CN113955731A - Preparation method of granular feed-grade monocalcium phosphate - Google Patents
Preparation method of granular feed-grade monocalcium phosphate Download PDFInfo
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- CN113955731A CN113955731A CN202111493919.5A CN202111493919A CN113955731A CN 113955731 A CN113955731 A CN 113955731A CN 202111493919 A CN202111493919 A CN 202111493919A CN 113955731 A CN113955731 A CN 113955731A
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- phosphoric acid
- tank
- monocalcium phosphate
- mixing
- pump
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- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 title claims abstract description 81
- 235000019691 monocalcium phosphate Nutrition 0.000 title claims abstract description 81
- 239000001506 calcium phosphate Substances 0.000 title claims abstract description 42
- 229910000150 monocalcium phosphate Inorganic materials 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 284
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 142
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 229940062672 calcium dihydrogen phosphate Drugs 0.000 claims abstract description 39
- 229910000389 calcium phosphate Inorganic materials 0.000 claims abstract description 39
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 24
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000012545 processing Methods 0.000 claims abstract description 10
- 238000000746 purification Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 87
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 54
- 238000002156 mixing Methods 0.000 claims description 54
- 238000003860 storage Methods 0.000 claims description 41
- 239000011575 calcium Substances 0.000 claims description 39
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 36
- 229960005069 calcium Drugs 0.000 claims description 36
- 229910052791 calcium Inorganic materials 0.000 claims description 36
- 238000005086 pumping Methods 0.000 claims description 35
- 238000012216 screening Methods 0.000 claims description 35
- 238000001035 drying Methods 0.000 claims description 33
- 238000003682 fluorination reaction Methods 0.000 claims description 28
- 238000001704 evaporation Methods 0.000 claims description 26
- 230000008020 evaporation Effects 0.000 claims description 26
- 239000000428 dust Substances 0.000 claims description 25
- 230000032683 aging Effects 0.000 claims description 21
- 238000006115 defluorination reaction Methods 0.000 claims description 20
- 239000003795 chemical substances by application Substances 0.000 claims description 19
- 229910052742 iron Inorganic materials 0.000 claims description 18
- 239000011347 resin Substances 0.000 claims description 18
- 229920005989 resin Polymers 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 18
- 230000002431 foraging effect Effects 0.000 claims description 14
- 238000003825 pressing Methods 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 13
- 238000004806 packaging method and process Methods 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 13
- -1 ferric trichloride modified zeolite Chemical class 0.000 claims description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000005453 pelletization Methods 0.000 claims description 7
- 239000013049 sediment Substances 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 7
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 7
- 229910021536 Zeolite Inorganic materials 0.000 claims description 6
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 6
- 238000007602 hot air drying Methods 0.000 claims description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 239000010457 zeolite Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 11
- 239000011574 phosphorus Substances 0.000 abstract description 11
- 241001465754 Metazoa Species 0.000 abstract description 4
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 abstract description 3
- 235000019700 dicalcium phosphate Nutrition 0.000 abstract description 3
- 241000276489 Merlangius merlangus Species 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 26
- 238000010586 diagram Methods 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 3
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 229910052785 arsenic Inorganic materials 0.000 description 3
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 3
- 229910052793 cadmium Inorganic materials 0.000 description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 241000251468 Actinopterygii Species 0.000 description 2
- 241000238557 Decapoda Species 0.000 description 2
- 239000003674 animal food additive Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/26—Compounds containing phosphorus
-
- 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
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/327—After-treatment
Abstract
The invention discloses a preparation method of granular feed-grade monocalcium phosphate, which comprises the following steps: 1) raw material purification, 2) preparation of monocalcium phosphate; 3) processing the granulated monocalcium phosphate; the content of water-soluble phosphorus in the granular calcium dihydrogen phosphate finished product produced by the method is controlled to be stable and controlled to be 17-18 wt%, the content of residual calcium carbonate is less than or equal to 1 wt%, and the content of free acid is less than 1.0 wt%, which fully indicates that the reaction completeness of the phosphoric acid, calcium hydrogen phosphate and coarse whiting is high; meanwhile, the product is granular, has good fluidity, is convenient for producing compound feed, and has high biological value of animals.
Description
Technical Field
The invention relates to the technical field of processing, in particular to a preparation method of granular feed-grade monocalcium phosphate.
Background
The feed-grade monocalcium phosphate is an excellent high-efficiency phosphate feed additive, has high phosphorus content and high water solubility, and is an excellent supplement for phosphorus and calcium of animals. The biological value of the feed-grade phosphate is highest, the feed-grade phosphate is particularly suitable for fish and shrimp aquatic animals, the utilization rate of calcium dihydrogen phosphate of the fish and shrimp is as high as 94-98%, and the utilization rate of phosphorus in calcium hydrogen phosphate is only 50%, so the feed-grade calcium dihydrogen phosphate plays an important role in developing aquatic products, and the feed additive of the variety is widely used at home and abroad.
Through market research, 17% -18% of granular feed-grade calcium hydrophosphate has certain market demand and stable customers, and meanwhile, 17% -18% of granular feed-grade calcium hydrophosphate has certain price advantage compared with powdery feed-grade calcium hydrophosphate, and in order to meet the market demand, a preparation method for quickly producing granular feed-grade calcium hydrophosphate in batches is needed.
Disclosure of Invention
The invention provides a preparation method of granular feed-grade monocalcium phosphate.
The scheme of the invention is as follows:
a preparation method of granular feed-grade monocalcium phosphate comprises the following steps:
1) raw material purification, namely conveying purchased concentrated phosphoric acid into a crude phosphoric acid underground pump tank, and pumping the concentrated phosphoric acid into a crude phosphoric acid storage tank through a crude phosphoric acid underground pump; the phosphoric acid in the crude phosphoric acid storage tank flows into a crude phosphoric acid underground pump tank through a bottom valve; then adjusting a three-way valve at the outlet of a crude phosphoric acid underground pump, pumping phosphoric acid in a crude phosphoric acid storage tank into a filter press through a crude phosphoric acid pump, carrying out filter pressing separation on sediments in the crude phosphoric acid, enabling separated filtrate to flow into a de-weighting reaction tank through a chute for de-weighting, adding sodium sulfide into the de-weighting reaction tank for reaction, recovering and washing tail gas generated by the reaction, pumping the de-weighted phosphoric acid into a de-fluorination reaction tank through the de-weighting phosphoric acid pump tank, adding a defluorinating agent into the de-fluorination reaction tank for defluorination reaction, pumping into the filter press through a de-fluorination phosphoric acid pump for filter pressing after defluorination is finished, enabling the filter-pressed fine phosphoric acid to flow into the de-fluorination phosphoric acid tank through the chute, and then pumping into a fine phosphoric acid storage tank through the pump;
2) preparing monocalcium phosphate, namely adding a finished calcium hydrophosphate product and heavy calcium carbonate powder into a bucket elevator in proportion through a bin and a metering screw respectively, uniformly mixing the calcium hydrophosphate and the heavy calcium carbonate in an input calcium hydrophosphate bin, inputting the uniformly mixed material into a mixing reaction tank through the metering screw, mixing and reacting the uniformly mixed material with the fine phosphoric acid metered and taken out from the step 1), feeding the reacted material into an aging chamber for aging, transferring the aged material to an aging site for aging by using a loader after the aging is finished, and simultaneously uniformly mixing the aged material with a returned calcium hydrophosphate returned to a system through a returned material; after the mixing is finished, carrying out flash evaporation drying, packaging, metering and checking to obtain powdery monocalcium phosphate; coarse granular calcium dihydrogen phosphate generated in the flash evaporation drying process is conveyed to a material returning system for curing and mixing after being screened and crushed;
3) the processing contains the process of graininess calcium dihydrogen phosphate, pelletizes the raw materials after step 2) qualified powdery calcium dihydrogen phosphate mixes with the auxiliary material, and the pelletization is accomplished and is carried out primary plastic, once sieves after the primary plastic is accomplished, once sieves and carries out secondary screening, the secondary screening is sieved for graininess feed level calcium dihydrogen phosphate, the primary screening is not sieved and carries out secondary plastic, carry out secondary screening afterwards, the secondary screening is not sieved is added in the middle of the auxiliary material.
As a preferable technical scheme, the tail gas in the step 1) is recovered and washed by absorbing the tail gas through a draught fan, and the tail gas is sent to a washing tower through a circulating pump tank and is washed and then discharged.
As a preferable technical scheme, the mixing reaction in the step 2) and the gas and dust generated in the process need to be washed, recovered and discharged.
As a preferable technical scheme, the material mixed in the step 2) is subjected to flash evaporation and drying, then is sent into a cyclone for cyclone dust removal, the separated powder is subjected to Goll dust removal and is sent into a storage bin for packaging, the miscellaneous materials subjected to cyclone dust removal and treatment are sieved, and the coarse granular calcium dihydrogen phosphate which is not sieved is sent into the storage bin through the sieving, is crushed and then is conveyed to a return system for curing and material mixing.
As a preferable technical scheme, the defluorinating agent comprises active silica, diatomite, alumina, iron-loaded resin and zeolite modified by ferric trichloride.
According to a preferable technical scheme, the defluorination agent comprises active silica, diatomite, alumina, iron-loaded resin and ferric trichloride modified zeolite, and the mass ratio of the active silica to the diatomite to the alumina to the iron-loaded resin to the ferric trichloride modified zeolite is 30-40: 10-15: 8-11: 20-26: 3-7.
As an optimal technical scheme, the inlet of the flash evaporation drying is 300-400 ℃, and the outlet is 50-60 ℃.
As a preferred technical scheme, the flash drying provides hot air drying through a hot-blast stove.
Due to the adoption of the technical scheme, the preparation method of the granular feed-grade monocalcium phosphate comprises the following steps: 1) raw material purification, namely conveying purchased concentrated phosphoric acid into a crude phosphoric acid underground pump tank, and pumping the concentrated phosphoric acid into a crude phosphoric acid storage tank through a crude phosphoric acid underground pump; the phosphoric acid in the crude phosphoric acid storage tank flows into a crude phosphoric acid underground pump tank through a bottom valve; then adjusting a three-way valve at the outlet of a crude phosphoric acid underground pump, pumping phosphoric acid in a crude phosphoric acid storage tank into a filter press through a crude phosphoric acid pump, carrying out filter pressing separation on sediments in the crude phosphoric acid, enabling separated filtrate to flow into a de-weighting reaction tank through a chute for de-weighting, adding sodium sulfide into the de-weighting reaction tank for reaction, recovering and washing tail gas generated by the reaction, pumping the de-weighted phosphoric acid into a de-fluorination reaction tank through the de-weighting phosphoric acid pump tank, adding a defluorinating agent into the de-fluorination reaction tank for defluorination reaction, pumping into the filter press through a de-fluorination phosphoric acid pump for filter pressing after defluorination is finished, enabling the filter-pressed fine phosphoric acid to flow into the de-fluorination phosphoric acid tank through the chute, and then pumping into a fine phosphoric acid storage tank through the pump; 2) preparing monocalcium phosphate, namely adding a finished calcium hydrophosphate product and heavy calcium carbonate powder into a bucket elevator in proportion through a bin and a metering screw respectively, uniformly mixing the calcium hydrophosphate and the heavy calcium carbonate in an input calcium hydrophosphate bin, inputting the uniformly mixed material into a mixing reaction tank through the metering screw, mixing and reacting the uniformly mixed material with the fine phosphoric acid metered and taken out from the step 1), feeding the reacted material into an aging chamber for aging, transferring the aged material to an aging site for aging by using a loader after the aging is finished, and simultaneously uniformly mixing the aged material with a returned calcium hydrophosphate returned to a system through a returned material; after the mixing is finished, carrying out flash evaporation drying, packaging, metering and checking to obtain powdery monocalcium phosphate; coarse granular calcium dihydrogen phosphate generated in the flash evaporation drying process is conveyed to a material returning system for curing and mixing after being screened and crushed; 3) the processing contains the process of graininess calcium dihydrogen phosphate, pelletizes the raw materials after step 2) qualified powdery calcium dihydrogen phosphate mixes with the auxiliary material, and the pelletization is accomplished and is carried out primary plastic, once sieves after the primary plastic is accomplished, once sieves and carries out secondary screening, the secondary screening is sieved for graininess feed level calcium dihydrogen phosphate, the primary screening is not sieved and carries out secondary plastic, carry out secondary screening afterwards, the secondary screening is not sieved is added in the middle of the auxiliary material.
The invention has the beneficial effects that:
the content of water-soluble phosphorus in the granular calcium dihydrogen phosphate finished product produced by the method is controlled to be stable and controlled to be 17-18 wt%, the content of residual calcium carbonate is less than or equal to 1 wt%, and the content of free acid is less than 1.0 wt%, which fully indicates that the reaction completeness of the phosphoric acid, calcium hydrogen phosphate and coarse whiting is high; meanwhile, the product is granular, has good fluidity, is convenient for producing compound feed, and has high biological value of animals.
The caking is not easy, and the storage is facilitated; the invention has simple operation and control, low drying energy consumption and low production cost; the method is environment-friendly and energy-saving, and generates little dust with little influence on the environment; and can be recycled.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a diagram of a feedstock purification framework in an example of the present invention;
FIG. 2 is a diagram of the upper half of the preparation of monocalcium phosphate in an embodiment of the present invention;
FIG. 3 is a bottom half frame diagram of the preparation of monocalcium phosphate in an embodiment of the present invention;
FIG. 4 is a block diagram of a process for processing a granular calcium dihydrogen phosphate-containing material according to an embodiment of the present invention.
Detailed Description
In order to make up for the above deficiencies, the present invention provides a method for preparing granular feed grade monocalcium phosphate to solve the above problems in the background art.
A preparation method of granular feed-grade monocalcium phosphate comprises the following steps:
1) raw material purification, namely conveying purchased concentrated phosphoric acid into a crude phosphoric acid underground pump tank, and pumping the concentrated phosphoric acid into a crude phosphoric acid storage tank through a crude phosphoric acid underground pump; the phosphoric acid in the crude phosphoric acid storage tank flows into a crude phosphoric acid underground pump tank through a bottom valve; then adjusting a three-way valve at the outlet of a crude phosphoric acid underground pump, pumping phosphoric acid in a crude phosphoric acid storage tank into a filter press through a crude phosphoric acid pump, carrying out filter pressing separation on sediments in the crude phosphoric acid, enabling separated filtrate to flow into a de-weighting reaction tank through a chute for de-weighting, adding sodium sulfide into the de-weighting reaction tank for reaction, recovering and washing tail gas generated by the reaction, pumping the de-weighted phosphoric acid into a de-fluorination reaction tank through the de-weighting phosphoric acid pump tank, adding a defluorinating agent into the de-fluorination reaction tank for defluorination reaction, pumping into the filter press through a de-fluorination phosphoric acid pump for filter pressing after defluorination is finished, enabling the filter-pressed fine phosphoric acid to flow into the de-fluorination phosphoric acid tank through the chute, and then pumping into a fine phosphoric acid storage tank through the pump;
2) preparing monocalcium phosphate, namely adding a finished calcium hydrophosphate product and heavy calcium carbonate powder into a bucket elevator in proportion through a bin and a metering screw respectively, uniformly mixing the calcium hydrophosphate and the heavy calcium carbonate in an input calcium hydrophosphate bin, inputting the uniformly mixed material into a mixing reaction tank through the metering screw, mixing and reacting the uniformly mixed material with the fine phosphoric acid metered and taken out from the step 1), feeding the reacted material into an aging chamber for aging, transferring the aged material to an aging site for aging by using a loader after the aging is finished, and simultaneously uniformly mixing the aged material with a returned calcium hydrophosphate returned to a system through a returned material; after the mixing is finished, carrying out flash evaporation drying, packaging, metering and checking to obtain powdery monocalcium phosphate; coarse granular calcium dihydrogen phosphate generated in the flash evaporation drying process is conveyed to a material returning system for curing and mixing after being screened and crushed;
3) the processing contains the process of graininess calcium dihydrogen phosphate, pelletizes the raw materials after step 2) qualified powdery calcium dihydrogen phosphate mixes with the auxiliary material, and the pelletization is accomplished and is carried out primary plastic, once sieves after the primary plastic is accomplished, once sieves and carries out secondary screening, the secondary screening is sieved for graininess feed level calcium dihydrogen phosphate, the primary screening is not sieved and carries out secondary plastic, carry out secondary screening afterwards, the secondary screening is not sieved is added in the middle of the auxiliary material.
The tail gas in the step 1) is recovered and washed by absorbing the tail gas through a draught fan, and the tail gas is sent into a washing tower through a circulating pump tank to be washed and then discharged.
The mixing reaction in the step 2) and the gas and dust generated in the process need to be washed, recovered and discharged.
And 2) after flash evaporation and drying are carried out on the mixed materials in the step 2), the mixed materials are sent into a cyclone for cyclone dust removal, the separated powder materials are subjected to Goll dust removal and sent into a storage bin for packaging, the mixed materials subjected to cyclone dust removal treatment are sieved and sent into the storage bin, and the coarse granular calcium dihydrogen phosphate which does not pass through the sieving is crushed and then is conveyed to a return system for curing and mixing.
The defluorinating agent comprises active silicon dioxide, diatomite, alumina, iron-loaded resin and zeolite modified by ferric trichloride.
The defluorination agent comprises active silica, diatomite, alumina, iron-loaded resin and ferric trichloride modified zeolite, and the mass ratio of the active silica to the diatomite to the iron-loaded resin to the ferric trichloride modified zeolite is 30-40: 10-15: 8-11: 20-26: 3-7.
The inlet of the flash evaporation drying is 300-400 ℃, and the outlet is 50-60 ℃.
The flash drying provides hot air drying through a hot-blast stove.
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1
A preparation method of granular feed-grade monocalcium phosphate comprises the following steps:
1) raw material purification, namely conveying purchased concentrated phosphoric acid into a crude phosphoric acid underground pump tank, and pumping the concentrated phosphoric acid into a crude phosphoric acid storage tank through a crude phosphoric acid underground pump; the phosphoric acid in the crude phosphoric acid storage tank flows into a crude phosphoric acid underground pump tank through a bottom valve; then adjusting a three-way valve at the outlet of a crude phosphoric acid underground pump, pumping phosphoric acid in a crude phosphoric acid storage tank into a filter press through a crude phosphoric acid pump, carrying out filter pressing separation on sediments in the crude phosphoric acid, enabling separated filtrate to flow into a de-weighting reaction tank through a chute for de-weighting, adding sodium sulfide into the de-weighting reaction tank for reaction, recovering and washing tail gas generated by the reaction, pumping the de-weighted phosphoric acid into a de-fluorination reaction tank through the de-weighting phosphoric acid pump tank, adding a defluorinating agent into the de-fluorination reaction tank for defluorination reaction, pumping into the filter press through a de-fluorination phosphoric acid pump for filter pressing after defluorination is finished, enabling the filter-pressed fine phosphoric acid to flow into the de-fluorination phosphoric acid tank through the chute, and then pumping into a fine phosphoric acid storage tank through the pump;
2) preparing monocalcium phosphate, namely adding a finished calcium hydrophosphate product and heavy calcium carbonate powder into a bucket elevator in proportion through a bin and a metering screw respectively, uniformly mixing the calcium hydrophosphate and the heavy calcium carbonate in an input calcium hydrophosphate bin, inputting the uniformly mixed material into a mixing reaction tank through the metering screw, mixing and reacting the uniformly mixed material with the fine phosphoric acid metered and taken out from the step 1), feeding the reacted material into an aging chamber for aging, transferring the aged material to an aging site for aging by using a loader after the aging is finished, and simultaneously uniformly mixing the aged material with a returned calcium hydrophosphate returned to a system through a returned material; after the mixing is finished, carrying out flash evaporation drying, packaging, metering and checking to obtain powdery monocalcium phosphate; coarse granular calcium dihydrogen phosphate generated in the flash evaporation drying process is conveyed to a material returning system for curing and mixing after being screened and crushed;
3) the processing contains the process of graininess calcium dihydrogen phosphate, pelletizes the raw materials after step 2) qualified powdery calcium dihydrogen phosphate mixes with the auxiliary material, and the pelletization is accomplished and is carried out primary plastic, once sieves after the primary plastic is accomplished, once sieves and carries out secondary screening, the secondary screening is sieved for graininess feed level calcium dihydrogen phosphate, the primary screening is not sieved and carries out secondary plastic, carry out secondary screening afterwards, the secondary screening is not sieved is added in the middle of the auxiliary material.
The tail gas in the step 1) is recovered and washed by absorbing the tail gas through a draught fan, and the tail gas is sent into a washing tower through a circulating pump tank to be washed and then discharged.
The mixing reaction in the step 2) and the gas and dust generated in the process need to be washed, recovered and discharged.
And 2) after flash evaporation and drying are carried out on the mixed materials in the step 2), the mixed materials are sent into a cyclone for cyclone dust removal, the separated powder materials are subjected to Goll dust removal and sent into a storage bin for packaging, the mixed materials subjected to cyclone dust removal treatment are sieved and sent into the storage bin, and the coarse granular calcium dihydrogen phosphate which does not pass through the sieving is crushed and then is conveyed to a return system for curing and mixing.
The defluorinating agent comprises active silicon dioxide, diatomite, alumina, iron-loaded resin and zeolite modified by ferric trichloride.
The defluorination agent comprises active silicon dioxide, diatomite, alumina, iron-loaded resin and ferric trichloride modified zeolite, and the mass ratio of the active silicon dioxide to the diatomite to the iron-loaded resin to the ferric trichloride modified zeolite is 30:10:8:20: 3.
The inlet of the flash evaporation drying is 300-400 ℃, and the outlet is 50-60 ℃.
The flash drying provides hot air drying through a hot-blast stove.
The quality indexes of the granular monocalcium phosphate product produced by the above method are shown in the following table 1:
| item | Index (I) |
| Phosphorus (P) content/%) | ≥17 |
| Content of citrate soluble phosphorus (P)/%) | ≥16 |
| Calcium (Ca) content/%) | ≥21 |
| Fluorine (F) content/ppm | ≤1600 |
| Arsenic (As) content/ppm | ≤20 |
| Lead (Pb) content/ppm | ≤20 |
| Cadmium (Cd) content/ppm | ≤10 |
| Particle size (0.2-2 mm test sieve)/%) | ≥90 |
Example 2
A preparation method of granular feed-grade monocalcium phosphate comprises the following steps:
1) raw material purification, namely conveying purchased concentrated phosphoric acid into a crude phosphoric acid underground pump tank, and pumping the concentrated phosphoric acid into a crude phosphoric acid storage tank through a crude phosphoric acid underground pump; the phosphoric acid in the crude phosphoric acid storage tank flows into a crude phosphoric acid underground pump tank through a bottom valve; then adjusting a three-way valve at the outlet of a crude phosphoric acid underground pump, pumping phosphoric acid in a crude phosphoric acid storage tank into a filter press through a crude phosphoric acid pump, carrying out filter pressing separation on sediments in the crude phosphoric acid, enabling separated filtrate to flow into a de-weighting reaction tank through a chute for de-weighting, adding sodium sulfide into the de-weighting reaction tank for reaction, recovering and washing tail gas generated by the reaction, pumping the de-weighted phosphoric acid into a de-fluorination reaction tank through the de-weighting phosphoric acid pump tank, adding a defluorinating agent into the de-fluorination reaction tank for defluorination reaction, pumping into the filter press through a de-fluorination phosphoric acid pump for filter pressing after defluorination is finished, enabling the filter-pressed fine phosphoric acid to flow into the de-fluorination phosphoric acid tank through the chute, and then pumping into a fine phosphoric acid storage tank through the pump;
2) preparing monocalcium phosphate, namely adding a finished calcium hydrophosphate product and heavy calcium carbonate powder into a bucket elevator in proportion through a bin and a metering screw respectively, uniformly mixing the calcium hydrophosphate and the heavy calcium carbonate in an input calcium hydrophosphate bin, inputting the uniformly mixed material into a mixing reaction tank through the metering screw, mixing and reacting the uniformly mixed material with the fine phosphoric acid metered and taken out from the step 1), feeding the reacted material into an aging chamber for aging, transferring the aged material to an aging site for aging by using a loader after the aging is finished, and simultaneously uniformly mixing the aged material with a returned calcium hydrophosphate returned to a system through a returned material; after the mixing is finished, carrying out flash evaporation drying, packaging, metering and checking to obtain powdery monocalcium phosphate; coarse granular calcium dihydrogen phosphate generated in the flash evaporation drying process is conveyed to a material returning system for curing and mixing after being screened and crushed;
3) the processing contains the process of graininess calcium dihydrogen phosphate, pelletizes the raw materials after step 2) qualified powdery calcium dihydrogen phosphate mixes with the auxiliary material, and the pelletization is accomplished and is carried out primary plastic, once sieves after the primary plastic is accomplished, once sieves and carries out secondary screening, the secondary screening is sieved for graininess feed level calcium dihydrogen phosphate, the primary screening is not sieved and carries out secondary plastic, carry out secondary screening afterwards, the secondary screening is not sieved is added in the middle of the auxiliary material.
The tail gas in the step 1) is recovered and washed by absorbing the tail gas through a draught fan, and the tail gas is sent into a washing tower through a circulating pump tank to be washed and then discharged.
The mixing reaction in the step 2) and the gas and dust generated in the process need to be washed, recovered and discharged.
And 2) after flash evaporation and drying are carried out on the mixed materials in the step 2), the mixed materials are sent into a cyclone for cyclone dust removal, the separated powder materials are subjected to Goll dust removal and sent into a storage bin for packaging, the mixed materials subjected to cyclone dust removal treatment are sieved and sent into the storage bin, and the coarse granular calcium dihydrogen phosphate which does not pass through the sieving is crushed and then is conveyed to a return system for curing and mixing.
The defluorinating agent comprises active silicon dioxide, diatomite, alumina, iron-loaded resin and zeolite modified by ferric trichloride.
The defluorination agent comprises active silicon dioxide, diatomite, alumina, iron-loaded resin and ferric trichloride modified zeolite, and the mass ratio of the active silicon dioxide to the diatomite to the iron-loaded resin to the ferric trichloride modified zeolite is 40:15:11:26: 7.
The inlet of the flash evaporation drying is 300-400 ℃, and the outlet is 50-60 ℃.
The flash drying provides hot air drying through a hot-blast stove.
The quality indexes of the granular monocalcium phosphate product produced by the above method are shown in the following table 2:
| item | Index (I) |
| Phosphorus (P) content/%) | ≥18 |
| Content of citrate soluble phosphorus (P)/%) | ≥17 |
| Calcium (Ca) content/%) | ≥22 |
| Fluorine (F) content/ppm | ≤1600 |
| Arsenic (As) content/ppm | ≤20 |
| Lead (Pb) content/ppm | ≤20 |
| Cadmium (Cd) content/ppm | ≤10 |
| Particle size (0.2-2 mm test sieve)/%) | ≥90 |
。
Example 3
A preparation method of granular feed-grade monocalcium phosphate comprises the following steps:
1) raw material purification, namely conveying purchased concentrated phosphoric acid into a crude phosphoric acid underground pump tank, and pumping the concentrated phosphoric acid into a crude phosphoric acid storage tank through a crude phosphoric acid underground pump; the phosphoric acid in the crude phosphoric acid storage tank flows into a crude phosphoric acid underground pump tank through a bottom valve; then adjusting a three-way valve at the outlet of a crude phosphoric acid underground pump, pumping phosphoric acid in a crude phosphoric acid storage tank into a filter press through a crude phosphoric acid pump, carrying out filter pressing separation on sediments in the crude phosphoric acid, enabling separated filtrate to flow into a de-weighting reaction tank through a chute for de-weighting, adding sodium sulfide into the de-weighting reaction tank for reaction, recovering and washing tail gas generated by the reaction, pumping the de-weighted phosphoric acid into a de-fluorination reaction tank through the de-weighting phosphoric acid pump tank, adding a defluorinating agent into the de-fluorination reaction tank for defluorination reaction, pumping into the filter press through a de-fluorination phosphoric acid pump for filter pressing after defluorination is finished, enabling the filter-pressed fine phosphoric acid to flow into the de-fluorination phosphoric acid tank through the chute, and then pumping into a fine phosphoric acid storage tank through the pump;
2) preparing monocalcium phosphate, namely adding a finished calcium hydrophosphate product and heavy calcium carbonate powder into a bucket elevator in proportion through a bin and a metering screw respectively, uniformly mixing the calcium hydrophosphate and the heavy calcium carbonate in an input calcium hydrophosphate bin, inputting the uniformly mixed material into a mixing reaction tank through the metering screw, mixing and reacting the uniformly mixed material with the fine phosphoric acid metered and taken out from the step 1), feeding the reacted material into an aging chamber for aging, transferring the aged material to an aging site for aging by using a loader after the aging is finished, and simultaneously uniformly mixing the aged material with a returned calcium hydrophosphate returned to a system through a returned material; after the mixing is finished, carrying out flash evaporation drying, packaging, metering and checking to obtain powdery monocalcium phosphate; coarse granular calcium dihydrogen phosphate generated in the flash evaporation drying process is conveyed to a material returning system for curing and mixing after being screened and crushed;
3) the processing contains the process of graininess calcium dihydrogen phosphate, pelletizes the raw materials after step 2) qualified powdery calcium dihydrogen phosphate mixes with the auxiliary material, and the pelletization is accomplished and is carried out primary plastic, once sieves after the primary plastic is accomplished, once sieves and carries out secondary screening, the secondary screening is sieved for graininess feed level calcium dihydrogen phosphate, the primary screening is not sieved and carries out secondary plastic, carry out secondary screening afterwards, the secondary screening is not sieved is added in the middle of the auxiliary material.
The tail gas in the step 1) is recovered and washed by absorbing the tail gas through a draught fan, and the tail gas is sent into a washing tower through a circulating pump tank to be washed and then discharged.
The mixing reaction in the step 2) and the gas and dust generated in the process need to be washed, recovered and discharged.
And 2) after flash evaporation and drying are carried out on the mixed materials in the step 2), the mixed materials are sent into a cyclone for cyclone dust removal, the separated powder materials are subjected to Goll dust removal and sent into a storage bin for packaging, the mixed materials subjected to cyclone dust removal treatment are sieved and sent into the storage bin, and the coarse granular calcium dihydrogen phosphate which does not pass through the sieving is crushed and then is conveyed to a return system for curing and mixing.
The defluorinating agent comprises active silicon dioxide, diatomite, alumina, iron-loaded resin and zeolite modified by ferric trichloride.
The defluorination agent comprises active silicon dioxide, diatomite, alumina, iron-loaded resin and ferric trichloride modified zeolite, and the mass ratio of the active silicon dioxide to the diatomite to the iron-loaded resin to the ferric trichloride modified zeolite is 35:12:9:22: 5.
The inlet of the flash evaporation drying is 300-400 ℃, and the outlet is 50-60 ℃.
The flash drying provides hot air drying through a hot-blast stove.
The quality indexes of the granular monocalcium phosphate product produced by the above method are shown in the following table 3:
| item | Index (I) |
| Phosphorus (P) content/%) | ≥17 |
| Content of citrate soluble phosphorus (P)/%) | ≥18 |
| Calcium (Ca) content/%) | ≥24 |
| Fluorine (F) content/ppm | ≤1200 |
| Arsenic (As) content/ppm | ≤10 |
| Lead (Pb) content/ppm | ≤15 |
| Cadmium (Cd) content/ppm | ≤10 |
| Particle size (0.2-2 mm test sieve)/%) | ≥90 |
。
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A preparation method of granular feed-grade monocalcium phosphate is characterized by comprising the following steps:
1) raw material purification, namely conveying purchased concentrated phosphoric acid into a crude phosphoric acid underground pump tank, and pumping the concentrated phosphoric acid into a crude phosphoric acid storage tank through a crude phosphoric acid underground pump; the phosphoric acid in the crude phosphoric acid storage tank flows into a crude phosphoric acid underground pump tank through a bottom valve; then adjusting a three-way valve at the outlet of a crude phosphoric acid underground pump, pumping phosphoric acid in a crude phosphoric acid storage tank into a filter press through a crude phosphoric acid pump, carrying out filter pressing separation on sediments in the crude phosphoric acid, enabling separated filtrate to flow into a de-weighting reaction tank through a chute for de-weighting, adding sodium sulfide into the de-weighting reaction tank for reaction, recovering and washing tail gas generated by the reaction, pumping the de-weighted phosphoric acid into a de-fluorination reaction tank through the de-weighting phosphoric acid pump tank, adding a defluorinating agent into the de-fluorination reaction tank for defluorination reaction, pumping into the filter press through a de-fluorination phosphoric acid pump for filter pressing after defluorination is finished, enabling the filter-pressed fine phosphoric acid to flow into the de-fluorination phosphoric acid tank through the chute, and then pumping into a fine phosphoric acid storage tank through the pump;
2) preparing monocalcium phosphate, namely adding a finished calcium hydrophosphate product and heavy calcium carbonate powder into a bucket elevator in proportion through a bin and a metering screw respectively, uniformly mixing the calcium hydrophosphate and the heavy calcium carbonate in an input calcium hydrophosphate bin, inputting the uniformly mixed material into a mixing reaction tank through the metering screw, mixing and reacting the uniformly mixed material with the fine phosphoric acid metered and taken out from the step 1), feeding the reacted material into an aging chamber for aging, transferring the aged material to an aging site for aging by using a loader after the aging is finished, and simultaneously uniformly mixing the aged material with a returned calcium hydrophosphate returned to a system through a returned material; after the mixing is finished, carrying out flash evaporation drying, packaging, metering and checking to obtain powdery monocalcium phosphate; coarse granular calcium dihydrogen phosphate generated in the flash evaporation drying process is conveyed to a material returning system for curing and mixing after being screened and crushed;
3) the processing contains the process of graininess calcium dihydrogen phosphate, pelletizes the raw materials after step 2) qualified powdery calcium dihydrogen phosphate mixes with the auxiliary material, and the pelletization is accomplished and is carried out primary plastic, once sieves after the primary plastic is accomplished, once sieves and carries out secondary screening, the secondary screening is sieved for graininess feed level calcium dihydrogen phosphate, the primary screening is not sieved and carries out secondary plastic, carry out secondary screening afterwards, the secondary screening is not sieved is added in the middle of the auxiliary material.
2. The method for preparing granular feed-grade monocalcium phosphate as claimed in claim 1, wherein the tail gas in step 1) is recovered and washed by a draught fan, and the tail gas is sent to a washing tower through a circulating pump tank and is washed and discharged.
3. The process for preparing granular feed grade monocalcium phosphate as claimed in claim 1, wherein: the mixing reaction in the step 2) and the gas and dust generated in the process need to be washed, recovered and discharged.
4. The process for preparing granular feed grade monocalcium phosphate as claimed in claim 1, wherein: and 2) after flash evaporation and drying are carried out on the mixed materials in the step 2), the mixed materials are sent into a cyclone for cyclone dust removal, the separated powder materials are subjected to Goll dust removal and sent into a storage bin for packaging, the mixed materials subjected to cyclone dust removal treatment are sieved and sent into the storage bin, and the coarse granular calcium dihydrogen phosphate which does not pass through the sieving is crushed and then is conveyed to a return system for curing and mixing.
5. The process for preparing granular feed grade monocalcium phosphate as claimed in claim 1, wherein: the defluorinating agent comprises active silicon dioxide, diatomite, alumina, iron-loaded resin and zeolite modified by ferric trichloride.
6. The process for producing granular feed grade monocalcium phosphate as claimed in claim 5, wherein: the defluorination agent comprises active silica, diatomite, alumina, iron-loaded resin and ferric trichloride modified zeolite, and the mass ratio of the active silica to the diatomite to the iron-loaded resin to the ferric trichloride modified zeolite is 30-40: 10-15: 8-11: 20-26: 3-7.
7. The process for producing granular feed grade monocalcium phosphate as claimed in claim 2, wherein: the inlet of the flash evaporation drying is 300-400 ℃, and the outlet is 50-60 ℃.
8. The process for preparing granular feed grade monocalcium phosphate as claimed in claim 7, wherein: the flash drying provides hot air drying through a hot-blast stove.
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