fluidized bed dryer after centrifuge carries out secondary centrifuging is sent into the crystallization isolated is dried, and the liquid isolated is successively
The Diammonium phosphate (DAP) solution that mother liquor adjusts qualification with the obtained index of step S7 is formed after progress mother liquor neutralization, filters pressing separation to be mixed into
Row concentration.
Produce the device of Diammonium phosphate (DAP), including clarifying tank, desulfurization pond, a neutralization bucket, belt feeder, secondary neutralization bucket, pressure
Filter, crystallizer, dashpot, centrifuge and fluidized bed dryer, phosphoric acid by wet process inject clarifying tank, and the outlet connection of clarifying tank is de-
The entrance in sulphur pond, the outlet in desulfurization pond pass sequentially through the entrance phase of a neutralization bucket, belt feeder and secondary neutralization bucket with filter press
Even, the white fertilizer of accessory substance is made after the solid drying that filter press is isolated, the Diammonium phosphate (DAP) clear liquid that filter press is isolated injects concentration
In the clear liquid entrance of tank, the outlet of concentration tank passes sequentially through crystallizer and dashpot and is connected with the feed inlet of centrifuge, centrifuge
The solid isolated, which is sent into fluidized bed dryer, is dried, and finished industrial grade Diammonium phosphate (DAP), the mother that centrifuge is isolated are obtained
Liquid injects the entrance of sedimentation separation bucket, and the crystallization that sedimentation separation bucket is isolated is connected with the feed inlet of centrifuge, sedimentation separation bucket
The liquid isolated is connected with the entrance of mother liquor neutralization bucket, and the outlet of mother liquor neutralization bucket passes through the mother of filters pressing separator and concentration tank
The connection of liquid entrance.
The belt feeder includes filter cloth rate of tension regulating device, and filter cloth rate of tension regulating device is mounted on the machine of belt feeder
On frame, including filter cloth tensioning wheel, fixing seat, the leading truck for adjusting screw rod and being symmetrically disposed on filter cloth tensioning wheel two sides, leading truck
It is fixedly mounted with fixing seat on the rack, the both ends of filter cloth tensioning wheel are connected separately with first bearing seat, and leading truck is equipped with
The guide chute matched with first bearing seat, fixing seat are equipped with the threaded hole matched with adjusting screw rod, adjust screw rod
The threaded hole that top passes through in fixing seat is connected with first bearing seat, adjusts screw rod and drives first bearing seat when threadingly hole rotates
It is slided up and down along guide chute, the rate of tension for completing filter cloth is adjusted.
The belt feeder includes belt tightening regulating device, and belt tightening regulating device includes leather belt roller and symmetrical
Pedestal set on leather belt roller two sides, the both ends of leather belt roller are installed on the base by second bearing seat respectively, the pedestal packet
Work shape bracket and floor stringer are included, work shape bracket is made of the first upright bar, the second upright bar and crossbeam, and floor stringer and crossbeam are mutually flat
It goes, bar shaped sliding block is equipped on the inside of floor stringer and crossbeam, the two sides of the second bearing seat are equipped with to be matched with bar shaped sliding block
Sliding slot；
It further include tensing screw rod, the first upright bar is equipped with the threaded hole matched with tension screw rod, tenses the top of screw rod
Threaded hole in the first upright bar is connected with second bearing seat, tenses screw rod and drives second bearing seat to exist when threadingly hole rotates
Traversing along bar shaped sliding block direction between floor stringer and crossbeam, the rate of tension for completing belt is adjusted.
The belt feeder includes Pneumatic type leather belt offset apparatus for correcting, and it includes correction that Pneumatic type leather belt, which deviates apparatus for correcting,
Roll shaft and corrective component, corrective component include at least one be set to belt side stroke inductive switch, microcontroller it is gentle
Dynamic to adjust component, stroke inductive switch is connected with the sampled signal input of microcontroller, the enabled letter of microcontroller
Number output end is connected with the pneumatic component that adjusts；The non-moving end of correction roll shaft is hinged on rack I, and the moved end for correcting roll shaft passes through gas
The dynamic component that adjusts is mounted on rack II；
The pneumatic adjusting component includes the first air bag group and the second air bag group, the first air bag group and the second air bag component
Be not set to the two sides of correction roll shaft moved end, the inflation/deflation driving circuit of the first air bag group and the second air bag group respectively with microcontroller
The enable signal output end of device MCU is connected.
The fluidized bed dryer includes vibrating feed device, vibrating feed device include loading hopper, fluidized bed into
Material mouth and the vibration drapery panel being obliquely installed, the discharge port of loading hopper are set to above the high order end of vibration drapery panel, vibration
The low order end of drapery panel is set to above fluidized bed feed inlet, is equipped with oscillation drive on the vibration drapery panel, institute
The both ends for stating vibration drapery panel are symmetrically arranged with resonant component, and every group of resonant component includes sunpender and spring, and the top of sunpender is fixed
It is mounted in reference seat, movable cushion block is socketed on sunpender, the bottom of sunpender is equipped with fixed cushion block, one end of spring and activity
Cushion block is fixedly connected, and the other end of spring is connect with fixed cushion block, and vibration drapery panel is fixedly connected with movable cushion block.
It is fixedly installed with U-shaped frame on the side wall of the vibration drapery panel, is equipped on the transverse slat and movable cushion block of U-shaped frame
The through-hole matched with sunpender, sunpender sequentially pass through U-shaped frame transverse slat, movable cushion block and spring and connect with fixed cushion block, activity mat
The upper top surface of block is fixedly connected with U-shaped frame transverse slat.
The beneficial effects of the present invention are:
1) this technique replaces thermal phosphoric acid to prepare PHOSPHORIC ACID TECH.GRADE diammonium using liquid extraction phosphoric acid, has reached reduction production
Cost, the purpose for promoting product competitiveness in the market.
2) filter progress replaces filter press using belt feeder, and same production capacity can reduce recruitment 90%, and greatly reduce worker
Labor intensity, after belt feeder, labor intensity is only original 10%.
3) this technique takes secondary neutralisation and Recycling Mother Solution to handle and carries out deep impurity-removing matter, can be good at solving wet process
Contaminant problem in phosphoric acid meets the production requirement of PHOSPHORIC ACID TECH.GRADE diamino, improves output capacity (85-90%), and keeps production continuous
Stable operation.To reach reduction production cost, the effect of product competitiveness in the market is promoted.
4) when Wet-process Phosphoric Acid Production comes out in addition to containing solid impurity, many of these dissolubility impurity are under storage requirement
In hypersaturated state, therefore has precipitating and be slowly precipitated.Supernatant purification is carried out before desulfurization defluorinate is handled, it can be with Precipitation
Dissolubility impurity in phosphoric acid by wet process, being capable of further purification of wet process phosphoric acid.
5) sliding for being driven tension wheel shaft bearing seat in filter cloth and belt tightening regulating device using screw rod, is improved
The accuracy of tightness adjustment process keeps the movement of bearing block more intuitive by the adjusting of screw rod, carries out convenient for operator micro-
It adjusts.
6) deviation angle of correction roll shaft is fine-tuned by correcting the inflation/deflation of air bag, so that it is inclined to drive belt to complete
Correction is moved, the automatic detection of belt offset is realized and is corrected certainly, intelligent, high degree of automation.
7) vibration drapery panel is additionally arranged between loading hopper and fluidized bed feed inlet, realize material further cloth and
It crushes, provides powerful guarantee for fluidized bed drying effect；Resonant component structure is simple, ingenious in design, and vibrates steady, operation
When without critical noisy.Fixed cushion block can be used adjustable mode and be mounted on sunpender, by the position-adjustable for adjusting fixed cushion block
Drapery panel height achievees the purpose that adjust cloth height.
Detailed description of the invention
Fig. 1 is present invention process method flow diagram；
Fig. 2 is filter cloth rate of tension regulating device structural schematic diagram one of the present invention；
Fig. 3 is filter cloth rate of tension regulating device structural schematic diagram two of the present invention；
Fig. 4 is inventive belt rate of tension regulating device structural schematic diagram；
Fig. 5 is the bearing block structure schematic diagram in inventive belt rate of tension regulating device；
Fig. 6 is that Pneumatic type leather belt of the present invention deviates apparatus for correcting structural schematic diagram；
Fig. 7 is vibrating feed device structural schematic diagram of the present invention；
Fig. 8 is the resonant component structural schematic diagram in vibrating feed device of the present invention.
Specific embodiment
Technical solution of the present invention is described in further detail with reference to the accompanying drawing, but protection scope of the present invention is not limited to
It is as described below.
[embodiment 1] as shown in Figure 1, Wet-process Phosphoric Acid Production Diammonium phosphate (DAP) method, comprising the following steps:
S1: phosphoric acid by wet process preparing phosphoric acid by wet process: is made with sulfuric acid decomposition phosphorus ore；
S2: phosphoric acid by wet process pretreatment: carrying out engaging sulphate to phosphoric acid by wet process and defluorinate handled, and then adds complexing agent to wet
Cation impurity in method phosphoric acid is handled；
In the phosphoric acid by wet process pre-treatment step, further includes a supernatant purifying step before desulfurization defluorinate processing, sink
Precipitation goes out the dissolubility impurity in phosphoric acid by wet process.It is many of these molten when Wet-process Phosphoric Acid Production comes out in addition to containing solid impurity
Solution property impurity is in hypersaturated state under storage requirement, therefore has precipitating and be slowly precipitated.It is carried out before desulfurization defluorinate is handled
Supernatant purification, can be with the dissolubility impurity in Precipitation phosphoric acid by wet process, being capable of further purification of wet process phosphoric acid.
S3: primary to neutralize: it is added polyacrylamide into pretreated phosphoric acid by wet process, molecular formula (C3H5NO) n, simultaneously
It neutralized, cured using gas ammonia；It is passed through gas ammonia while stirring, when the molar ratio of gas ammonia and phosphoric acid wait be passed through is 0.4, continues
20min is stirred, and carries out heating treatment, heating rate is 0.4 DEG C/min, and adjustment degree of neutralization to 0.6 stops heating, consolidate
Liquid mixture；
S4: belt feeder filtering: it will once neutralize obtained solidliquid mixture slurry and import belt feeder progress solid-liquid point
From liquid enters next process；
S5: secondary neutralization secondary neutralization: is carried out to the liquid being once obtained by filtration using gas ammonia；It is passed through gas while stirring
Ammonia, when the molar ratio of gas ammonia and phosphoric acid wait be passed through is 1.4, adjustment solution ph is 5.3, obtains diammonium phosphate slurry；
S6: secondary filter press filtering: importing filter press progress secondary filter for the secondary obtained slurry that neutralizes, isolated
Solid drying after be made the white fertilizer of accessory substance, isolated liquid be Diammonium phosphate (DAP) clear liquid；
S7: index is adjusted: PHOSPHORIC ACID TECH.GRADE is added in isolated Diammonium phosphate (DAP) clear liquid, molecular formula H3PO4 is referred to
Mark accurate adjustment；
S8: crystallization: qualified Diammonium phosphate (DAP) solution is adjusted to index and is concentrated, and crystallizer is added and is crystallized；
S9: separation drying: centrifuge is added in the Diammonium phosphate (DAP) after crystallization and is separated by solid-liquid separation, it is dry that solid is sent into fluidized bed
Dry device is dried, and finished industrial grade Diammonium phosphate (DAP) is obtained, and Recycling Mother Solution uses.
[embodiment 2] as shown in Figure 1, Wet-process Phosphoric Acid Production Diammonium phosphate (DAP) method, comprising the following steps:
S1: phosphoric acid by wet process preparing phosphoric acid by wet process: is made with sulfuric acid decomposition phosphorus ore；
S2: phosphoric acid by wet process pretreatment: carrying out engaging sulphate to phosphoric acid by wet process and defluorinate handled, and then adds complexing agent to wet
Cation impurity in method phosphoric acid is handled；
S3: primary to neutralize: polyacrylamide to be added into pretreated phosphoric acid by wet process, while using in gas ammonia progress
With curing；It is passed through gas ammonia while stirring, when the molar ratio of gas ammonia and phosphoric acid wait be passed through is 0.8, continues to stir 25min, go forward side by side
Row heating treatment, heating rate are 0.6 DEG C/min, and adjustment degree of neutralization to 0.8 stops heating, obtain solidliquid mixture；
S4: belt feeder filtering: it will once neutralize obtained solidliquid mixture slurry and import belt feeder progress solid-liquid point
From liquid enters next process；
S5: secondary neutralization secondary neutralization: is carried out to the liquid being once obtained by filtration using gas ammonia；It is passed through gas while stirring
Ammonia, when the molar ratio of gas ammonia and phosphoric acid wait be passed through is 1.6, adjustment solution ph is 5.6, obtains diammonium phosphate slurry；
S6: secondary filter press filtering: importing filter press progress secondary filter for the secondary obtained slurry that neutralizes, isolated
Solid drying after be made the white fertilizer of accessory substance, isolated liquid be Diammonium phosphate (DAP) clear liquid；
S7: index is adjusted: PHOSPHORIC ACID TECH.GRADE is added in isolated Diammonium phosphate (DAP) clear liquid and carries out index accurate adjustment；
S8: crystallization: qualified Diammonium phosphate (DAP) solution is adjusted to index and is concentrated, and crystallizer is added and is crystallized；
S9: separation drying: centrifuge is added in the Diammonium phosphate (DAP) after crystallization and is separated by solid-liquid separation, it is dry that solid is sent into fluidized bed
Dry device is dried, and finished industrial grade Diammonium phosphate (DAP) is obtained, and Recycling Mother Solution uses.
[embodiment 3] as shown in Figure 1, Wet-process Phosphoric Acid Production Diammonium phosphate (DAP) method, comprising the following steps:
S1: phosphoric acid by wet process preparing phosphoric acid by wet process: is made with sulfuric acid decomposition phosphorus ore；
S2: phosphoric acid by wet process pretreatment: carrying out engaging sulphate to phosphoric acid by wet process and defluorinate handled, and then adds complexing agent to wet
Cation impurity in method phosphoric acid is handled；
S3: primary to neutralize: polyacrylamide to be added into pretreated phosphoric acid by wet process, while using in gas ammonia progress
With curing；It is passed through gas ammonia while stirring, when the molar ratio of gas ammonia and phosphoric acid wait be passed through is 0.5, continues to stir 23min, go forward side by side
Row heating treatment, heating rate are 0.5 DEG C/min, and adjustment degree of neutralization to 0.7 stops heating, obtain solidliquid mixture；
S4: belt feeder filtering: it will once neutralize obtained solidliquid mixture slurry and import belt feeder progress solid-liquid point
From liquid enters next process；
S5: secondary neutralization secondary neutralization: is carried out to the liquid being once obtained by filtration using gas ammonia；It is passed through gas while stirring
Ammonia, when the molar ratio of gas ammonia and phosphoric acid wait be passed through is 1.5, adjustment solution ph is 5.5, obtains diammonium phosphate slurry；
S6: secondary filter press filtering: importing filter press progress secondary filter for the secondary obtained slurry that neutralizes, isolated
Solid drying after be made the white fertilizer of accessory substance, isolated liquid be Diammonium phosphate (DAP) clear liquid；
S7: index is adjusted: PHOSPHORIC ACID TECH.GRADE is added in isolated Diammonium phosphate (DAP) clear liquid and carries out index accurate adjustment；
S8: crystallization: qualified Diammonium phosphate (DAP) solution is adjusted to index and is concentrated, and crystallizer is added and is crystallized；
S9: separation drying: centrifuge is added in the Diammonium phosphate (DAP) after crystallization and is separated by solid-liquid separation, it is dry that solid is sent into fluidized bed
Dry device is dried, and finished industrial grade Diammonium phosphate (DAP) is obtained, and Recycling Mother Solution uses.
[embodiment 4] as shown in Figure 1, Wet-process Phosphoric Acid Production Diammonium phosphate (DAP) method, comprising the following steps:
S1: phosphoric acid by wet process preparing phosphoric acid by wet process: is made with sulfuric acid decomposition phosphorus ore；
S2: phosphoric acid by wet process pretreatment: carrying out engaging sulphate to phosphoric acid by wet process and defluorinate handled, and then adds complexing agent to wet
Cation impurity in method phosphoric acid is handled；
S3: primary to neutralize: polyacrylamide to be added into pretreated phosphoric acid by wet process, while using in gas ammonia progress
With curing；It is passed through gas ammonia while stirring, when the molar ratio of gas ammonia and phosphoric acid wait be passed through is 0.6, continues to stir 22min, go forward side by side
Row heating treatment, heating rate are 0.5 DEG C/min, and adjustment degree of neutralization to 0.6 stops heating, obtain solidliquid mixture；
S4: belt feeder filtering: it will once neutralize obtained solidliquid mixture slurry and import belt feeder progress solid-liquid point
From liquid enters next process；
S5: secondary neutralization secondary neutralization: is carried out to the liquid being once obtained by filtration using gas ammonia；It is passed through gas while stirring
Ammonia, when the molar ratio of gas ammonia and phosphoric acid wait be passed through is 1.6, adjustment solution ph is 5.4, obtains diammonium phosphate slurry；
S6: secondary filter press filtering: importing filter press progress secondary filter for the secondary obtained slurry that neutralizes, isolated
Solid drying after be made the white fertilizer of accessory substance, isolated liquid be Diammonium phosphate (DAP) clear liquid；
S7: index is adjusted: PHOSPHORIC ACID TECH.GRADE is added in isolated Diammonium phosphate (DAP) clear liquid and carries out index accurate adjustment；
S8: crystallization: qualified Diammonium phosphate (DAP) solution is adjusted to index and is concentrated, and crystallizer is added and is crystallized；
S9: separation drying: centrifuge is added in the Diammonium phosphate (DAP) after crystallization and is separated by solid-liquid separation, it is dry that solid is sent into fluidized bed
Dry device is dried, and finished industrial grade Diammonium phosphate (DAP) is obtained, and Recycling Mother Solution uses.
As shown in Figure 1, the device of production Diammonium phosphate (DAP), including it is clarifying tank, desulfurization pond, a neutralization bucket, belt feeder, secondary
Neutralization bucket, filter press, crystallizer, dashpot, centrifuge and fluidized bed dryer, phosphoric acid by wet process inject clarifying tank, clarifying tank
The entrance in outlet connection desulfurization pond, the outlet in desulfurization pond passes sequentially through a neutralization bucket, belt feeder and secondary neutralization bucket and filters pressing
The entrance of machine is connected, and the white fertilizer of accessory substance is made after the solid drying that filter press is isolated, the Diammonium phosphate (DAP) that filter press is isolated is clear
Liquid injects in the clear liquid entrance of concentration tank, and the outlet of concentration tank passes sequentially through the feed inlet phase of crystallizer and dashpot with centrifuge
Even, the solid that centrifuge is isolated, which is sent into fluidized bed dryer, is dried, and finished industrial grade Diammonium phosphate (DAP), centrifuge point are obtained
The entrance of the mother liquor injection sedimentation separation bucket separated out, the crystallization that sedimentation separation bucket is isolated are connected with the feed inlet of centrifuge, sink
The liquid isolated of drop separating barrel is connected with the entrance of mother liquor neutralization bucket, the outlet of mother liquor neutralization bucket pass through filters pressing separator with it is dense
The mother liquor entrance of contracting tank connects.
As shown in Fig. 2, belt feeder includes filter cloth rate of tension regulating device, filter cloth rate of tension regulating device is mounted on belt feeder
Rack 1 on, including filter cloth tensioning wheel 2, fixing seat 5, adjust screw rod 6 and be symmetrically disposed on the guiding of 2 two sides of filter cloth tensioning wheel
Frame 3, leading truck 3 and fixing seat 5 are fixedly mounted in rack 1, and the both ends of filter cloth tensioning wheel 2 are connected separately with first bearing seat
4, leading truck 3 is equipped with the guide chute 7 matched with first bearing seat 4, and fixing seat 5 is equipped with to be matched with adjusting screw rod 6
Threaded hole, adjust screw rod 6 top pass through fixing seat 5 on threaded hole be connected with first bearing seat 4, adjusting screw rod 6 along spiral shell
Driving first bearing seat 4 is slided up and down along guide chute 7 when pit rotates, and the rate of tension for completing filter cloth is adjusted.
As a further improvement, cooperating location hole as shown in figure 3, be additionally provided with location hole 3.1 on the side wing of leading truck 3
3.1 use positioning pin 3.2, adjust in filter cloth tensioning wheel 2 to (rate of tension is moderate) behind appropriate location, it is fixed that positioning pin 3.2 is passed through
Position hole 3.1 is simultaneously pressed in first bearing seat 4, can reach the purpose for further fixing filter cloth tensioning wheel 2.
As shown in figure 4, belt feeder includes belt tightening regulating device, belt tightening regulating device includes leather belt roller 8
With the pedestal for being symmetrically set in 8 two sides of leather belt roller, the both ends of leather belt roller 8 pass through the installation of second bearing seat 13 on the base respectively, institute
The pedestal stated includes work shape bracket and floor stringer 9, and work shape bracket is made of the first upright bar 10, the second upright bar 11 and crossbeam 12, auxiliary
Beam 9 is helped to be parallel to each other with crossbeam 12, the inside of floor stringer 9 and crossbeam 12 is equipped with bar shaped sliding block 14, the second bearing seat 13
To be equipped with the sliding slot 15(that matches with bar shaped sliding block 14 as shown in Figure 5 for two sides)；It further include tensing screw rod 16, in the first upright bar 10
Equipped with the threaded hole matched with tension screw rod 16, threaded hole and second of the top of screw rod 16 in the first upright bar 3 is tensed
Bearing block 13 is connected, and tenses screw rod 16 and drives the edge between floor stringer 9 and crossbeam 12 of second bearing seat 13 when threadingly hole rotates
14 direction of bar shaped sliding block is traversing, and the rate of tension for completing belt is adjusted.
As shown in fig. 6, belt feeder includes Pneumatic type leather belt offset apparatus for correcting, Pneumatic type leather belt offset apparatus for correcting includes
Roll shaft 18 and corrective component are corrected, corrective component includes two stroke inductive switch 19, the microcontrollers for being set to 17 two sides of belt
MCU20 and pneumatic adjusting component, stroke inductive switch 19 are connected with the sampled signal input of microcontroller 20, microcontroller
The enable signal output end of device MCU20 is connected with the pneumatic component that adjusts；The non-moving end of correction roll shaft 18 is hinged on rack I24,
The moved end for correcting roll shaft 18 is mounted on rack II21 by pneumatically adjusting component；The pneumatic adjusting component includes the first gas
Capsule group 22 and the second air bag group 23, the first air bag group 22 and the second air bag group 23 are respectively arranged at the two of correction 18 moved end of roll shaft
The inflation/deflation driving circuit of side, the first air bag group 22 and the second air bag group 23 is defeated with the enable signal of microcontroller 20 respectively
Outlet is connected.
The course of work that Pneumatic type leather belt deviates apparatus for correcting is as follows: when 17 angle of belt shifts, first by setting
Stroke inductive switch 19 in 17 two sides of belt senses the information of the offset, and stroke inductive switch 19 transmits a signal to micro-control
Device MCU20 processed, and analysis is handled by microcontroller 20 and exports control signal to positioned at the first of correction 18 moved end two sides of roll shaft
Air bag group 22 and the second air bag group 23 push correction roll shaft 18 to enclose by the inflation/deflation of the first air bag group 22 and the second air bag group 23
Thin tail sheep rotation occurs around its non-moving end, to realize the adjustment of correction 18 angle of roll shaft.
As shown in fig. 7, the fluidized bed dryer includes vibrating feed device, vibrating feed device includes loading hopper
25, fluidized bed feed inlet 26 and the vibration drapery panel 27 being obliquely installed, the discharge port of loading hopper 25 are set to vibration drapery panel
Above 27 high order end, the low order end of vibration drapery panel 27 is set to 26 top of fluidized bed feed inlet, the vibration drapery panel
Oscillation drive is installed, oscillation drive is specially eccentric motor 33, and eccentric motor 33 passes through clevis mounting 34 on 27
It is fixedly mounted on the bottom plate of vibration drapery panel 27.The protective plate 35 increased is additionally provided on the side wall of the vibration drapery panel 27.
The both ends of the vibration drapery panel 27 are symmetrically arranged with resonant component, and every group of resonant component includes sunpender 28 and spring 29, sunpender 28
Top be fixedly mounted in reference seat 30, movable cushion block 31 is socketed on sunpender 28, the bottom of sunpender 28 is equipped with fixed pad
One end of block 32, spring 29 is fixedly connected with movable cushion block 31, and the other end of spring 29 is connect with fixed cushion block 32, vibrates cloth
Plate 27 is fixedly connected with movable cushion block 31.
Specifically, as shown in figure 8, being fixedly installed with U-shaped frame 37, U-shaped frame 37 on the side wall of the vibration drapery panel 27
Transverse slat and movable cushion block 31 on be equipped with the through-hole matched with sunpender 28, sunpender 28 sequentially passes through 37 transverse slat of U-shaped frame, activity
Cushion block 31 and spring 29 are connect with fixed cushion block 32, and the upper top surface of movable cushion block 31 is fixedly connected with 37 transverse slat of U-shaped frame.
As shown in figure 8, the top of sunpender 28 is fixedly mounted in reference seat 30 by L shape connecting rod 36, it is socketed on sunpender 28
There is movable cushion block 31,32 center of fixation cushion block is equipped with the through-hole matched with sunpender 28, the bottom surface of fixed cushion block 32
It is fixed with adjusting nut 38, the bottom of sunpender 28 is the screw rod cooperated with adjusting nut 38.By the position for adjusting fixed cushion block 32
The height for setting adjustable vibration drapery panel 27, achievees the purpose that adjust cloth height.
The working principle of vibrating feed device is as follows: powdered Diammonium phosphate (DAP) material falls on vibration cloth from loading hopper 25
First time cloth is completed on plate 27, the work of eccentric motor 33 drives entire vibration drapery panel 27 to generate extensional vibration and completes material
Secondary material distributing, material, which gradually slides to enter in fluidized bed feed inlet 26 from inclined vibration drapery panel 27, completes cloth three times.
The above is only a preferred embodiment of the present invention, it should be understood that the present invention is not limited to described herein
Form should not be regarded as an exclusion of other examples, and can be used for other combinations, modifications, and environments, and can be at this
In the text contemplated scope, modifications can be made through the above teachings or related fields of technology or knowledge.And those skilled in the art institute into
Capable modifications and changes do not depart from the spirit and scope of the present invention, then all should be in the protection scope of appended claims of the present invention
It is interior.
Claims (7)
1. the method for Wet-process Phosphoric Acid Production Diammonium phosphate (DAP), which comprises the following steps:
S1: phosphoric acid by wet process preparing phosphoric acid by wet process: is made with sulfuric acid decomposition phosphorus ore；
S2: phosphoric acid by wet process pretreatment: carrying out engaging sulphate to phosphoric acid by wet process and defluorinate handled, and then adds complexing agent to wet process phosphorus
Cation impurity in acid is handled；
S3: primary to neutralize: deep purifying agent being added into pretreated phosphoric acid by wet process, while being neutralized using gas ammonia, is ripe
Change；It is passed through gas ammonia while stirring, when the molar ratio of gas ammonia and phosphoric acid wait be passed through is 0.4-0.8, continues to stir 20-25min, and
Heating treatment is carried out, heating rate is 0.4-0.6 DEG C/min, and adjustment degree of neutralization to 0.6-0.8 stops heating, and it is mixed to obtain solid-liquid
Close object；
S4: belt feeder filtering: will once neutralize obtained solidliquid mixture slurry importing belt feeder and be separated by solid-liquid separation, liquid
Body enters next process；
The belt feeder includes filter cloth rate of tension regulating device, and filter cloth rate of tension regulating device is mounted on the rack of belt feeder
(1) on, including filter cloth tensioning wheel (2), fixing seat (5), screw rod (6) is adjusted and are symmetrically disposed on filter cloth tensioning wheel (2) two sides
Leading truck (3), leading truck (3) and fixing seat (5) are fixedly mounted on rack (1), and the both ends of filter cloth tensioning wheel (2) connect respectively
It is connected to first bearing seat (4), leading truck (3) is equipped with the guide chute (7) matched with first bearing seat (4), fixing seat (5)
Be equipped with and adjust screw rod (6) threaded hole for matching, adjust screw rod (6) top pass through threaded hole on fixing seat (5) with
First bearing seat (4) be connected, adjust screw rod (6) threadingly hole rotate when drive first bearing seat (4) along guide chute (7) up and down
Sliding, the rate of tension for completing filter cloth are adjusted；
The belt feeder includes belt tightening regulating device, and belt tightening regulating device includes leather belt roller (8) and symmetrical
Pedestal set on leather belt roller (8) two sides, the both ends of leather belt roller (8) pass through second bearing seat (13) installation on the base respectively, institute
The pedestal stated includes work shape bracket and floor stringer (9), and work shape bracket is by the first upright bar (10), the second upright bar (11) and crossbeam (12)
It constituting, floor stringer (9) is parallel to each other with crossbeam (12), bar shaped sliding block (14) are equipped on the inside of floor stringer (9) and crossbeam (12),
The two sides of the second bearing seat (13) are equipped with the sliding slot (15) matched with bar shaped sliding block (14)；It further include tensing screw rod
(16), the first upright bar (10) is equipped with and tenses screw rod (16) threaded hole for matching, and the top for tensing screw rod (16) passes through the
Threaded hole in one upright bar (10) is connected with second bearing seat (13), tenses screw rod (16) and drives the second axis when threadingly hole rotates
Hold that seat (13) is traversing along bar shaped sliding block (14) direction between floor stringer (9) and crossbeam (12), the rate of tension for completing belt is adjusted；
The belt feeder includes Pneumatic type leather belt offset apparatus for correcting, and it includes correction roll shaft that Pneumatic type leather belt, which deviates apparatus for correcting,
(18) and corrective component, corrective component include that at least one is set to the stroke inductive switch (19) of belt (17) side, microcontroller
Device MCU(20) and pneumatic adjusting component, the sampled signal input phase of stroke inductive switch (19) and microcontroller (20)
Even, the enable signal output end of microcontroller (20) is connected with the pneumatic component that adjusts；The non-moving end for correcting roll shaft (18) is hinged
On rack I(24), the moved end for correcting roll shaft (18) is mounted on rack II(21 by pneumatically adjusting component) on；
The pneumatic adjusting component includes the first air bag group (22) and the second air bag group (23), the first air bag group (22) and second
Air bag group (23) is respectively arranged at the two sides of correction roll shaft (18) moved end, and the first air bag group (22) and second air bag group (23) are filled
Deflation driving circuit is connected with the enable signal output end of microcontroller (20) respectively；
S5: secondary neutralization secondary neutralization: is carried out to the liquid being once obtained by filtration using gas ammonia；It is passed through gas ammonia while stirring, to
When the molar ratio of the gas ammonia and phosphoric acid that are passed through is 1.4-1.6, adjustment solution ph is 5.3-5.6, obtains diammonium phosphate slurry；
S6: secondary filter press filtering: the secondary obtained slurry that neutralizes is imported into filter press progress secondary filter, isolated consolidates
The white fertilizer of accessory substance is made after body drying, isolated liquid is Diammonium phosphate (DAP) clear liquid；
S7: index is adjusted: regulator is added in isolated Diammonium phosphate (DAP) clear liquid and carries out index accurate adjustment；
S8: crystallization: qualified Diammonium phosphate (DAP) solution is adjusted to index and is concentrated, and crystallizer is added and is crystallized；
S9: separation drying: centrifuge is added in the Diammonium phosphate (DAP) after crystallization and is separated by solid-liquid separation, solid is sent into fluidized bed dryer
It is dried, obtains finished industrial grade Diammonium phosphate (DAP), Recycling Mother Solution uses.
2. the method for Wet-process Phosphoric Acid Production Diammonium phosphate (DAP) according to claim 1, it is characterised in that: the phosphoric acid by wet process
It further include a supernatant purifying step before desulfurization defluorinate processing in pre-treatment step, the dissolution in Precipitation phosphoric acid by wet process
Property impurity.
3. the method for Wet-process Phosphoric Acid Production Diammonium phosphate (DAP) according to claim 1, it is characterised in that: the deep purifying
Agent is polyacrylamide, and the regulator is PHOSPHORIC ACID TECH.GRADE.
4. the method for Wet-process Phosphoric Acid Production Diammonium phosphate (DAP) according to claim 1, it is characterised in that: mother liquor follows in step S9
The step of ring uses are as follows: the mother liquor for separating centrifuge continues sedimentation separation, and centrifuge is sent into the crystallization isolated
Feeding fluidized bed dryer is dried after carrying out secondary centrifuging, and the liquid isolated successively carries out mother liquor neutralization, filters pressing separation
Formation mother liquor is mixed with the Diammonium phosphate (DAP) solution that the index that step S7 is obtained adjusts qualification and is concentrated afterwards.
5. such as the device of method of any of claims 1-4 production Diammonium phosphate (DAP), it is characterised in that: including supernatant
Bucket, desulfurization pond, a neutralization bucket, belt feeder, secondary neutralization bucket, filter press, crystallizer, dashpot, centrifuge and fluidized bed are dry
Dry device, phosphoric acid by wet process inject clarifying tank, and the entrance in the outlet connection desulfurization pond of clarifying tank, the outlet in desulfurization pond passes sequentially through once
Neutralization bucket, belt feeder and secondary neutralization bucket are connected with the entrance of filter press, and the belt feeder includes that filter cloth rate of tension adjusts dress
It sets, filter cloth rate of tension regulating device is mounted in the rack (1) of belt feeder, including filter cloth tensioning wheel (2), fixing seat (5), adjusting
The fixed peace of screw rod (6) and the leading truck (3) for being symmetrically disposed on filter cloth tensioning wheel (2) two sides, leading truck (3) and fixing seat (5)
On rack (1), the both ends of filter cloth tensioning wheel (2) are connected separately with first bearing seat (4), and leading truck (3) is equipped with and the
The guide chute (7) that one bearing block (4) matches, fixing seat (5) are equipped with the threaded hole matched with adjusting screw rod (6), adjust
The threaded hole that the top of section screw rod (6) passes through on fixing seat (5) is connected with first bearing seat (4), adjusts screw rod (6) threadingly hole
First bearing seat (4) are driven to slide up and down along guide chute (7) when rotation, the rate of tension for completing filter cloth is adjusted；
The belt feeder includes belt tightening regulating device, and belt tightening regulating device includes leather belt roller (8) and symmetrical
Pedestal set on leather belt roller (8) two sides, the both ends of leather belt roller (8) pass through second bearing seat (13) installation on the base respectively, institute
The pedestal stated includes work shape bracket and floor stringer (9), and work shape bracket is by the first upright bar (10), the second upright bar (11) and crossbeam (12)
It constituting, floor stringer (9) is parallel to each other with crossbeam (12), bar shaped sliding block (14) are equipped on the inside of floor stringer (9) and crossbeam (12),
The two sides of the second bearing seat (13) are equipped with the sliding slot (15) matched with bar shaped sliding block (14)；It further include tensing screw rod
(16), the first upright bar (10) is equipped with and tenses screw rod (16) threaded hole for matching, and the top for tensing screw rod (16) passes through the
Threaded hole in one upright bar (10) is connected with second bearing seat (13), tenses screw rod (16) and drives the second axis when threadingly hole rotates
Hold that seat (13) is traversing along bar shaped sliding block (14) direction between floor stringer (9) and crossbeam (12), the rate of tension for completing belt is adjusted；
The belt feeder includes Pneumatic type leather belt offset apparatus for correcting, and it includes correction roll shaft that Pneumatic type leather belt, which deviates apparatus for correcting,
(18) and corrective component, corrective component include that at least one is set to the stroke inductive switch (19) of belt (17) side, microcontroller
Device MCU(20) and pneumatic adjusting component, the sampled signal input phase of stroke inductive switch (19) and microcontroller (20)
Even, the enable signal output end of microcontroller (20) is connected with the pneumatic component that adjusts；The non-moving end for correcting roll shaft (18) is hinged
On rack I(24), the moved end for correcting roll shaft (18) is mounted on rack II(21 by pneumatically adjusting component) on；
The pneumatic adjusting component includes the first air bag group (22) and the second air bag group (23), the first air bag group (22) and second
Air bag group (23) is respectively arranged at the two sides of correction roll shaft (18) moved end, and the first air bag group (22) and second air bag group (23) are filled
Deflation driving circuit is connected with the enable signal output end of microcontroller (20) respectively；
The white fertilizer of accessory substance is made after the solid drying that filter press is isolated, the Diammonium phosphate (DAP) clear liquid that filter press is isolated injects concentration
In the clear liquid entrance of tank, the outlet of concentration tank passes sequentially through crystallizer and dashpot and is connected with the feed inlet of centrifuge, centrifuge
The solid isolated, which is sent into fluidized bed dryer, is dried, and finished industrial grade Diammonium phosphate (DAP), the mother that centrifuge is isolated are obtained
Liquid injects the entrance of sedimentation separation bucket, and the crystallization that sedimentation separation bucket is isolated is connected with the feed inlet of centrifuge, sedimentation separation bucket
The liquid isolated is connected with the entrance of mother liquor neutralization bucket, and the outlet of mother liquor neutralization bucket passes through the mother of filters pressing separator and concentration tank
The connection of liquid entrance.
6. device according to claim 5, it is characterised in that: the fluidized bed dryer includes vibrating feed device,
Vibrating feed device includes loading hopper (25), fluidized bed feed inlet (26) and the vibration drapery panel (27) being obliquely installed, charging
The discharge port of funnel (25) is set to above the high order end of vibration drapery panel (27), and the low order end of vibration drapery panel (27) is set to
Above fluidized bed feed inlet (26), oscillation drive, the vibration drapery panel are installed on the vibration drapery panel (27)
(27) both ends are symmetrically arranged with resonant component, and every group of resonant component includes sunpender (28) and spring (29), the top of sunpender (28)
It is fixedly mounted on reference seat (30), is socketed on sunpender (28) movable cushion block (31), the bottom of sunpender (28) is equipped with fixation
One end of cushion block (32), spring (29) is fixedly connected with movable cushion block (31), the other end of spring (29) and fixed cushion block (32)
Connection, vibration drapery panel (27) are fixedly connected with movable cushion block (31).
7. device according to claim 6, it is characterised in that: be fixedly mounted on the side wall of the vibration drapery panel (27)
Have U-shaped frame (37), is equipped with the through-hole matched with sunpender (28), sunpender on the transverse slat and movable cushion block (31) of U-shaped frame (37)
(28) it sequentially passes through U-shaped frame (37) transverse slat, movable cushion block (31) and spring (29) to connect with fixed cushion block (32), movable cushion block
(31) upper top surface is fixedly connected with U-shaped frame (37) transverse slat.
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| CN108033434B (en) * | 2017-11-03 | 2020-05-08 | 云南中正化学工业有限公司 | Method for producing high-quality industrial diammonium phosphate by triple purification method |
| CN108383552A (en) * | 2018-03-19 | 2018-08-10 | 成都理工大学 | A kind of production method of potassium acid phosphate |
| CN110681487A (en) * | 2019-09-27 | 2020-01-14 | 瓮福达州化工有限责任公司 | Iron removing system and preparation process thereof |
| CN118026116B (en) * | 2024-04-02 | 2024-09-06 | 新洋丰农业科技股份有限公司 | Method for preparing diammonium phosphate from monoammonium phosphate mother liquor |
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| JP4239502B2 (en) * | 2002-07-23 | 2009-03-18 | 三菱マテリアル株式会社 | Phosphorus recovery method |
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| CN102730657A (en) * | 2012-06-27 | 2012-10-17 | 贵州川恒化工有限责任公司 | Method for defluorination, purification and separation of wet-process phosphoric acid |
| CN102863267A (en) * | 2012-09-08 | 2013-01-09 | 湖北三宁化工股份有限公司 | Method for producing monoammonium phosphate and coproducing N-P binary compound fertilizer by using wet-process phosphoric acid |
| CN104229764A (en) * | 2014-09-01 | 2014-12-24 | 云南云天化国际化工有限公司 | Method for continuously producing water-soluble monoammonium phosphate by using wet-process phosphoric acid |
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