CN1579930A - New method for concentrating and purifying wet phosphoric acid by humid heat joint - Google Patents
New method for concentrating and purifying wet phosphoric acid by humid heat joint Download PDFInfo
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- CN1579930A CN1579930A CN 03135557 CN03135557A CN1579930A CN 1579930 A CN1579930 A CN 1579930A CN 03135557 CN03135557 CN 03135557 CN 03135557 A CN03135557 A CN 03135557A CN 1579930 A CN1579930 A CN 1579930A
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- Prior art keywords
- phosphoric acid
- wet
- concentrating
- process phosphoric
- heat
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 216
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 107
- 238000000034 method Methods 0.000 title claims abstract description 89
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002485 combustion reaction Methods 0.000 claims abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 11
- 229910052731 fluorine Inorganic materials 0.000 claims description 11
- 239000011737 fluorine Substances 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- OBSZRRSYVTXPNB-UHFFFAOYSA-N tetraphosphorus Chemical compound P12P3P1P32 OBSZRRSYVTXPNB-UHFFFAOYSA-N 0.000 claims description 4
- 239000005909 Kieselgur Substances 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 claims 1
- 235000012239 silicon dioxide Nutrition 0.000 claims 1
- 238000005507 spraying Methods 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 description 12
- 229910019142 PO4 Inorganic materials 0.000 description 11
- 239000011574 phosphorus Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000036571 hydration Effects 0.000 description 5
- 238000006703 hydration reaction Methods 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 238000006115 defluorination reaction Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- 230000002745 absorbent Effects 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000003556 assay Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 3
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- ZHQXROVTUTVPGO-UHFFFAOYSA-N [F].[P] Chemical compound [F].[P] ZHQXROVTUTVPGO-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 2
- 235000019691 monocalcium phosphate Nutrition 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002918 waste heat Substances 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 229910000150 monocalcium phosphate Inorganic materials 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention discloses a new method which combines moist heat and inspissations to purify wet-method phosphoric acid. Its characters are: using a low-density wet method phosphoric acid to absorb phosphorus pentoxide produced by phosphor' combustion, at the same time, using the heat energy produced by phosphor' combustion to vaporize redundant moisture in wet method phosphoric acid. After this, the wet method phosphoric acid can be condensed. And also the steam make fluorin in wet-method phosphoric acid transgress in gaseity. After this, the wet-method phosphoric acid can be purified.
Description
The technical field is as follows:
the invention relatesto a method for producing phosphoric acid in the chemical field, in particular to a novel method for concentrating wet-process phosphoric acid and defluorinating and purifying the phosphoric acid by utilizing hydration of thermal-process phosphorus pentoxide and evaporation and concentration of combustion waste heat of yellow phosphorus.
Background art:
at present, many wet-process phosphoric acid concentration processes have adverse factors that the concentration of phosphoric acid is increased and the viscosity and specific heat capacity of phosphoric acid are respectively increased along with the concentration process, have strong corrosivity on production equipment, have high requirements on the material of the equipment, and are suitable for industrial productionThe process conditions are also quite harsh, and a large amount of heat is required in the concentration process, the energy consumption is high, and the defluorination is extremely difficult. In the feed-grade phosphate industry, the general method is to use limestone or lime milk as an alkaline agent to adjust the pH value of a solution so as to precipitate fluorine in wet acid. However, in this case, the concentration of phosphoric acid after defluorination is reduced to about 10% (as H)3PO4A meter); secondly, the yield of phosphorus is reduced by the white fertilizer generated in the process, so that the concentration and purification of the wet-process phosphoric acid are greatly limited.
The invention content is as follows:
the invention aims to provide a new method for purifying wet-process phosphoric acid by combining wet-process phosphoric acid and concentration, which overcomes a plurality of defects in the method, does not need to add new equipment, does not need external heat, only utilizes the existing hot-process phosphoric acid device and process route, takes the wet-process phosphoric acid as an absorbent of hot-process phosphorus pentoxide gas, and can further concentrate the wet-process phosphoric acid and achieve the expected defluorination effect on the premise of not influencing the yield and consumption of the hot-process phosphoric acid.
The purpose of the invention is realized as follows:
the technical scheme of the invention comprises the following steps: adding a proper amount of 10-50% (by P) into a concentrated acid circulating tank in a thermal phosphoric acid process2O5Measured) is used as a phosphorus pentoxide absorbent, and simultaneously, the wet-process phosphoric acid is used as a coolant for hot air flow in the absorption tower, so that the moisture in the wet-process phosphoric acid is removed by utilizing the principles that the phosphorus pentoxide gas needs to absorb water during hydration and needs to evaporate water during cooling in the production process of the hot-process phosphoric acid, and the aim of concentrating the wet-process phosphoric acid is fulfilled. Adding a proper amount of active silica-containing substance (such as one or a mixture of diatomite, white carbon black, active silica and the like) into a hot-process phosphoric acid concentration tank, wherein the adding amount is calculated according to the fluorine content in wet-process phosphoric acid. In the form of HF to SiO2And (2) controlling the circulating acid temperature to be below 85 ℃ for circulating for 1-2 hours, decomposing fluorine in the wet-process phosphoric acid into silicon tetrafluoride gas along with the increase of the concentration of the phosphoric acid and the increase of the time, and finally realizing a new method for purifying the wet-process phosphoric acid by wet-heat combined concentration.
The wet-process phosphoric acid concentration can be gradually concentrated to more than 85% (as H)3PO4Meter), and can remove the wet-process phosphoric acidMore than 95 percent of fluorine, and the phosphorus-fluorine ratio (P) of finished phosphoric acid2O5the/F) can reach the required value. And because of the addition of the thermal phosphoric acid, the adverse factor that the viscosity of the phosphoric acid suddenly rises when the phosphoric acid is concentrated by a pure wet process is avoided, the specific heat capacity of the phosphoric acid is improved, the corrosivity in the concentration process of the phosphoric acid is reduced, external heat is not required, a large amount of energy consumption can be saved, and 1.1 ton of water in the wet process phosphoric acid can be concentrated and removed when 85% phosphoric acid is produced by each ton of yellow phosphorus. The finished phosphoric acid can be used as raw material for producing feed grade calcium hydrophosphate, feed grade calcium biphosphate and other phosphate series products, thereby leading the wet-process phosphoric acid to be more widely applied in the phosphate series products.
The mechanism on which the invention is based is as follows:
1. yellow phosphorus burns to produce phosphorus pentoxide and a large amount of heat:
2. phosphorus pentoxide hydration consumes excess water in wet-process phosphoric acid and produces phosphoric acid:
3. the water in the wet-process phosphoric acid is evaporated into water vapor after absorbing heat;
water (liquid state) + Q → Water (vapor state)
4. The fluorine brought in by the wet-process phosphoric acid is decomposed into silicon tetrafluoride and hydrogen fluoride gas:
5. the silica added to the wet-process phosphoric acid converts the hydrogen fluoride, which is highly corrosive, into the less corrosive fluorosilicic acid:
the invention has the advantages that:
(1) the existing thermal phosphoric acid production device is utilized, no additional equipment is needed, and the capacity of the existing device for producing the thermal phosphoric acid is not influenced;
(2) the wet-process phosphoric acid is used as a hydration absorbent of the hot-process phosphoric acid, and the dual concentration effects of hydration dehydration of phosphorus pentoxide gas and evaporation dehydration of absorbed waste heat in the production process of the hot-process phosphoric acid are ingeniously utilized, so that the aim of concentrating the wet-process phosphoric acid is fulfilled;
(3) the steam generated in the heat exchange process of the phosphorus pentoxide high-temperature hot gas flow and the solution is skillfully utilized, certain phosphoric acid concentration is controlled, and sufficient silicon is ensured, so that fluorine in the wet-process phosphoric acid escapes in a gaseous form, and the aim of defluorination is fulfilled;
(4) no phosphorus pentoxide loss exists in the concentration process, and the yield of phosphorus in wet-process phosphoric acid reaches 100 percent;
(5) the viscosity of the phosphoric acid is reduced along with the increase of the content of the phosphoric acid in the mixed acid bya hot method in the concentration process, the specific heat capacity is increased, the fluidity is good, the heat transfer effect is good, the defects of high viscosity, low specific heat capacity, serious scaling, poor heat transfer effect and the like along with the increase of the concentration in the process of independently concentrating the wet method phosphoric acid are avoided, and the material requirements on equipment are reduced along with the decrease of the viscosity and the content of impurities;
(6) after the diatomite is added, a large amount of fluorine in the wet-process phosphoric acid escapes in the form of silicon tetrafluoride along with concentration, so that the corrosivity to system equipment is reduced;
(7) the phosphorus-fluorine ratio of the concentrated finished product phosphoric acid can reach a required value, the quality of the phosphoric acid is good, and the phosphoric acid can be used as a production raw material of phosphate series products such as feed-grade calcium hydrophosphate, feed-grade monocalcium phosphate and the like, so that the application of wet-process phosphoric acid is expanded;
(8) no need of external heat, low energy consumption, low concentration cost and good economic benefit.
The technical effects are as follows:
the invention realizes the production process of the wet and hot combined phosphoric acid, can realize different proportions of the wet phosphoric acid and the hot phosphoric acid by adjusting the initial concentration of the wet phosphoric acid, can greatly reduce the production cost of 85 percent phosphoric acid, and can meet the production requirements of various phosphorus products including feed-grade products by various sanitary indexes in the product. In addition, the process has the advantages of low investment, low material requirement,low energy consumption, easy control of operation and the like.
Description of the drawings:
FIG. 1 is a schematic view of a new process flow of concentrating and purifying wet-process phosphoric acid by combining wet heat and moisture
The specific implementation mode is as follows:
the technical contents of the present invention will be further described by specific embodiments with reference to the accompanying drawings.
Example 1:
injecting wet-process phosphoric acid (with content of H) into a phosphoric acid circulating tank3O469.18%, FO.315%) and simultaneously adding diatomite and wet-process phosphoric acid to form a suspension, and using the suspension as P produced by combustion of yellow phosphorus2O5When the specific gravity of the phosphoric acid reaches 1.61, the phosphoric acid is pumped into a finished phosphoric acid storage tank.
Assay analysis results of concentrated phosphoric acid:
phosphoric acid (with H)3PO4Calculated) 85.41% fluoride (calculated as F) 0.068%
Phosphorus to fluorine ratio (P)5O5/F)909.99
The phosphoric acid meets the requirements of feed-grade phosphate production.
Example 2:
injecting wet-process phosphoric acid (with content of H) into a phosphoric acid circulating tank3PO440.23%, fo.98%) and simultaneously adding diatomaceous earth and wet-process phosphoric acid to form a suspension which is used as P produced by combustion of yellow phosphorus2O5When the specific gravity of the phosphoric acid reaches 1.62, the phosphoric acid is pumped into a finished phosphoric acid storage tank.
Assay analysis results of concentrated phosphoric acid:
phosphoric acid (with H)3PO4Calculated) 85.26% fluoride (calculated as F) 0.059%
Phosphorus to fluorine ratio (P)2O5/F)1046.96
The phosphoric acid meets the requirements of feed-grade phosphate production.
Example 3:
injecting wet-process phosphoric acid (with content of H) into a phosphoric acid circulating tank3PO419.34%, F1.57%) with the addition of diatomsMixing soil with wet-process phosphoric acid to form a suspension, and using the suspension as P produced by combustion of yellow phosphorus2O5When the specific gravity of the phosphoric acid reaches 1.62, the phosphoric acid is pumped into a finished phosphoric acid storage tank.
Assay analysis results of concentrated phosphoric acid:
phosphoric acid (with H)3PO4Calculated) 85.34% fluoride (calculated as F) 0.066%
Phosphorus to fluorine ratio (P)2O5/F)936.80
The phosphoric acid meets the requirements of feed-grade phosphate production.
Claims (4)
1. A new method for concentrating and purifying wet-process phosphoric acid by combining wet process and heat is characterized in that a substance containing active silicon dioxide is added into the wet-process phosphoric acid, then the wet-process phosphoric acid is used for spraying and absorbing phosphorus pentoxide generated by yellow phosphorus combustion, and finally the purposes of concentrating and purifying the wet-process phosphoric acid are achieved, and the wet-heat mixed phosphoric acid with low impurity content is obtained.
2. The new method for concentrating and purifying wet-process phosphoric acid by wet-heat combination according to claim 1, wherein the concentration of the wet-process phosphoric acid is 10-50% (expressed as P)2O5Meter).
3. The new method for concentrating and purifying wet-process phosphoric acid by combining wet process and heat as claimed in claim 1, wherein the active silica-containing material is one or a mixture of diatomaceous earth, white carbon black, active silica, etc.
4. The new method for concentrating and purifying wet-process phosphoric acid by combining wet process and heat technology according to claim 1, wherein the active silica-containing substance is added in an amount of HF to SiO 2-6 to 1 (molar ratio) calculated on the fluorine content in the wet-process phosphoric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03135557 CN1238249C (en) | 2003-08-08 | 2003-08-08 | New method for concentrating and purifying wet phosphoric acid by humid heat joint |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03135557 CN1238249C (en) | 2003-08-08 | 2003-08-08 | New method for concentrating and purifying wet phosphoric acid by humid heat joint |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1579930A true CN1579930A (en) | 2005-02-16 |
| CN1238249C CN1238249C (en) | 2006-01-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03135557 Expired - Fee Related CN1238249C (en) | 2003-08-08 | 2003-08-08 | New method for concentrating and purifying wet phosphoric acid by humid heat joint |
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| CN (1) | CN1238249C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107226460A (en) * | 2016-03-25 | 2017-10-03 | 云南派博科技有限公司 | The method that peroxophosphoric acid is produced using phosphorus calory burning concentration of dilute phosphoric acid |
| CN108313995A (en) * | 2018-04-13 | 2018-07-24 | 云南磷化集团有限公司 | Wet-process phosphoric acid concentration defluorinate integral method |
-
2003
- 2003-08-08 CN CN 03135557 patent/CN1238249C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107226460A (en) * | 2016-03-25 | 2017-10-03 | 云南派博科技有限公司 | The method that peroxophosphoric acid is produced using phosphorus calory burning concentration of dilute phosphoric acid |
| CN108313995A (en) * | 2018-04-13 | 2018-07-24 | 云南磷化集团有限公司 | Wet-process phosphoric acid concentration defluorinate integral method |
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| Publication number | Publication date |
|---|---|
| CN1238249C (en) | 2006-01-25 |
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