CN105439646A - Method for producing phosphorus magnesia fertilizer by using wet phosphoric acid residues - Google Patents
Method for producing phosphorus magnesia fertilizer by using wet phosphoric acid residues Download PDFInfo
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Abstract
The present invention discloses a method for producing a phosphorus magnesia fertilizer by using wet phosphoric acid residues. Further liquid-solid separation of remaining acid from wet phosphoric acid is performed by using pressing filtration, and the obtained supernatant acid is used for production of high level phosphorus ammonium or a compound fertilizer. A filter cake is filtered, and the washing solution is sent to a reaction tank of wet phosphoric acid apparatus for use; powdery magnesia that contains available magnesium and is alkaline is added into the solid phase to neutralize the acid; and the free acid content is reduced to be lower than 5%; then the phosphorus magnesia fertilizer product containing both available phosphorus and available magnesium is produced. The method disclosed by the present inventive is simple in process and good in economic benefit, and the product of a granular shape or a powdery shape can be directly applied, or the product can be used as a raw material for producing a compound-mixed fertilizer. Effective P2O5 contained in the product contains 10-35% of water soluble P2O5, 65-90% of citric acid soluble phosphorus, and the product also contains 1-15% of MgO. The balance supply of crop nutrition is facilitated, the absorption of the crop on phosphorus is promoted, the utilization rate of phosphorus in the fertilizer and the fertilizer efficiency are increased, and the crop quality is improved, so that the method has a good application prospect.
Description
Technical field
The invention belongs to the phosphate fertilizer in chemical fertilizer, production of compound fertilizer technical field, relate to the recycling of the phosphoric acid slag produced in Wet-process Phosphoric Acid Production, specifically relate to a kind of method utilizing phosphoric acid by wet process slag to produce phosphorus fertiliser containing magnesium.
Background technology
Wet-process Phosphoric Acid Production, when carrying out solid-liquor separation (filter, wash) to reaction slurry, inevitably has partial solid phase phosphogypsum and wears filter, enter in liquid phase dilute phosphoric acid; In wet-process phosphoric acid concentration process, along with moisture evaporation, a large amount of amounts of insoluble iron, aluminium, magnesium phosphoric acid salt are separated out in supersaturation; When producing the high-concentration phosphate compound fertilizerses such as premium grads diammonium phosphate, need to carry out ageing, clarification to wet method strong phosphoric acid, in ageing, clarifying process, along with temperature declines, time lapse, constantly can separate out again, produce phosphoric acid postprecipitation salt.Wet method strong phosphoric acid clarifying process, the solid formation that said process produces to be separated as much as possible exactly and enter clarifying tank underflow, namely be called in the industry in what acid (or the acid of what slag), to guarantee that in the clear acid in upper strata, solid formation content is lower, produce total nutrient and water-soluble phosphorus accounts for available phosphorus ratio product up to standard.
In recent years, along with phosphate rock resource dilution, quality declines, and in phosphorus ore, the foreign matter content such as iron, aluminium, magnesium rises, and the what acid number amount produced during the clarification of wet method strong phosphoric acid is comparatively large, and what acid rises to 0.30 ~ 0.40:1.0 with the ratio of clear acid.The clear acid in upper strata is mainly used to produce premium grads diammonium phosphate (or monoammonium phosphate) and other high-concentration compound fertilizer product.The acid of underflow what, is mainly used to the products such as production inferior grade diammonium phosphate (monoammonium phosphate), coarse whiting, rich calcium at present.In recent years, inferior grade diammonium phosphate (monoammonium phosphate) market outlet is bad, and the produce market such as coarse whiting, rich calcium is unstable again, brings difficulty to the digestibility and utilization of what acid, Some Enterprises is forced to stop production because of the what swollen groove of acid, also there is risk of environmental pollution.How to utilize what acid economically, produce phosphate fertilizer, Chemical Mixed Fertilizer product innovation, just become the major issue that phosphoric acid by wet process, high-concentration phosphate compound fertilizers industry are urgently to be resolved hurrily.
Magnesium is one of main composition composition of plant materials inner chlorophyll, and it can be grown by Promoting plant growth, is the necessary important moderate-element of plant growth.And magnesium and phosphorus have stronger synergistic effect, the existence of magnesium, obviously can promote that crop is to the absorption of phosphorus, improves crop yield and quality, improves fertilizer efficiency and the absorption rate of phosphate fertilizer.
Summary of the invention
The object of the invention is to the deficiency for existing phosphoric acid by wet process slag Application way, a kind of method utilizing phosphoric acid by wet process slag to produce phosphorus fertiliser containing magnesium is provided.Adopt in magnesium oxide (being commonly called as magnesia) and the free acid of phosphoric acid by wet process slag, generate primary magnesium phosphate and/or phosphoric acid hydrogen two magnesium, obtain a kind of New Phosphorus compound fertilizer containing available phosphorus (based on citric acid soluble phosphorus, also having a small amount of water-soluble phosphorus) and the efficient oxidation magnesium.
Object of the present invention is achieved by the following technical programs.
Except as otherwise noted, percentage ratio of the present invention is mass percent.
A kind of method utilizing phosphoric acid by wet process slag to produce phosphorus fertiliser containing magnesium, it is characterized in that: solid-liquor separation is carried out to the acid of phosphoric acid by wet process what, filter cake obtains phosphoric acid slag through washing, add powdery magnesia in the ratio of phosphoric acid slag and magnesia mass ratio 100:1.5 ~ 25, mix, neutralize, after granulation, drying, obtain granular phosphorus fertiliser containing magnesium product again.
Or phosphoric acid slag is mixed with magnesia, neutralize, pile postpone and obtain powdery phosphorus fertiliser containing magnesium product.
The sour solid content for obtaining in phosphoric acid by wet process clarifying process of described phosphoric acid by wet process what is the underflow what acid of 10 ~ 40%.
Described solid-liquor separation preferably adopts pressure filter to carry out.
The clear acid that the solid content obtained after solid-liquor separation is less than 3.0%, for the production of more premium grads diammonium phosphate or monoammonium phosphate, and other high-concentration compound fertilizer product.
The washing lotion produced during filter cake washing is sent wet-process phosphoric acid reaction groove back to and is reclaimed.
Described granulation adopts roller pelletizer or granulating disc.
Thinking of the present invention is: by press filtration to phosphoric acid by wet process what acid solid-liquor separation further, the clear acid obtained is for the production of premium grads diammonium phosphate, monoammonium phosphate etc.Filter cake is through washing, and washing lotion is delivered to Wet Phosphoric Acid Plant reactive tank and utilized, and washs the solid formation and phosphoric acid slag that obtain, its effective P
2o
5content (butt) is general between 20 ~ 38%, free acid (P
2o
5meter) content (butt) about 5 ~ 25%, can damage crop, directly can not be used as fertilizer.So add be rich in effective magnesium and be again alkalescence powdery magnesia phosphoric acid by wet process slag is neutralized, by free acid (P
2o
5meter) content is reduced to less than 5%, and then produce the granular phosphorus fertiliser containing magnesium product simultaneously containing available phosphorus and effective magnesium through granulation, drying; Or do not carry out granulation after neutralization, obtain powdery phosphorus fertiliser containing magnesium product.
Relative to prior art, the present invention has the following advantages:
1, present invention process is simple, practical, efficient, and no matter good product performance, be granular or powder-like product all can directly be used, and also can be used as the raw material producing Chemical Mixed Fertilizer, has good market application foreground.
The contained effectively P of the phosphorus fertiliser containing magnesium of 2, producing
2o
5in, 10 ~ 35% is water-soluble P
2o
5(quick-acting phosphorus), 65 ~ 90% is citric acid soluble phosphorus (slow phosphorus), and product also contains effective MgO of 1 ~ 15%, be conducive to the balance supply of crop alimentary, utilize, promote that crop is to the absorption of phosphorus, improve utilization ratio and the fertilizer efficiency of phosphorus in fertilizer, improve crop quality.
3, to the underflow what acid obtained in phosphoric acid by wet process clarifying process, carry out solid-liquor separation further, how clear acid can be obtained, and then more premium grads diammonium phosphate complex fertilizer products such as (or) monoammonium phosphates can be produced, increase economic benefit.
4, the present invention only simply need transform the compound fertilizer facility of existing manufacturing enterprise, can realize producing, and has obvious economic benefit and environmental benefit.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
Embodiment 1
As shown in Figure 1, getting the solid content obtained in phosphoric acid by wet process clarifying process is that press filtration is carried out in 10 ~ 40% underflow what acid, and liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces other compound fertilizer of high concentration such as premium grads diammonium phosphate or monoammonium phosphate.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns wet-process phosphoric acid reaction groove.After washing, obtain effective P
2o
5be the phosphoric acid slag of 25%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:8 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 23.15%, water-soluble P
2o
5: 5.79%, free P
2o
5: 0.00%, effective MgO:6.85%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 22.11%, water-soluble P
2o
5: 5.53%, free P
2o
5: 0.00%, effective MgO:6.54%, free H
2o:7.50%.
Embodiment 2
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 25%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:5 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 23.81%, water-soluble P
2o
5: 7.14%, free P
2o
5: 0.00%, effective MgO:4.76%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 22.74%, water-soluble P
2o
5: 6.82%, free P
2o
5: 0.00%, effective MgO:4.55%, free H
2o:7.50%.
Embodiment 3
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 25%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:1.5 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 24.63%, water-soluble P
2o
5: 8.62%, free P
2o
5: 3.50%, effective MgO:2.17%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 23.52%, water-soluble P
2o
5: 8.23%, free P
2o
5: 3.34%, effective MgO:2.07%, free H
2o:7.50%.
Embodiment 4
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 25%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:12 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 22.32%, water-soluble P
2o
5: 4.46%, free P
2o
5: 0.00%, effective MgO:9.46%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 21.32%, water-soluble P
2o
5: 4.26%, free P
2o
5: 0.00%, effective MgO:9.04%, free H
2o:7.50%.
Embodiment 5
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 25%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:18 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 21.19%, water-soluble P
2o
5: 3.18%, free P
2o
5: 0.00%, effective MgO:13.05%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 20.23%, water-soluble P
2o
5: 3.03%, free P
2o
5: 0.00%, effective MgO:12.46%, free H
2o:7.50%.
Embodiment 6
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 25%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:25 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 20.00%, water-soluble P
2o
5: 2.00%, free P
2o
5: 0.00%, effective MgO:16.80%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 19.10%, water-soluble P
2o
5: 1.91%, free P
2o
5: 0.00%, effective MgO:16.04%, free H
2o:7.50%.
Embodiment 7
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 32%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:8 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 29.63%, water-soluble P
2o
5: 7.41%, free P
2o
5: 0.00%, effective MgO:6.67%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 28.15%, water-soluble P
2o
5: 7.04%, free P
2o
5: 0.00%, effective MgO:6.33%, free H
2o:8.00%.
Embodiment 8
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 32%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:5 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 30.48%, water-soluble P
2o
5: 9.14%, free P
2o
5: 1.20%, effective MgO:4.57%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 28.95%, water-soluble P
2o
5: 8.69%, free P
2o
5: 1.14%, effective MgO:4.34%, free H
2o:8.00%.
Embodiment 9
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 32%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:1.5 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 31.53%, water-soluble P
2o
5: 11.03%, free P
2o
5: 4.50%, effective MgO:1.97%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 29.95%, water-soluble P
2o
5: 10.48%, free P
2o
5: 4.28%, effective MgO:1.87%, free H
2o:8.00%.
Embodiment 10
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 32%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:12 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 28.57%, water-soluble P
2o
5: 5.71%, free P
2o
5: 0.00%, effective MgO:9.29%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 27.14%, water-soluble P
2o
5: 5.43%, free P
2o
5: 0.00%, effective MgO:8.82%, free H
2o:8.00%.
Embodiment 11
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 32%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:18 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 27.12%, water-soluble P
2o
5: 4.07%, free P
2o
5: 0.00%, effective MgO:12.88%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 25.76%, water-soluble P
2o
5: 3.86%, free P
2o
5: 0.00%, effective MgO:12.24%, free H
2o:8.00%.
Embodiment 12
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 32%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:25 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 25.60%, water-soluble P
2o
5: 2.56%, free P
2o
5: 0.00%, effective MgO:16.64%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 24.32%, water-soluble P
2o
5: 2.43%, free P
2o
5: 0.00%, effective MgO:15.81%, free H
2o:8.00%.
Embodiment 13
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 38%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:8 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 35.19%, water-soluble P
2o
5: 8.80%, free P
2o
5: 0.00%, effective MgO:6.48%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 33.25%, water-soluble P
2o
5: 8.31%, free P
2o
5: 0.00%, effective MgO:6.13%, free H
2o:8.50%.
Embodiment 14
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 38%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:5 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 36.19%, water-soluble P
2o
5: 10.86%, free P
2o
5: 1.50%, effective MgO:4.38%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 34.20%, water-soluble P
2o
5: 10.26%, free P
2o
5: 1.42%, effective MgO:4.14%, free H
2o:8.50%.
Embodiment 15
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 38%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:1.5 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 37.44%, water-soluble P
2o
5: 13.10%, free P
2o
5: 4.90%, effective MgO:1.77%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 35.38%, water-soluble P
2o
5: 12.38%, free P
2o
5: 4.63%, effective MgO:1.68%, free H
2o:8.50%.
Embodiment 16
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 38%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:12 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 33.93%, water-soluble P
2o
5: 6.79%, free P
2o
5: 0.00%, effective MgO:9.11%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 32.06%, water-soluble P
2o
5: 6.41%, free P
2o
5: 0.00%, effective MgO:8.61%, free H
2o:8.50%.
Embodiment 17
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 38%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:18 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 32.20%, water-soluble P
2o
5: 4.83%, free P
2o
5: 0.00%, effective MgO:12.71%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 30.43%, water-soluble P
2o
5: 4.56%, free P
2o
5: 0.00%, effective MgO:12.01%, free H
2o:8.50%.
Embodiment 18
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 38%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:25 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P
2o
5: 30.40%, water-soluble P
2o
5: 3.04%, free P
2o
5: 0.00%, effective MgO:16.48%, free H
2o:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P
2o
5: 28.73%, water-soluble P
2o
5: 2.87%, free P
2o
5: 0.00%, effective MgO:15.57%, free H
2o:8.50%.
Embodiment 19
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 20%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:8 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P2O5:18.52%, water-soluble P_2O_5: 4.63%, free P2O5: 0.00%, effective MgO:6.85%, free H2O:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P2O5:17.69%, water-soluble P_2O_5: 4.42%, free P2O5: 0.00%, effective MgO:6.54%, free H2O:7.50%.
Embodiment 20
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 20%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:5 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P2O5:19.05%, water-soluble P_2O_5: 5.71%, free P2O5: 0.00%, effective MgO:4.76%, free H2O:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P2O5:18.19%, water-soluble P_2O_5: 5.46%, free P2O5: 0.00%, effective MgO:4.55%, free H2O:7.50%.
Embodiment 21
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 20%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:1.5 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P2O5:19.70%, water-soluble P_2O_5: 6.90%, free P2O5: 3.50%, effective MgO:2.17%, free H2O:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P2O5:18.82%, water-soluble P_2O_5: 6.59%, free P2O5: 3.34%, effective MgO:2.07%, free H2O:7.50%.
Embodiment 22
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 20%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:12 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P2O5:17.86%, water-soluble P_2O_5: 3.57%, free P2O5: 0.00%, effective MgO:9.46%, free H2O:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P2O5:17.05%, water-soluble P_2O_5: 3.41%, free P2O5: 0.00%, effective MgO:9.04%, free H2O:7.50%.
Embodiment 23
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 20%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:18 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P2O5:16.95%, water-soluble P_2O_5: 2.54%, free P2O5: 0.00%, effective MgO:13.05%, free H2O:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P2O5:16.19%, water-soluble P_2O_5: 2.43%, free P2O5: 0.00%, effective MgO:12.46%, free H2O:7.50%.
Embodiment 24
As shown in Figure 1, get solid content be 10 ~ 40% the acid of phosphoric acid by wet process slag carry out press filtration, liquid phase is the clear acid that solid content is less than 3.0%, sends to and produces premium grads diammonium phosphate other compound fertilizer of high concentration such as (or) monoammonium phosphates.Filter-press residues (being commonly called as filter cake) washs with water, and washings returns phosphoric acid extraction reactive tank.After washing, obtain effective P
2o
5be the phosphoric acid slag of 20%, add magnesia in the ratio of phosphoric acid slag and magnesia 100:25 (mass ratio), stir, mix, deliver to tablets press and carry out granulation, then carry out drying, cooling, metering packing, obtain granular phosphorus fertiliser containing magnesium finished product.Product analysis result is as follows: effectively P2O5:16.00%, water-soluble P_2O_5: 1.60%, free P2O5: 0.00%, effective MgO:16.80%, free H2O:3.00%.
During not granulation, reaction of banking up, obtain powdery phosphorus fertiliser containing magnesium product, product analysis result is as follows: effectively P2O5:15.28%, water-soluble P_2O_5: 1.53%, free P2O5: 0.00%, effective MgO:16.04%, free H2O:7.50%.
Claims (6)
1. the method utilizing phosphoric acid by wet process slag to produce phosphorus fertiliser containing magnesium, it is characterized in that: solid-liquor separation is carried out to the acid of phosphoric acid by wet process what, filter cake obtains phosphoric acid slag through washing, add powdery magnesia in the ratio of phosphoric acid slag and magnesia mass ratio 100:1.5 ~ 25, mix, neutralize, after granulation, drying, obtain granular phosphorus fertiliser containing magnesium product again; Or phosphoric acid slag is mixed with magnesia, neutralize, pile postpone and obtain powdery phosphorus fertiliser containing magnesium product.
2. the method utilizing phosphoric acid by wet process slag to produce phosphorus fertiliser containing magnesium according to claim 1, is characterized in that: the sour solid content for obtaining in phosphoric acid by wet process clarifying process of described phosphoric acid by wet process what is the underflow what acid of 10 ~ 40%.
3. the method utilizing phosphoric acid by wet process slag to produce phosphorus fertiliser containing magnesium according to claim 1, is characterized in that: described solid-liquor separation preferably adopts pressure filter to carry out.
4. the method utilizing phosphoric acid by wet process slag to produce phosphorus fertiliser containing magnesium according to claim 1, is characterized in that: through washing its effective P of phosphoric acid slag obtained
2o
5content is 20 ~ 38%.
5. the method utilizing phosphoric acid by wet process slag to produce phosphorus fertiliser containing magnesium according to claim 1, it is characterized in that: the clear acid that the solid content obtained after solid-liquor separation is less than 3.0%, for the production of premium grads diammonium phosphate or monoammonium phosphate, and other high-concentration compound fertilizer product.
6. the method utilizing phosphoric acid by wet process slag to produce phosphorus fertiliser containing magnesium according to claim 1, is characterized in that: the washing lotion produced during filter cake washing is sent wet-process phosphoric acid reaction groove back to and reclaimed.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106831053A (en) * | 2017-02-10 | 2017-06-13 | 云南三环中化化肥有限公司 | A kind of production method of graininess, function intensified type phosphorus containing magnesium ammonium |
| CN111018571A (en) * | 2019-11-22 | 2020-04-17 | 中国农业大学 | Method for activating and utilizing low-grade phosphate ore |
| CN113277885A (en) * | 2021-06-09 | 2021-08-20 | 四川大学 | Resource utilization method of phosphoric acid residues |
| CN115626841A (en) * | 2022-11-07 | 2023-01-20 | 云南云天化股份有限公司 | Preparation method of calcium-magnesium-rich citrate soluble phosphate fertilizer special for macadamia nuts |
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| CN106831053A (en) * | 2017-02-10 | 2017-06-13 | 云南三环中化化肥有限公司 | A kind of production method of graininess, function intensified type phosphorus containing magnesium ammonium |
| CN111018571A (en) * | 2019-11-22 | 2020-04-17 | 中国农业大学 | Method for activating and utilizing low-grade phosphate ore |
| CN113277885A (en) * | 2021-06-09 | 2021-08-20 | 四川大学 | Resource utilization method of phosphoric acid residues |
| CN115626841A (en) * | 2022-11-07 | 2023-01-20 | 云南云天化股份有限公司 | Preparation method of calcium-magnesium-rich citrate soluble phosphate fertilizer special for macadamia nuts |
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