CN219897355U - Wet process phosphoric acid anion removing device - Google Patents
Wet process phosphoric acid anion removing device Download PDFInfo
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- CN219897355U CN219897355U CN202321247180.4U CN202321247180U CN219897355U CN 219897355 U CN219897355 U CN 219897355U CN 202321247180 U CN202321247180 U CN 202321247180U CN 219897355 U CN219897355 U CN 219897355U
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 178
- 238000000034 method Methods 0.000 title claims abstract description 43
- 238000000605 extraction Methods 0.000 claims abstract description 129
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 82
- 238000003860 storage Methods 0.000 claims abstract description 67
- 239000002253 acid Substances 0.000 claims abstract description 37
- 230000003009 desulfurizing effect Effects 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000006477 desulfuration reaction Methods 0.000 claims abstract description 15
- 230000023556 desulfurization Effects 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000004042 decolorization Methods 0.000 claims abstract description 4
- 238000004458 analytical method Methods 0.000 claims description 13
- 230000001804 emulsifying effect Effects 0.000 claims description 2
- 150000001450 anions Chemical class 0.000 abstract description 10
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 abstract description 2
- 238000000746 purification Methods 0.000 description 18
- 239000002904 solvent Substances 0.000 description 18
- 238000002156 mixing Methods 0.000 description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000002086 nanomaterial Substances 0.000 description 7
- 239000002367 phosphate rock Substances 0.000 description 7
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 239000010452 phosphate Substances 0.000 description 5
- 239000003337 fertilizer Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000003456 ion exchange resin Substances 0.000 description 3
- 229920003303 ion-exchange polymer Polymers 0.000 description 3
- -1 iron-magnesium-aluminum Chemical compound 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- RMNODSGCFHVNDC-UHFFFAOYSA-N phenyl bis(2-propan-2-ylphenyl) phosphate Chemical compound CC(C)C1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C(C)C)OC1=CC=CC=C1 RMNODSGCFHVNDC-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- TUUQISRYLMFKOG-UHFFFAOYSA-N trihexyl 2-acetyloxypropane-1,2,3-tricarboxylate Chemical compound CCCCCCOC(=O)CC(C(=O)OCCCCCC)(OC(C)=O)CC(=O)OCCCCCC TUUQISRYLMFKOG-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Abstract
The utility model provides a wet-process phosphoric acid anion removing device, wherein an outlet of a concentrated phosphoric acid pipeline and an outlet of an extractant storage tank are respectively connected with an inlet of an extraction device; the outlet of the extraction device is connected with the inlet of the desulfurizing tower; the outlet of the desulfurizing tower is connected with the inlet of the back extraction device; the outlet of the back extraction device is connected with the inlet of the back extraction acid storage tank. The concentrated phosphoric acid pipeline is connected with the upper inlet of the extraction device, the extractant storage tank is connected with the lower inlet of the extraction device, and the materials in the concentrated phosphoric acid pipeline and the materials in the extractant storage tank are subjected to countercurrent contact extraction. Countercurrent contact extraction is carried out on concentrated phosphoric acid and an extractant under a closed environment, so as to obtain a light phase and a heavy phase; the light phase is treated by desulfurization, desalted water back extraction, decolorization and concentration to obtain the phosphoric acid with anions removed. The device is convenient to manage on site in the aspect of operation of removing sulfate radical without adding ore pulp, no phosphogypsum is produced, and the acid loss is low.
Description
Technical Field
The utility model belongs to the technical field of wet phosphoric acid purification by a sulfuric acid method, and relates to a purification device for obtaining high-purity wet phosphoric acid.
Background
At present, the basic reserve of phosphorite in China is 32.4 hundred million tons, and it has been ascertained that phosphorite resources are distributed in 27 provinces (autonomous regions), but the distribution is centralized, and the distribution is mainly in five provinces of Hubei, sichuan, guizhou, yunnan and Hunan, the total reserve of phosphorite resources in five provinces exceeds 80%, but with the consumption of phosphorite resources, most of the phosphorite resources exhibit low grade characteristics, and the utilization of low grade phosphorite resources is greatly dependent on the technical level of wet phosphoric acid. The wet phosphoric acid has the characteristics of low-grade phosphorite utilization and low process energy consumption compared with the hot phosphoric acid, but has the inherent defects of high impurity content of phosphoric acid and high purification difficulty.
With the rise of new energy, the demand for high-purity phosphoric acid is increasing, so that the purification of phosphoric acid is particularly urgent. The phosphoric acid purifying method has a plurality of chemical precipitation, solvent extraction, crystallization, ion exchange and the like, and the solvent extraction is taken as a main flow process route in China at present, wherein the extraction process taking Vat Fu as a main flow process can continuously and industrially produce food grade phosphoric acid, and the Sichuan Dai and Hua Shi solvent extraction purifying processes meet the industrial phosphoric acid requirement.
Analysis of the wet phosphoric acid produced by collophanite in the Hubei area shows that the content of the iron-magnesium-aluminum sesquioxide in the acid is high, the MER value (the percentage ratio of the sum of the percentage of the sesquioxide in the phosphoric acid to the percentage of phosphorus pentoxide) is as high as 8 percent, and when dilute phosphoric acid is concentrated, the acid viscosity is high, the energy consumption is high during concentration due to the influence of iron-magnesium-aluminum ions, the acid concentration is difficult, and the subsequent extraction efficiency is greatly improved.
In addition, electrodialysis is often adopted in the purification process of wet phosphoric acid, but anions enter together with phosphate radical due to concentration difference and electric field force in the process, so that the anion removal rate is not high. When the ion exchange resin is used for the treatment, the ion exchange resin needs to be replaced for a long period of time, and the efficiency of the ion exchange resin is low. Therefore, the removal of anionic impurities is still a problem to be solved by those skilled in the art.
Disclosure of Invention
In order to solve the problems, the main purpose is to provide a device for removing anions by wet phosphoric acid extraction aiming at the defects existing in the prior extraction technology. Can effectively remove anion impurities under the condition of high impurity content of wet-process phosphoric acid to obtain high-purity wet-process purified phosphoric acid. In the wet-process phosphoric acid purification process, the extraction rate is high, the yield of the raffinate acid is low, and the method is suitable for a new production technology of large-scale production.
The outlet of the concentrated phosphoric acid pipeline and the outlet of the extractant storage tank are respectively connected with the inlet of the extraction device;
the outlet of the extraction device is connected with the inlet of the desulfurizing tower;
the outlet of the desulfurizing tower is connected with the inlet of the back extraction device;
the outlet of the back extraction device is connected with the inlet of the back extraction acid storage tank.
The extraction device and the back extraction acid storage tank are respectively selected from any one of a pipeline type dispersing machine, a pipeline type emulsifying machine, a turntable tower type extraction tower and a turbine extraction tower.
The concentrated phosphoric acid pipeline is connected with the upper inlet of the extraction device, the extractant storage tank is connected with the lower inlet of the extraction device, and the materials in the concentrated phosphoric acid pipeline and the materials in the extractant storage tank are subjected to countercurrent contact extraction.
The outlet of the desulfurizing tower is connected with the upper inlet of the back extraction device, and the process water storage tank is connected with the lower inlet of the back extraction device, so that countercurrent contact back extraction of materials in the desulfurizing tower and materials in the process water storage tank is realized.
The outlet of the back extraction acid storage tank is connected with the inlet of the centrifuge;
the outlet of the centrifugal machine is connected with the inlet of the decoloring tank;
the outlet of the decoloring tank is connected with the inlet of the concentrating device;
the outlet of the concentration device is connected with the inlet of the phosphoric acid storage tank.
The outlet of the extraction device is connected with the inlet of the analysis tower through a pipeline, and the outlet of the analysis tower is connected with the inlet of the filter.
In another technical scheme, the outlet of the extraction device is connected with the inlet of the desulfurization and decoloration tower;
the outlet of the desulfurization and decoloration tower is connected with the inlet of the back extraction device; the outlet of the back extraction device is connected with the inlet of the back extraction acid storage tank; the outlet of the back extraction acid storage tank is connected with the inlet of the centrifuge; the outlet of the centrifugal machine is connected with the inlet of the concentration device.
The outlet of the extraction device and the outlet of the desulfurizing tower are respectively connected with the inlet of the analyzing tower through pipelines, the outlet of the analyzing tower is connected with the inlet of the filter, and the outlet of the filter is respectively connected to the dilute phosphoric acid storage tank and the filter residue product area.
The outlet of the back extraction device is connected with the inlet of the extractant storage tank.
In another scheme, an outlet of the extraction device and an outlet of the desulfurization and decoloration tower are respectively connected with an inlet of the analysis tower through pipelines, an outlet of the analysis tower is connected with an inlet of a filter, and an outlet of the filter is respectively connected to a dilute phosphoric acid storage tank and a filter residue product area.
The outlet of the filter is respectively connected to the dilute phosphoric acid storage tank and the filter residue product area.
The outlet of the back extraction device is connected with the inlet of the extractant storage tank.
The outlet of the solvent storage tank is connected with the inlet of the ultra-high speed mixing device, and the outlet of the ultra-high speed mixing device is connected with the inlet of the extractant storage tank.
The overspeed mixing device is selected from a variable-frequency high-speed stirrer, and the variable-frequency high-speed stirrer can realize a switching rate of 500r/min-1000 r/min.
Aiming at the device, the utility model provides a wet-process phosphoric acid anion removal process, which comprises the following steps: step 1, extraction: and (3) delivering the concentrated phosphoric acid obtained by pre-purification to a purification tower and an extracting agent for countercurrent extraction reaction to obtain a light phase 2 and a heavy phase 2 containing phosphorus pentoxide.
And 2, fine desulfurization: and (3) carrying out reaction fine desulfurization on the light phase 2 obtained in the step 1 of the intermediate purification process by using a desulfurizing agent, and washing to obtain a light phase 3 and a heavy phase 3.
Step 3, back extraction: and (3) carrying out back extraction on the light phase 2 obtained in the step 2 of the intermediate purification process by using desalted water to obtain a light phase 4 and a heavy phase 4. The light phase 4 returns to the purification and extraction process for cyclic reaction, and the heavy phase 4 is the stripping acid with the concentration of 38-42% obtained after intermediate purification.
And 4, raffinate acid analysis: and (3) the heavy phase 2 obtained in the step (1) in the intermediate purification process is subjected to solvent analysis to obtain raffinate, and the raffinate is filtered to obtain clear liquid, and the clear liquid returns to a clear liquid tank in the pre-purification process to participate in the pre-extraction reaction. And delivering the filtered phosphorus-containing waste residue to a fertilizer process to produce the fertilizer.
Step 5, stripping acid analysis: and (3) carrying out solvent analysis and concentration on the strip acid obtained in the step (3) in the intermediate purification process to obtain the phosphoric acid with 42-45% of concentration without solvent.
And step 6, decoloring: and (3) decoloring the phosphoric acid obtained in the step 5 in the intermediate purification step to obtain decolored acid.
And 7, concentrating: and (3) carrying out flash evaporation on the decolorized acid obtained in the step (6) in the intermediate purification process to concentrate the acid to concentrated phosphoric acid with the phosphorus pentoxide content of 61-65%.
The utility model has the beneficial effects that
In the technological process of the utility model, sulfate radical is removed without adding ore pulp in pretreatment, the operation is convenient to manage on site, phosphogypsum is not produced, and the acid loss is low.
High extraction rate and less by-product raffinate.
The post-purification can adjust the process according to the device requirement, and can reduce the dependence on materials aiming at the production of phosphoric acid with different qualities, and the requirements can be met by common domestic 316L or 2205.
The technical scheme of the utility model has short extraction time and high efficiency, and the anion, in particular sulfate ion, namely fluoride ion, has good removal effect, and the anion content is lower than 100ppm, more preferably lower than 50ppm, more preferably lower than 30ppm, more preferably lower than 10ppm, more preferably lower than 5ppm, more preferably lower than 1ppm, more preferably lower than 100ppb.
Drawings
FIG. 1 is a schematic diagram of a wet process phosphoric acid anion removal apparatus of example 1, a concentrated phosphoric acid pipeline, 2 an extraction apparatus, 3 a desulfurizing tower, 4 a resolution tower, 5 a filter, 6 a dilute phosphoric acid pipeline, 7 a residue product zone, 8 a stripping apparatus, 9 an extractant storage tank, 10 a strip acid storage tank, 11 a centrifuge, 12 a decolorizing tank, 13 a concentration apparatus, 14 a phosphoric acid storage tank, 15 a super high speed mixing apparatus, 16 a solvent storage tank.
FIG. 2 is a schematic diagram of a wet process phosphoric acid anion removal apparatus of example 2, concentrated phosphoric acid pipeline, 2, extraction apparatus, 3', desulfurization and decolorization column, 4, resolution column, 5, filter, 6, dilute phosphoric acid pipeline, 7, residue product zone, 8 stripping apparatus, 9, extractant storage tank, 10, strip acid storage tank, 11, centrifuge, 13, concentration apparatus, 14, phosphoric acid storage tank, 15, ultra high speed mixing apparatus, 16, solvent storage tank.
Detailed Description
Example 1
The outlets of the concentrated phosphoric acid pipeline 1 and the extractant storage tank 9 are respectively connected with the inlet of the extraction device 2;
the outlet of the extraction device 2 is connected with the inlet of the desulfurizing tower 3;
the outlet of the desulfurizing tower 3 is connected with the inlet of the back extraction device 8;
the outlet of the stripping device 8 is connected with the inlet of a stripping acid storage tank 10.
The extraction device 2 and the back extraction acid storage tank 10 are respectively selected from a turntable tower type extraction tower.
The concentrated phosphoric acid pipeline 1 is connected with the upper inlet of the extraction device 2, the extractant storage tank 9 is connected with the lower inlet of the extraction device 2, and the materials in the concentrated phosphoric acid pipeline 1 and the materials in the extractant storage tank 9 are subjected to countercurrent contact extraction.
The outlet of the desulfurizing tower 3 is connected with the upper inlet of the back extraction device 8, and the process water storage tank 17 is connected with the lower inlet of the back extraction device 8, so that countercurrent contact back extraction of the materials in the desulfurizing tower 3 and the materials in the process water storage tank 17 is realized.
The outlet of the back extraction acid storage tank 10 is connected with the inlet of the centrifuge 11;
the outlet of the centrifugal machine 11 is connected with the inlet of the decoloring tank 12;
the outlet of the decoloring tank 12 is connected with the inlet of the concentrating device 13;
the outlet of the concentration device 13 is connected to the inlet of the phosphoric acid storage tank 14.
The outlet of the extraction device 2 and the outlet of the desulfurizing tower 3 are respectively connected with the inlet of the analyzing tower 4 through pipelines, and the outlet of the analyzing tower 4 is connected with the inlet of the filter 5.
The outlet of the filter 5 is connected via a dilute phosphoric acid conduit 6 to a dilute phosphoric acid storage tank, and the outlet of the filter 5 is also connected to a residue product zone 7.
The outlet of the stripping device 8 is connected to the inlet of an extractant reservoir 15.
The outlet of the solvent storage tank 16 is connected with the inlet of the ultra-high speed mixing device 15, and the outlet of the ultra-high speed mixing device 15 is connected with the inlet of the extractant storage tank 9.
The overspeed mixing device 9 is selected from a variable frequency high-speed stirrer, and the variable frequency high-speed stirrer can realize a switching rate of 500r/min-1000 r/min.
Example 2
The outlets of the concentrated phosphoric acid pipeline 1 and the extractant storage tank 9 are respectively connected with the inlet of the extraction device 2;
the outlet of the extraction device 2 is connected with the inlet of the desulfurization and decoloration tower 3';
the outlet of the desulfurization and decolorization tower 3' is connected with the inlet of the back extraction device 8;
the outlet of the stripping device 8 is connected with the inlet of a stripping acid storage tank 10.
The extraction device 2 and the back extraction acid storage tank 10 are respectively selected from a turntable tower type extraction tower.
The concentrated phosphoric acid pipeline 1 is connected with the upper inlet of the extraction device 2, the extractant storage tank 9 is connected with the lower inlet of the extraction device 2, and the materials in the concentrated phosphoric acid pipeline 1 and the materials in the extractant storage tank 9 are subjected to countercurrent contact extraction.
The outlet of the desulfurizing tower 3 is connected with the upper inlet of the back extraction device 8, and the process water storage tank 17 is connected with the lower inlet of the back extraction device 8, so that countercurrent contact back extraction of the materials in the desulfurizing and decolorizing tower 3' and the materials in the process water storage tank 17 is realized.
The outlet of the back extraction acid storage tank 10 is connected with the inlet of the centrifuge 11;
the outlet of the centrifugal machine 11 is connected with the inlet of the concentration device 13;
the outlet of the concentration device 13 is connected to the inlet of the phosphoric acid storage tank 14.
The outlet of the extraction device 2 and the outlet of the desulfurization and decoloration tower 3' are respectively connected with the inlet of the analysis tower 4 through pipelines, and the outlet of the analysis tower 4 is connected with the inlet of the filter 5.
The outlet of the filter 5 is connected via a dilute phosphoric acid conduit 6 to a dilute phosphoric acid storage tank, and the outlet of the filter 5 is also connected to a residue product zone 7.
The outlet of the stripping device 8 is connected to the inlet of an extractant reservoir 15.
The outlet of the solvent storage tank 16 is connected with the inlet of the ultra-high speed mixing device 15, and the outlet of the ultra-high speed mixing device 15 is connected with the inlet of the extractant storage tank 9.
The overspeed mixing device 9 is selected from a variable frequency high-speed stirrer, and the variable frequency high-speed stirrer can realize a switching rate of 500r/min-1000 r/min.
Example 3
The following procedure was carried out using the apparatus of example 1:
TABLE 1 phosphoric acid parameter index
Configuration of the extractant: bis (2-isopropylphenyl) phenyl phosphate and methyl isobutyl ketone in a volume ratio of 1:20, and mixing at 400r/min for 5min to form transparent suspension.
Desulfurizing agent: the mass concentration of the dilute phosphoric acid solution of the barium carbonate is 20-35%, and the mass fraction of the barium carbonate in the dilute phosphoric acid solution of the barium carbonate is 30-40%.
The wet-process phosphoric acid from which anions are to be removed is the wet-process phosphoric acid of number 1 in table 1 above.
The temperature in the extraction tower is controlled to be 45+/-5 ℃, the pressure in the extraction tower is controlled to be 0.01-0.05Mpa, wet phosphoric acid and an extraction solvent are respectively preheated to be 45+/-5 ℃, the wet phosphoric acid and the extraction solvent enter the extraction tower from the upper part and the lower part of the extraction tower together according to the volume ratio of 1:2.1 for contact extraction, the wet phosphoric acid and the extraction solvent are respectively emulsified and dispersed into 200 mu m granularity through a turntable tower in the contact extraction process, and the heavy phase 1 and the light phase 1 are collected after the contact reaction is carried out for 3 min.
Adding a desulfurizing agent into the light phase 1 for stirring and desulfurizing to obtain a heavy phase 2 and a light phase 2, wherein the volume ratio of the light phase 1 to the desulfurizing agent is 10:1.
and (3) mixing the heavy phase 1 and the heavy phase 2 to obtain raffinate acid, and analyzing and filtering to obtain dilute phosphoric acid and phosphate solid filter residues, wherein the phosphate solid filter residues are used for producing fertilizer.
The light phase 2 is back extracted by adding 10% volume of water relative to the light phase 2 to obtain a heavy phase 3 (back extraction acid) and a light phase 3 (residual acid), wherein the light phase 3 continuously enters from the bottom of the extraction tower by taking 80% (volume fraction) as an extraction solvent, and meanwhile, the fresh extractant with 20% volume fraction is supplemented.
And (3) carrying out vacuum rectification and desolventizing on the heavy phase 3 at the absolute pressure of 10-30KPaA and the temperature of 85-100 ℃ to obtain the phosphoric acid with 42-50% of solvent-free concentration.
The phosphoric acid is decolorized by active carbon and then concentrated by vacuum flash evaporation at 90-120 ℃ and absolute pressure of 10-25KPaA to obtain the concentrated phosphoric acid with 64-65% phosphorus pentoxide content.
The extraction efficiency of the extractant, the anion removal efficiency, and the reaction results for the time of recycling the extractant are shown in table 2.
Example 4
The following procedure was carried out using the apparatus of example 2
Configuration of the extractant: acetyl trihexyl citrate and methyl isobutyl ketone in a volume ratio of 1:20, and mixing at high speed at 800r/min for 3min to form transparent suspension.
The desulfurization and decoloration agent is a super carbon nanomaterial; the preparation method of the super carbon nanomaterial comprises the following steps:
mixing carbon nanofibers, KOH and barium carbonate, ball milling for 2 hours at 300r/min, sieving with a 600-mesh sieve, dehydrating the mixture obtained after ball milling at 200 ℃, heating to 600 ℃ in an inert atmosphere, calcining for 2 hours, and cooling to obtain the super carbon nanomaterial. The mass ratio of the carbon material to the alkali to the desulfurization material is 1:1:0.5.
The wet-process phosphoric acid from which anions are to be removed is the wet-process phosphoric acid of number 4 in table 1 above.
The temperature in the extraction tower is controlled to be 45+/-5 ℃, the pressure in the extraction tower is controlled to be 0.01-0.05Mpa, wet phosphoric acid and an extraction solvent are respectively preheated to be 45+/-5 ℃, the wet phosphoric acid and the extraction solvent enter the extraction tower from the upper part and the lower part of the extraction tower together according to the volume ratio of 1:1.9 for contact extraction, the wet phosphoric acid and the extraction solvent are respectively dispersed into 250 mu m granularity in the contact extraction process, and the heavy phase 1 and the light phase 1 are collected after the contact reaction is carried out for 4 min.
Mixing the light phase 1 with a dilute phosphoric acid solution of the super carbon nano material, wherein the mass concentration of the dilute phosphoric acid is 38%, and the mass fraction of the super carbon nano material in the dilute phosphoric acid solution of the super carbon nano material is 30%. The volume ratio of the light phase to the super carbon nanomaterial is 8:0.6.
the light phase 1 is desulfurized and decolored to obtain a heavy phase 2 '(back extraction acid) and a light phase 2'.
And (3) resolving the heavy phase 1 and the heavy phase 2' to obtain raffinate, and filtering the raffinate to obtain the diluted phosphoric acid and phosphate mixture with the mass concentration of 8.5%. The phosphate mixture is used for preparing fertilizer and realizing circulation.
Adding water into the light phase 2' for back extraction to obtain a heavy phase 3' (back extraction acid) and a light phase 3' back extraction liquid; the light phase 3' back extraction liquid is reused as a new extractant after being supplemented with a fresh extractant; the back extraction liquid accounts for 12% of the new extractant by volume.
The heavy phase 3' (back extraction acid) is treated by vacuum rectification to remove solvent, and the vacuum rectification condition is that the solvent is removed under the absolute pressure of 10-30KPaA and the temperature of 85-100 ℃;
and carrying out vacuum flash evaporation on the decolorized material and the material obtained after solvent removal at 90-120 ℃ under the absolute pressure of 10-25KPaA to obtain phosphoric acid with the concentration of 66-65%.
Claims (8)
1. The wet process phosphoric acid anion removing device is characterized in that,
the outlets of the concentrated phosphoric acid pipeline (1) and the extractant storage tank (9) are respectively connected with the inlet of the extraction device (2);
the outlet of the extraction device (2) is connected with the inlet of the desulfurizing tower (3);
the outlet of the desulfurizing tower (3) is connected with the inlet of the back extraction device (8);
the outlet of the back extraction device (8) is connected with the inlet of a back extraction acid storage tank (10).
2. The wet process phosphoric acid anion removal device according to claim 1, wherein,
the extraction device (2) and the back extraction acid storage tank (10) are respectively selected from any one of a pipeline type dispersing machine, a pipeline type emulsifying machine, a turntable tower type extraction tower and a turbine extraction tower.
3. The wet process phosphoric acid anion removal device according to claim 2, wherein,
the concentrated phosphoric acid pipeline (1) is connected with the upper inlet of the extraction device (2), the extractant storage tank (9) is connected with the lower inlet of the extraction device (2), and the materials in the concentrated phosphoric acid pipeline (1) are countercurrent contact-type extracted with the materials in the extractant storage tank (9).
4. The wet process phosphoric acid anion removing device according to claim 2, wherein an outlet of the desulfurizing tower (3) is connected with an upper inlet of the back extraction device (8), and a process water storage tank (17) is connected with a lower inlet of the back extraction device (8), so that countercurrent contact back extraction of materials in the desulfurizing tower (3) and materials in the process water storage tank (17) is realized.
5. The wet process phosphoric acid anion removal device according to claim 1, wherein,
the outlet of the back extraction acid storage tank (10) is connected with the inlet of the centrifuge (11);
the outlet of the centrifugal machine (11) is connected with the inlet of the decoloring tank (12);
the outlet of the decoloring tank (12) is connected with the inlet of the concentrating device (13);
the outlet of the concentration device (13) is connected with the inlet of the phosphoric acid storage tank (14).
6. The wet process phosphoric acid anion removing device according to claim 1, wherein the outlet of the extraction device (2) is connected with the inlet of the desulfurization and decolorization tower (3');
the outlet of the desulfurization and decoloration tower (3') is connected with the inlet of the back extraction device (8);
the outlet of the back extraction acid storage tank (10) is connected with the inlet of the centrifuge (11); the outlet of the centrifuge (11) is connected with the inlet of the concentration device (13).
7. The wet process phosphoric acid anion removal device according to claim 5, wherein,
the outlet of the extraction device (2) and the outlet of the desulfurizing tower (3) are respectively connected with the inlet of the analyzing tower (4) through pipelines, the outlet of the analyzing tower (4) is connected with the inlet of the filter (5), and the outlet of the filter (5) is respectively connected to the dilute phosphoric acid storage tank and the filter residue product area;
the outlet of the back extraction device (8) is connected with the inlet of the extractant storage tank (9).
8. The wet process phosphoric acid anion removal device according to claim 6, wherein,
the outlet of the extraction device (2) and the outlet of the desulfurization and decoloration tower (3') are respectively connected with the inlet of the analysis tower (4) through pipelines, the outlet of the analysis tower (4) is connected with the inlet of the filter (5), and the outlet of the filter (5) is respectively connected to the dilute phosphoric acid storage tank and the filter residue product area.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202321247180.4U CN219897355U (en) | 2023-05-23 | 2023-05-23 | Wet process phosphoric acid anion removing device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321247180.4U CN219897355U (en) | 2023-05-23 | 2023-05-23 | Wet process phosphoric acid anion removing device |
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