CN104944397B - A kind of technique that potassium dihydrogen phosphate is prepared by purification of wet process phosphoric acid low cost - Google Patents

A kind of technique that potassium dihydrogen phosphate is prepared by purification of wet process phosphoric acid low cost Download PDF

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CN104944397B
CN104944397B CN201510279076.7A CN201510279076A CN104944397B CN 104944397 B CN104944397 B CN 104944397B CN 201510279076 A CN201510279076 A CN 201510279076A CN 104944397 B CN104944397 B CN 104944397B
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sulfate
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CN104944397A (en
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陈锂
陈庚
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Wuhan Huiding Science & Technology Co Ltd
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Abstract

The invention discloses a kind of technique that potassium dihydrogen phosphate is prepared by purification of wet process phosphoric acid low cost, (1) synthos preparations: P2O5The purification of phosphoric acid of mass fraction 30%~48% is reacted with 200% calcium salt of stoichiometry;(2) polyoxyethylene alkyl amine of solution quality 0.1%~1.3% and the composite assistant of propylene glycol block polyether composition desulfurization: are added in the potassium acid sulfate or potassium sulfate solution of mass fraction 10%~30%, at 40~90 DEG C, stoichiometrically 1: l ratio be added step (1) synthos to pH be 4.5~4.8,50~90 DEG C keep the temperature 4 hours, sulfuric acid calcium is filtered, mother liquor is concentrated, crystallization, washing, dry potassium dihydrogen phosphate.Composite assistant is added in potassium acid sulfate or potassium sulfate are reacted with calcium salt in the present invention, and the calcium sulphate crystal of generation is regular, easily filters, and in calcium sulphate crystal adsorption, reduces calcium sulphate crystal surface free energy, phosphorus potassium lost rate is low.

Description

A kind of technique that potassium dihydrogen phosphate is prepared by purification of wet process phosphoric acid low cost
Technical field
The invention belongs to phosphate preparation technical fields, and in particular to one kind is by potassium sulfate or potassium acid sulfate and phosphoric acid by wet process The method for preparing potassium dihydrogen phosphate.
Background technique
Potassium dihydrogen phosphate is widely used in the industries such as chemical industry, medicine, food and farming and animal husbandry, especially agriculturally, due to phosphorus Acid dihydride potassium has nutritional ingredient high, and amount of application is few, is suitable for various soil and crop, and can be used for soaking seed, soaks root, blade face spray It applies and pours, therefore rapidly developed and be widely applied in recent years.
It is technically not difficult to prepare potassium dihydrogen phosphate, it is important to production cost, around reducing cost, the life developed at present Production. art mainly has: neutralisation, double decomposition, extraction, ion-exchange, electrolysis method and direct method.
Wherein direct method is that potassium chloride and sulfuric acid reaction are generated to potassium acid sulfate and hydrogen chloride, and hydrogen chloride is secondary after being absorbed with water Produce hydrochloric acid;Potassium acid sulfate and excessive sulfuric acid are reacted with phosphorus ore generates potassium dihydrogen phosphate, hydrofluoric acid, phosphoric acid mixed solution and phosphorus Gypsum;Silica defluorinate is added into mixed solution, is filtered to remove ardealite, filtrate is that potassium dihydrogen phosphate is mixed with phosphoric acid Liquid after concentration, is added methanol extraction and goes out potassium dihydrogen phosphate, distillation filtrate recycles methanol, and the technique is by Irish Ge Erding fertilizer Company's invention, it is considered to be the most economical method of production potassium dihydrogen phosphate.The states such as subsequent Israel, the U.S., Japan carry out in succession Process optimization, the improvements of Rotem company, Israel are without using solvent extraction and separation potassium dihydrogen phosphate.Direct method is most Big advantage is that have used more cheap rock phosphate in powder, sulfuric acid and potassium chloride be raw material, but more demanding to rock phosphate in powder, it is necessary to using excellent Matter rock phosphate in powder, although China's phosphate rock resource is abundant, grade is not high, after sulfuric acid to leach, gained phosphoric acid liquid rich in magnesium, calcium, iron, The plurality of impurities such as aluminium, sulfate radical, fluosilicic acid root, fluorine ion, complicated components, it is difficult to purify, therefore qualified di(2-ethylhexyl)phosphate can not be produced Hydrogen potassium.In recent years, domestic to have carried out serial improvement and optimization to this technique, applied for a collection of patent: CN103265000A is disclosed It is directly reacted with potassium sulfate with calcium dihydrogen phosphate and generates potassium dihydrogen phosphate;CN102424374A, CN103058158A are disclosed It is directly reacted with potassium acid sulfate with calcium monohydrogen phosphate and generates potassium dihydrogen phosphate;CN103332668A is disclosed with potassium acid sulfate and is raised calcium Directly reaction generates potassium dihydrogen phosphate;CN102963874A is disclosed, and calcium carbonate generation is added into potassium sulfate and phosphoric acid mixed liquor Potassium dihydrogen phosphate.
" direct method " most essential reaction is that calcium sulfate precipitation is generated after reacting by calcium salt with sulfate radical to prepare phosphoric acid Potassium dihydrogen, the greatest drawback of such technique are that calcium sulfate precipitation can be mingled with a large amount of phosphate radical and potassium ion, are formed so-called total Crystalline substance precipitating, general phosphate radical mass fraction is 10% or more, and potassium ion mass fraction is 5% or more;And phosphate radical and potassium ion Be filtered in company with calcium sulfate precipitation, buried as waste material, can not reuse, cause significant loss, improve cost of material, make this Technique loses the superiority of low raw-material cost, is influenced by this technical problem, which fails always industrialized production, and the country is still Continue to use traditional neutralisation or ion-exchange production potassium dihydrogen phosphate.
Summary of the invention
Object of the present invention is to for above-mentioned potassium dihydrogen phosphate production status and existing industrial technology problem and solution sulfuric acid Calcium precipitate is mingled with phosphate radical and potassium ion problem, provides that a kind of raw material is sufficient, be easy to get, simple process, can significantly reduce raw material and disappears Consumption, inexpensive and what is be convenient for industrialized production prepares potassium dihydrogen phosphate technique by purification of wet process phosphoric acid.
The object of the invention implementation is a kind of technique that potassium dihydrogen phosphate is prepared by purification of wet process phosphoric acid low cost, tool Steps are as follows for body:
(1) prepared by synthos: purification of wet process phosphoric acid is added in reactor, is added according to the ratio of stoichiometry 200% Calcium salt is transferred to measuring tank after reacting 2~3 hours between 40~70 DEG C;
The purification of wet process phosphoric acid P2O5Mass fraction is 30%~48%;
The calcium salt is calcium oxide, calcium hydroxide or calcium carbonate;
(2) it desulfurization: in the potassium acid sulfate or potassium sulfate addition reaction kettle for being 10%~30% by mass fraction, is stirring Under, composite assistant is added according to 0.1%~1.3% ratio of potassium acid sulfate or potassium sulfate solution quality, is heated to 40~90 DEG C Afterwards, the synthos of step (1) are added according to 1: l ratio of stoichiometry, controls the pH of solution terminal between 4.5~4.8, adds Material is finished, and keeps the temperature 4 hours at 50~90 DEG C, is filtered to remove calcium sulfate, mother liquor is transferred to enrichment process;
The composite assistant is made of non-ionic surfactant polyoxyethylene alkylamine and propylene glycol block polyether, group Point and mass fraction are as follows: polyoxyethylene alkyl amine 1%~99%, propylene glycol block polyether 1~99%;
The polyoxyethylene alkyl amine are as follows: lauryl amine polyoxyethylene ether or octadecylamine polyoxyethylene ether, wherein polyoxy second Alkene ether number=2~30;
The propylene glycol block polyether are as follows: L35, L44, L45, L64, P65, F68 or F38;
(3) concentration and crystallization: 103 DEG C are heated to by step (2) is mother liquid obtained, concentration is evaporated, until there is a little solid It when appearance, is transferred in crystallization kettle, under slow stirring, is gradually cooled to room temperature, filter, the desulfurization work of filtrate return step (2) Sequence, crystal are transferred to washing procedure;
(4) washing and drying: the crystal of step (3) being transferred in washing kettle, is washed with deionized three times, centrifugation point From, be drying to obtain potassium dihydrogen phosphate product;
Second and third secondary washing water is recycled, first and second time is prepared in potassium dihydrogen phosphate wash crystallization as next round and washes Wash water, third time wash water fresh deionized water.
The present invention is added one kind and is gathered by nonionic surfactant in potassium acid sulfate or potassium sulfate and calcium salt reaction process The composite assistant of ethylene oxide alkylamine and propylene glycol block polyether composition, make the calcium sulphate crystal generated it is regular, in thicker plagioclase Web crystal;Composite assistant and in calcium sulphate crystal adsorption, reduces the surface free energy of calcium sulphate crystal, to eliminate sulphur Sour calcium precipitate is mingled with phosphate radical and potassium ion, realizes that phosphate radical and potassium ion maximum utilize.
Of the invention significantly has the technical effect that
1, it solves calcium sulfate precipitation and is mingled with phosphate radical and potassium ion technical problem, P in gained calcium sulfate precipitation2O5Quality Score is 0.23%~1.77%, K2The mass fraction of O is 0.01%~0.05%, and phosphorus potassium lost is less, and entire reaction is envelope Closure system, exclusive outside sulfuric acid calcium precipitate, without other emissions, therefore phosphorus potassium utilization rate is high, significantly reduces consumption of raw materials;
2, it realizing with the purpose of cheap calcium salt removing sulfate radical, gained potassium dihydrogen phosphate product meets industrial grade standard, It is theoretically most economical potassium dihydrogen phosphate production line;
3, calcium sulfate precipitation has certain hydrophobicity, is easy to filter and wash, is convenient for work because being adsorbed with surfactant Industry metaplasia produces;
4, using purification of wet process phosphoric acid and potassium acid sulfate or potassium sulfate as raw material, raw material is easy to get, sufficient, simple process, changes Existing PHOSPHORIC ACID TECH.GRADE potassium dihydrogen production technology.
Specific embodiment
The present invention is added one kind and is gathered by nonionic surfactant in potassium acid sulfate or potassium sulfate and calcium salt reaction process The composite assistant of ethylene oxide alkylamine and propylene glycol block polyether composition, make the calcium sulphate crystal generated it is regular, in thicker plagioclase Web crystal, composite assistant and in calcium sulphate crystal adsorption reduce the surface free energy of calcium sulphate crystal, to eliminate sulfuric acid Calcium precipitate is mingled with phosphate radical and potassium ion, realizes that phosphate radical and potassium ion maximum utilize.
The composite assistant is made of non-ionic surfactant polyoxyethylene alkylamine and propylene glycol block polyether, group Point and mass fraction are as follows: polyoxyethylene alkyl amine 1%~99%, propylene glycol block polyether 1~99%.Preferably polyoxyethylene Alkylamine 24%~60%, propylene glycol block polyether 40%~76%.
Non-ionic surfactant polyoxyethylene alkylamine and propylene glycol block polyether will form not with degree of polymerization difference Same product, kind is more, in the present invention, each kind to show certain effect, such product can be used as this hair Bright composite assistant, but in polyoxyethylene alkyl amine class product, with lauryl amine polyoxyethylene ether or octadecylamine polyoxyethylene ether, Polyoxyethylene ether number=2~30 are optimal.
The present invention is described in detail with specific embodiment below.
Embodiment 1:
(1) prepared by synthos: purification of wet process phosphoric acid being added in reactor, is added according to the ratio of stoichiometry 200% Enter calcium oxide, after 70 DEG C are reacted 3 hours, is transferred to measuring tank.P in purification of wet process phosphoric acid2O5Mass fraction is 30%.
(2) desulfurization: the potassium sulfate that mass fraction is 10% is added in reaction kettle, under stiring, according to potassium sulfate solution Composite assistant, composite assistant composition is added in 0.1% ratio of quality are as follows: and lauryl amine polyoxyethylene ether (2) mass fraction is 1%, L35 mass fraction is 99%.Then after reaction solution being heated to 40 DEG C, the phosphorus of step (1) is added according to 1: l ratio of stoichiometry Acid calcium salt controls the pH of solution terminal between 4.5~4.8, and charging is finished, and keeps the temperature 4 hours at 50 DEG C, is filtered to remove calcium sulfate, Mother liquor is transferred to enrichment process.To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.03%, P2O5%= 0.91%.
(3) concentration and crystallization: being heated to 103 DEG C for above-mentioned mother liquor, be evaporated concentration, when there is a little solid to occur, It is transferred in crystallization kettle while hot, under slow stirring, is gradually cooled to room temperature, filter, the desulfurization process of filtrate return step (2), Crystal is transferred to washing procedure.
(4) washing and drying: crystal is transferred in washing kettle, is washed with deionized three times, centrifuge separation, filtrate is returned It returns in crystallization kettle, crystal is drying to obtain potassium dihydrogen phosphate product;
Second and third secondary washing water is recycled, first and second time prepared in potassium dihydrogen phosphate wash crystallization as next round is washed Wash water.
Potassium dihydrogen phosphate product is analyzed, as a result are as follows: K2O%=35.12%, P2O5%=50.98%, SO4 2-% =0.22%.
Embodiment 2: with embodiment 1, the difference is that:
(1) prepared by synthos: purification of wet process phosphoric acid being added in reactor, is added according to 200% ratio of stoichiometry Calcium carbonate is transferred to measuring tank after 50 DEG C are reacted 2 hours.P in purification of wet process phosphoric acid2O5Mass fraction is 48%.
(2) desulfurization: the potassium sulfate of mass fraction 20% is added in reaction kettle, under stiring, according to potassium sulfate solution matter Composite assistant, composite assistant composition is added in 1.0% ratio of amount are as follows: and lauryl amine polyoxyethylene ether (2) mass fraction is 49%, L35 mass fraction is 51%.After reaction solution is heated to 50 DEG C, the synthos of step (1) are added, charging is finished, and keeps the temperature 4 at 70 DEG C Hour.To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.047%, P2O5%=1.32%.
(4) washing and dry: crystal is transferred in washing kettle, with second and third washing washing first and second time, go from Sub- water washing third time, centrifuge separation, first time filtrate return in crystallization kettle, and crystal is drying to obtain potassium dihydrogen phosphate product;
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=35.61%, P2O5%=50.17%, SO4 2-%=0.31%.
Embodiment 3: with embodiment 2, the difference is that:
(1) prepared by synthos: purification of wet process phosphoric acid being added in reactor, is added according to the ratio of stoichiometry 200% Enter calcium hydroxide, after 40 DEG C are reacted 2 hours, is transferred to measuring tank.P in purification of wet process phosphoric acid2O5Mass fraction is 41%.
(2) desulfurization: the potassium sulfate of mass fraction 10% is added in reaction kettle, under stiring, according to potassium sulfate solution matter Composite assistant, composite assistant composition is added in 1.3% ratio of amount are as follows: and lauryl amine polyoxyethylene ether (15) mass fraction is 99%, L35 mass fraction is 1%.After reaction solution is heated to 90 DEG C, the synthos of step (1) are added, charging is finished, and keeps the temperature 4 at 90 DEG C Hour.
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.05%, P2O5%=1.48%.
Washing analyzes result with the potassium dihydrogen phosphate after drying are as follows: K2O%=36.11%, P2O5%=49.73%, SO4 2-%=0.36%.
Embodiment 4, with embodiment 2, the difference is that:
(1) prepared by synthos: purification of wet process phosphoric acid being added in reactor, is added according to 200% ratio of stoichiometry Calcium carbonate is transferred to measuring tank after 60 DEG C are reacted 2 hours.P in purification of wet process phosphoric acid2O5Mass fraction is 35%.
(2) desulfurization: the potassium sulfate that mass fraction is 20% is added in reaction kettle, under stiring, according to potassium sulfate solution Composite assistant, composite assistant composition is added in 0.7% ratio of quality are as follows: and lauryl amine polyoxyethylene ether (30) mass fraction is 99%, L35 mass fraction is 1%.After reaction solution is heated to 50 DEG C, the synthos of step (1) are added, charging is finished, and keeps the temperature 4 at 70 DEG C Hour.
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.01%, P2O5%=0.42%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=35.04%, P2O5%=51.97%, SO4 2-%=0.16%.
Embodiment 5, with embodiment 2, the difference is that:
(2) desulfurization: the potassium acid sulfate that mass fraction is 30% is added in reaction kettle, under stiring, according to potassium acid sulfate Composite assistant, composite assistant composition is added in 0.7% ratio of solution quality are as follows: lauryl amine polyoxyethylene ether (30) mass fraction is 99%, L44 mass fraction are 1%.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.03%, P2O5%=1.12%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=34.72%, P2O5%=52.67%, SO4 2-%=0.36%.
Embodiment 6, with embodiment 2, the difference is that:
(2) desulfurization: the potassium sulfate that mass fraction is 18% is added in reaction kettle, under stiring, according to potassium sulfate solution Composite assistant, composite assistant composition is added in 0.7% ratio of quality are as follows: and lauryl amine polyoxyethylene ether (15) mass fraction is 50%, L44 mass fraction is 50%.After reaction solution is heated to 80 DEG C, the synthos of step (1) are added, charging is finished, and keeps the temperature 4 at 60 DEG C Hour.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.02%, P2O5%=1.02%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=33.41%, P2O5%=53.54%, SO4 2-%=0.31%.
Embodiment 7, with embodiment 2, the difference is that:
(2) desulfurization: the potassium sulfate that mass fraction is 15% is added in reaction kettle, under stiring, according to potassium sulfate solution Composite assistant, composite assistant composition is added in 0.2% ratio of quality are as follows: and lauryl amine polyoxyethylene ether (2) mass fraction is 39%, L45 mass fraction is 61%.After reaction solution is heated to 60 DEG C, the synthos of step (1) are added, charging is finished, and keeps the temperature 4 at 80 DEG C Hour.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.03%, P2O5%=1.63%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=34.41%, P2O5%=52.92%, SO4 2-%=0.24%.
Embodiment 8, with embodiment 2, the difference is that:
(2) desulfurization: the potassium acid sulfate that mass fraction is 25% is added in reaction kettle, under stiring, according to potassium acid sulfate Composite assistant, composite assistant composition are as follows: lauryl amine polyoxyethylene ether (30) mass fraction is is added in 0.3% ratio of solution quality 60%, L64 mass fraction are 40%.After reaction solution is heated to 50 DEG C, the synthos of step (1) are added, charging is finished, at 70 DEG C Heat preservation 4 hours.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.02%, P2O5%=0.96%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=34.94%, P2O5%=51.95%, SO4 2-%=0.42%.
Embodiment 9, with embodiment 2, the difference is that:
(2) desulfurization: the potassium acid sulfate that mass fraction is 25% is added in reaction kettle, under stiring, according to potassium acid sulfate Composite assistant, composite assistant composition is added in 0.5% ratio of solution quality are as follows: lauryl amine polyoxyethylene ether (30) mass fraction is 21%, L64 mass fraction are 79%.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.04%, P2O5%=1.77%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=33.27%, P2O5%=52.87%, SO4 2-%=0.36%.
Embodiment 10, with embodiment 2, the difference is that:
(2) desulfurization: under stiring, composite assistant, composite assistant group is added according to 1.1% ratio of potassium sulfate solution quality Become: lauryl amine polyoxyethylene ether (30) mass fraction is that 39%, P65 mass fraction is 61%.After reaction solution is heated to 50 DEG C, The synthos of step (1) are added, charging is finished, and keeps the temperature 4 hours at 70 DEG C.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.01%, P2O5%=0.76%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=34.12%, P2O5%=52.21%, SO4 2-%=0.22%.
Embodiment 11, with embodiment 2, the difference is that:
(2) desulfurization: under stiring, composite assistant, composite assistant group is added according to 1.3% ratio of potassium sulfate solution quality Become: lauryl amine polyoxyethylene ether (2) mass fraction is that 60%, F68 mass fraction is 40%.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.01%, P2O5%=0.67%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=35.16%, P2O5%=53.01%, SO4 2-%=0.17%.
Embodiment 12, with embodiment 2, the difference is that:
(2) desulfurization: under stiring, composite assistant, composite assistant group is added according to 1.3% ratio of potassium sulfate solution quality Become: lauryl amine polyoxyethylene ether (15) mass fraction is that 51%, F38 mass fraction is 49%.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.03%, P2O5%=0.93%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=35.23%, P2O5%=52.89%, SO4 2-%=0.31%.
Embodiment 13, with embodiment 2, the difference is that:
(2) desulfurization: under stiring, the potassium acid sulfate that mass fraction is 30% is added in reaction kettle, according to potassium acid sulfate Composite assistant, composite assistant composition is added in 0.1% ratio of solution quality are as follows: octadecylamine polyoxyethylene ether (2) mass fraction is 1%, F68 mass fraction are 99%.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.01%, P2O5%=0.39%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=35.07%, P2O5%=51.93%, SO4 2-%=0.24%.
Embodiment 14, with embodiment 2, the difference is that:
(2) desulfurization: under stiring, the potassium acid sulfate that mass fraction is 20% is added in reaction kettle, according to potassium acid sulfate Composite assistant, composite assistant composition is added in 1.3% ratio of solution quality are as follows: octadecylamine polyoxyethylene ether (2) mass fraction is 51%, L35 mass fraction are 49%.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.01%, P2O5%=0.23%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=36.37%, P2O5%=50.43%, SO4 2-%=0.29%.
Embodiment 15, with embodiment 2, the difference is that:
(2) desulfurization: under stiring, the potassium sulfate that mass fraction is 10% is added in reaction kettle, according to potassium sulfate solution Composite assistant, composite assistant composition is added in 0.8% ratio of quality are as follows: and octadecylamine polyoxyethylene ether (10) mass fraction is 51%, L44 mass fraction is 49%.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.03%, P2O5%=0.31%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=35.49%, P2O5%=51.02%, SO4 2-%=0.31%.
Embodiment 16, with embodiment 2, the difference is that:
(2) composite assistant, composite assistant composition are as follows: 18 desulfurization: is added according to 1.3% ratio of potassium sulfate solution quality Amine polyoxyethylene ether (15) mass fraction is that 50%, L45 mass fraction is 50%.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.01%, P2O5%=0.23%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=36.37%, P2O5%=50.43%, SO4 2-%=0.29%.
Embodiment 17, with embodiment 2, the difference is that:
(2) composite assistant, composite assistant composition are as follows: 18 desulfurization: is added according to 1.3% ratio of potassium sulfate solution quality Amine polyoxyethylene ether (30) mass fraction is that 50%, P65 mass fraction is 50%.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.05%, P2O5%=0.31%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=37.49%, P2O5%=49.51%, SO4 2-%=0.49%.
Embodiment 18, with embodiment 2, the difference is that:
(2) composite assistant, composite assistant composition are as follows: 18 desulfurization: is added according to 1.3% ratio of potassium sulfate solution quality Amine polyoxyethylene ether (2) mass fraction is that 24%, L64 mass fraction is 76%.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.01%, P2O5%=0.79%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=36.23%, P2O5%=50.11%, SO4 2-%=0.32%.
Embodiment 19, with embodiment 2, the difference is that:
(2) composite assistant, composite assistant composition are as follows: 18 desulfurization: is added according to 0.8% ratio of potassium sulfate solution quality Amine polyoxyethylene ether (20) mass fraction is that 51%, F38 mass fraction is 49%.
Items analysis result is as follows:
To K in calcium sulfate2O、P2O5Content is analyzed, as a result are as follows: K2O%=0.01%, P2O5%=0.27%.
Potassium dihydrogen phosphate analyzes result are as follows: K2O%=36.49%, P2O5%=50.02%, SO4 2-%=0.43%.

Claims (2)

1. a kind of technique for preparing potassium dihydrogen phosphate by purification of wet process phosphoric acid low cost, it is characterised in that: specific step is as follows:
(1) prepared by synthos: purification of wet process phosphoric acid is added in reactor, and oxidation is added according to the ratio of stoichiometry 200% Calcium, calcium hydroxide or calcium carbonate are transferred to measuring tank after reacting 2~3 hours between 40~70 DEG C;
The purification of wet process phosphoric acid P2O5Mass fraction is 30%~48%;
(2) it desulfurization: in the potassium acid sulfate or potassium sulfate addition reaction kettle for being 10%~30% by mass fraction, under stiring, presses Composite assistant is added according to 0.1%~1.3% ratio of potassium acid sulfate or potassium sulfate solution quality to press after being heated to 40~90 DEG C The synthos of step (1) are added according to 1: l ratio of stoichiometry, control the pH of solution terminal between 4.5~4.8, charging is finished, 4 hours are kept the temperature at 50~90 DEG C, is filtered to remove calcium sulfate, mother liquor is transferred to enrichment process;
The composite assistant is made of non-ionic surfactant polyoxyethylene alkylamine and propylene glycol block polyether, component and Mass fraction are as follows: polyoxyethylene alkyl amine 1%~99%, propylene glycol block polyether 1~99%;
The polyoxyethylene alkyl amine are as follows: lauryl amine polyoxyethylene ether or octadecylamine polyoxyethylene ether, wherein polyoxyethylene ether Number=2~30;
The propylene glycol block polyether are as follows: L35, L44, L45, L64, P65, F68 or F38;
(3) concentration and crystallization: being heated to 103 DEG C for step (2) is mother liquid obtained, be evaporated concentration, until there is a little solid appearance When, it is transferred in crystallization kettle, under slow stirring, is gradually cooled to room temperature, filter, the desulfurization process of filtrate return step (2), knot Brilliant object is transferred to washing procedure;
(4) washing and drying: the crystal of step (3) being transferred in washing kettle, is washed with deionized three times, centrifuge separation, It is drying to obtain potassium dihydrogen phosphate product;
Second and third secondary washing water is recycled, first and second time in potassium dihydrogen phosphate wash crystallization washing is prepared as next round Water, third time wash water fresh deionized water.
2. a kind of technique for preparing potassium dihydrogen phosphate by purification of wet process phosphoric acid low cost according to claim 1, feature It is: the component and mass fraction of non-ionic surfactant polyoxyethylene alkylamine and propylene glycol block polyether are as follows: polyoxy second Allylic alkylation amine 24%~60%, propylene glycol block polyether 40%~76%.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101054170A (en) * 2007-04-13 2007-10-17 宜昌市仁和矿业有限责任公司 Method for preparing potassium dihydrogen phosphate from calcium hydrogen phosphate
CN102963874A (en) * 2012-11-26 2013-03-13 四川川恒化工股份有限公司 Method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101054170A (en) * 2007-04-13 2007-10-17 宜昌市仁和矿业有限责任公司 Method for preparing potassium dihydrogen phosphate from calcium hydrogen phosphate
CN102963874A (en) * 2012-11-26 2013-03-13 四川川恒化工股份有限公司 Method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
聚氧乙烯烷基胺的性能及其应用;李兰廷;《精细与专用化学品》;20040806;第12卷(第15期);6-11

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