CN106395778B - The method for producing potassium dihydrogen phosphate using wet phosphoric acid refining by-product scourage - Google Patents
The method for producing potassium dihydrogen phosphate using wet phosphoric acid refining by-product scourage Download PDFInfo
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- CN106395778B CN106395778B CN201610783674.2A CN201610783674A CN106395778B CN 106395778 B CN106395778 B CN 106395778B CN 201610783674 A CN201610783674 A CN 201610783674A CN 106395778 B CN106395778 B CN 106395778B
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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
- C01B25/30—Alkali metal phosphates
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Abstract
The present invention is a kind of method producing potassium dihydrogen phosphate using wet phosphoric acid refining by-product scourage, filtrated stock will first be crystallized, scourage, water carries out adjusting acid to produce mixed liquor, the stoichiometry for pressing sulfate radical in mixed liquor again carries out desulfurization, then potassium chloride is added to generate potassium dihydrogen phosphate by the stoichiometry of phosphoric acid in the filtrate after desulfurization, after stirring, activated carbon is added into slurry, decoloring assistant carries out decoloration removing impurities, after filtering, normal pressure concentration is carried out successively, vacuum cooled crystallizes, to obtain crystal and mother liquor, potassium dihydrogen phosphate product is obtained after crystal drying, mother liquor is then sent back in the tune acid technique of next round and is recycled.The present invention can not only realize the efficient utilization to scourage obtained by solvent extraction refined wet process phosphoric acid, can improve the utilization rate of mother liquor, save product cost, and technological process is simple, cost of material is relatively low, better economic benefit.
Description
Technical field
The present invention relates to a kind of production technologies of potassium dihydrogen phosphate more particularly to a kind of utilization wet phosphoric acid refining by-product to wash
The method of remaining aquatic production potassium dihydrogen phosphate, the scourage system generated when it is particularly applicable to take solvent extraction refined wet process phosphoric acid
Potassium dihydrogen phosphate is taken, and technological process is simple, cost is relatively low.
Background technology
There are two types of the raw materials for production of potassium dihydrogen phosphate, and one is thermal phosphoric acids, and one is phosphoric acid by wet processes.Using thermal phosphoric acid
The method for producing industrial grade potassium dihydrogen phosphate directly neutralized with highly basic, although the purity of product is very high, production cost is higher,
And production cost can be greatly reduced using Wet-process Phosphoric Acid Production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen, byproduct or filter residue can be with
Agrochemical is produced, therefore, current numerous domestic is become using the optimization of Wet-process Phosphoric Acid Production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen technique
The research hotspot of scientific research institution.
Currently, the phosphoric acid,diluted used in technique using Wet-process Phosphoric Acid Production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen is mostly passed through by rock phosphate in powder
Sulfuric acid extraction is made, then ground phosphate rock either calcium carbonate or calcium oxide or other sylvite, calcium salt progress are added in phosphoric acid,diluted
Desulfurization pretreatment, then by extraction or double decomposition, crystallization to produce potassium dihydrogen phosphate, this technology has the following defects：
Production raw material type used is more and expensive；Crystallization cost is higher, and the utilization rate of crystalline mother solution is not high；Technique
Flow is complicated, and limited for the hoisting power of major product potassium dihydrogen phosphate yield, whole production cost is higher.
Invention content
The purpose of the present invention is overcome cost of material existing in the prior art is higher, technological process is complicated defect and ask
Topic, provides that a kind of cost of material is relatively low, technological process simply utilizes wet phosphoric acid refining by-product scourage to produce biphosphate
The method of potassium.
In order to achieve the above object, technical solution of the invention is：It is a kind of to utilize wet phosphoric acid refining by-product scourage
The method for producing potassium dihydrogen phosphate, the method include the following steps successively：
Adjust sour technique：First scourage, water are uniformly mixed to obtain mixed liquor, P in the mixed liquor2O5Mass percent
A concentration of 18-22%；The sylvite washings that the scourage is configured from solvent extraction refined wet process phosphoric acid participate in reaction
The product obtained afterwards, the scourage include P2O5With sulfate radical, P2O5Mass percent concentration be 35-45%, sulfate radical
Content is 35-65g/L；
Sulfur removal technology：Ground phosphate rock or calcium carbonate are first added in above-mentioned mixed liquor or barium carbonate carries out desulfurization, then to desulfurization
Solution afterwards is filtered, and filtrate is sent to reactive tank；
Hybrid technique：In reactive tank, the 85-95% for first pressing the stoichiometry of phosphoric acid in above-mentioned filtrate adds potassium chloride, phosphorus
The stoichiometry of acid is by P2O5Content convert, while addition while stir, then by the solution after stirring send to decolourize slot；
Decoloration removing impurities technique：It decolourizes in slot, activated carbon first is added in solution after agitation, decoloring assistant carries out decoloration and takes off
It is miscellaneous, then the slurry after decoloration removing impurities is filtered to produce slurry clear liquid；
Normal pressure concentration technology：Normal pressure concentration first is carried out to above-mentioned slurry clear liquid, then the slurry after concentration is sent cold to vacuum
But crystallization tank；
Crystallization and filtering technique：In vacuum cooled crystallization tank, vacuum cooled crystallization first is carried out to the slurry after above-mentioned concentration,
The slurries after crystallization are filtered again to obtain crystal and mother liquor, then crystal is dried to obtain product potassium dihydrogen phosphate.
The crystallization is with filtering technique, and the mother liquor includes potassium dihydrogen phosphate and sulfate radical, and the matter of potassium dihydrogen phosphate
Amount percent concentration is 35-45%, and the content of sulfate radical is 40-48g/L, meanwhile, the mother liquor of filtering gained is sent to next
In the tune acid technique of wheel, be uniformly mixed together with scourage, water to obtain mixed liquor.
In the sulfur removal technology, by mixed liquor sulfate radical stoichiometry 50-85% addition ground phosphate rock or calcium carbonate or
Barium carbonate carries out desulfurization, and desulfurization time is 2-4 hours, and temperature is 75-90 DEG C.
In the sulfur removal technology, the solution after desulfurization is filtered, and filtrate is sent to reactive tank, filter residue sends to phosphoric acid
Workshop merges with ardealite.
In the hybrid technique, mixing time is 1-2 hours, and temperature is 70-80 DEG C.
In the normal pressure concentration technology, the proportion after the concentration of slurry clear liquid normal pressure is 1.30-1.35, the temperature of normal pressure concentration
Degree is 140-170 DEG C.
In the normal pressure concentration technology, normal pressure concentration is carried out to slurry clear liquid in the evaporator of inner liner polytetrafluoroethylene,
Meanwhile the steam generated when being concentrated to normal pressure carries out water cycle washing to recycle hydrogen chloride, and give to the fertile workshop of system.
The crystallization is with filtering technique, and the time of vacuum cooled crystallization is 2.5-4.5 hours, crystallization temperature 40-
50 DEG C, after crystallization, the slurries after crystallization are filtered to obtain crystal and mother liquor with centrifuge, crystal is by fluidized bed drying.
In the decoloration removing impurities technique, activated carbon, decoloring assistant additive amount respectively be liquor capacity 1-5 ‰.
The decoloring assistant is the aqueous solution that mass percent concentration is 1-15%, and the solvent of this kind of aqueous solution is water, molten
Matter is potassium acetate, potassium thiosulfate, potassium sulfide, polyvinyl alcohol, polyoxyethylene alkyl amine, acrylamide, silicone surfactant
Any one or arbitrary two kinds of mass ratioes in JSY-6504, poly- alkyl phenol-ethylene oxide are 1:1 mixture being configured to or
Arbitrary three kinds in mass ratio 1:1.75:3 mixtures being configured to.
Compared with prior art, beneficial effects of the present invention are：
1, in method of the present invention using wet phosphoric acid refining by-product scourage production potassium dihydrogen phosphate, based on scourage
Raw material object is wanted, which participates in obtaining after reacting from the sylvite washings that solvent extraction refined wet process phosphoric acid is configured
Product, advantage includes：First, cheap, it is conducive to reduce cost of material；Secondly, the impurity contained in scourage is seldom,
The metal impurities that the overwhelming majority easily precipitates all are removed during wet phosphoric acid refining, conducive to follow-up step is simplified, especially
Conducive to being smoothed out for follow-up sulfur removal technology；Again, this scourage is due to being that sylvite washings participate in product obtained by the reaction,
Inside contains potassium, and the presence of potassium is not only conducive to the generation of follow-up potassium dihydrogen phosphate, but also conducive to potassium chloride in reduction hybrid technique
Addition, further decreases cost of material.Therefore, the present invention can be realized to scourage obtained by solvent extraction refined wet process phosphoric acid
Efficient utilization, improve the rate of recovery of phosphorus and potassium, and reduce the cost of material of production potassium dihydrogen phosphate, simplify whole technique stream
Journey.
2, in method of the present invention using wet phosphoric acid refining by-product scourage production potassium dihydrogen phosphate, in crystallization and filtering
In technique, the mother liquor generated may participate in the tune acid technique in next round production, be recycled, advantage includes：First,
Impurity content in mother liquor is seldom, and the content of potassium dihydrogen phosphate is higher, to its Returning utilization, can not only recycle very considerable phosphorus
Acid dihydride potassium avoids the loss of a large amount of phosphorus, potassium, improves the utilization rate of mother liquor, and can save the cost and knot for adjusting sour technique
Brilliant cost；Secondly, mother liquor is returned directly in the tune acid technique of the first step, it is made to be subjected to the desulfurization of second step, to promote
Make the lasting removing of foreign ion in mother liquor, especially sulfate radical, avoid the accumulation of impurity in mother liquor, remains each in crystalline mother solution
The stabilization of component content has ensured the consecutive production of technological process.Therefore, the utilization rate of the present invention not only mother liquor is very high, and
And conducive to crystallization cost and cost of material is reduced, it is conducive to the consecutive production of overall flow.
3, in method of the present invention using wet phosphoric acid refining by-product scourage production potassium dihydrogen phosphate, overall flow is successively
Including adjusting sour technique, sulfur removal technology, hybrid technique, decoloration removing impurities technique, normal pressure concentration technology, crystallization and filtering technique, and tie
It is recycled in the brilliant tune acid technique that may participate in next round with the mother liquor in filtering technique.Wherein, adjust acid in the first stepping
Row can comprehensively utilize scourage and mother liquor, unified to produce starting point, process control easy to produce, and mother liquor can be promoted to participate in
Subsequent desulfurization avoids the accumulation of impurity in mother liquor to damage the continuity of production；Sulfur removal technology is mixed to remove sulfate radical
It is to generate potassium dihydrogen phosphate to close technique, and why first desulfurization remixes, be in order on the basis of removing a large amount of sulfate radicals,
The higher potassium chloride of purity is added to realize the effect of combination among the strong ones, potassium element is not only wasted if first mixing desulfurization again,
And the addition of potassium chloride can not be determined by the phosphorus acid content of solution, because the addition of ground phosphate rock can make on phosphorus acid content
It rises, increases the difficulty of technological operation；As for last decoloration removing impurities technique, normal pressure concentration technology, crystallization and filtering technique be for
Obtain the pure crystalline solid of color, design to improve the quality of final products, meanwhile, final step arrangement crystallization with
Filtering technique is conducive to recycle also for the tune acid technique convenient for the mother liquor participation next round first step generated.Cause
This, not only technological process is simple by the present invention, and front and back step connecting is strong, and conducive to cost is saved, and that improves raw material utilizes effect
Rate enhances the cost performance of integrated artistic.
4, in method of the present invention using wet phosphoric acid refining by-product scourage production potassium dihydrogen phosphate, in sulfur removal technology
It is interior, carry out desulfurization, the behaviour by the 50-85% addition ground phosphate rock or calcium carbonate or barium carbonate of sulfate radical stoichiometry in mixed liquor
Work can make product up to standard, meet quality requirement, and be avoided that unnecessary waste, increase production cost.Therefore, of the invention
Sexual valence is relatively high, and economic benefit is stronger.
5, in method of the present invention using wet phosphoric acid refining by-product scourage production potassium dihydrogen phosphate, in decoloration removing impurities work
In skill, addition activated carbon, decoloring assistant this two substance carry out decoloration removing impurities, and the two cooperates, and decoloring assistant can assist living
Property carbon decoloring remove nonferrous metal ion, and flocculate convenient for filtering precipitation, finally, avoid foreign ion and chlorion from matching and generate
Soluble-salt damages the quality of product.Therefore, decoloration removing impurities effect of the invention is preferable, is conducive to improve product quality.
Description of the drawings
Fig. 1 is the flow diagram of the present invention.
Fig. 2 is the dimensional structure diagram of A type outer containers in A type mixing arrangements.
Fig. 3 is the sectional view of A type outer containers in A type mixing arrangements.
Fig. 4 is the enlarged diagram at C in Fig. 3.
Fig. 5 is the structural schematic diagram of A type blenders in A type mixing arrangements.
Fig. 6 is the enlarged diagram at D in Fig. 5.
Fig. 7 is the enlarged diagram at E in Fig. 5.
Fig. 8 is the vertical view of trigone blade in Fig. 5.
Fig. 9 is the explosive view of Type B outer container in Type B mixing arrangement.
Figure 10 is the relative position schematic diagram of Type B outer container in Type B mixing arrangement, Type B blender.
Figure 11 is the connection diagram of tube cavity, air guide column on Type B outer container in Type B mixing arrangement.
Figure 12 is the vertical view of upper drive disk in Figure 10.
Figure 13 is the change schematic diagram of the first design of reciprocal telescopic device on Type B blender.
Figure 14 is the structural schematic diagram of second of design of reciprocal telescopic device on Type B blender.
Specific implementation mode
Below in conjunction with description of the drawings, the present invention is described in further detail with specific implementation mode.
Referring to Fig. 1 to Figure 14, a method of potassium dihydrogen phosphate being produced using wet phosphoric acid refining by-product scourage, it is described
Method includes the following steps successively：
Adjust sour technique：First scourage, water are uniformly mixed to obtain mixed liquor, P in the mixed liquor2O5Mass percent
A concentration of 18-22%；The sylvite washings that the scourage is configured from solvent extraction refined wet process phosphoric acid participate in reaction
The product obtained afterwards, the scourage include P2O5With sulfate radical, P2O5Mass percent concentration be 35-45%, sulfate radical
Content is 35-65g/L；
Sulfur removal technology：Ground phosphate rock or calcium carbonate are first added in above-mentioned mixed liquor or barium carbonate carries out desulfurization, then to desulfurization
Solution afterwards is filtered, and filtrate is sent to reactive tank；
Hybrid technique：In reactive tank, the 85-95% for first pressing the stoichiometry of phosphoric acid in above-mentioned filtrate adds potassium chloride, phosphorus
The stoichiometry of acid is by P2O5Content convert, while addition while stir, then by the solution after stirring send to decolourize slot；
Decoloration removing impurities technique：It decolourizes in slot, activated carbon first is added in solution after agitation, decoloring assistant carries out decoloration and takes off
It is miscellaneous, then the slurry after decoloration removing impurities is filtered to produce slurry clear liquid；
Normal pressure concentration technology：Normal pressure concentration first is carried out to above-mentioned slurry clear liquid, then the slurry after concentration is sent cold to vacuum
But crystallization tank；
Crystallization and filtering technique：In vacuum cooled crystallization tank, vacuum cooled crystallization first is carried out to the slurry after above-mentioned concentration,
The slurries after crystallization are filtered again to obtain crystal and mother liquor, then crystal is dried to obtain product potassium dihydrogen phosphate.
The crystallization is with filtering technique, and the mother liquor includes potassium dihydrogen phosphate and sulfate radical, and the matter of potassium dihydrogen phosphate
Amount percent concentration is 35-45%, and the content of sulfate radical is 40-48g/L, meanwhile, the mother liquor of filtering gained is sent to next
In the tune acid technique of wheel, be uniformly mixed together with scourage, water to obtain mixed liquor.
In the sulfur removal technology, by mixed liquor sulfate radical stoichiometry 50-85% addition ground phosphate rock or calcium carbonate or
Barium carbonate carries out desulfurization, and desulfurization time is 2-4 hours, and temperature is 75-90 DEG C.
In the sulfur removal technology, the solution after desulfurization is filtered, and filtrate is sent to reactive tank, filter residue sends to phosphoric acid
Workshop merges with ardealite.
In the hybrid technique, mixing time is 1-2 hours, and temperature is 70-80 DEG C.
In the normal pressure concentration technology, the proportion after the concentration of slurry clear liquid normal pressure is 1.30-1.35, the temperature of normal pressure concentration
Degree is 140-170 DEG C.
In the normal pressure concentration technology, normal pressure concentration is carried out to slurry clear liquid in the evaporator of inner liner polytetrafluoroethylene,
Meanwhile the steam generated when being concentrated to normal pressure carries out water cycle washing to recycle hydrogen chloride, and give to the fertile workshop of system.
The crystallization is with filtering technique, and the time of vacuum cooled crystallization is 2.5-4.5 hours, crystallization temperature 40-
50 DEG C, after crystallization, the slurries after crystallization are filtered to obtain crystal and mother liquor with centrifuge, crystal is by fluidized bed drying.
In the decoloration removing impurities technique, activated carbon, decoloring assistant additive amount respectively be liquor capacity 1-5 ‰.
The decoloring assistant is the aqueous solution that mass percent concentration is 1-15%, and the solvent of this kind of aqueous solution is water, molten
Matter is potassium acetate, potassium thiosulfate, potassium sulfide, polyvinyl alcohol, polyoxyethylene alkyl amine, acrylamide, silicone surfactant
Any one or arbitrary two kinds of mass ratioes in JSY-6504, poly- alkyl phenol-ethylene oxide are 1:1 mixture being configured to or
Arbitrary three kinds in mass ratio 1:1.75:3 mixtures being configured to.
The principle of the present invention is described as follows：
One, mixed liquor：
P in mixed liquor2O5Mass percent concentration the reason of being limited to 18-22% it is as follows：
First, it is influenced by scourage and mother liquid concentration, P in mixed liquor2O5Concentration can not possibly it is too high, otherwise can increase
Phosphorus damage when desulfurization is filtered, and if it is too low if, mean and excessive water be added, then can increase the load of equipment below, increase
Cost；
Secondly, concentration too it is high not only result in it is follow-up can not be completely dissolved when potassium chloride is added, many solutes are straight
Precipitation is connect, and can be caused when mother liquor participates in adjusting acid, the potassium dihydrogen phosphate in mother liquor is precipitated in mixing channel to result in blockage now
As.
Two, scourage：
The production that scourage participates in obtaining after reaction from the sylvite washings that solvent extraction refined wet process phosphoric acid is configured
Object (in solvent extraction refined wet process phosphoric acid, scourage will be obtained after being washed with washings to satisfying), miscellaneous
Matter is less, meanwhile, potassium dihydrogen phosphate is influenced maximum to be exactly P2O5, sulfate radical, therefore only need to the concentration of both substances into
Row limits.
P in scourage2O5Mass percent concentration be 35-45%：The dense upper limit of acid is limited by solvent extraction, molten
Agent extraction can not possibly allow scourage acid dense excessively high for control cost, because scourage acid is dense excessively high, what is directly illustrated is exactly
The failure of solvent extraction, and such as tartaric acid is dense too low, it will cause the increases of potassium dihydrogen phosphate subsequent concentration process cost, because
Water is more, and the concentration water to be removed is more, and load increases, and cost improves.
The content of sulfate radical is 35-65g/L：It is equally limited by solvent extraction, solvent extraction directly determines to wash remaining
The concentration of sulfate radical in water.
Three, mother liquor：
The mass percent concentration of potassium dihydrogen phosphate is 35-45% in mother liquor, and the content of sulfate radical is 40-48g/L：Phosphorus
Acid dihydride potassium, sulfate radical concentration be to be determined by last round of crystallization and filtering technique, be in order to ensure in last round of technique
Crystallization effect and passively obtain.
Potassium dihydrogen phosphate：Its concentration is the equalization point of the quality and yield of last round of product potassium dihydrogen phosphate, if concentration mistake
Height, more potassium dihydrogen phosphate crystals will be precipitated in it in vacuum cooled crystallization tank, and adjoint sulfate radical also can be with sulphur therewith
Acid salts are precipitated, and influence the purity of potassium dihydrogen phosphate product, meanwhile, when highly concentrated mother liquor Returning utilization, it will produce crystallization
Block pipeline；If concentration is too low, illustrate in crystallization process, crystallization content is few, causes the yield of potassium dihydrogen phosphate not up to standard.
Sulfate radical：Its concentration, if excessive concentration, is illustrated to find the equalization point of potassium dihydrogen phosphate quality and benefit
The sulfate radical content of the potassium dihydrogen phosphate crystal of last round of precipitation is high, and product quality can be unqualified；If concentration is too low, although can protect
Demonstrate,proving product quality, this detection is upper absolutely qualified in sulfate radical, but it can increase desulphurization cost of the enterprise in production,
After all, for product when selling, price is sulfate radical content that is the same, thus need to only meeting Industry code requirements, if sternly
In industry requirement, then it can increase desulphurization cost, to reduce product profit.
Four, each operating procedure：
1, sulfur removal technology：
The purpose of the step is to remove the sulfate radical in mixed liquor, and forming crystallization to prevent the later stage influences the quality of finished product
And yield.
Desulfurization time is 2-4 hours：Time is longer, and desulfurization effect is better, but to consider cost performance.
Temperature is 75-90 DEG C：Desulfurization effect in this temperature section is best.
2, hybrid technique：
The purpose of the step is potassium dihydrogen phosphate in order to obtain.
Mixing time is 1-2 hours：In order to mix fully, make that the reaction was complete.
70-80℃：A bit, the solubility higher of solute, the dispersibility of solute in a solvent is better, and reaction is got over for temperature height
Fully；Temperature is too high, and high energy consumption, temperature is too low, and the reaction time extends.
3, decoloration removing impurities technique：
Activated carbon be in order to adsorbing and removing by solvent extraction refined wet process phosphoric acid process bands Lai a small amount of organic matter, make molten
Liquid color is limpid, decoloring assistant be in order to remove a small amount of non-ferrous metal impurity brought by equipment and pipeline in production process and with
Activated carbon forms certain flocculation and facilitates filtering.The foreign ion of removing is more, the solubility generated with chlorion pairing
Salt is fewer, does not interfere with the quality of product more, chlorion just can only with hydrogen ion together with, form chlorination when normal pressure concentrates
Hydrogen is precipitated.
Activated carbon, decoloring assistant additive amount respectively be liquor capacity 1-5 ‰：Within the scope of this, decolorizing effect is best, this
Outside, concentration is low, and addition will increase, and concentration is high, and volatility is too strong, and smell is too big, causes environmental pollution.
The rate of filtration is preferably 4.50-6.00m3/m2hr：Speed is too small, and filtration time can increase, and speed is too fast, filtering
Pressure is too big, is also easy to produce filtering and penetrates.
4, normal pressure concentration technology：
The purpose that normal pressure is concentrated into proportion 1.30-1.35 is to obtain the biphosphate that purity is high, yield is big after cooling down
Potassium crystal, while recycling quality and yield that hydrogen chloride gas improves crystallization.Proportion is too low, and concentration is not thorough, and can cause to crystallize
Amount is few, influences yield；Proportion is too high, can cause since crystallization causes clogging rapidly to the cold in conveyance conduit, and be also easy to produce
Impurity is carried secretly.
The temperature of normal pressure concentration is 140-170 DEG C：Temperature is too low, and hydrogen chloride cannot volatilize completely, and temperature is excessively high, energy consumption
Too high, equipment life also shortens.
Polytetrafluoroethylene (PTFE)：It is corrosion-resistant using polytetrafluoroethylene material high temperature resistant, on-deformable characteristic.
5, crystallization and filtering technique：
Vacuum cooled crystallization is conducive to the formation of potassium dihydrogen phosphate crystal particle and grows up, while recycling extra hydrogen chloride
Gas, to obtain the higher potassium dihydrogen phosphate of purity after drying.
The time of vacuum cooled crystallization is 2.5-4.5 hours：First be it is up to standard in order to meet crystal grain size, second
Be in order to meet crystallization after slurry mobility.
Crystallization temperature is 40-50 DEG C：At a temperature of this, the potassium dihydrogen phosphate crystal form of precipitation is beautiful, wall not easy to stick.
Product quality：What standard generally referred to used by industrial potassium dihydrogen phosphate production at present is chemical industry standard
HG2321-92, the product potassium dihydrogen phosphate that the present invention produces can reach sulfate radical≤0.1%, P2O5Content 49.5-
The standard of 52.3%, K2O content 34.0-35.2%, have reached Grade A standard.
Five, mixing arrangement is refined --- adjust the hybrid manipulation in sour technique or hybrid technique in following A types mixing arrangement or B
It carries out, to enhance mixed effect, the uniformity of mixture being improved, referring to Fig. 1 to Figure 14 in type mixing arrangement：
(1), A types mixing arrangement：
A type mixing arrangements include A type outer container A1 with A type blender A2, A type blenders A2 include teeter column A21 and its
The quantity of the stirring accessory of upper setting, A type blenders A2 is two, and face is arranged in an axial direction in A type outer containers A1,
In, outer after lower concave part A112 in the top drawing-in for the teeter column A21 being located above to be extended down to right over it, underlying teeter column
It is outer after upper recess A142 in the bottom drawing-in of A21 to be extended down to immediately below it；
A type outer containers A1 include from top to bottom top outer container A11, in upper outer container A12, in lower outer container A13, bottom
Outer container A14, the top bottoms outer container A11 upper outer container A12 rotary-tops in coordinate, in the upper bottoms outer container A12 in
The cooperation of lower outer container A13 rotary-tops, in the lower bottoms outer container A13 coordinate with bottom outer container A14 rotary-tops；Hold outside top
Device A11 is the recessed upper half spherical structure in middle part, including upper left protrusion A111, middle lower concave part A112, the upper right protrusion A113 communicated,
Middle lower concave part A112 is located at the center position of top outer container A11；In upper outer container A12 be frustum structure wide at the top and narrow at the bottom, in
Gusset on upper outer container A12 between its top surface, bottom surface is the arcwall face of indent；In lower outer container A13 be up-narrow and down-wide
Frustum structure, in gusset on lower outer container A13 positioned at its top surface, bottom surface between for indent arcwall face；Bottom outer container
A14 is the lower half spherical structure of middle part fovea superior, including lower-left protrusion A141, middle upper recess A142, the bottom right protrusion A143 communicated, in
Upper recess A142 is located at the center position of bottom outer container A14；The top bottoms outer container A11, in the upper bottoms outer container A12, in
Be both provided with railroad A3 on the lower bottoms outer container A13, at the top of upper outer container A12, at the top of lower outer container A13, bottom
The chute device A4 being slidably matched with railroad A3 is both provided on the tops outer container A14；Railroad A3 includes sliding
The base of the rail seat A31 and external slide rail A32 connected thereon, interior sliding rail A33, external slide rail A32, interior sliding rail A33 are concentric ring structure, outer cunning
Rail A32, interior sliding rail A33 include slide track bar A34 and bulb A35, and the tops slide track bar A34 are connected with the bottoms sliding rail pedestal A31,
The bottom ends slide track bar A34 are connect with bulb A35, and bulb A35 diameters are more than slide track bar A34 diameters；Chute device A4 includes sliding slot base
Seat A41 and external chute A42, the internal chute A43 connected thereon, external chute A42, internal chute A43 are concentric ring structure, external chute
A42, internal chute A43 include hollow sliding slot pipe A44 and ball-and-socket A45, the sliding slot bottom ends pipe A44 and the top sliding slot pedestal A41 phase
Connection, the middle parts sliding slot pipe A44 are provided with the ball-and-socket A45 communicated therewith, slide track bar A34 diameters, sliding slot pipe A44 diameters, bulb A35
Diameter, ball-and-socket A45 diameters are sequentially increased, and are interference fit between bulb A35, sliding slot pipe A44.In use, first by mixed raw material
It is put into A type outer containers A1, raw material can be powder, liquid combination or liquid, (only restriction raw material type, not limiting raw material can only for liquid combination
Two kinds), restart top outer container A11, in upper outer container A12, in lower outer container A13, bottom outer container A14 rotations, together
Shi Qidong A type blenders A2 rotates to obtain final mixture.When railroad, chute device assembly, first by bulb plug
Into sliding slot pipe, and under push away, until fill in ball-and-socket, sliding slot pipe packet is outside slide track bar, sliding slot pipe, slide track bar and the cunnings of inside and outside two circle
Base of the rail seat, sliding slot pedestal constitute a sliding pair, and sliding pair advantage includes：It can ensure that smoothness, the stabilization of sliding, it can be pre- anti-skidding
Rail, sliding slot deform, and can provide a relatively independent, closed space to avoid external interference and impact, and setting lubrication
Oil is to enhance lubrication.
Preferred embodiment one, top outer container A11, in upper outer container A12, in lower outer container A13, bottom outer container A14 all
For hollow structure, including concentric exine shells A15, inner wall shell A16, wherein exine shells A15, inner wall shell in the outer container A11 of top
It is connect at the top of the bottoms A16 and sliding rail pedestal A31 on the outer container A11 of top；In exine shells A15, inner wall shell in upper outer container A12
The upper bottoms outer container A12 upper hopper chute pedestal A41 are connect at the top of A16, and exine shells A15, the inner wall bottoms shell A16 are above outer in hold
Connection at the top of sliding rail pedestal A31 on device A12；In in lower outer container A13 at the top of exine shells A15, inner wall shell A16 in lower outer container
The bottoms A13 upper hopper chute pedestal A41 connect, and sliding rail pedestal A31 on outer container A13 is played in exine shells A15, the inner wall bottoms shell A16 in
Top connects；Exine shells A15, the bottoms inner wall shell A16 top and bottom outer container A14 upper hopper chute pedestal A41 in the outer container A14 of bottom
Portion connects.When mixing, setting heater to being mixed raw material to heat in exine shells A15, inner wall shell A16.
Preferred embodiment two, top outer container A11, in upper outer container A12, in lower outer container A13, bottom outer container A14
All offer multiple admission line A17 communicated with external feed stream device on gusset, admission line A17 through exine shells A15,
The A16 settings of inner wall shell.When mixing, swirling eddy is sprayed to enhance mixed effect, air inlet into outer container by admission line A17
The external feed stream device that pipeline A17 is connect may be either employed in published all air intake apparatus or Type B mixing arrangement
Air guide column B5 structures.
Preferred embodiment three, A type blenders A2 include hollow teeter column A21 and the stirring accessory being arranged thereon, the stirring
Accessory includes hollow oblique branch pipe A22 and drum chassis A23, the quantity at least two of oblique branch pipe A22, and teeter column A21,
The venthole A7 of multiple one-way valve structures is all offered on oblique branch pipe A22, drum chassis A23；The bottom end of the oblique branch pipe A22 with
Column chamber A211 in teeter column A21 is communicated, the middle part phase at the position and branch pipe sliding block A221 of its nearly bottom end on oblique branch pipe A22 gussets
Connection, the branch pipe sliding slot A213 that the upper and lower ends of branch pipe sliding block A221 open up along the post jamb A212 of teeter column A21 are slided
Cooperation；The drum chassis A23 includes hollow top bottom-disc A231, low bottom-disc A232, the top bottom-disc A231, low bottom-disc A232
Middle part connected with teeter column A21 perforation, position on teeter column A21 positioned at top bottom-disc A231, low bottom-disc A232 between and
The inner end of multiple spring A233 is connected, and the outer end of spring A233 is connected with one end of trigone blade A234, trigone blade
The other end of A234 is between top bottom-disc A231, low bottom-disc A232.
Preferred embodiment four, the bottom ends oblique branch pipe A22 are communicated with teeter column A21 inner prop chambers A211, the inside on the tops oblique branch pipe A22
It is provided with reciprocating rotary device comprising bifurcated pipe A24, leaf pipe A25, rotation fan A26, the bottoms bifurcated pipe A24 are through oblique branch pipe A22
The oblique mouth of pipe A222 opened up on top is inserted into the inside on the tops oblique branch pipe A22, is located at oblique branch pipe on the middle part of bifurcated pipe A24
Position except A22 is connected with multiple leaf pipe A25, is connected in the middle part of the top of bifurcated pipe A24 and rotation fan A26, rotation fan
Multiple rotating fan blades A261 are provided on A26, oblique branch pipe A22, bifurcated pipe A24, leaf pipe A25 are sequentially communicated, and oblique branch pipe A22, are divided
The venthole A7 of multiple one-way valve structures is both provided on breeches pipe A24, leaf pipe A25；The bottom of bifurcated pipe A24 is following two knots
Any one in structure：The first：The bottom of bifurcated pipe A24 is connected with the convex ball outer end A51 on convex ball A5, convex ball inner end
A52 between convex ball outer end A51, the bottom ends oblique branch pipe A22, the width of oblique mouth of pipe A222, convex ball outer end A51 width, convex
The width of ball inner end A52, oblique branch pipe A22 diameter expand successively；Second：The bottom of bifurcated pipe A24 and the middle parts fork sliding block A6
On the slider bore A61 that opens up be connected, the both ends of fork sliding block A6 are slidably matched with the inner wall of oblique branch pipe A22, and it is upper to pitch sliding block A6
Position between bifurcated pipe A24, oblique branch pipe A22 is connected with one end of fork spring A62, the other end of fork spring A62 with tiltedly
The inner wall on the tops branch pipe A22 is connected, and pitches spring A62, the junction of oblique branch pipe A22 is uniformly arranged around oblique mouth of pipe A222.It is excellent
The occupation mode of scheme three, four is selected to include：First, teeter column A21 is driven to rotate to drive oblique branch pipe A22, drum chassis A23
Rotation, spring A233, trigone blade A234 are got rid of by outer to expand stirring range and strength；Secondly, A type blenders A2 ventilations, warp
Gas is sprayed by the arbitrary combination in teeter column A21, oblique branch pipe A22, drum chassis A23, bifurcated pipe A24 or leaf pipe A25 outward,
Which position whether opening of venthole A7 opens, all depending on application demand；Again, when teeter column A21 rotates, bifurcated
Pipe A24 reciprocatingly slides in it, reciprocatingly slides and combines or pitch spring A62, fork by convex ball A5, bifurcated pipe A24, oblique branch pipe A22
Sliding block A6, bifurcated pipe A24, oblique branch pipe A22 combinations are realized.
(2), Type B mixing arrangement：
Type B mixing arrangement includes Type B outer container B1 and Type B blender B2；Wherein, Type B outer container B1 is cuboid structure,
It is provided with rotating shaft holder B3 on the middle part of its top surface, a rotating pipe seat is each provided on the middle part of bottom surface and four sides
B4；Type B blender B2 includes mixing drum B21 and the stirring accessory being arranged thereon, the top drawing-in rotating shaft holder of mixing drum B21
It is extended down on after B3 right over it, is extended down to inside Type B outer container B1 under the bottom ends mixing drum B21；The rotating shaft holder B3 includes
Outer ring seat B31 and interior rotating basis B32, the periphery of outer ring seat B31 are fixedly connected with the top surface of Type B outer container B1, outer ring seat B31
Inner circumferential and interior rotating basis B32 periphery rotatable engagement, the inner circumferential of interior rotating basis B32 with through its internal mixing drum
The outer wall of B21 connects；The rotating pipe seat B4 includes outer ring seat B31, interior cake seat B42 and multiple tube cavity B41, outer ring seat
The periphery of B31 is connect with the bottom surface of Type B outer container B1 or side, and the inner circumferential of outer ring seat B31 and the periphery rotation of interior cake seat B42 are matched
It closes, multiple through tube cavity B41 is provided with to be communicated with external feed stream device in the middle part of interior cake seat B42.In use, first
Mixed raw material is put into Type B outer container B1, raw material is powder, liquid combination or liquid, (only restriction raw material type, does not limit for liquid combination
Raw material can only be two kinds), restart rotating pipe seat B4 and spray swirling eddy into Type B outer container B1, and starts Type B blender
B2 is rotated to obtain final mixture.
Preferred embodiment one, tube cavity B41 are connected with external feed stream device after being inserted into its internal air guide column B5, lead
Air column B5 be hollow structure, including be sequentially communicated preceding interpolating unit B51, in determine portion B52, outer portion of company B53, preceding interpolating unit B51 diameters are small
Determine portion's B52 diameters in, preceding interpolating unit B51, in determine portion B52 and be located inside tube cavity B41, outer portion of company B53 is located at tube cavity
Outside B41；On preceding interpolating unit B51 it is close in determine to be cased with ring slider B43, the internal ring wall B44 of ring slider B43 outside the position of portion B52
It is in contact with preceding interpolating unit B51 outer walls, the plumbing chase that the tops external annulus B45 of ring slider B43 open up along duct wall B46
B47 is slided, and the position on its nearly top is connected with the one end sliding block spring B48 on the sides external annulus B45, and sliding block spring B48 is another
End is connect with the duct wall B46 by plumbing chase B47, and sliding block spring B48 determines portion B52 settings in being higher than；In determine on portion B52 it is close outer
The position of company portion B53 is provided with upper protruding block B54 to carry out limit cooperation, wall card slot with the wall card slot B49 opened up in duct wall B46
The nearly tube cavity B41 external ports settings of B49；The position of nearly tube cavity B41 external ports offers outer arc slot on outer portion of company B53
B55 with arc inserted sheet B56 to carry out insertion sealed cooperation, and arc inserted sheet B56 height is more than or equal to outer portion of company B53 diameters, outside
Position is internally provided with check valve sheet B57, outer portion of company B53 between outer arc slot B55, outer portion of the company outer ends B53 on company portion B53
The upper position above check valve sheet B57 offers outer straight slot B58 to inlay cooperation with outer logical plug B59.When assembly, first will before
Interpolating unit B51 is inserted into 43 middle part of annular slide block B, then determines portion B52 in moving ahead, to withstand ring slider B43 along plumbing chase B47 forward
Sliding, advancing slip ring slider B43 will be drawn before sliding block spring B48, until upper protruding block B54 is caught in wall card slot B49, assembly is completed.
When midway being needed to add, first arc inserted sheet B56 to determine portion B52, outer portion of company B53 in partition, then is pushed aside along outer arc slot B55 underthrusts
Outer logical plug B59 to open outer straight slot B58, cleaned, and after cleaning, then is added by the inner cavity for then externally connecting portion B53 through outer straight slot B58
Enter to need substance (powder state or liquid) to be added, after addition, block outer straight slot B58, then on pull out arc inserted sheet B56 in unicom
Determine portion B52, outer portion of company B53, then from the outer end air inlet of outer portion of company B53 to rush in additive in outer container.
Preferred embodiment two, Type B outer container B1 include be that four assembles post B11 of hollow, rectangular body structure packaged match with six
Plate B12, assembles post B11, buck plate B12 are connected with each other to constitute enclosed Type B outer container B1；Buck plate B12 includes equal
Capable interior heat-conducting plate B13, covering closing plate B14, interior heat-conducting plate B13, installation opening B15 and outer shroud are offered on covering closing plate B14
Seat B31 periphery be connected, on interior heat-conducting plate B13, covering closing plate B14 positioned at installation opening B15 surroundings position be provided with it is multiple
Fever slot B16 is to assemble heater, and the surrounding of installation opening B15 is provided with interval ring body B17, and interval ring body B17 is located at fever
Between slot B16, installation opening B15.When mixing, heater heats mixed raw material.Assembles post B11, buck plate B12 are real
Existing modularization assembling.
Preferred embodiment three, the stirring accessory on Type B blender B2 include the consistent upper drive disk B22 of structure, lower drive disk
B23, upper drive disk B22, lower drive disk B23 include a bore B24 of center position setting and are uniformly arranged around its surrounding
Multiple drive hole B25, bore B24 and be inserted into its internal mixing drum B21 and be fixedly connected, in the axial direction, upper drive disk B22,
Drive hole B25 or more on lower drive disk B23 corresponds coaxial arrangement, and upper and lower corresponding two drive hole B25 are one group, often
Group drive hole B25 be connected with the upper and lower side of driving tube B26, the side of driving tube B26 is provided with reciprocal telescopic device, be with
Any one in lower two kinds of structures：The first：Reciprocal telescopic device includes pipe close slot B6 and soft net B61, the driving tube
The inside of the sides B26 offers pipe close slot B6 to fill in soft net B61, the week of pipe close slot B6 and the sides driving tube B26 junction
Side is fixedly connected with the periphery of soft net B61, and multiple thin footpath hole B62 are evenly arranged on soft net B61；Second：Back and forth stretch
Compression apparatus includes rotating seat B7, rotation rod B71, rotating frame B72 and rotation net B73, the side of the driving tube B26 and rotating seat
The inner end of B7 is fixedly connected, the upper and lower ends rotatable engagement of the inside and rotation rod B71 of rotating seat B7, the side of rotation rod B71
It is connected with the arch B74 of rotating frame B72, frame bottom B75, frame inside portion B76, frame inside portion B76 and outer frame side B77 phases
Parallel, the upper and lower ends of outer frame side B77 are connected with arch B74, frame bottom B75, the outer ends arch B74, frame bottom B75
Outer end and outer frame side B77 surround the frame slot B78 of an outward opening to fill in rotation net B73 altogether, the inner side edge of rotation net B73
It is connected with the side of outer frame side B77, the outer side edges of rotation net B73 are connected with the inside portion of perpendicular net B731, erect net item
The upper and lower ends of B731 are connected with the outer end of top net B732, spacer screen B733 respectively, top net B732, spacer screen B733
Inner end is located at the inside of frame top sliding slot B741, frame bottom sliding slot B751, and top net B732 is slided along frame top sliding slot B741
Cooperation, spacer screen B733 is slidably matched along frame bottom sliding slot B751, and frame top sliding slot B741 is opened in the interior of arch B74
Portion, frame bottom sliding slot B751 are opened in the inside of frame bottom B75.The occupation mode of preferred embodiment three includes：First, mixing drum B21,
Upper drive disk B22, lower drive disk B23 itself are stirred, and the venthole opened up thereon sprays swirling eddy stirring outward；Secondly,
The reciprocal telescopic movement that the reciprocal telescopic device of rotation occurs is any one in following two methods of operation：(1), it uses
Before, soft net B61 is filled in pipe close slot B6, in use, under the action of outer knockout press, soft net B61 be thrown out of pipe close slot B6 with
Mixture in outer container is stirred；Also powder state additive and soft net B61 can be filled in into pipe close slot B6 together initial
It is interior, then under the action of outer knockout press, additive, soft net B61 are thrown out of together；(2), before use, top net B732, spacer screen item
The inner end of B733 is inserted into respectively inside frame top sliding slot B741, frame bottom sliding slot B751, meanwhile, erecting net B731, outer frame side B77 will
Rotation net B73 is sandwiched in frame slot B78, and when operation, outer knockout press caused by rotating, which will push up, nets a B732, spacer screen B733 respectively along frame
Top sliding slot B741, frame bottom sliding slot B751 are thrown away, and a perpendicular net B731 is also thrown out of, and rotation net B73 is flared, then, the rotation of rotation
Turn net B73 to be stirred the mixture in outer container；Also net B731, outer frame side B77 can be erected by rotation net initial
When B73 is sandwiched in frame slot B78, powder state additive and rotation net B73 are filled in together in frame slot B78, then in the effect of outer knockout press
Under, additive, rotation net B73 are thrown out of together.
Embodiment 1：
Referring to Fig. 1 to Figure 14, a method of potassium dihydrogen phosphate being produced using wet phosphoric acid refining by-product scourage, successively
Include the following steps：
Adjust sour technique：First scourage, water are uniformly mixed to obtain mixed liquor, P in mixed liquor2O5Mass percent it is dense
Degree is 18%；The scourage participates in obtaining after reacting from the sylvite washings that solvent extraction refined wet process phosphoric acid is configured
Product, which includes P2O5With sulfate radical, P2O5Mass percent concentration be 35%, the content of sulfate radical is 35g/
L；
Sulfur removal technology：First into above-mentioned mixed liquor by the 85% addition ground phosphate rock or carbon of sulfate radical stoichiometry in mixed liquor
Sour calcium or barium carbonate carry out desulfurization, and desulfurization time is 2-4 hours, and temperature is 75-90 DEG C, then is carried out to the solution after desulfurization
Filter, filtrate are sent to reactive tank, and filter residue is sent to phosphoric acid workshop and merged with ardealite；
Hybrid technique：First press 85% addition potassium chloride of the stoichiometry of phosphoric acid in above-mentioned filtrate, the stoichiometry of phosphoric acid
By P2O5Content convert, while addition while stir, mixing time be 1-2 hour, temperature be 70-80 DEG C, then will stir after
Solution send to decoloration slot；
Decoloration removing impurities technique：Activated carbon first is added in solution after agitation, decoloring assistant carries out decoloration removing impurities, activated carbon
Additive amount be the 1 ‰ of liquor capacity, the additive amount of decoloring assistant is the 5 ‰ of liquor capacity, then to the slurry after decoloration removing impurities
It is filtered to produce slurry clear liquid；The decoloring assistant is the aqueous solution that mass percent concentration is 1-15%, this kind water-soluble
The solvent of liquid be water, solute be potassium acetate, potassium thiosulfate, potassium sulfide, polyvinyl alcohol, polyoxyethylene alkyl amine, acrylamide,
Any one or arbitrary two kinds of mass ratioes in silicone surfactant JSY-6504, poly- alkyl phenol-ethylene oxide are 1:1 matches
Manufactured mixture is three kinds in mass ratio 1 arbitrary:1.75:3 mixtures being configured to；
Normal pressure concentration technology：Normal pressure concentration first is carried out to above-mentioned slurry clear liquid, the temperature of normal pressure concentration is 170 DEG C, normal pressure
Proportion after concentration is 1.30, meanwhile, the steam generated when being concentrated to normal pressure carries out water cycle washing to recycle hydrogen chloride, and send
It is sent to vacuum cooled crystallization tank to the fertile workshop of system, then by the slurry after concentration；
Crystallization and filtering technique：First to after above-mentioned concentration slurry carry out vacuum cooled crystallization, vacuum cooled crystallization when
Between be 2.5-4.5 hour, crystallization temperature is 40-50 DEG C, then is filtered the slurries after crystallization to obtain crystal and mother liquor,
Mother liquor includes potassium dihydrogen phosphate and sulfate radical, and the mass percent concentration of potassium dihydrogen phosphate is 35%, and the content of sulfate radical is
Then 40g/L dries to obtain product potassium dihydrogen phosphate crystal, parameter is：K2O 34.0%, P2O549.5%, SO4 2-
0.10%.
Embodiment 2：
Substance with embodiment 1, the difference is that：
Adjust sour technique：P in mixed liquor2O5Mass percent concentration be 22%；P in scourage2O5Mass percent it is dense
Degree is 45%, and the content of sulfate radical is 65g/L；
Sulfur removal technology：It is carried out by the 50% addition ground phosphate rock or calcium carbonate or barium carbonate of sulfate radical stoichiometry in mixed liquor
Desulfurization；
Hybrid technique：By 95% addition potassium chloride of the stoichiometry of phosphoric acid in filtrate；；
Decoloration removing impurities technique：The additive amount of activated carbon is the 5 ‰ of liquor capacity, and the additive amount of decoloring assistant is liquor capacity
1 ‰；
Normal pressure concentration technology：The temperature of normal pressure concentration is 140 DEG C, and the proportion after normal pressure concentration is 1.35；
Crystallization and filtering technique：The mass percent concentration of potassium dihydrogen phosphate is 45% in mother liquor, and the content of sulfate radical is
The parameter of 48g/L, product potassium dihydrogen phosphate is：K2O 35.2%, P2O552.3%, SO4 2-0.08%.
Embodiment 3：
Substance with embodiment 1, the difference is that：
Adjust sour technique：P in mixed liquor2O5Mass percent concentration be 20%；P in scourage2O5Mass percent it is dense
Degree is 40%, and the content of sulfate radical is 50g/L；
Sulfur removal technology：It is carried out by the 68% addition ground phosphate rock or calcium carbonate or barium carbonate of sulfate radical stoichiometry in mixed liquor
Desulfurization；
Hybrid technique：By 90% addition potassium chloride of the stoichiometry of phosphoric acid in filtrate；；
Decoloration removing impurities technique：The additive amount of activated carbon is the 2 ‰ of liquor capacity, and the additive amount of decoloring assistant is liquor capacity
3 ‰；
Normal pressure concentration technology：The temperature of normal pressure concentration is 155 DEG C, and the proportion after normal pressure concentration is 1.33；
Crystallization and filtering technique：The mass percent concentration of potassium dihydrogen phosphate is 40% in mother liquor, and the content of sulfate radical is
The parameter of 44g/L, product potassium dihydrogen phosphate is：K2O 34.6%, P2O550.9%, SO4 2-0.09%.
Embodiment 4：
Substance with embodiment 1, the difference is that：
Adjust sour technique：P in mixed liquor2O5Mass percent concentration be 19%；P in scourage2O5Mass percent it is dense
Degree is 44%, and the content of sulfate radical is 63g/L；
Sulfur removal technology：It is carried out by the 80% addition ground phosphate rock or calcium carbonate or barium carbonate of sulfate radical stoichiometry in mixed liquor
Desulfurization；
Hybrid technique：By 92% addition potassium chloride of the stoichiometry of phosphoric acid in filtrate；；
Decoloration removing impurities technique：The additive amount of activated carbon is the 4 ‰ of liquor capacity, and the additive amount of decoloring assistant is liquor capacity
1 ‰；
Normal pressure concentration technology：The temperature of normal pressure concentration is 160 DEG C, and the proportion after normal pressure concentration is 1.34；
Crystallization and filtering technique：The mass percent concentration of potassium dihydrogen phosphate is 39% in mother liquor, and the content of sulfate radical is
The parameter of 43g/L, product potassium dihydrogen phosphate is：K2O 34.8%, P2O551.9%, SO4 2-0.09%.
Embodiment 5：
Substance with embodiment 1, the difference is that：
Adjust sour technique：P in mixed liquor2O5Mass percent concentration be 21%；P in scourage2O5Mass percent it is dense
Degree is 37%, and the content of sulfate radical is 40g/L；
Sulfur removal technology：It is carried out by the 65% addition ground phosphate rock or calcium carbonate or barium carbonate of sulfate radical stoichiometry in mixed liquor
Desulfurization；
Hybrid technique：By 88% addition potassium chloride of the stoichiometry of phosphoric acid in filtrate；；
Decoloration removing impurities technique：The additive amount of activated carbon is the 4 ‰ of liquor capacity, and the additive amount of decoloring assistant is liquor capacity
4 ‰；
Normal pressure concentration technology：The temperature of normal pressure concentration is 150 DEG C, and the proportion after normal pressure concentration is 1.31；
Crystallization and filtering technique：The mass percent concentration of potassium dihydrogen phosphate is 43% in mother liquor, and the content of sulfate radical is
The parameter of 47g/L, product potassium dihydrogen phosphate is：K2O 34.5%, P2O551.2%, SO4 2-0.08%.
Embodiment 6：
Substance with embodiment 1, the difference is that：
Adjust sour technique：First mother liquor, scourage, water are uniformly mixed to obtain mixed liquor, P in mixed liquor2O5Quality percentage
Specific concentration is 20%；P in scourage2O5Mass percent concentration be 36%, the content of sulfate radical is 44g/L；Phosphoric acid in mother liquor
The mass percent concentration of potassium dihydrogen is 37.8%, and the content of sulfate radical is 43g/L；
Sulfur removal technology：It is carried out by the 80% addition ground phosphate rock or calcium carbonate or barium carbonate of sulfate radical stoichiometry in mixed liquor
Desulfurization；
Hybrid technique：By 95% addition potassium chloride of the stoichiometry of phosphoric acid in filtrate；；
Decoloration removing impurities technique：The additive amount of activated carbon is the 4 ‰ of liquor capacity, and the additive amount of decoloring assistant is liquor capacity
4 ‰；
Normal pressure concentration technology：The temperature of normal pressure concentration is 155 DEG C, and the proportion after normal pressure concentration is 1.33；
Crystallization and filtering technique：The mass percent concentration of potassium dihydrogen phosphate is 35% in mother liquor, and the content of sulfate radical is
The parameter of 40g/L, product potassium dihydrogen phosphate is：K2O 34.9%, P2O550.9%, SO4 2-0.10%.
Embodiment 7：
Substance with embodiment 6, the difference is that：
Adjust sour technique：P in mixed liquor2O5Mass percent concentration be 22%；P in scourage2O5Mass percent it is dense
Degree is 39%, and the content of sulfate radical is 45g/L；The mass percent concentration of potassium dihydrogen phosphate is 38.5% in mother liquor, sulfate radical
Content be 45g/L；
Sulfur removal technology：It is carried out by the 70% addition ground phosphate rock or calcium carbonate or barium carbonate of sulfate radical stoichiometry in mixed liquor
Desulfurization；
Hybrid technique：By 85% addition potassium chloride of the stoichiometry of phosphoric acid in filtrate；；
Decoloration removing impurities technique：The additive amount of activated carbon is the 5 ‰ of liquor capacity, and the additive amount of decoloring assistant is liquor capacity
5 ‰；
Normal pressure concentration technology：The temperature of normal pressure concentration is 170 DEG C, and the proportion after normal pressure concentration is 1.35；
Crystallization and filtering technique：The mass percent concentration of potassium dihydrogen phosphate is 39% in mother liquor, and the content of sulfate radical is
The parameter of 43g/L, product potassium dihydrogen phosphate is：K2O 35.1%, P2O551.7%, SO4 2-0.08%.
Embodiment 8：
Substance with embodiment 6, the difference is that：
Adjust sour technique：P in mixed liquor2O5Mass percent concentration be 21%；P in scourage2O5Mass percent it is dense
Degree is 41%, and the content of sulfate radical is 40g/L；The mass percent concentration of potassium dihydrogen phosphate is 41.3% in mother liquor, sulfate radical
Content be 46g/L；
Sulfur removal technology：It is carried out by the 60% addition ground phosphate rock or calcium carbonate or barium carbonate of sulfate radical stoichiometry in mixed liquor
Desulfurization；
Hybrid technique：By 88% addition potassium chloride of the stoichiometry of phosphoric acid in filtrate；；
Decoloration removing impurities technique：The additive amount of activated carbon is the 3 ‰ of liquor capacity, and the additive amount of decoloring assistant is liquor capacity
4 ‰；
Normal pressure concentration technology：The temperature of normal pressure concentration is 165 DEG C, and the proportion after normal pressure concentration is 1.32；
Crystallization and filtering technique：The mass percent concentration of potassium dihydrogen phosphate is 42% in mother liquor, and the content of sulfate radical is
The parameter of 45g/L, product potassium dihydrogen phosphate is：K2O 35.2%, P2O552.3%, SO4 2-0.10%.
Embodiment 9：
Substance with embodiment 6, the difference is that：
Adjust sour technique：P in mixed liquor2O5Mass percent concentration be 18%；P in scourage2O5Mass percent it is dense
Degree is 35%, and the content of sulfate radical is 35g/L；The mass percent concentration of potassium dihydrogen phosphate is 35% in mother liquor, sulfate radical
Content is 40g/L；
Sulfur removal technology：It is carried out by the 50% addition ground phosphate rock or calcium carbonate or barium carbonate of sulfate radical stoichiometry in mixed liquor
Desulfurization；
Hybrid technique：By 90% addition potassium chloride of the stoichiometry of phosphoric acid in filtrate；；
Decoloration removing impurities technique：The additive amount of activated carbon is the 1 ‰ of liquor capacity, and the additive amount of decoloring assistant is liquor capacity
1 ‰；
Normal pressure concentration technology：The temperature of normal pressure concentration is 140 DEG C, and the proportion after normal pressure concentration is 1.35；
Crystallization and filtering technique：The mass percent concentration of potassium dihydrogen phosphate is 36% in mother liquor, and the content of sulfate radical is
The parameter of 42g/L, product potassium dihydrogen phosphate is：K2O 34.2%, P2O551.1%, SO4 2-0.09%.
Embodiment 10：
Substance with embodiment 6, the difference is that：
Adjust sour technique：P in mixed liquor2O5Mass percent concentration be 19%；P in scourage2O5Mass percent it is dense
Degree is 45%, and the content of sulfate radical is 65g/L；The mass percent concentration of potassium dihydrogen phosphate is 45% in mother liquor, sulfate radical
Content is 48g/L；
Sulfur removal technology：It is carried out by the 85% addition ground phosphate rock or calcium carbonate or barium carbonate of sulfate radical stoichiometry in mixed liquor
Desulfurization；
Hybrid technique：By 94% addition potassium chloride of the stoichiometry of phosphoric acid in filtrate；；
Decoloration removing impurities technique：The additive amount of activated carbon is the 2 ‰ of liquor capacity, and the additive amount of decoloring assistant is liquor capacity
5 ‰；
Normal pressure concentration technology：The temperature of normal pressure concentration is 170 DEG C, and the proportion after normal pressure concentration is 1.30；
Crystallization and filtering technique：The mass percent concentration of potassium dihydrogen phosphate is 42% in mother liquor, and the content of sulfate radical is
The parameter of 45g/L, product potassium dihydrogen phosphate is：K2O 35.2%, P2O552.3%, SO4 2-0.08%.
Embodiment 11：
Substance with embodiment 6, the difference is that：
Adjust sour technique：P in mixed liquor2O5Mass percent concentration be 20%；P in scourage2O5Mass percent it is dense
Degree is 40%, and the content of sulfate radical is 50g/L；The mass percent concentration of potassium dihydrogen phosphate is 40% in mother liquor, sulfate radical
Content is 44g/L；
Sulfur removal technology：It is carried out by the 70% addition ground phosphate rock or calcium carbonate or barium carbonate of sulfate radical stoichiometry in mixed liquor
Desulfurization；
Hybrid technique：By 90% addition potassium chloride of the stoichiometry of phosphoric acid in filtrate；；
Decoloration removing impurities technique：The additive amount of activated carbon is the 4 ‰ of liquor capacity, and the additive amount of decoloring assistant is liquor capacity
3 ‰；
Normal pressure concentration technology：The temperature of normal pressure concentration is 160 DEG C, and the proportion after normal pressure concentration is 1.34；
Crystallization and filtering technique：The mass percent concentration of potassium dihydrogen phosphate is 44% in mother liquor, and the content of sulfate radical is
The parameter of 46g/L, product potassium dihydrogen phosphate is：K2O 34.8%, P2O551.8%, SO4 2-0.08%.
Claims (9)
1. a kind of method producing potassium dihydrogen phosphate using wet phosphoric acid refining by-product scourage includes decoloration removing impurities work successively
Skill, normal pressure concentration technology, crystallization and filtering technique, it is characterised in that：The method further include before removing impurities technique of decolourizing according to
The tune acid technique of secondary progress, sulfur removal technology, hybrid technique, and the operation of each technique is as follows：
Adjust sour technique：First scourage, water are uniformly mixed to obtain mixed liquor, P in the mixed liquor2O5Mass percent concentration
For 18-22%；The scourage participates in obtaining after reacting from the sylvite washings that solvent extraction refined wet process phosphoric acid is configured
The product arrived, the scourage include P2O5With sulfate radical, P2O5Mass percent concentration be 35-45%, the content of sulfate radical is
35-65g/L；
Sulfur removal technology：First add ground phosphate rock or calcium carbonate in above-mentioned mixed liquor or barium carbonate carry out desulfurization, then to desulfurization after
Solution is filtered, and filtrate is sent to reactive tank；
Hybrid technique：In reactive tank, the 85-95% for first pressing the stoichiometry of phosphoric acid in above-mentioned filtrate adds potassium chloride, phosphoric acid
Stoichiometry is by P2O5Content convert, while addition while stir, then by the solution after stirring send to decolourize slot；
Decoloration removing impurities technique：It decolourizes in slot, first addition activated carbon, decoloring assistant carry out decoloration removing impurities in solution after agitation,
The slurry after decoloration removing impurities is filtered to produce slurry clear liquid again；
Normal pressure concentration technology：Normal pressure concentration first is carried out to above-mentioned slurry clear liquid, then the slurry after concentration is sent to vacuum cooled knot
Brilliant slot；
Crystallization and filtering technique：In vacuum cooled crystallization tank, vacuum cooled crystallization first is carried out to the slurry after above-mentioned concentration, then right
Slurries after crystallization are filtered to obtain crystal and mother liquor, then dry crystal to obtain product potassium dihydrogen phosphate；It is described
Crystallization is with filtering technique, and the mother liquor includes potassium dihydrogen phosphate and sulfate radical, and the mass percent concentration of potassium dihydrogen phosphate
Content for 35-45%, sulfate radical is 40-48g/L, meanwhile, the mother liquor of filtering gained is sent to the tune acid technique of next round
In, be uniformly mixed together with scourage, water to obtain mixed liquor.
2. a kind of method producing potassium dihydrogen phosphate using wet phosphoric acid refining by-product scourage according to claim 1,
It is characterized in that：
In the sulfur removal technology, by the 50-85% addition ground phosphate rock or calcium carbonate or carbonic acid of sulfate radical stoichiometry in mixed liquor
Barium carries out desulfurization, and desulfurization time is 2-4 hours, and temperature is 75-90 DEG C.
3. a kind of method producing potassium dihydrogen phosphate using wet phosphoric acid refining by-product scourage according to claim 2,
It is characterized in that：
In the sulfur removal technology, the solution after desulfurization is filtered, and filtrate is sent to reactive tank, filter residue sends to phosphoric acid workshop
Merge with ardealite.
4. a kind of method producing potassium dihydrogen phosphate using wet phosphoric acid refining by-product scourage according to claim 1,
It is characterized in that：
In the hybrid technique, mixing time is 1-2 hours, and temperature is 70-80 DEG C.
5. a kind of method producing potassium dihydrogen phosphate using wet phosphoric acid refining by-product scourage according to claim 1,
It is characterized in that：
In the normal pressure concentration technology, the proportion after the concentration of slurry clear liquid normal pressure is 1.30-1.35, and the temperature of normal pressure concentration is
140-170℃.
6. a kind of method producing potassium dihydrogen phosphate using wet phosphoric acid refining by-product scourage according to claim 5,
It is characterized in that：
In the normal pressure concentration technology, normal pressure concentration is carried out to slurry clear liquid in the evaporator of inner liner polytetrafluoroethylene, meanwhile,
The steam generated when being concentrated to normal pressure carries out water cycle washing to recycle hydrogen chloride, and send to the fertile workshop of system.
7. a kind of method producing potassium dihydrogen phosphate using wet phosphoric acid refining by-product scourage according to claim 1,
It is characterized in that：
The crystallization is with filtering technique, and the time of vacuum cooled crystallization is 2.5-4.5 hours, and crystallization temperature is 40-50 DEG C,
After crystallization, the slurries after crystallization are filtered to obtain crystal and mother liquor with centrifuge, crystal is by fluidized bed drying.
8. a kind of method producing potassium dihydrogen phosphate using wet phosphoric acid refining by-product scourage according to claim 1,
It is characterized in that：In the decoloration removing impurities technique, activated carbon, decoloring assistant additive amount respectively be liquor capacity 1-5 ‰.
9. a kind of method producing potassium dihydrogen phosphate using wet phosphoric acid refining by-product scourage according to claim 8,
It is characterized in that：The decoloring assistant is the aqueous solution that mass percent concentration is 1-15%, and the solvent of this kind of aqueous solution is water,
Solute is potassium acetate, potassium thiosulfate, potassium sulfide, polyvinyl alcohol, polyoxyethylene alkyl amine, acrylamide, silicone surfactants
In agent JSY-6504, poly- alkyl phenol-ethylene oxide any one or it is arbitrary two kinds in mass ratio be 1:1 mixing being configured to
Object is three kinds in mass ratio 1 arbitrary:1.75:3 mixtures being configured to.
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