CN1907843A - Method of classification utilizing wet-process phosphoric acid - Google Patents
Method of classification utilizing wet-process phosphoric acid Download PDFInfo
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- CN1907843A CN1907843A CN 200610021637 CN200610021637A CN1907843A CN 1907843 A CN1907843 A CN 1907843A CN 200610021637 CN200610021637 CN 200610021637 CN 200610021637 A CN200610021637 A CN 200610021637A CN 1907843 A CN1907843 A CN 1907843A
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Abstract
A method for stage-by-stage utilization of wet-process phosphoric acid includes: (1) preparing initial-cleaning phosphoric acid by extracting upper clear liquor, (2) using one part of phosphoric acid obtained from step 1 to manufacture inductrial phosphate, (3) using the other part of the initial-cleaning phosphoric acid to prepare industrial cleaning phosphoric acid, (4) preparing ammonium phosphate compound fertilizer by the remnant after extraction. In addition, the industrial cleaning phosphoric acid can be further concentrated to industrial phosphoric acid, and food grade cleaning phosphoric acid can be manufactured from the rest by defluorination, dearsenication, and removal of heavy metals. Said food grade cleaning phosphoric acid is classified into three parts, one used for food grade and medicinal grade phosphoric acid production by concentration, one used for food grade phosphoric acid, and one for electronic grade phosphoric acid. This method can reduce apparatus investment and regulate the type and yield of products according to requirments of market.
Description
Technical field
The invention belongs to wet phosphoric acid purifying and phosphoric acid by wet process Application Areas, particularly a kind of method for preparing technical grade, food grade, electron-level phosphoric acid and compound manure, industrial phosphoric acid salt, phosphoric acid for food salt with phosphoric acid by wet process.
Background technology
" phosphoric acid, phosphate fertilizer and composite fertilizer " (chief editor Jiang Shanxiang, Chemical Industry Press, in March, 1999) introduced the manufacture level phosphoric acid that French Luo Na-Rhone-Poulenc adopted in the book and the solvent extration of food grade phosphoric acid---Central Liqueur flow process (is seen this book P
429～P
430), this flow process is to contain 40～50%P
2O
5Phosphoric acid by wet process be raw material, processing step comprise after clarification, decolouring, extraction, washing, water are stripped, are stripped ester mutually again with the salt solution back extraction, purify ester dearsenification, two and imitate evaporation concentration, defluorinate.
Chinese patent ZL03117850.2 discloses and has a kind ofly prepared the method for PHOSPHORIC ACID TECH.GRADE and food grade phosphoric acid with phosphoric acid by wet process, and the processing step of preparation PHOSPHORIC ACID TECH.GRADE comprises pre-treatment, desulfurization, filtering separation, extraction, dark desulfurization, washing, back extraction successively and concentrates; The method for preparing food grade phosphoric acid, its processing step are to increase dark defluorinate operation on the basis of the processing step of above-mentioned preparation PHOSPHORIC ACID TECH.GRADE, and dark defluorinate operation is placed on after the back extraction operation.
Chinese patent ZL92106621.X discloses a kind of production method of diammonium phosphate, and its processing step is: a, dilute phosphoric acid and gas ammonia carry out neutralization reaction one time, make degree of neutralization reach 1.1～1.2; B, slip concentrate; C, slip and gas ammonia after concentrating carry out the secondary neutralization reaction, make the slip degree of neutralization bring up to 1.5～1.8; D, the slip after the secondary neutralization reaction is delivered to spray granulation drier carry out granulation, drying.
Logical common alkali of phosphatic preparation and phosphoric acid neutralization, reaction post crystallization, the dry the finished product that get.Chinese patent ZL99127183.1 discloses the phosphatic method of a kind of production, this method is raw material with the raw phosphoric acid, extracting-back extraction hockets, what back extraction obtained mutually is phosphate solution, being heated to 80～150 ℃ reclaims wherein dissolved organic phase evaporation, back extraction adds alkali lye or pure phosphoric acid accurate adjustment mutually again, promptly obtains phosphoric acid salt.
Foregoing shows, with regard to prior art, preparing compound manure and technical grade and food grade phosphoric acid, phosphoric acid salt with phosphoric acid by wet process all is to adopt one to overlap independently technical process and produce a kind of product, its weak point is: 1, producing a kind of product then needs a cover complete device, then need many cover complete device if produce multiple product, certainly will increase facility investment like this, take more soils; 2, make enterprise be difficult in time adjust the kind and the output of product according to the needs in market.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, the method that provides a kind of phosphoric acid by wet process classification to utilize adopts this kind method, can reduce facility investment and be convenient in time adjust according to the needs in market the kind of product.
The method that phosphoric acid by wet process classification of the present invention utilizes, its technical scheme is as follows:
(1) supernatant liquid of extracting phosphoric acid by wet process (foreign matter content is low) defluorinate, decolouring, desulfurization extract after handling and filtering, back extraction, are prepared into purifying phosphoric acid just;
(2) part of the first purifying phosphoric acid of step (1) preparation is adopted neutralization reaction, slip concentrate, the technical process manufacture phosphoric acid salt of crystallisation by cooling;
(3) another part of the first purifying phosphoric acid that step (1) is prepared adopts the technical process of washing, back extraction to prepare the technical grade purifying phosphoric acid;
(4) remaining phosphoric acid by wet process and raffinate adopts ammonium phosphate production process to prepare ammonium phosphate compound fertilizer after the extracting.
Except that above-mentioned technology, also can continue classification, a part that is about to prepared technical grade purifying phosphoric acid concentrates manufacture level phosphoric acid, another part defluorinate, dearsenification, the removing heavy-metal of prepared technical grade purifying phosphoric acid is handled obtained the food grade purifying phosphoric acid.
Prepared food grade purifying phosphoric acid is divided into three parts, wherein a part concentrates production food grade, Phosphoric acid (medicine grade), a part adopts that neutralization reaction, slip concentrate, phosphoric acid for food salt is produced in the technical process of crystallisation by cooling, centrifugation, and a part adopts the multistage crystallization method to produce electron-level phosphoric acid.
The processing parameter of first each step of purifying phosphoric acid of preparation is as follows:
(1) defluorinate, decolouring, desulfurization are handled
Defluorinating agent is yellow soda ash and silicon-dioxide or salt of wormwood and silicon-dioxide, extraordinarily go into by 1～1.5 of fluorine content stoichiometric ratio in the phosphoric acid, discoloring agent is that activated carbon is or/and diatomite, add-on is 0.1～1% of a phosphoric acid quality, sweetening agent is a barium carbonate or/and hydrated barta, and the sweetening agent add-on is by SO in the organic phase
4 2-Stoichiometric ratio adds, 60～100 ℃ of temperature of reaction, 3～6 hours reaction times;
(2) filtering separation
Adopt flame filter press to separate the solid impurity of removing in the phosphoric acid;
(3) extraction
The extraction agent that extraction process uses is the mixture of tributyl phosphate, isopropyl ether and kerosene, the volume percent of tributyl phosphate is 60～70%, the volume percent of isopropyl ether is 10～20%, the volume percent of kerosene is 20～40%, the extraction process parameter: organic phase compares 3～6: 1 with water, 50～60 ℃ of temperature, organic phase are external phase;
(4) back extraction
The extraction agent that the back extraction operation is used is soft water, processing parameter: organic phase compares 6～10: 1 with water, and 50～60 ℃ of temperature, organic phase are external phase.
The processing parameter of each step of manufacture phosphoric acid salt is as follows:
According to the phosphatic kind of manufacture, adopt different neutralizing agents and select different processing parameters for use.As the manufacture monoammonium phosphate, then adopt following neutralizing agent and select following processing parameter for use.
(1) neutralization reaction
Add gas ammonia (NH
3) neutralization, the degree of neutralization of slip is controlled at 1～1.05, and water content is controlled at 55～60%;
(2) slip concentrates
The employing multiple-effect concentrates, and the terminal point water content of enriching slurry is controlled at 22～25%;
(3) crystallisation by cooling, centrifugation, drying
The dry gas inlet temperature is 130～135 ℃, and the temperature of exit gas is 60～70 ℃.
The processing parameter of each step of preparation technical grade purifying phosphoric acid is as follows:
Washing is carried out in washing tower, and washings is a purifying phosphoric acid, is added with the NH of phosphoric acid quality 0.5～1% in the washings
4H
2PO
4, processing parameter: organic phase compares 18～20: 1 with washings, and 50～60 ℃ of temperature, organic phase are external phase; The extraction agent that the back extraction operation is used is soft water, processing parameter: organic phase compares 6～10: 1 with water, and 50～60 ℃ of temperature, organic phase are external phase.
Manufacture level phosphoric acid process parameter is as follows:
Adopt and force vacuum concentration equipment to concentrate, vacuum tightness is 80～85kpa.
The processing parameter of preparation food grade purifying phosphoric acid is as follows:
Defluorinating agent is yellow soda ash or salt of wormwood or/and silicon-dioxide, and defluorinating agent is extraordinarily gone into by 1～1.5 of fluorine content stoichiometric ratio in the phosphoric acid, and the removing heavy-metal agent is Na
2S, add-on is generally 1～3 times of theoretical amount, and dearsenic agent is P
2S
5, extraordinarily to go into 1～3 of arsenic content, 60～100 ℃ of temperature of reaction in 3～6 hours reaction times, are got rid of excessive H
2S filters the back and uses.
Production food grade, Phosphoric acid (medicine grade) processing parameter are as follows:
Used thickening equipment is a rotatory evaporator, and vacuum tightness is 88～95kpa, can repeatedly concentrate.
The processing parameter of producing each step of phosphoric acid for food salt is as follows:
Kind according to producing phosphoric acid for food salt adopts different neutralizing agents and selects different processing parameters for use.As produce KH
2PO
4, then adopt following neutralizing agent and select following processing parameter for use.
(1) neutralization reaction
Add chemical pure KOH, the pH value of slip is controlled at 4.2～4.6, and water content is controlled at 50～60%;
(2) slip concentrates
The employing vacuum concentration (vacuum tightness 90～120kpa), the terminal point water content of slip is controlled at 25～30%;
(3) crystallisation by cooling
Cooling temperature is controlled at 10～30 ℃;
(4) centrifugation
Centrifugation is after washing, dry product, and wash water returns the neutralization reaction operation.
The processing parameter of producing each processing step of electron-level phosphoric acid is as follows:
The food grade purifying phosphoric acid is concentrated into mass concentration 90～120%P at 230～440 ℃ of high temperature
2O
5, be cooled to 0～20 ℃ of crystallization then and go out the phosphoric acid crystal, filter the phosphoric acid crystal, with the phosphoric acid crystal heat fused that obtains, adopt above-mentioned processing parameter again high temperature concentrate, crystallisation by cooling, filtration, repeat at least 3 times and can obtain electron-level phosphoric acid.High temperature is concentrated in the graphite concentration kettle and carries out.
The fertilizer grade ammonium phosphate production process has " Phosphoric Acid Concentration method " and " slurry concentrated process ", and ammonium phosphate compound fertilizer has monoammonium phosphate and diammonium phosphate.Both can adopt " Phosphoric Acid Concentration method " and " slurry concentrated process " coproduction monoammonium phosphate and diammonium phosphate (seeing Chinese patent ZL 02113425.1), and can adopt " Phosphoric Acid Concentration method ", " slurry concentrated process " to produce monoammonium phosphate, diammonium phosphate again respectively.
Diammonium phosphate adopts " Phosphoric Acid Concentration method " to produce, processing step be Phosphoric Acid Concentration, in and granulating and drying; Phosphoric Acid Concentration is 25%～28%P with the extraction gained
2O
5Dilute phosphoric acid is concentrated into 46～50%P
2O
5Concentration; In and granulating and drying; slip pre-neutralization degree is controlled at 1.4～1.5, and ammonification is to degree of neutralization 1.8～1.9 in the tablets press, and water content is controlled at 3～4%; the dry gas temperature out is controlled at about 90 ℃, and the water content that goes out the drying machine product is controlled at 1～2% (mass percent).Monoammonium phosphate adopts " in and slurry concentrated process " to produce, and processing step is neutralization reaction (comprising that the washings neutralization directly neutralizes with dilute phosphoric acid), and the multiple-effect slip concentrates, spray-fluidized-bed drying or spray granulating drying; Neutralization reaction, the degree of neutralization of slip is controlled at 1.0～1.05, and water content is controlled at 50～55%; The multiple-effect slip concentrates, and the water content of enriching slurry is controlled at 20～24%; Spray-fluidized-bed drying, drying tower inlet temperature are controlled at 130～135 ℃, 60～70 ℃ of tower exit temperatures; Spray granulating drying, dry gas inlet temperature are controlled at 550～600 ℃, and the dry gas temperature out should be controlled at 100～110 ℃.
The present invention has following beneficial effect:
1, adopts the production of the method for the invention tissue, significantly reduced facility investment.For example, adopting the described method of prior art is the independent manufacture level of raw material phosphoric acid with the phosphoric acid by wet process, 2500 tons/year output, facility investment needs about 5,500,000 yuans, independent manufacture level monoammonium phosphate, 10,000 tons/year output, facility investment needs about 8,000,000 yuans, and facility investment amounts to about 1350 yuans (with present Chinese market calculation of price); And adopt the method for the invention is feedstock production PHOSPHORIC ACID TECH.GRADE and monoammonium phosphate with the phosphoric acid by wet process, the output of PHOSPHORIC ACID TECH.GRADE is 2500 tons/year, the output of industrial grade monoammonium phosphate is 10,000 tons/year, and the total value of facility investment is (with present Chinese market calculation of price) about 9,000,000 yuans only.
2, adopt the method for the invention, a set of equipment can be produced multiple product, is convenient to produce according to the needs tissue in market, in time adjusts the kind and the output of product.
3, the production line of the method for the invention formation is the integral body that organically combines, and the residue that produces in the product preparation of back can return products production operation utilization the preceding in the production line.
4, the method for the invention adopts defluorinate, decolouring, desulfurization, filtration, extraction, stripping process step, can obtain high-quality purifying phosphoric acid just.
5, technical grade, food grade phosphoric acid and the phosphate ratio that adopts the method for the invention to produce has the like product purity raising of chemical method and the production of other method now, and cost reduces.
Description of drawings
Fig. 1 is first kind of process flow sheet of the method for phosphoric acid by wet process classification utilization of the present invention;
Fig. 2 is second kind of process flow sheet of the method for phosphoric acid by wet process classification utilization of the present invention;
Fig. 3 is the third process flow sheet of the method for phosphoric acid by wet process classification utilization of the present invention.
Embodiment
Embodiment 1
In the present embodiment, raw materials used phosphoric acid by wet process composed as follows:
P
2O
5SO
4 2-F Fe As heavy metal (in Pb) colourity
27.80％ 2.19％ 1.68％?0.71％ 0.0014％ 0.0025％ ＞300
The technical process of present embodiment as shown in Figure 1, the production of fertilizer grade monoammonium phosphate and diammonium phosphate, industrial phosphoric acid salt, technical grade purifying phosphoric acid forms organic whole.
Phosphoric acid by wet process is 400,000 tons, and the supernatant liquid defluorinate that 100,000 tons of foreign matter contents of extracting are low, decolouring, desulfurization extract after handling and filtering, back extraction obtains purifying phosphoric acid just.Just purifying phosphoric acid 50% is used to prepare industrial phosphoric acid salt, and first purifying phosphoric acid 50% obtains the technical grade purifying phosphoric acid after washing, back extraction.Remaining 300,000 tons of phosphoric acid by wet processes after the extracting, to wherein 100,000 tons of employings " concentrated phosphoric acid method " production diammonium phosphate, with wherein 200,000 tons be used to wash tail gas that the production diammonium phosphate produced and be raw material with this tail gas washing liquid, adopt " in and slurry concentrated process " to produce monoammonium phosphate.
1, the processing step and the processing parameter of the first purifying phosphoric acid of preparation
Extract after adopting defluorinate, decolouring, desulfurization to handle and filter the phosphoric acid by wet process, back extraction obtains purifying phosphoric acid just.
(1) desulfurization, defluorinate, decolouring are handled
Carry out in treatment trough, defluorinating agent is selected yellow soda ash and silicon-dioxide for use, and yellow soda ash is extraordinarily gone into by 1.0 of fluorine content stoichiometric ratio in the phosphoric acid, and silicon-dioxide is extraordinarily gone into by 0.3 of fluorine content stoichiometric ratio in the phosphoric acid; Discoloring agent is selected gac and diatomite for use, and add-on is respectively 0.2% of phosphoric acid quality, and the sweetening agent barium carbonate is by SO in the organic phase
4 2-Stoichiometric ratio adds, and temperature of reaction is 60 ℃, and the reaction times is 6 hours.
(2) filtering separation
Adopt flame filter press to separate the solid impurity of removing in the phosphoric acid.
(3) extraction
Extraction is carried out in extraction tower, and extraction agent is the mixture of tributyl phosphate, isopropyl ether, kerosene, and the percent by volume of tributyl phosphate is 60%, and the volume percent of isopropyl ether is 10%, and the volume percent of kerosene is 30%.Processing parameter: compare 4: 1 of organic phase and water, 50 ℃ of temperature, organic phase are external phase.
(4) back extraction
Back extraction is carried out in the back extraction tower, and extraction agent is a soft water, compare 6: 1 of organic phase and water, and 60 ℃ of temperature, water is an external phase.
2, phosphatic processing step of manufacture and processing parameter
Manufacture phosphoric acid salt is raw material with first purifying phosphoric acid, and processing step is followed successively by neutralization reaction, concentrated, the crystallisation by cooling of slip.
(1) neutralization reaction
Add gas ammonia (NH
3) neutralization, the degree of neutralization of slip is controlled at 1.05, and water content is controlled at 56%;
(2) slip concentrates
The employing economic benefits and social benefits concentrate, and the terminal point water content of enriching slurry is controlled at 25%;
(3) crystallisation by cooling, centrifugation, drying
The dry gas inlet temperature is 135 ℃, and the temperature of exit gas is 65 ℃.
The industrial phosphoric acid salt NH that is produced
4H
2PO
4, relevant components contents is as follows:
NH
4H
2PO
4Moisture F Fe As heavy metal (in Pb) water-insoluble
99～99.5％ ＜0.3％ 0.02％ ≤0.003％ ≤0.0015％ ≤0.0010％ ≤0.1％
3, the processing step and the processing parameter of preparation technical grade purifying phosphoric acid
Adopt the technical process of washing, back extraction to obtain the technical grade purifying phosphoric acid first purifying phosphoric acid.
(1) washing
Washing is carried out in washing tower, and washings is a purifying phosphoric acid, is added with phosphoric acid quality 0.6%NH in the washings
4H
2PO
4, compare 20: 1 of organic phase and washings, 50 ℃ of temperature, organic phase are external phase;
(2) back extraction
Back extraction is carried out in the back extraction tower, and extraction agent is a soft water, compare 6: 1 of organic phase and water, and 60 ℃ of temperature, organic phase are external phase, the gained purifying phosphoric acid is the technical grade purifying phosphoric acid.
4, prepare ammonium phosphate compound fertilizer with phosphoric acid by wet process remaining after the extracting
(1) processing step and the processing parameter of employing " concentrated phosphoric acid method " production diammonium phosphate
The processing step of production diammonium phosphate comprise successively Phosphoric Acid Concentration, in and granulating and drying; Phosphoric Acid Concentration is with 27.80%P
2O
5Dilute phosphoric acid be concentrated into 42%P
2O
5Concentrated phosphoric acid; In and the processing parameter of granulating and drying be: ammonification goes out tablets press water content 3% to degree of neutralization 1.8 in the slip pre-neutralization degree 1.45, tablets press, 90 ℃ of dry gas temperature outs, the water content that goes out the drying machine product is controlled at 1.5%.The granular diammonium phosphate product of being produced: N18%, effectively P
2O
546%, H
2O 1.5%.
(2) adopt " in and slurry concentrated process " to produce the processing step and the processing parameter of powdery monoammonium phosphate
The processing step of producing powdery monoammonium phosphate comprises that successively washings neutralization, two effect slips concentrate, spray-fluidized-bed drying; The washings neutralization, the slip degree of neutralization is controlled at 1.03, and water content is controlled at 52%, and the equipment of employing is pump circulation ammonification evaporation reaction device; Two imitate the concentrated solvent or diluent slurry with moisture 44% of slip is concentrated into moisture 22% enriching slurry; Spray-fluidized-bed drying is finished in spray-drying tower, 130 ℃ of air inlet temperature of stabilizer, 60 ℃ of tower exit temperatures.The powdery monoammonium phosphate product of being produced: N 11%, effectively P
2O
552%, H
2O 1.5%.
Embodiment 2
As shown in Figure 2, on the basis of embodiment 1, continue classification, 50% of the technical grade purifying phosphoric acid that embodiment 1 is prepared concentrates manufacture level phosphoric acid, and 50% remaining technical grade purifying phosphoric acid carries out defluorinate, dearsenification, removing heavy-metal to be handled and obtain the food grade purifying phosphoric acid.
1, the processing parameter of manufacture level phosphoric acid
The technical grade purifying phosphoric acid concentrated be PHOSPHORIC ACID TECH.GRADE.Concentrate to adopt and force vacuum concentration equipment, vacuum tightness is 80kpa, and the relevant components contents of institute's PHOSPHORIC ACID TECH.GRADE that obtains is as follows:
P
2O
5SO
4 2-F Fe As heavy metal (in Pb) colourity
61.50％ 0.0010％ 0.02％ 0.0020％ 0.0004％ 0.0006％ ＜20
2, the processing parameter of preparation food grade purifying phosphoric acid
The technical grade purifying phosphoric acid is carried out dark defluorinate, dearsenification, removing heavy-metal handle and promptly obtain the food grade purifying phosphoric acid, dearsenification, defluorinate, removing heavy-metal carry out in reactive tank, and dearsenic agent is P
2S
5, extraordinarily to go into 2 of arsenic content, the removing heavy-metal agent is Na
2S, add-on is 1.5 times of theoretical amount, defluorinating agent is selected salt of wormwood and silicon-dioxide for use, salt of wormwood is extraordinarily gone into by 1.2 of fluorine content stoichiometric ratio in the phosphoric acid, silicon-dioxide is extraordinarily gone into by 0.3 of fluorine content stoichiometric ratio in the phosphoric acid, and temperature of reaction is 90 ℃, and the reaction times is 3 hours.
Embodiment 3
As shown in Figure 3, on the basis of embodiment 2, continue classification, 50% of the food grade purifying phosphoric acid of embodiment 2 preparation is used to prepare food grade, Phosphoric acid (medicine grade), and 40% of food grade purifying phosphoric acid is used to prepare phosphoric acid for food salt, and food grade purifying phosphoric acid 10% is used to prepare electron-level phosphoric acid.
1, produces the processing parameter of food grade phosphoric acid, Phosphoric acid (medicine grade)
The food grade purifying phosphoric acid concentrated be food grade phosphoric acid.Be concentrated under the vacuum condition and carry out, vacuum tightness is 93kpa, and equipment used is a rotatory evaporator.Prepared food grade phosphoric acid, relevant components contents is as follows:
P
2O
5SO
4 2-F Fe As heavy metal (in Pb) colourity
61.50％ 0.0010％ 0.001％ 0.0020％ 0.0001％ 0.0001％ ＜20
Above-mentioned food grade phosphoric acid also can be used as Phosphoric acid (medicine grade) and uses.
2, produce the processing step and the processing parameter of phosphoric acid for food salt
With the food grade purifying phosphoric acid adopt that neutralization reaction, slip concentrate, the technical process of crystallisation by cooling, centrifugation obtains phosphoric acid for food salt.
(1) neutralization reaction
Add chemical pure KOH, the pH value of slip is controlled at 4.4, and water content is controlled at 55%;
(2) slip concentrates
Adopt vacuum concentration (vacuum tightness is 95kpa), the terminal point water content of enriching slurry is controlled at 26%;
(3) crystallisation by cooling
Cooling temperature is controlled at 30 ℃;
(4) centrifugation
Centrifugation is after washing, dry product, and wash water returns the neutralization reaction operation.
Prepared phosphoric acid for food salt KH
2PO
4, relevant components contents is as follows:
KH
2PO
4SO
4 2-F Fe As heavy metal (in Pb)
99.20％ 0.0010％ 0.001％ 0.0020％ 0.0001％ 0.0001％
3, produce the processing step and the processing parameter of electron-level phosphoric acid
Adopt the level Four crystallization process to produce electron-level phosphoric acid, the food grade purifying phosphoric acid is concentrated into 98%P at 340 ℃ of high temperature
2O
5, be cooled to 8 ℃ of crystallizations then and go out the phosphoric acid crystal, filter the phosphoric acid crystal, with the phosphoric acid crystal heat fused that obtains, adopt above-mentioned processing parameter again high temperature concentrate, crystallisation by cooling, filtration, repeat 4 times and can obtain electron-level phosphoric acid.High temperature is concentrated in the graphite concentration kettle and carries out.
Prepared electron-level phosphoric acid, F, SO
4With the content of metal ion below 1ppm.
Preparation just purifying phosphoric acid, technical grade purifying phosphoric acid, food grade purifies the residue that phosphorus produces, and is used to produce the fertilizer grade monoammonium phosphate.
The invention is not restricted to the foregoing description, the turnout of various products can be according to the market demand adjustment.
Claims (4)
1, a kind of method of phosphoric acid by wet process classification utilization is characterized in that:
(1) the supernatant liquid defluorinate of extracting phosphoric acid by wet process, decolouring, desulfurization extract after handling and filtering, back extraction is prepared into purifying phosphoric acid just,
(2) part of the first purifying phosphoric acid of step (1) preparation is adopted neutralization reaction, slip concentrate, the technical process manufacture phosphoric acid salt of crystallisation by cooling,
(3) another part of the first purifying phosphoric acid that step (1) is prepared adopts the technical process of washing, back extraction to prepare the technical grade purifying phosphoric acid,
(4) remaining phosphoric acid by wet process and raffinate adopts ammonium phosphate production process to prepare ammonium phosphate compound fertilizer after the extracting.
2, the method for phosphoric acid by wet process classification utilization according to claim 1, it is characterized in that the part of prepared technical grade purifying phosphoric acid is concentrated manufacture level phosphoric acid, another part defluorinate, dearsenification, the removing heavy-metal of prepared technical grade purifying phosphoric acid are handled obtained the food grade purifying phosphoric acid.
3, the method for phosphoric acid by wet process classification utilization according to claim 2, it is characterized in that prepared food grade purifying phosphoric acid is divided into three parts, wherein a part concentrates production food grade, Phosphoric acid (medicine grade), a part adopts that neutralization reaction, slip concentrate, phosphoric acid for food salt is produced in the technical process of crystallisation by cooling, centrifugation, and a part adopts the multistage crystallization method to produce electron-level phosphoric acid.
4, the method for phosphoric acid by wet process classification utilization according to claim 3, it is characterized in that adopting the multistage crystallization method to produce electron-level phosphoric acid is that the food grade purifying phosphoric acid is concentrated into mass concentration 90～120%P at 230～440 ℃ of high temperature
2O
5, be cooled to 0～20 ℃ of crystallization then and go out the phosphoric acid crystal, filter the phosphoric acid crystal, with the phosphoric acid crystal heat fused that obtains, adopt above-mentioned processing parameter again high temperature concentrate, crystallisation by cooling, filtration, repeat at least 3 times and can obtain electron-level phosphoric acid.
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| CN101857213A (en) * | 2010-06-04 | 2010-10-13 | 广西明利集团有限公司 | Method for preparing food-grade diammonium phosphate from wet-process phosphoric acid |
| CN102583284A (en) * | 2012-02-09 | 2012-07-18 | 昆明川金诺化工股份有限公司 | Method for removing slag before solvent extraction in process of producing industrial-grade phosphoric acid by wet-process phosphoric acid |
| CN102583285A (en) * | 2012-02-28 | 2012-07-18 | 瓮福（集团）有限责任公司 | Method for preparing high-concentration phosphoric acid from fertilizer-grade phosphoric acid |
| CN104072208A (en) * | 2014-07-16 | 2014-10-01 | 云南常青树化工有限公司 | Preparation method for water soluble fertilizer |
| CN105366655A (en) * | 2015-12-10 | 2016-03-02 | 四川蓝海化工（集团）有限公司 | Preparation method of capacitor grade phosphoric acid crystals |
| CN113772646A (en) * | 2021-09-30 | 2021-12-10 | 武汉工程大学 | Wet-process phosphoric acid two-stage membrane deep purification process |
| CN118206087A (en) * | 2024-04-03 | 2024-06-18 | 新洋丰农业科技股份有限公司 | Method for preparing fertilizer grade and battery grade monoammonium phosphate by using wet-process phosphoric acid |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042216C (en) * | 1992-07-17 | 1999-02-24 | 莱西市磷肥厂 | Enriching slurry process for production of diammonium phosphate |
| CN1094111C (en) * | 1999-12-30 | 2002-11-13 | 清华大学 | Alternate extraction-counter extraction process of producing phosphate |
| CN1204044C (en) * | 2003-05-12 | 2005-06-01 | 四川大学 | Method for preparing industrial grade and food grade phosphoric acid by wet method phosphoric acid |
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| CN101857213A (en) * | 2010-06-04 | 2010-10-13 | 广西明利集团有限公司 | Method for preparing food-grade diammonium phosphate from wet-process phosphoric acid |
| CN101857213B (en) * | 2010-06-04 | 2013-02-20 | 广西钦州桂金诺磷化工有限公司 | Method for preparing food-grade diammonium phosphate from wet-process phosphoric acid |
| CN102583284A (en) * | 2012-02-09 | 2012-07-18 | 昆明川金诺化工股份有限公司 | Method for removing slag before solvent extraction in process of producing industrial-grade phosphoric acid by wet-process phosphoric acid |
| CN102583285A (en) * | 2012-02-28 | 2012-07-18 | 瓮福（集团）有限责任公司 | Method for preparing high-concentration phosphoric acid from fertilizer-grade phosphoric acid |
| CN102583285B (en) * | 2012-02-28 | 2013-11-13 | 瓮福（集团）有限责任公司 | Method for preparing high-concentration phosphoric acid from fertilizer-grade phosphoric acid |
| CN104072208A (en) * | 2014-07-16 | 2014-10-01 | 云南常青树化工有限公司 | Preparation method for water soluble fertilizer |
| CN105366655A (en) * | 2015-12-10 | 2016-03-02 | 四川蓝海化工（集团）有限公司 | Preparation method of capacitor grade phosphoric acid crystals |
| CN113772646A (en) * | 2021-09-30 | 2021-12-10 | 武汉工程大学 | Wet-process phosphoric acid two-stage membrane deep purification process |
| CN113772646B (en) * | 2021-09-30 | 2024-05-07 | 武汉工程大学 | Wet-process phosphoric acid two-stage membrane deep purification process |
| CN118206087A (en) * | 2024-04-03 | 2024-06-18 | 新洋丰农业科技股份有限公司 | Method for preparing fertilizer grade and battery grade monoammonium phosphate by using wet-process phosphoric acid |
| CN118206087B (en) * | 2024-04-03 | 2024-09-20 | 新洋丰农业科技股份有限公司 | Method for preparing fertilizer grade and battery grade monoammonium phosphate by using wet-process phosphoric acid |
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