CN114735668A - Production method of fire-fighting-grade monoammonium phosphate - Google Patents
Production method of fire-fighting-grade monoammonium phosphate Download PDFInfo
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- CN114735668A CN114735668A CN202210339001.3A CN202210339001A CN114735668A CN 114735668 A CN114735668 A CN 114735668A CN 202210339001 A CN202210339001 A CN 202210339001A CN 114735668 A CN114735668 A CN 114735668A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 title claims abstract description 14
- 235000019837 monoammonium phosphate Nutrition 0.000 title claims abstract description 14
- 239000006012 monoammonium phosphate Substances 0.000 title claims abstract description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 172
- 239000002002 slurry Substances 0.000 claims abstract description 99
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 86
- 238000011282 treatment Methods 0.000 claims abstract description 66
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 55
- 239000000706 filtrate Substances 0.000 claims abstract description 42
- 239000012535 impurity Substances 0.000 claims abstract description 31
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000006477 desulfuration reaction Methods 0.000 claims abstract description 27
- 230000023556 desulfurization Effects 0.000 claims abstract description 27
- 230000005484 gravity Effects 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000000047 product Substances 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 14
- 239000006228 supernatant Substances 0.000 claims abstract description 14
- 238000000605 extraction Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000006115 defluorination reaction Methods 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims description 23
- 238000000746 purification Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000002367 phosphate rock Substances 0.000 claims description 15
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 3
- 230000007613 environmental effect Effects 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 abstract description 16
- 239000003795 chemical substances by application Substances 0.000 abstract description 12
- 239000004254 Ammonium phosphate Substances 0.000 abstract description 11
- 229910000148 ammonium phosphate Inorganic materials 0.000 abstract description 11
- 235000019289 ammonium phosphates Nutrition 0.000 abstract description 11
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 abstract description 11
- 238000004062 sedimentation Methods 0.000 abstract description 10
- 239000002893 slag Substances 0.000 description 10
- 239000002253 acid Substances 0.000 description 7
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- ZRIUUUJAJJNDSS-UHFFFAOYSA-N ammonium phosphates Chemical compound [NH4+].[NH4+].[NH4+].[O-]P([O-])([O-])=O ZRIUUUJAJJNDSS-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 239000013618 particulate matter Substances 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 206010003497 Asphyxia Diseases 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 229920004449 Halon® Polymers 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical class [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 description 1
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical class O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000019700 dicalcium phosphate Nutrition 0.000 description 1
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002221 fluorine Chemical class 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 229910021645 metal ion Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000012066 reaction slurry Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- VKFFEYLSKIYTSJ-UHFFFAOYSA-N tetraazanium;phosphonato phosphate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])(=O)OP([O-])([O-])=O VKFFEYLSKIYTSJ-UHFFFAOYSA-N 0.000 description 1
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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
- C01B25/26—Phosphates
- C01B25/28—Ammonium phosphates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The application discloses a production method of fire-fighting grade monoammonium phosphate, which can improve the purity of an ammonium phosphate dry powder extinguishing agent. The method comprises the following steps: carrying out desulfurization treatment on target dilute phosphoric acid and ore pulp in a phosphoric acid extraction tank; carrying out concentration defluorination treatment on the target dilute phosphoric acid after desulfurization treatment to obtain target concentrated phosphoric acid; carrying out cooling treatment and sedimentation treatment on the target concentrated phosphoric acid, and carrying out impurity removal treatment on the supernatant of the concentrated phosphoric acid with the preset specific gravity after sedimentation treatment to obtain a first filtrate; sending the first filtrate to a neutralization reactor to perform neutralization reaction with ammonia gas to obtain ammoniated slurry; removing impurities from the ammoniated slurry to obtain a second filtrate; sending the second filtrate to a neutralization reactor to perform neutralization reaction with ammonia gas to obtain ammoniated neutralized slurry; concentrating the ammoniated neutralized slurry to obtain concentrated slurry; and carrying out guniting and drying treatment on the concentrated slurry to obtain a finished product.
Description
Technical Field
The application relates to the technical field of phosphorus chemical industry, in particular to a production method of fire-fighting-grade monoammonium phosphate.
Background
Ammonium phosphate dry powder fire extinguishing agent, ABC dry powder fire extinguishing agent for short, is a substitute for Halon material for protecting ozone layer. Wherein the ammonium phosphate dry powder extinguishing agent is mainly divided into three types: dry powder based on ammonium phosphate or ammonium pyrophosphate; mixed dry powder using ammonium phosphate salt or ammonium sulfate salt as base material; dry powder based on ammonium phosphate salts. The ammonium phosphate dry powder extinguishing agent has been widely used due to the characteristics of high extinguishing efficiency, high speed, wide raw material sources, no toxicity to the environment, human and livestock, no need of special power, wide use temperature and the like.
The effects of suffocation, cooling, radiation and chemical inhibition on flaming combustion are the embodiments of the fire extinguishing efficiency of the ammonium phosphate salt dry powder. Where chemical inhibition is the rationale for fire suppression, it serves the primary fire suppression role. Ammonium dihydrogen phosphate decomposes endothermically in the combustion flame into ammonia and phosphoric acid, with subsequent formation of phosphorus pentoxide. Each step of reaction is endothermic reaction, so that the cooling effect is better; the free ammonia produced by decomposition can react with the free radicals produced in the flame combustion reaction, reduce and terminate the free radicals produced by the combustion reaction, and reduce the combustion reaction rate.
At present, the main raw materials for producing the ammonium phosphate dry powder extinguishing agent generally use thermal monoammonium phosphate, the raw materials account for 70-80% of the total cost of the product, and ammonium dihydrogen phosphate in the ammonium phosphate dry powder extinguishing agent produced by using the thermal monoammonium phosphate accounts for a lower proportion, so that the purity of the ammonium phosphate dry powder extinguishing agent is reduced.
Disclosure of Invention
The application provides a production method of fire-fighting grade monoammonium phosphate, which can improve the purity of an ammonium phosphate dry powder extinguishing agent.
The application provides a production method of fire-fighting grade monoammonium phosphate, which is characterized by comprising the following steps:
s1, adding a preset amount of target dilute phosphoric acid and ore pulp into a phosphoric acid extraction tank to obtain phosphorus ore pulp, and performing desulfurization treatment on the phosphorus ore pulp;
s2, carrying out concentration defluorination treatment on the phosphorite slurry subjected to desulfurization treatment in the step S1 to obtain target concentrated phosphoric acid;
s3, cooling and settling the target concentrated phosphoric acid, and removing impurities from the supernatant of the concentrated phosphoric acid with the preset specific gravity through a plate-and-frame filter pressing purification system to obtain a first filtrate;
s4, sending the first filtrate to a neutralization reactor to perform neutralization reaction with ammonia gas to obtain ammoniated slurry;
s5, removing impurities from the ammoniated slurry through a plate-and-frame filter-pressing purification system to obtain a second filtrate;
s6, sending the second filtrate to a neutralization reactor to perform neutralization reaction with ammonia gas to obtain ammoniated neutralized slurry;
s7, concentrating the ammoniated neutralized slurry to obtain concentrated slurry;
and S8, carrying out guniting and drying treatment on the concentrated slurry to obtain a finished product.
Alternatively, the temperature in the desulfurization treatment in step S1 is: at 78-82 ℃, the reaction time is as follows: 30-60 min.
Optionally, the temperature of the temperature reduction process in step S3 is: dropping to below 45 ℃.
Optionally, the specific gravity phosphoric acid supernatant in step S3 is: 1.55 to 1.65.
Optionally, the neutralization degree of the neutralization reaction of the first filtrate and ammonia gas in the step S4 is as follows: 0.2-0.9, and the specific gravity of the neutralized slurry is as follows: 1.45-1.55, the water content of the slurry is: 40-60%, the slurry reaction temperature is: 120 to 135 ℃.
Optionally, the neutralization degree of the neutralization reaction of the second filtrate and ammonia gas in step S6 is: 0.95-1.10, and the specific gravity of the neutralized slurry is as follows: 1.40-1.50, the water content of the slurry is: 25-35%, and the slurry reaction temperature is as follows: 120 to 135 ℃.
Alternatively, the environmental conditions of the concentration process of step S7 are: and performing closed cycle heat exchange between vacuum steam with the pressure not more than 0.5 Mpa.
Alternatively, the temperature in the slurry spray drying process of step S8 is: 200-350 ℃, the pressure is 101KPa, and the drying time is as follows: 5-30 min.
Optionally, the slurry in step S1 is prepared from a concentrate;
the ore pulp fineness range is as follows: 80-100 meshes and 50-200 meshes.
Optionally, in the step S1, the content of P2O5 in the diluted phosphoric acid is: 23 to 26 percent.
According to the technical scheme, the method has the following beneficial effects:
in the application, a preset amount of target dilute phosphoric acid and ore pulp are added into a phosphoric acid extraction tank, a wet-process phosphoric acid extraction method is adopted to carry out desulfurization treatment on the target dilute phosphoric acid, the target dilute phosphoric acid after desulfurization treatment is concentrated and defluorinated to obtain target concentrated phosphoric acid, the target concentrated phosphoric acid is cooled and settled to play a role of primary impurity removal, then the supernatant of the concentrated phosphoric acid with the preset specific gravity after cooling treatment and settling treatment is subjected to impurity removal treatment through a plate-and-frame filter-pressing purification system to obtain a first filtrate, the first filtrate is sent to a neutralization reactor to carry out neutralization reaction with ammonia gas to obtain ammoniated slurry, the ammoniated slurry is subjected to impurity removal treatment through the plate-and-frame filter-pressing purification system to obtain a second filtrate, more impurities are removed through impurity removal treatment twice to improve the purification degree of a finished product, the second filtrate is sent to a neutralization reactor to carry out neutralization reaction with the ammonia gas, and (3) obtaining ammoniated neutralized slurry, concentrating the ammoniated neutralized slurry to obtain concentrated slurry, spraying and drying the concentrated slurry to obtain a finished product, and improving the purity of the ammonium phosphate dry powder extinguishing agent by a wet-process phosphoric acid extraction desulfurization method, phosphoric acid concentration defluorination, phosphoric acid temperature reduction impurity removal and multiple filter pressing impurity removal treatments.
Drawings
FIG. 1 is a schematic diagram of a process for the production of fire-fighting grade monoammonium phosphate in the present application.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the technical solution in the embodiment of the present invention will be clearly and completely described below with reference to the drawings in the embodiment of the present invention, and it is obvious that the described embodiment is only a part of the embodiment of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, shall fall within the scope of the present invention.
In order to solve the technical problem, the application provides a production method of fire-fighting grade monoammonium phosphate, which can improve the purity of the ammonium phosphate dry powder extinguishing agent, and the following examples are specifically referred.
Referring to fig. 1, fig. 1 is a process for producing fire-fighting grade monoammonium phosphate, comprising the steps of:
s1, adding a preset amount of target dilute phosphoric acid and ore pulp into the phosphoric acid extraction tank to obtain phosphorite pulp, and performing desulfurization treatment on the phosphorite pulp;
s2, carrying out concentration defluorination treatment on the phosphorite slurry subjected to desulfurization treatment in the step S1 to obtain target concentrated phosphoric acid;
s3, performing cooling treatment and sedimentation treatment on the target concentrated phosphoric acid, and performing impurity removal treatment on the supernatant of the concentrated phosphoric acid with the preset specific gravity after the cooling treatment and the sedimentation treatment through a plate-and-frame filter pressing purification system to obtain a first filtrate;
s4, sending the first filtrate to a neutralization reactor to perform neutralization reaction with ammonia gas to obtain ammoniated slurry;
s5, removing impurities from the ammoniated slurry through a plate-and-frame filter pressing purification system to obtain a second filtrate;
s6, sending the second filtrate to a neutralization reactor to perform neutralization reaction with ammonia gas to obtain ammoniated neutralized slurry;
s7, concentrating the ammoniated neutralized slurry to obtain concentrated slurry;
and S8, carrying out guniting and drying treatment on the concentrated slurry to obtain a finished product.
Therefore, in the application, the phosphoric acid extraction tank carries out desulfurization by adding the phosphoric ore pulp in a metering manner, the quality of high-quality phosphoric acid provides high-quality raw material guarantee for the production of ammonium fire-fighting phosphate, the dilute phosphoric acid after desulfurization treatment is concentrated and defluorinated, and when the concentration of the phosphoric acid is increased to 48-52 percent P2O5The lowest sulfate radical in phosphoric acid is controlled to be less than 1.5 percent to obtain target concentrated phosphoric acid, impurities such as Fe, Al and the like in the phosphoric acid can form ferric aluminum phosphate salt precipitates in the aging process of the concentrated phosphoric acid, fluorine in the phosphoric acid can also form some fluorine salt precipitates with fine crystal particles, separation is carried out through the concentrated phosphoric acid precipitation, and a phosphoric acid deep purification measure is adopted to improve the purity of the ammonium fire-fighting product. The results of the desulfurization treatment test are shown in Table 1.
TABLE 1 desulfurization treatment test results
The proportion of the adding amount of the dilute phosphoric acid and the ore pulp is based on the added dilute phosphoric acid, and the adding amount of the ore pulp is calculated according to the index of sulfate radical in the dilute phosphoric acid and is 110 percent of the theoretical amount.
The filter-pressing clean system of sheet frame is an edulcoration sediment system equipment, can both effectually get rid of to obvious particulate matter still slight particulate matter, and its theory of operation is: when the device is started to work, the automatic valves AV2 and AV3 are opened, the automatic valve AV1 is closed, the phosphorization liquid containing the slag is pumped into a plate-and-frame filter press by a pump P1 for pressurization and filtration, and the supernatant flows back to the phosphorization tank through filter cloth; after working for a period of time, the phosphorization slag is continuously accumulated in the filter cavity, the resistance is increased, the pressure of the pipeline is increased, and when the preset pressure is reached, the pressure sensor sends out a signal, so that the automatic valve AV1 is opened, and the automatic valve AV2 is closed; then the automatic valve AV4 is opened, the compressed air is automatically introduced for dehydration, after the dehydration reaches the preset time, the automatic valve AV3 is closed, the automatic valve AV4 is closed, the AV5 is opened, and the pressure inside the filter press is released; and then starting a slag unloading program, and enabling the full-automatic slag unloading device to play a role so as to clear the phosphated slag cake from the plate frame and fall into the slag collecting disc, and then automatically pressing the plate frame to start the next working cycle. Because the automation degree of the equipment is higher, the equipment can automatically work without being attended after being started, and in addition, the filter press can be provided with an automatic filter cloth cleaning device, so that the working efficiency can be greatly improved, and the manual operation cost can be reduced; the plate-and-frame filter press has the advantages of simple structure, high integral tightness, large handling capacity, strong circulation, higher filtering precision and lower leakage detection probability, thereby improving the filtering quality. That is, carry out impurity removal treatment through sheet frame filter-pressing clean system to play the effect that further improves fire-fighting ammonium product purity.
The method comprises the steps of performing filter pressing on concentrated phosphoric acid sedimentation supernatant with preset specific gravity and acid temperature within a preset range by using a plate-and-frame filter press, separating solid materials, enabling separated slag to enter filter pressing filter residues and a sedimentation slag acid storage tank, mixing slag acid, stirring, and pumping out a tank area slag acid tank through a pump for adjusting nutrients, wherein a primary purified acid radical after filter pressing is diluted by adding water to the specific gravity within the range of 1.30-1.45 according to the slurry-ammonium pulping effect, so that the high-neutralization-degree preneutralized slurry has good fluidity.
In the invention, a preset amount of target dilute phosphoric acid and ore pulp are added into a phosphoric acid extraction tank, a wet-process phosphoric acid extraction method is adopted to carry out desulfurization treatment on the target dilute phosphoric acid, the target dilute phosphoric acid after desulfurization treatment is concentrated and defluorinated to obtain target concentrated phosphoric acid, the target concentrated phosphoric acid is cooled and settled to play a role of preliminary impurity removal, then the supernatant of the concentrated phosphoric acid with the preset specific gravity after cooling treatment and settling treatment is subjected to impurity removal treatment by a plate-and-frame filter-pressing purification system to obtain a first filtrate, the first filtrate is sent to a neutralization reactor to carry out neutralization reaction with ammonia gas to obtain ammoniated slurry, the ammoniated slurry is subjected to impurity removal treatment by the plate-and-frame filter-pressing purification system to obtain a second filtrate, more impurities are removed by twice impurity removal treatment to improve the purification degree of finished products, the second filtrate is sent to the neutralization reactor to carry out neutralization reaction with the ammonia gas, and (3) obtaining ammoniated neutralized slurry, concentrating the ammoniated neutralized slurry to obtain concentrated slurry, spraying and drying the concentrated slurry to obtain a finished product, and performing wet-process phosphoric acid extraction desulfurization, phosphoric acid concentration defluorination, phosphoric acid temperature reduction impurity removal and multiple filter pressing impurity removal treatments to improve the purity of the ammonium phosphate salt dry powder extinguishing agent. The quality index of the obtained finished product is shown in table 2.
TABLE 2 quality index of the finished product
Alternatively, the temperature in the desulfurization treatment in step S1 is: at 78-82 ℃, the reaction time is as follows: 30-60 min.
Alternatively, P in dilute phosphoric acid in step S12O5The mass content is as follows: 23 to 26 percent.
Optionally, the slurry in step S1 is prepared from a concentrate;
the fineness range of the ore pulp is as follows: 80-100 meshes and 50-200 meshes.
In the production process of wet-process phosphoric acid, excessive sulfuric acid is added to improve the decomposition rate of phosphorite, so that the wet-process phosphoric acid contains excessive sulfate radicals. When phosphoric acid is used for producing calcium hydrogen phosphate, excessive sulfate radicals can generate fine calcium sulfate precipitates to block filter cloth, influence subsequent processes and reduce the quality of products, so the sulfate radicals in the wet-process phosphoric acid must be removed.
In the invention, in order to fully react the ore pulp, the phosphorite is crushed and screened, and then is ground by a ball grinder to prepare the ore pulp, so that the fineness of the ore pulp is between 80 and 100 meshes and between 50 and 200 meshes.
Optionally, the temperature of the temperature reduction process in step S3 is: and dropped to below 45 deg.c.
Optionally, the specific gravity concentrated phosphoric acid supernatant liquid preset in the step S3 is: 1.55 to 1.65.
When a mixture of several soluble solid substances has different solubility in the same solvent or the change trend of the solubility with temperature, the substances can be separated by changing the temperature. In the invention, the impurity is removed by adopting cooling treatment, namely, concentrated phosphoric acid is cooled to be lower than 45 ℃ at normal temperature and normal pressure and naturally settled, so that a large amount of phosphogypsum, iron, aluminum and other metal ion compounds in the concentrated phosphoric acid are precipitated and separated out, thereby obtaining the concentrated phosphoric acid with higher purity, and the supernatant of the settled concentrated phosphoric acid with the specific gravity of about 1.55-1.65 and the acid temperature of lower than 45 ℃ is subjected to impurity removal by utilizing a plate-and-frame filter-pressing purification system.
Optionally, the neutralization degree of the neutralization reaction of the first filtrate and ammonia gas in the step S4 is as follows: 0.2-0.9, and the specific gravity of the neutralized slurry is as follows: 1.45-1.55, the water content of the slurry is: 40-60%, the slurry reaction temperature is: 120 to 135 ℃.
Optionally, the neutralization degree of the neutralization reaction of the second filtrate and ammonia gas in step S6 is: 0.95-1.10, and the specific gravity of the neutralized slurry is as follows: 1.40-1.50, the water content of the slurry is: 25-35%, and the slurry reaction temperature is as follows: 120 to 135 ℃.
In this application, in order to improve the purity of the monoammonium fire fighting product, besides improving the quality of phosphoric acid, the reduction of the neutralization degree of the ammonia-acid slurry is also a key step, and the neutralization degree of the neutralization reaction of the first filtrate and ammonia gas is as follows: 0.2-0.9, and the specific gravity of the neutralized slurry is as follows: 1.45-1.55, the water content of the slurry is: 40% -60%, and the neutralization degree of the second filtrate and ammonia gas neutralization reaction slurry is controlled as follows: 0.95-1.10, and the specific gravity of the neutralized slurry is as follows: 1.40-1.50, the water content of the slurry is: 25% -35%, and the first filtrate and the second filtrate are respectively adopted with different neutralization degrees, neutralization slurry specific gravity and slurry water content when reacting with ammonia gas, so that the neutralized slurry material has good fluidity and the product nutrient moisture is effectively controlled under different reaction conditions.
Alternatively, the environmental conditions of the concentration process of step S7 are: and performing closed cycle heat exchange between vacuum steam with the pressure of not more than 0.5 MPa.
The ammoniated neutralized slurry flows in a preset flow channel after entering a steam room until flowing out in the form of steam or water. The addition of external impurities in the concentration process can be reduced by concentrating under closed circulation heat exchange, so that the purity of concentrated slurry is improved, and the purity of a product is further improved.
Alternatively, the temperature in the slurry spray drying process of step S8 is: 200-350 ℃, the pressure is 101KPa, and the drying time is as follows: 5-30 min.
The following embodiments will be described in further detail with reference to the following examples, which are implemented on the premise of the technology of the present invention, and the detailed embodiments and the specific operation procedures are given to illustrate the inventive concept of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1:
(1) adding target dilute phosphoric acid and ore pulp into a phosphoric acid extraction tank, wherein the target dilute phosphoric acid is converted into 100 percent P2O5The adding amount is 42 tons/hour, the ore pulp is ore pulp containing 35 percent of water, the adding amount is 6 cubic meters/hour to obtain phosphorite pulp, and the phosphorite pulp is subjected to desulfurization treatment at the temperature of 78 ℃, and the desulfurization reaction time is 30 min;
(2) concentrating and defluorinating the phosphorite slurry subjected to desulfurization treatment in the step (1) to obtain target concentrated phosphoric acid;
(3) cooling the target concentrated phosphoric acid to 44 ℃, simultaneously performing natural sedimentation treatment, and performing impurity removal treatment on the supernatant of the concentrated phosphoric acid with the preset specific gravity of 1.55 after cooling treatment and sedimentation treatment through a plate-and-frame filter pressing purification system to obtain a first filtrate;
(4) sending the first filtrate to a neutralization reactor to perform neutralization reaction with ammonia gas at the neutralization degree of 0.2 and the slurry specific gravity of 1.45, the slurry water content of 40 percent and the slurry reaction temperature of 120 ℃ to obtain ammoniated slurry;
(5) removing impurities from the ammoniated slurry through a plate-and-frame filter pressing purification system to obtain a second filtrate;
(6) sending the second filtrate to a neutralization reactor to perform neutralization reaction with ammonia gas at the neutralization degree of 0.95, the specific gravity of the neutralized slurry is 1.40, the water content of the slurry is 25%, and the reaction temperature of the slurry is 120 ℃ to obtain ammoniated neutralized slurry;
(7) carrying out closed cycle heat exchange on ammoniated neutralized slurry in vacuum steam for concentration treatment to obtain concentrated slurry;
(8) and (3) carrying out guniting and drying treatment on the concentrated slurry at the temperature of 200 ℃ and the pressure of 101Kpa for 30min to obtain a finished product.
Example 2:
(1) adding target dilute phosphoric acid and ore pulp into a phosphoric acid extraction tank, wherein the target dilute phosphoric acid is converted into 100 percent P2O5The adding amount is 42 tons/hour, the ore pulp is ore pulp containing 35 percent of water, the adding amount is 10 cubic meters/hour to obtain phosphorite pulp, and the phosphorite pulp is subjected to desulfurization treatment at the temperature of 80 ℃, and the desulfurization reaction time is 32 min;
(2) concentrating and defluorinating the phosphorite slurry subjected to desulfurization treatment in the step (1) to obtain target concentrated phosphoric acid;
(3) cooling the target concentrated phosphoric acid to 42 ℃, simultaneously performing natural sedimentation treatment, and performing impurity removal treatment on the supernatant of the concentrated phosphoric acid with the preset specific gravity of 1.60 after cooling treatment and sedimentation treatment through a plate-and-frame filter pressing purification system to obtain a first filtrate;
(4) sending the first filtrate to a neutralization reactor, reacting with ammonia gas at a neutralization degree of 0.4, a specific gravity of slurry of 1.50, a water content of the slurry of 50%, and a slurry reaction temperature of 125 ℃ to perform neutralization reaction to obtain ammoniated slurry;
(5) removing impurities from the ammoniated slurry through a plate-and-frame filter pressing purification system to obtain a second filtrate;
(6) sending the second filtrate to a neutralization reactor to perform neutralization reaction with ammonia gas at the neutralization degree of 0.98, the specific gravity of neutralized slurry of 1.45, the water content of the slurry of 30 percent and the reaction temperature of the slurry of 125 ℃ to obtain ammoniated neutralized slurry;
(7) carrying out closed cycle heat exchange on ammoniated neutralized slurry in vacuum steam for concentration treatment to obtain concentrated slurry;
(8) and (3) carrying out guniting and drying treatment on the concentrated slurry at the temperature of 220 ℃ and the pressure of 101Kpa for 25min to obtain a finished product.
Although the invention has been illustrated and described with respect to specific embodiments, it should be appreciated that many other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (10)
1. A production method of fire-fighting grade monoammonium phosphate is characterized by comprising the following steps:
s1, adding a preset amount of target dilute phosphoric acid and ore pulp into a phosphoric acid extraction tank to obtain phosphorite pulp, and performing desulfurization treatment on the phosphorite pulp;
s2, carrying out concentration defluorination treatment on the phosphorite slurry subjected to desulfurization treatment in the step S1 to obtain target concentrated phosphoric acid;
s3, cooling and settling the target concentrated phosphoric acid, and removing impurities from the supernatant of the concentrated phosphoric acid with the preset specific gravity through a plate-and-frame filter pressing purification system to obtain a first filtrate;
s4, sending the first filtrate to a neutralization reactor to perform neutralization reaction with ammonia gas to obtain ammoniated slurry;
s5, removing impurities from the ammoniated slurry through a plate-and-frame filter-pressing purification system to obtain a second filtrate;
s6, sending the second filtrate to a neutralization reactor to perform neutralization reaction with ammonia gas to obtain ammoniated neutralized slurry;
s7, concentrating the ammoniated neutralized slurry to obtain concentrated slurry;
and S8, carrying out guniting and drying treatment on the concentrated slurry to obtain a finished product.
2. The production method according to claim 1, wherein the temperature in the desulfurization treatment in step S1 is: at 78-82 ℃, the reaction time is as follows: 30-60 min.
3. The production method according to claim 1, wherein the temperature of the temperature reduction treatment in step S3 is: dropping to below 45 ℃.
4. The production method according to claim 1, wherein the phosphoric acid supernatant of the preset specific gravity in step S3 is: 1.55 to 1.65.
5. The production method according to claim 1, wherein the neutralization degree of the neutralization reaction of the first filtrate and ammonia gas in step S4 is: 0.2-0.9, and the specific gravity of the neutralized slurry is as follows: 1.45-1.55, the water content of the slurry is: 40-60%, the slurry reaction temperature is: 120 to 135 ℃.
6. The production method according to claim 1, wherein the neutralization degree of the neutralization reaction of the second filtrate with ammonia gas in step S6 is: 0.95-1.10, and the specific gravity of the neutralized slurry is as follows: 1.40-1.50, the water content of the slurry is: 25-35%, and the slurry reaction temperature is as follows: 120 to 135 ℃.
7. The production method according to claim 1, wherein the environmental conditions of the concentration process of step S7 are: and performing closed cycle heat exchange between vacuum steam with the pressure not more than 0.5 Mpa.
8. The production method according to any one of claims 1 to 7, wherein the temperature in the slurry-spraying drying process of step S8 is: 200-350 ℃, and the pressure is as follows: 101KPa, drying time: 5-30 min.
9. The production method according to any one of claims 1 to 7, wherein the slurry is prepared from a concentrate in step S1;
the ore pulp fineness ranges are as follows: 80-100 meshes and 50-200 meshes.
10. According to claims 1 to 7The process according to any one of the above processes, wherein P in the diluted phosphoric acid in the step S12O5The mass content is as follows: 23 to 26 percent.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020256A (en) * | 2010-11-22 | 2011-04-20 | 马健 | Method for producing industrial and agricultural monoammonium phosphate and magnesium ammonium phosphate with wet-process phosphoric acid |
| CN102701167A (en) * | 2012-06-13 | 2012-10-03 | 中化化肥有限公司重庆磷复肥工程技术研究中心 | Method for producing industrial ammonium dihydrogen phosphate |
| CN104229764A (en) * | 2014-09-01 | 2014-12-24 | 云南云天化国际化工有限公司 | Method for continuously producing water-soluble monoammonium phosphate by using wet-process phosphoric acid |
| CN106800283A (en) * | 2015-11-26 | 2017-06-06 | 贵州川恒化工股份有限公司 | The production method of powdery fire-fighting level MAP |
| CN107539971A (en) * | 2017-09-12 | 2018-01-05 | 甘肃瓮福化工有限责任公司 | A kind of production technology of MAP |
-
2022
- 2022-04-01 CN CN202210339001.3A patent/CN114735668A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020256A (en) * | 2010-11-22 | 2011-04-20 | 马健 | Method for producing industrial and agricultural monoammonium phosphate and magnesium ammonium phosphate with wet-process phosphoric acid |
| CN102701167A (en) * | 2012-06-13 | 2012-10-03 | 中化化肥有限公司重庆磷复肥工程技术研究中心 | Method for producing industrial ammonium dihydrogen phosphate |
| CN104229764A (en) * | 2014-09-01 | 2014-12-24 | 云南云天化国际化工有限公司 | Method for continuously producing water-soluble monoammonium phosphate by using wet-process phosphoric acid |
| CN106800283A (en) * | 2015-11-26 | 2017-06-06 | 贵州川恒化工股份有限公司 | The production method of powdery fire-fighting level MAP |
| CN107539971A (en) * | 2017-09-12 | 2018-01-05 | 甘肃瓮福化工有限责任公司 | A kind of production technology of MAP |
Non-Patent Citations (1)
| Title |
|---|
| 陈德清;王娜;张敏;神兴明;刘鹏;: "湿法磷酸净化生产工业磷酸一铵研究" * |
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