CN101367672B - Manufacturing method of high concentration enrich superphosphate phosphorus fertilizer - Google Patents
Manufacturing method of high concentration enrich superphosphate phosphorus fertilizer Download PDFInfo
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- CN101367672B CN101367672B CN2008100689305A CN200810068930A CN101367672B CN 101367672 B CN101367672 B CN 101367672B CN 2008100689305 A CN2008100689305 A CN 2008100689305A CN 200810068930 A CN200810068930 A CN 200810068930A CN 101367672 B CN101367672 B CN 101367672B
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Abstract
The invention discloses a manufacturing method of high concentration rich superphosphate fertilizer, which comprises: phosphoric acid is used as raw material, steam is steamed to make the temperature of the phosphoric acid reach 55 to 65 DEG C, then phosphorite powder is added to be mixed, the amount of the phosphorite powder is 105 percent of calculated theoretical calculation amount according to phosphoric acid amount, after mixed reaction with the phosphoric acid in a mixer with 30s, 94 percent to 98 percent sulphuric acid is added, the mixed acid of the amount of the sulphuric acid mixed with the phosphoric acid is 62 percent to 68 percent, the sulphuric acid, the phosphoric acid and the phosphorite powder are severely mixed in a reactor for 1 min, material slurry flows into a turning chemical chamber to be solidified, the solidified time is 30 to 40min, the solidified temperature is 95 DEG C, after piling up and curing, powder-shaped material is added with water for pelleting, and the high concentration rich superphosphate fertilizer is obtained after drying and screening. The manufacturing method has the advantages of simple process flow, little equipment, simple and convenient operation, low manufacturing cost and easy realization of industrial manufacture.
Description
Technical field
The present invention relates to chemical field, relate in particular to a kind of method of producing phosphate fertilizer.
Background technology
Enrich superphosphate phosphorus fertilizer (hereinafter to be referred as rich calcium) can be considered effective P
2O
5The phosphate fertilizer product of content between coarse whiting and calcium superphosphate, normally the acidification reaction by Rock Phosphate (72Min BPL) and sulfuric acid and phosphate mixture makes, and the main component of product is Ca (H
2PO
4)
2H
2O and CaSO
4, next also has a spot of free P
2O
5And H
2O, effectively P
2O
5According to the customer demand difference, mainly contain specification such as 24%, 26%, 28%, 30%, 32%, 34%.Its production method is similar to normal superphosphate, also can produce with the coarse whiting device.
As far back as the twenties, the Soviet Union and the U.S. have just carried out making the research of rich calcium.In the fifties, the development of rich calcium enters the period of great prosperity, and EJFOX etc. have carried out theoretical analysis to the problem of running in the rich calcium production, discusses from selection that calculates water content, mixing acid and concentration the acidifying of sour consumption etc.They find: compare with the result of single acid treatment phosphorus ore, when nitration mixture is handled water content and temperature of reaction all must be controlled at one more among a small circle in.LDYates etc. on this basis to the mixing of phosphoric acid, change into maturing process and carried out comparatively deep research.But these researchs all are based upon with high concentrations of phosphoric acid (about 50%) and the higher concentrate of grade.
Russian patent SU343969 discloses the production method of rich calcium, reduce the phosphoric acid consumption and strengthen ground phosphate rock consumption production double superphosphate, this method phosphoric acid concentration that need raise just can reach when producing rich calcium P2O5 requirement to phosphorus, at sulphur, may be physics when phosphorus nitration mixture and ground phosphate rock are mixing cured is the sposh shape, material is difficult to solidify, can not become powder-like product, adopt rotary drum or disk granulation all to be difficult for producing, need on fluidized-bed, to use the hot-air dry granulation, or the slip spray drying granulation is handled, need to increase drying plant and dry required auxiliary facilitys such as thermal source, thereby improved production cost.
In the patent No. is CN92109010.2, " a kind of production method of enrich superphosphate phosphorus fertilizer " disclosed, detailed process is to be mixed into the nitration mixture that concentration is 64%-70% with 27.02-30% (weight) with 93% or 98% sulfuric acid, treat that its temperature is cooled to 70-80 ℃ and mixes with 90% mistake 100-150 purpose ground phosphate rock, the breeze amount is the 100-102.8% (weight) according to the Theoretical Calculation amount of mixing acid amount calculating, set time 30-60min, curing time 8-12 days, 50 ℃.This method hybrid reaction temperature height, time are longer, and set time is longer, and curing temperature is higher, and this method can only be produced the rich calcium product of lower concentration.
Domestic scholars is coated with quick end, Huo Danqun has carried out the research of decomposing the rich calcium of the peaceful phosphorus ore system in Sichuan with mixture of sulfuric phosphoric acid; Zhang Zhengqing has studied slip solidified control in the rich CAL; Virgin Yun Qing etc. has carried out mixing acid and has decomposed the research that golden river phosphorus ore is produced rich calcium; The extensive production technology of also studying rich calcium of Huang Qing.But their research all is confined to produce the rich calcium of lower concentration, general concentration (effective P
2O
5) can only reach about 24%, and Production Flow Chart is long, and productive expense is higher, operation control difficulty.The rich calcium that China produces at present is confined to w (P more
2O
5Effectively) 20%～30%, relevant w (P
2O
5Effectively) 〉=34% production of the rich calcium of high density and test rarely seen report.
Summary of the invention
A kind of technical process that the objective of the invention is to overcome above-mentioned shortcoming and provide is simple, equipment is few, easy and simple to handle, production cost is low and be easy to realize the production method of the high concentration enrich superphosphate phosphorus fertilizer of suitability for industrialized production.
A kind of production method of high concentration enrich superphosphate phosphorus fertilizer, comprise: be raw material with phosphoric acid, feeding steam makes the phosphoric acid temperature reach 55-65 ℃, adding ground phosphate rock then mixes, the amount of breeze is according to 105% of the Theoretical Calculation amount of phosphoric acid amount calculating, in mixing tank with phosphoric acid hybrid reaction 30s after, add 94%-98% sulfuric acid, the nitration mixture concentration when the vitriolic amount is mixed with phosphoric acid is 62-68%, with sulfuric acid, phosphoric acid and ground phosphate rock acutely mix 1min in reactor after, slip flows into the revolution chamber of changing into and solidifies, be 30-40min set time, and 95 ℃ of solidification values are stored up again, after the slaking, pulverulent material adds water granulation, drying, screening promptly.
The production method of above-mentioned a kind of high concentration enrich superphosphate phosphorus fertilizer, wherein: between the maturation period double superphosphate is carried out turning, every day 1-2 time, curing temperature is 40-45 ℃, curing time 7-10 days.
The production method of above-mentioned a kind of high concentration enrich superphosphate phosphorus fertilizer, wherein: phosphoric acid is raffinate phosphoric acid and sludge phosphoric acid, P
2O
5Content is 40-43%, solid content 2-8%.
The production method of above-mentioned a kind of high concentration enrich superphosphate phosphorus fertilizer, wherein: the effective P of product
2O
534～35%, water-soluble P
2O
5Be more than 30%, free P
2O
5≤ 5%, solubility S5～7%, particle be 2～4mm 〉=90%, mean compressive strength reaches more than the 35N.
The present invention compared with prior art, as can be known from the above technical solutions: use with impure amount, the higher sludge phosphoric acid (perhaps raffinate phosphoric acid) of solid content to be raw material, phosphoric acid concentration is lower, by changing phosphoric acid and vitriolic interpolation order, makes the time of acidification reaction be reduced to 1.5min; What produce fluorine in process of production is distributed as step of reaction 0.012～0.06%, change into chamber 2.62～6.0%, slaking 0.4～1.2 in the warehouse, particulate state (or powdery) product drying 13～18%, cooling, fragmentation, screening etc. 1～4%, residue in the product 71.7～79.1%, escape into gas phase and amount to 17～28.3%, can be by receiving the fluorine system recoveries.And top temperature is lower than 1000 ℃ in producing, and the control of not only save energy, and humidity is proper, does not need to adorn dust removal installation.Effective P of the rich calcium product of the high density that the present invention obtains
2O
534～35%, water-soluble P
2O
5Be more than 30%, solubility S5～7% not only provides abundanter effective P than general calcium
2O
5, and provide abundanter sulfur fertilizer (CaSO than coarse whiting
4.nH
2O).
Embodiment
Embodiment 1
Raw material: 1) phosphoric acid: raffinate phosphoric acid, w (P
2O
5) 42.6%, solid content 4%;
2) sulfuric acid: industrial sulphuric acid, w (H
2SO
4) 98%;
3) ground phosphate rock: chemical constitution following (by weight)
| Form | P 2O 5 | CaO | MgO | SiO 2 | Fe 2O 3 | F | Al 2O 3 | CO 2 | Ore powder granularity-100 order |
| Content (%) | 32.58 | 49.56 | 2.29 | 4.21 | 0.32 | 3.1 | 0.35 | 3.12 | 92.5 |
Contain P
2O
5Be 42.6%, the raffinate phosphoric acid 29.4kg of solid content 4%, measure by under meter, feeding steam makes the phosphoric acid temperature reach 55 ℃, add ground phosphate rock 30kg then, in mixing tank with phosphoric acid hybrid reaction 30s after, add sulfuric acid 7.5kg, with sulfuric acid, phosphoric acid and ground phosphate rock in reactor violent mix 1min after, slip flows into the revolution chamber of changing into and solidifies, and be 35min set time, 95 ℃ of solidification values; Cutter is delivered to the slaking of slaking warehouse with the fresh double superphosphate cutting of solidified after smashing, curing temperature is 45 ℃; Between the maturation period, need carry out turning, every day 1-2 time to double superphosphate; After the slaking 9 days, treat the free P in the sampling analysis work in-process
2O
5Drop to 5-6%, effectively P
2O
5, when index such as moisture meets the requirements, maturing process finishes; After overcuring, pulverulent material adds the water granulation, drying, the screening just can obtain this product, particle be 2～4mm 〉=90%, mean compressive strength reaches more than the 35N, the analytical results of quality product is as follows:
| Rich calcium product | W(P 2O 5 is total)％ | W(P 2O 5 is effective)％ | W(P 2O 5 is water-soluble)％ | W(P 2O 5 is free)％ | W(S)％ | W (moisture) % | Granularity (2-4mm), % |
| Granular | 37.12 | 35.10 | 32.76 | 4.8 | 5.3 | 1.8 | 94.5 |
| Powdery | 36.62 | 34.45 | 32.21 | 5.2 | 5.22 | 4.27 |
Embodiment 2
Raw material: 1) phosphoric acid: raffinate phosphoric acid, w (P
2O
5) 41.4%, solid content 6%;
2) sulfuric acid: industrial sulphuric acid, w (H
2SO
4) 98%;
3) phosphorus ore: chemical constitution following (by weight)
| Form | P 2O 5 | CaO | MgO | SiO 2 | Fe 2O 3 | F | Al 2O 3 | CO 2 | Ore powder granularity-100 order |
| Content (%) | 31.37 | 50.52 | 3.29 | 4.16 | 0.41 | 2.9 | 0.38 | 3.2 | 96.0 |
Contain P
2O
5Be 41.4%, the raffinate phosphoric acid 30.5kg of solid content 6%, measure by under meter, feeding steam makes the phosphoric acid temperature reach 60 ℃, add the ground phosphate rock 30kg of metering in proportion then, in mixing tank with phosphoric acid hybrid reaction 30s after, add the sulfuric acid 7.6kg of metering in proportion, with sulfuric acid, phosphoric acid and ground phosphate rock in reactor violent mix 1min after, slip flows into the revolution chamber of changing into and solidifies, and be 40min set time, 95 ℃ of solidification values.Cutter is delivered to the slaking of slaking warehouse with the fresh double superphosphate cutting of solidified after smashing, curing temperature is 42 ℃.Between the maturation period, need carry out turning, every day 1-2 time to double superphosphate.After the slaking 10 days, treat the free P in the sampling analysis work in-process
2O
5Drop to 5-6%, effectively P
2O
5, when index such as moisture meets the requirements, maturing process finishes.After overcuring, pulverulent material adds the water granulation, drying, the screening just can obtain this product, particle be 2-4mm 〉=90%, mean compressive strength reaches more than the 35N, the analytical results of quality product is as follows
| Rich calcium product | W(P 2O 5 is total)％ | W(P 2O 5 is effective)％ | W(P 2O 5 is water-soluble)％ | W(P 2O 5 is free)％ | W(S)％ | W (moisture) % | Granularity (2-4mm), % |
| Granular | 37.0 | 34.56 | 32.2 | 4.4 | 5.31 | 2.1 | 94.8 |
| Powdery | 36.46 | 34.24 | 31.8 | 5.12 | 5.20 | 4.68 |
Embodiment 3
Raw material: 1) phosphoric acid: sludge phosphoric acid, w (P
2O
5) 40.8%, solid content 8%;
2) sulfuric acid: industrial sulphuric acid, w (H
2SO
4) 98%;
3) phosphorus ore: chemical constitution following (by weight)
| Form | P 2O 5 | CaO | MgO | SiO 2 | Fe 2O 3 | F | Al 2O 3 | CO 2 | Ore powder granularity-100 order |
| Content (%) | 30.82 | 44.28 | 1.25 | 15.36 | 0.36 | 2.88 | 0.52 | 2.96 | 95.0 |
Contain P
2O
5Be 40.8%, the sludge phosphoric acid 31.0kg of solid content 8%, measure by under meter, feeding steam makes the phosphoric acid temperature reach 65 ℃, add the ground phosphate rock 30kg of metering in proportion then, in mixing tank with phosphoric acid hybrid reaction 30s after, add the sulfuric acid 7.5kg of metering in proportion, with sulfuric acid, phosphoric acid and ground phosphate rock in reactor violent mix 1min after, slip flows into the revolution chamber of changing into and solidifies, and be 30min set time, 95 ℃ of solidification values.Cutter is delivered to the slaking of slaking warehouse with the fresh double superphosphate cutting of solidified after smashing, curing temperature is 40 ℃.Between the maturation period, need carry out turning, every day 1-2 time to double superphosphate.After the slaking 7 days, treat the free P in the sampling analysis work in-process
2O
5Drop to 5-6%, effectively P
2O
5, when index such as moisture meets the requirements, maturing process finishes.After overcuring, pulverulent material adds the water granulation, drying, the screening just can obtain this product, particle be 2～4mm 〉=90%, mean compressive strength reaches more than the 35N, the analytical results of quality product is as follows:
| Rich calcium product | W(P 2O 5 is total)％ | W(P 2O 5 is effective)％ | W(P 2O 5 is water-soluble)％ | W(P 2O 5 is free)％ | W(S)％ | W (moisture) % | Granularity (2-4mm), % |
| Granular | 37.2 | 34.34 | 32.0 | 4.36 | 5.26 | 2.2 | 92.6 |
| Powdery | 36.28 | 34.15 | 31.4 | 5.10 | 5.21 | 4.56 |
Claims (3)
1. the production method of a high concentration enrich superphosphate phosphorus fertilizer comprises:
With phosphoric acid is raw material, feeding steam makes the phosphoric acid temperature reach 55-65 ℃, adding ground phosphate rock then mixes, the amount of breeze is according to 105% of the Theoretical Calculation amount of phosphoric acid amount calculating, in mixing tank with phosphoric acid hybrid reaction 30s after, add 94%-98% sulfuric acid, nitration mixture concentration when the vitriolic amount is mixed with phosphoric acid is 62-68%, with sulfuric acid, behind the violent mixing 1min, slip flows into the revolution chamber of changing into and solidifies in reactor for phosphoric acid and ground phosphate rock, and be 30-40min set time, 95 ℃ of solidification values, store up again, after the slaking, pulverulent material adds water granulation, drying, screening promptly.
2. the production method of a kind of high concentration enrich superphosphate phosphorus fertilizer as claimed in claim 1, it is characterized in that: between the maturation period double superphosphate is carried out turning, every day 1-2 time, curing temperature is 40-45 ℃, curing time 7-10 days.
3. the production method of a kind of high concentration enrich superphosphate phosphorus fertilizer as claimed in claim 1 or 2, it is characterized in that: phosphoric acid is raffinate phosphoric acid and sludge phosphoric acid, P
2O
5Content is 40-43%, solid content 2-8%.
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| CN101367672B true CN101367672B (en) | 2010-12-15 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583289B (en) * | 2012-02-10 | 2013-05-22 | 瓮福（集团）有限责任公司 | Method of producing triple superphosphate by using raffinate acid resulted from phosphoric acid purification |
| WO2014045301A2 (en) * | 2012-08-30 | 2014-03-27 | Indo Gulf Fertilizers | A process for preparing phosphates from rock phosphate |
| CN104071757B (en) * | 2014-07-16 | 2016-08-24 | 云南常青树化工有限公司 | A kind of preparation method of double superphosphate |
| CN104692836B (en) * | 2015-03-31 | 2017-09-08 | 防城港盛农磷化有限公司 | The calcium superphosphate slurry preparation method and its production equipment of single many oar stirring curings of groove |
| CN104788131A (en) * | 2015-04-29 | 2015-07-22 | 铜陵化学工业集团有限公司 | Method for producing superphosphate by utilizing low-grade phosphate ore mixed acid process |
| CN106242644A (en) * | 2016-08-15 | 2016-12-21 | 瓮福（集团）有限责任公司 | A kind of preparation method of normal superphosphate |
| CN106380231A (en) * | 2016-08-30 | 2017-02-08 | 甘肃瓮福化工有限责任公司 | Method for producing calcium superphosphate with phosphate rock tailings and phosphoric acid sludge |
| CN106699453A (en) * | 2016-12-18 | 2017-05-24 | 贵州越都化工有限公司 | Enriched superphosphate and preparation method for same |
| CN109593003A (en) * | 2019-01-31 | 2019-04-09 | 云南云天化以化磷业研究技术有限公司 | A kind of production method improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer |
| CN111606739A (en) * | 2020-06-17 | 2020-09-01 | 云南磷化集团海口磷业有限公司 | Sulfur-containing enriched calcium superphosphate production device and preparation method |
| CN114773122A (en) * | 2022-03-25 | 2022-07-22 | 云南磷化集团海口磷业有限公司 | Sulfur-coated calcium superphosphate rich in medium and trace elements and preparation method thereof |
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