CN109650362A - With the method for centrifugal extractor purification of wet process phosphoric acid - Google Patents
With the method for centrifugal extractor purification of wet process phosphoric acid Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- 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
- C01B25/18—Phosphoric acid
- C01B25/234—Purification; Stabilisation; Concentration
- C01B25/237—Selective elimination of impurities
- C01B25/2372—Anionic impurities, e.g. silica or boron compounds
- C01B25/2375—Fluoride or fluosilicate anion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0476—Moving receptacles, e.g. rotating receptacles
- B01D11/048—Mixing by counter-current streams provoked by centrifugal force, in rotating coils or in other rotating spaces
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- C—CHEMISTRY; METALLURGY
- 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
- C01B25/18—Phosphoric acid
- C01B25/234—Purification; Stabilisation; Concentration
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- C—CHEMISTRY; METALLURGY
- 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
- C01B25/18—Phosphoric acid
- C01B25/234—Purification; Stabilisation; Concentration
- C01B25/237—Selective elimination of impurities
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- C—CHEMISTRY; METALLURGY
- 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
- C01B25/46—Preparation involving solvent-solvent extraction
- C01B25/461—Preparation involving solvent-solvent extraction the phosphoric acid present in the medium obtained after reaction being first extracted from the liquid phase formed or separated then re-extracted as free acid by using water or as a phosphate by using a basic compound
- C01B25/465—Preparation involving solvent-solvent extraction the phosphoric acid present in the medium obtained after reaction being first extracted from the liquid phase formed or separated then re-extracted as free acid by using water or as a phosphate by using a basic compound the extracting agent being an ester or a mixture of esters
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Abstract
Disclosed by the invention is a kind of method with centrifugal extractor purification of wet process phosphoric acid of chemical production technical field, main includes pretreatment, extraction, washing, back extraction, desulfurization and concentration several stages, wherein main improvement is to use centrifugal extractor in extraction, washing and back extraction three phases.Using centrifugal extractor as extraction equipment, low, P is required to raw material phosphoric acid concentration2O5Content only needs 30~40%, and common half water phosphoric acid by wet process, which only makees simple process, to be met the requirements, no additional energy, and the prior art requires phosphoric acid concentration that must control 40~58%；Extraction section temperature does not need additionally to control, normal-temperature reaction, is that can reach 75% or more extraction yield, and compare rotating disc column and have to reach 6~8:1 compared to 4:1；Using centrifugal extractor, it is sufficiently mixed two-phase under high-speed condition, extraction efficiency is high, and split-phase effect is good, compared with rotating disc column etc., is able to achieve quick split-phase and without entrainment.
Description
Technical field
The present invention relates to chemical production technical fields more particularly to a kind of purification of wet process phosphoric acid to produce technical grade, food-grade
The method of phosphoric acid.
Background technique
Wet phosphoric acid purifying solvent extraction process is the process of a liquid-liquid two-phase mass transfer, and extraction equipment will reach high
Separating effect and intensity, the raising dependent on mass transfer rate.And the approach of mass transfer rate is improved nothing more than will disperse sufficiently to increase
Big two-phase contact interface；Increase two-phase lubrication degree to improve mass tranfer coefficient；It takes reflux type to contact and reduces back-mixing to increase
Big mass transfer force.
The extraction equipment applied in industry at present is relatively more, can be classified as two class of fractional extraction and differential extraction.Mixing clarification
Device and sieve-plate tower belong to fractional extraction, and packed tower, rotating disc column and pulse extraction column belong to differential extraction.But not in industrialization
It is ideal.
1, mixer-settler extractor
This equipment is the equipment and most common for phosphoric acid by wet process extraction earliest, by mixed zone and Disengagement zone two
Part forms.The operating reliability of this equipment is strong, and the flow-rate ratio of two-phase can be in a wide range of interior variation, the mixing and separation of two-phase
Very sufficiently, every grade of efficiency is very high, is close to theoretical stage sometimes.The disadvantage is that investment and running expense are high.
2, sieve-plate tower
Light phase goes out from tower top, and heavy phase goes out from tower bottom；Organic solvent from tower lower bottom into, phosphoric acid by wet process from tower top into.Sieve
Sieve plate effect in plate tower strengthens mass transfer, second is that having understood difference substantially first is that dispersed phase is made to be subjected to dispersion repeatedly and collecting and distributing
The back-mixing of plate interlayer liquid, improves mass transfer force.
Sieve-plate tower, which is applied to the lower system of interfacial tension, can achieve higher efficiency, but lower for interfacial tension
System, it is difficult to realize effective dispersion.
3, rotating disc column
Rotating disc column is a kind of extraction tower with external energy, and turntable is driven by external motor.Light phase goes out from tower top, heavy phase
Go out from tower bottom；Organic solvent from tower lower bottom into, phosphoric acid by wet process from tower top into.
Rotating disc column efficiency with higher is able to satisfy the requirement of mass production ability, and ability consumption is low, compares in industrial application
Extensively, it is applied in phosphoric acid by wet process extracting and purifying technique on a large scale in recent years.The disadvantage is that low separation efficiency, is easy to appear folder
Band；
4, pulse-column
Pulse-column is a kind of input external enwergy, promotes the extraction tower of liquid-liquid system dispersion.The external energy of input promotes in tower
Medium pulsing movement, enhance dispersant liquid drop in disturbance and phase interface rapid liquidity, with improve interphase mass transfer speed
Rate.
Mechanical stirring or back and forth movement structural member, impulse movement not be arranged specially for having the prominent advantages that for pulse-column in tower
Dynamic source may be provided at outside tower, avoid corroding.The processing capacity of this tower is not high, and the power of consumption is big, and axial backmixing is also than nothing
It increased when pulse.
Summary of the invention
To overcome existing extraction equipment above shortcomings in purification of wet process phosphoric acid, technology to be solved by this invention
Problem is: provide it is a kind of using centrifugal extractor come the method for purification of wet process phosphoric acid.
The technical solution adopted by the present invention to solve the technical problems is:
With the method for centrifugal extractor purification of wet process phosphoric acid, comprising the following steps:
A, it pre-processes: defluorinating agent being added into Wet Phosphoric Acid Market and carries out defluorinate, add active carbon decoloring, filtering is backward
Hydrogen peroxide is added in filtrate to decolourize, obtains pretreatment phosphoric acid；
B, extract: will pretreatment phosphoric acid from heavy phase import enter the first centrifugal extractor, by extractant from light phase import into
Enter the first centrifugal extractor and carries out counter-current extraction；
C, it washs: the organic phase obtained after step b extraction being entered into the second centrifugal extractor from light phase import, by phosphoric acid,diluted
Enter the second centrifugal extractor from heavy phase import to be washed；
D, it is stripped: the organic phase after step c washing being entered into third centrifugal extractor from light phase import, by pure water from heavy phase
Import enters third centrifugal extractor and is stripped；
E, desulfurization: back extraction gained phosphoric acid is entered into desulphurization plant, is reacted with it and is filtered with desulfurizing agent, filter residue is sulfuric acid
Salt, filtrate are phosphoric acid；
F, it is concentrated: the phosphoric acid after desulfurization is pumped into concentrator by clear liquid, form concentration under vacuum heating conditions
Purifying phosphoric acid.
Further, the concentration for the pretreatment phosphoric acid being added in step b is 30~40%, phosphoric acid and extractant are pre-processed
Volume ratio be 1:4~6, extraction temperature be 20~50 DEG C.
Further, extractant in step b be one of tributyl phosphate or butylphosphoric acid ester with diluent kerosene,
The mixture of one of MIBK, n-butanol or diisopropyl ether.
Further, 15~30:1 of phase volume ratio of organic phase and phosphoric acid,diluted, wash temperature is 40~65 in step c
℃。
Further, 5~8:1 of phase volume ratio of organic phase and pure water, back extraction temperature is 40~65 DEG C in step d.
Further, first centrifugal extractor, the second centrifugal extractor and third centrifugal extractor are three
And the above concatenated three-level extraction mechanism of centrifugal extractor, the revolving speed of centrifugal extractors at different levels are not less than 3000r/min.
Further, further include Matter Transfer technique, the washing acid generated after being washed in step c with it is pre- in step b
It is extracted after processing phosphoric acid mixing；Resulting phosphoric acid is stripped in step d takes a portion to be used as the phosphoric acid,diluted in step c；
Resulting solvent is stripped in step d as the extractant in step b.
Further, further include recycle heat technique, step d is stripped resulting high-temperature solvent and is generating with step b
Containing extractant is used as after sour solvent heat exchange, containing after heat exchange enters step c after sour solvent is heated by steam and being washed.
The beneficial effects of the present invention are:
1, using centrifugal extractor as extraction equipment, low, P is required to raw material phosphoric acid concentration2O5Content only needs 30~
40%, common half water phosphoric acid by wet process, which only makees simple process, to be met the requirements, no additional energy, and the prior art requires phosphoric acid dense
Degree must be controlled 40~58%；
2, extraction section temperature does not need additionally to control, normal-temperature reaction, is the extraction yield that can reach 75% or more compared to 4:1,
And it compares rotating disc column and has to reach 6~8:1；
3, using centrifugal extractor, it is sufficiently mixed two-phase under high-speed condition, extraction efficiency is high, and split-phase effect is good, with
Rotating disc column etc. is compared, and is able to achieve quick split-phase and without entrainment.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.
The method of present invention centrifugal extractor purification of wet process phosphoric acid, comprising the following steps:
A, it pre-processes: defluorinating agent being added into Wet Phosphoric Acid Market and carries out defluorinate, add active carbon decoloring, filtering is backward
Hydrogen peroxide is added in filtrate to decolourize, obtains pretreatment phosphoric acid；
B, extract: will pretreatment phosphoric acid from heavy phase import enter the first centrifugal extractor, by extractant from light phase import into
Enter the first centrifugal extractor to be extracted, one of tributyl phosphate or butylphosphoric acid ester and diluent can be used in the extractant
The mixture of one of kerosene, MIBK, n-butanol or diisopropyl ether；
C, it washs: the organic phase obtained after step b extraction being entered into the second centrifugal extractor from light phase import, by phosphoric acid,diluted
Enter the second centrifugal extractor from heavy phase import and carries out countercurrent washing；
D, it is stripped: the organic phase after step c washing being entered into third centrifugal extractor from light phase import, by pure water from heavy phase
Import enters third centrifugal extractor and is stripped；
E, desulfurization: back extraction gained phosphoric acid is entered into desulphurization plant, is reacted with it and is filtered with desulfurizing agent, filter residue is sulfuric acid
Salt, filtrate are phosphoric acid；
F, it is concentrated: the phosphoric acid after desulfurization is pumped into concentrator by clear liquid, form concentration under vacuum heating conditions
Purifying phosphoric acid.
Wherein, specific process parameter control requirement are as follows:
The concentration for the pretreatment phosphoric acid being added in step b is 30~40%, and the volume ratio for pre-processing phosphoric acid and extractant is
1:4~6, extraction temperature are 20~50 DEG C；
In step c, 15~30:1 of phase volume ratio of organic phase and phosphoric acid,diluted, wash temperature is 40~65 DEG C；
In step d, 5~8:1 of phase volume ratio of organic phase and pure water, back extraction temperature is 40~65 DEG C.
Compared to the rotating disc column in traditional handicraft, lower, P is required to raw material phosphoric acid concentration using centrifugal extractor2O5Content
30~40% are only needed, and rotating disc column requires phosphoric acid concentration that must control 40~58%, since concentration requirement is low, to common half water
Phosphoric acid by wet process, which only makees simple process, to be met the requirements, no additional energy.Phase since centrifugal extractor revolving speed is higher, when extraction
Also lower, the volume ratio 4:1 than requiring, and rotating disc column needs 6~8:1.In washing and strip stages, it equally should be high speed and revolve
The centrifugal extractor turned can be such that two-phase is sufficiently mixed, and extraction efficiency is high, and split-phase effect is good, therefore required compared to also relatively
It is low.
Centrifugal extractor is taken up a large area since common extraction equipment extraction efficiency is low, and centrifugal extractor ruler
Very little small, separate unit Centrifugical extraction is high-efficient, thus the application use the first centrifugal extractor, the second centrifugal extractor and third from
Heart extracter is the concatenated three-level extraction mechanism of three centrifugal extractors, just can increase extraction road using three-level counter-current extraction
Diameter reduces extraction time, to improve effect of extracting.If desired centrifugal extractor number can then be increased by further increasing extraction yield
Amount makes organic phase and the water phase realize mixing, split-phase to provide enough centrifugal force, and the revolving speed of centrifugal extractors at different levels should not
Lower than 3000r/min.
In entire production process, for energy-saving and emission-reduction, material utilization rate is improved, is provided with Matter Transfer technique and heat
Circulation technology.Entire technical process is as shown in Figure 1, wherein Matter Transfer technique includes: the washing generated after washing in step c
Acid is extracted after mixing with the pretreatment phosphoric acid in step b；Resulting phosphoric acid is stripped in step d takes a portion to be used as step
Phosphoric acid,diluted in rapid c；Resulting solvent is stripped in step d as the extractant in step b.Recycle heat technique includes: by step
Rapid d is stripped resulting high-temperature solvent and contains after sour solvent exchanges heat with what step b was generated as extractant, contains sour solvent after heat exchange
C is entered step after heating by steam to be washed.
Below by specific embodiment, the invention will be further described.
Embodiment one:
Sour index is pre-processed to be as follows:
| Material name | P2O5% | CaO% | MgO% | Fe2O3% | Al2O3% | F% | SO42-% | Specific gravity |
| Pretreatment acid | 39.02 | 0.074 | 1.76 | 0.32 | 0.2 | 0.083 | 3.62 | 1.47 |
1, it extracts: preparing the mixed solvent containing tributyl phosphate and kerosene, specific gravity 0.93, centrifugal extractor revolving speed is extremely
After 3000r/min, pretreatment acid is sent into the first order through metering pump with 555ml/min and extracts centrifuge heavy liquid inlet, mixed solvent
The third level is sent into 2220ml/min with metering pump and extracts centrifuge light phase inlet, carries out three-level counter-current extraction, extraction phase is than 4:
1, temperature is 20 DEG C -25 DEG C, and raffinate is discharged by third level heavy out；It is light by first order extraction centrifuge containing sour solvent
It is mutually exchanged heat after outlet discharge by heat exchanger and circulation solvent, then enters washing section after heating by steam；
2, wash: after centrifugal extractor revolving speed to 3000r/min, gained diluted acid enters the extraction of the washing section first order after back extraction
Centrifuge heavy liquid inlet enters third level extraction centrifuge light phase inlet containing sour solvent after extraction section heating, carries out three
20:1 is compared in stage countercurrent washing, washing, and temperature is 40-45 DEG C, and washing acid is discharged by third level heavy out and pre-processes acid
Mixing；Being discharged containing sour solvent from first order extraction centrifuge light phase export after washing, into stripping section；
3, be stripped: after centrifugal extractor revolving speed to 3000r/min, pure water enters stripping section first order extraction centrifuge heavy phase
Entrance enters third level extraction centrifuge light phase inlet containing sour solvent from washing section, carries out three-level countercurrent reextraction, be stripped phase
Than 5:1, temperature is 40-45 DEG C, is collected after diluted acid is discharged by third level heavy out after back extraction at rear end defluorinate, concentration
Reason；Solvent after back extraction is from first order extraction centrifuge light phase export discharge, and into first-class heat exchanger and after extracting, solvent exchanges heat
Enter extraction section afterwards to be recycled.
Runing time 24 hours, consumption pretreatment acid 1174.82kg, output raffinate 470.13kg converted extraction yield
77.92%, table specific as follows:
Gained phosphoric acid,diluted index is as follows:
| P2O5% | Ca% | Fe% | Mg% | F% | SO4 2-% | As% | Coloration | Specific gravity |
| 22.03 | It is not detected | 0.0004 | It is not detected | 0.007 | 0.24 | 0.0002 | Less than 20 | 1.19 |
Embodiment two:
Sour index is pre-processed to be as follows:
| Material name | P2O5% | CaO% | MgO% | Fe2O3% | Al2O3% | F% | SO42-% | Specific gravity |
| Pretreatment acid | 39.02 | 0.074 | 1.76 | 0.32 | 0.2 | 0.083 | 3.62 | 1.47 |
1, it extracts: preparing the mixed solvent containing tributyl phosphate and kerosene, specific gravity 0.93, centrifugal extractor revolving speed is extremely
After 3000r/min, pretreatment acid is sent into the first order through metering pump with 555ml/min and extracts centrifuge heavy liquid inlet, mixed solvent
The third level is sent into 2220ml/min with metering pump and extracts centrifuge light phase inlet, carries out three-level counter-current extraction, extraction phase is than 4:
1, temperature is 35 DEG C -40 DEG C, and raffinate is discharged by third level heavy out；It is light by first order extraction centrifuge containing sour solvent
It is mutually exchanged heat after outlet discharge by heat exchanger and circulation solvent, then enters washing section after heating by steam；
2, wash: after centrifugal extractor revolving speed to 3000r/min, gained diluted acid enters the extraction of the washing section first order after back extraction
Centrifuge heavy liquid inlet enters third level extraction centrifuge light phase inlet containing sour solvent after extraction section heating, carries out three
25:1 is compared in stage countercurrent washing, washing, and temperature is 60-65 DEG C, and washing acid is discharged by third level heavy out and pre-processes acid
Mixing；Being discharged containing sour solvent from first order extraction centrifuge light phase export after washing, into stripping section；
3, be stripped: after centrifugal extractor revolving speed to 3000r/min, pure water enters stripping section first order extraction centrifuge heavy phase
Entrance enters third level extraction centrifuge light phase inlet containing sour solvent from washing section, carries out three-level countercurrent reextraction, be stripped phase
Than 5:1, temperature is 60-65 DEG C, is collected after diluted acid is discharged by third level heavy out after back extraction at rear end defluorinate, concentration
Reason；Solvent after back extraction is from first order extraction centrifuge light phase export discharge, and into first-class heat exchanger and after extracting, solvent exchanges heat
Enter extraction section afterwards to be recycled.
Runing time 24 hours, consumption pretreatment acid 1174.82kg, output raffinate 503.19kg converted extraction yield
75.5%, table specific as follows:
| Consumption decoloration acid kg | Consumption decoloration acid P2O5% | Raffinate quality kg | Raffinate P2O5% | Extraction yield % |
| 1174.82 | 39.02 | 503.19 | 22.32 | 75.5 |
Gained phosphoric acid,diluted index is as follows:
| P2O5% | Ca% | Fe% | Mg% | F% | SO4 2-% | As% | Coloration | Specific gravity |
| 23.23 | It is not detected | 0.0006 | It is not detected | 0.01 | 0.58 | 0.0005 | Less than 20 | 1.20 |
Embodiment two:
Sour index is pre-processed to be as follows:
| Material name | P2O5% | CaO% | MgO% | Fe2O3% | Al2O3% | F% | SO42-% | Specific gravity |
| Pretreatment acid | 39.02 | 0.074 | 1.76 | 0.32 | 0.2 | 0.083 | 3.62 | 1.47 |
1, it extracts: preparing the mixed solvent containing tributyl phosphate and kerosene, specific gravity 0.93, centrifugal extractor revolving speed is extremely
After 3000r/min, pretreatment acid is sent into the first order through metering pump with 370ml/min and extracts centrifuge heavy liquid inlet, mixed solvent
The third level is sent into 2220ml/min with metering pump and extracts centrifuge light phase inlet, carries out three-level counter-current extraction, extraction phase is than 6:
1, temperature is 45 DEG C -50 DEG C, and raffinate is discharged by third level heavy out；It is light by first order extraction centrifuge containing sour solvent
It is mutually exchanged heat after outlet discharge by heat exchanger and circulation solvent, then enters washing section after heating by steam；
2, wash: after centrifugal extractor revolving speed to 3000r/min, gained diluted acid enters the extraction of the washing section first order after back extraction
Centrifuge heavy liquid inlet enters third level extraction centrifuge light phase inlet containing sour solvent after extraction section heating, carries out three
15:1 is compared in stage countercurrent washing, washing, and temperature is 60-65 DEG C, and washing acid is discharged by third level heavy out and pre-processes acid
Mixing；Being discharged containing sour solvent from first order extraction centrifuge light phase export after washing, into stripping section；
3, be stripped: after centrifugal extractor revolving speed to 3000r/min, pure water enters stripping section first order extraction centrifuge heavy phase
Entrance enters third level extraction centrifuge light phase inlet containing sour solvent from washing section, carries out three-level countercurrent reextraction, be stripped phase
Than 8:1, temperature is 60-65 DEG C, is collected after diluted acid is discharged by third level heavy out after back extraction at rear end defluorinate, concentration
Reason；Solvent after back extraction is from first order extraction centrifuge light phase export discharge, and into first-class heat exchanger and after extracting, solvent exchanges heat
Enter extraction section afterwards to be recycled.
Runing time 24 hours, consumption pretreatment acid 783.22kg, output raffinate 285.83kg converted extraction yield
79.63%, table specific as follows.
| Consumption decoloration acid kg | Consumption decoloration acid P2O5% | Raffinate quality kg | Raffinate P2O5% | Extraction yield % |
| 783.22 | 39.02 | 285.83 | 21.78 | 79.63 |
Gained phosphoric acid,diluted index is as follows:
| P2O5% | Ca% | Fe% | Mg% | F% | SO4 2-% | As% | Coloration | Specific gravity |
| 19.95 | It is not detected | 0.0002 | It is not detected | 0.006 | 0.18 | 0.0003 | Less than 20 | 1.18 |
In conclusion can guarantee higher extraction yield using this technique, and split-phase effect is good, with the phases such as rotating disc column
Than being able to achieve quick split-phase and without entrainment, there is good practicability and application prospect.
Claims (8)
1. with the method for centrifugal extractor purification of wet process phosphoric acid, characterized in that the following steps are included:
A, it pre-processes: defluorinating agent being added into Wet Phosphoric Acid Market and carries out defluorinate, active carbon decoloring is added, to filtrate after filtering
Middle addition hydrogen peroxide decolourizes, and obtains pretreatment phosphoric acid；
B, it extracts: pretreatment phosphoric acid from heavy phase import being entered into the first centrifugal extractor, extractant is entered the from light phase import
One centrifugal extractor carries out counter-current extraction；
C, it washs: the organic phase obtained after step b extraction being entered into the second centrifugal extractor from light phase import, by phosphoric acid,diluted from again
Phase import enters the second centrifugal extractor and is washed；
D, it is stripped: the organic phase after step c washing being entered into third centrifugal extractor from light phase import, by pure water from heavy phase import
It is stripped into third centrifugal extractor；
E, desulfurization: back extraction gained phosphoric acid is entered into desulphurization plant, is reacted with it and is filtered with desulfurizing agent, filter residue is sulfate, filter
Liquid is phosphoric acid；
F, it is concentrated: the phosphoric acid after desulfurization being pumped into concentrator by clear liquid, forms the net of concentration under vacuum heating conditions
Change phosphoric acid.
2. the method for using centrifugal extractor purification of wet process phosphoric acid as described in claim 1, it is characterized in that: being added in step b
The concentration for pre-processing phosphoric acid is 30~40%, and the volume ratio for pre-processing phosphoric acid and extractant is 1:4~6, extraction temperature is 20~
50℃。
3. the method for using centrifugal extractor purification of wet process phosphoric acid as described in claim 1, it is characterized in that: the extraction in step b
Agent is one of tributyl phosphate or butylphosphoric acid ester and one of diluent kerosene, MIBK, n-butanol or diisopropyl ether
Mixture.
4. the method for using centrifugal extractor purification of wet process phosphoric acid as described in claim 1, it is characterized in that: in step c, organic phase
With 15~30:1 of phase volume ratio of phosphoric acid,diluted, wash temperature is 40~65 DEG C.
5. the method for using centrifugal extractor purification of wet process phosphoric acid as described in claim 1, it is characterized in that: in step d, organic phase
With 5~8:1 of phase volume ratio of pure water, being stripped temperature is 40~65 DEG C.
6. the method with centrifugal extractor purification of wet process phosphoric acid as described in Claims 1 to 5 any one claim, special
Sign is: first centrifugal extractor, the second centrifugal extractor and third centrifugal extractor are three and the above Centrifugical extraction
The revolving speed of the concatenated multitple extraction mechanism of machine, centrifugal extractors at different levels is not less than 3000r/min.
7. the method with centrifugal extractor purification of wet process phosphoric acid as described in Claims 1 to 5 any one claim, special
Sign is: further including Matter Transfer technique, after the washing acid generated after washing in step c is mixed with the pretreatment phosphoric acid in step b
It is extracted；Resulting phosphoric acid is stripped in step d takes a portion to be used as the phosphoric acid,diluted in step c；Gained is stripped in step d
Solvent be used as step b in extractant.
8. the method for using centrifugal extractor purification of wet process phosphoric acid as claimed in claim 7, it is characterized in that: further including recycle heat
Technique, step d are stripped resulting high-temperature solvent and contain after sour solvent exchanges heat as extractant, after heat exchange with what step b was generated
C is entered step after heating containing sour solvent by steam to be washed.
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| CN110116997A (en) * | 2019-06-25 | 2019-08-13 | 山东鲁北企业集团总公司 | A kind of method that wet phosphoric acid purifying removes iron |
| CN112875662A (en) * | 2021-03-24 | 2021-06-01 | 中国石油化工股份有限公司 | Method for purifying wet-process phosphoric acid by solvent extraction |
| CN113548651A (en) * | 2021-09-09 | 2021-10-26 | 中国石油化工股份有限公司 | Method for purifying wet-process phosphoric acid by solvent extraction |
| EP4015452A1 (en) | 2020-12-21 | 2022-06-22 | Técnicas Reunidas, S.A. | Process for producing technical grade phosphoric acid from sewage sludge ash |
| CN115672036A (en) * | 2022-11-18 | 2023-02-03 | 中国石油化工股份有限公司 | Methyl isobutyl ketone solvent recovery device and method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110116997A (en) * | 2019-06-25 | 2019-08-13 | 山东鲁北企业集团总公司 | A kind of method that wet phosphoric acid purifying removes iron |
| EP4015452A1 (en) | 2020-12-21 | 2022-06-22 | Técnicas Reunidas, S.A. | Process for producing technical grade phosphoric acid from sewage sludge ash |
| CN112875662A (en) * | 2021-03-24 | 2021-06-01 | 中国石油化工股份有限公司 | Method for purifying wet-process phosphoric acid by solvent extraction |
| CN112875662B (en) * | 2021-03-24 | 2023-02-24 | 中国石油化工股份有限公司 | Method for purifying wet-process phosphoric acid by solvent extraction |
| CN113548651A (en) * | 2021-09-09 | 2021-10-26 | 中国石油化工股份有限公司 | Method for purifying wet-process phosphoric acid by solvent extraction |
| CN115672036A (en) * | 2022-11-18 | 2023-02-03 | 中国石油化工股份有限公司 | Methyl isobutyl ketone solvent recovery device and method |
| CN115672036B (en) * | 2022-11-18 | 2024-06-07 | 中国石油化工股份有限公司 | Methyl isobutyl ketone solvent recovery device and method |
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