CN109593003A - A kind of production method improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer - Google Patents
A kind of production method improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer Download PDFInfo
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- CN109593003A CN109593003A CN201910095327.4A CN201910095327A CN109593003A CN 109593003 A CN109593003 A CN 109593003A CN 201910095327 A CN201910095327 A CN 201910095327A CN 109593003 A CN109593003 A CN 109593003A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B17/00—Other phosphatic fertilisers, e.g. soft rock phosphates, bone meal
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Abstract
The present invention provides a kind of production method for improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer, include the following steps: (1) hybrid reaction: by 10%~40% that ureasulfuric acid dosage is citric acid soluble phosphorus fertilizer amount, it is added in citrate acid soluble phosphatic fertilizer, 60~90 DEG C of hybrid reaction temperature, 50~90min of hybrid reaction, obtains material A；(2) solidify: material A solidifies 60~120min, obtains material B at 50~60 DEG C；(3) cure: material B cures 1~3 day at 45~55 DEG C, obtains compound fertilizer's head product.The present invention is mixed using ureasulfuric acid with citrate acid soluble phosphatic fertilizer, and the hydrogen ion, acid ion after ureasulfuric acid dissociation make citric acid soluble phosphorus be converted into water-soluble phosphorus, and urea is complexed with water-soluble phosphorus again, obtains the water-soluble phosphorus of complex status.After handling citrate acid soluble phosphatic fertilizer using the method for the present invention, water-soluble phosphorus content effectively improves in fertilizer；And simple process and low cost.
Description
Technical field
The invention belongs to technical field of fertilizer production, are specifically related to a kind of life for improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer
Production method.
Background technique
Citrate acid soluble phosphatic fertilizer also known as weak acid dissolubility phosphate fertilizer, are a kind of fertilizer for being relatively insoluble in water, and one kind is not easy to be absorbed by plants
Fertilizer, thus phosphorus utilization is very low, is unfavorable for its application in agricultural.
During Wet-process Phosphoric Acid Production, the impurity part of phosphorus ore association enters phosphoric acid, causes miscellaneous in phosphoric acid by wet process
Matter content is higher, need to remove or reduce the related impurities in phosphoric acid according to the difference of production product.Utilize Wet-process Phosphoric Acid Production water
During dissolubility compound fertilizer, phosphoric acid is handled with removal of impurities using in ammonia, generates a large amount of by-product filter residues in the dedoping step, wherein
Citric acid soluble phosphorus accounts for the 60~90% of total phosphorus；By-product filter residue can be used as citrate acid soluble phosphatic fertilizer and sell, but is further processed and utilizes, energy
Obtain better economic benefit.Wherein P in the filter residue of water soluble composite fertilizer by-product2O5Content is 20~45%, in conjunction with ureasulfuric acid
Afterwards, improve water-soluble phosphorus content, can be used as a kind of acid compound fertilizer and use, also can be used as factory formula fertilizer or in, low concentration it is multiple
The raw material in Hefei；Fundamentally widen the use scope of filter residue.
Chinese patent it is a kind of by Chinese holly Soluble phosphorus be converted into water-soluble phosphorus method (application number: 201610664630.8), wherein Chinese holly
Soluble phosphorus refers to filter residue or solution containing Chinese holly Soluble phosphorus, and Chinese holly Soluble phosphorus filter residue is from Wet-process Phosphoric Acid Production industrial grade phosphate or Quan Shui
When the products such as dissolubility compound fertilizer, in ammonia and in removal of impurities industrial process.Chinese holly Soluble phosphorus is mixed with sulfuric acid, nitric acid in patent, is being activated
It reacts to obtain mixed slurry under the action of agent (neopelex mixes in proportion with ammonium nitrate), adds stabilization
Agent obtains stable water-soluble phosphorus slurry, so that Chinese holly Soluble phosphorus be made to be converted into water-soluble phosphorus.Though Chinese holly Soluble phosphorus can be partially converted by the patent
Water-soluble phosphorus, but the neopelex foaming power in the activator added is strong, it is unfavorable to reacting；Activator is added in the process
With stabilizer increased costs, water-soluble phosphorus slurry is obtained, later use process is connected, long flow path is unfavorable for industrialized production.
Summary of the invention
The present invention in view of the deficiency of the prior art, provides a kind of life for improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer
Production method, after handling citrate acid soluble phosphatic fertilizer using this method, water-soluble phosphorus content effectively improves in fertilizer；And simple process,
It is at low cost.
Unless otherwise indicated, percentage of the present invention is mass fraction.
The purpose of the present invention is achieved by the following technical programs:
A kind of production method improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer, includes the following steps:
(3) hybrid reaction: being the 10%~40%, preferably 20%~30% of citric acid soluble phosphorus fertilizer amount by ureasulfuric acid dosage,
It is added in citrate acid soluble phosphatic fertilizer, 60~90 DEG C of hybrid reaction temperature, preferably 70~80 DEG C, 50~90min of hybrid reaction obtain object
Expect A；
(4) solidify: material A solidifies 60~120min, obtains material B at 50~60 DEG C；
(3) cure: material B cures 1~3 day at 45~55 DEG C, obtains compound fertilizer's head product.
In ureasulfuric acid of the present invention, 0.92~2.2:1 of mass ratio of solid urea and sulfuric acid, preferably 1.07~
1.38: 1, temperature when configuring ureasulfuric acid remains 80~90 DEG C.
Water-soluble phosphorus accounts for available phosphorus (P in the citrate acid soluble phosphatic fertilizer2O5Content) ratio be 25%~40%.
In (1) step of the invention, compound fertilizer's head product can also be directly obtained with 4.5~6.5h of hybrid reaction.
Water-soluble phosphorus accounts for available phosphorus (P in compound fertilizer's head product that the present invention obtains2O5Content) ratio be 65%~85%.
Ureasulfuric acid dosage is the 10%~40% of citric acid soluble phosphorus fertilizer amount in the present invention.Less than 10%, reaction mass is in dosage
Solid-state, and citric acid soluble phosphorus conversion ratio is low；Dosage is greater than 40%, dilutes total active constituent content, and contain free acid in material
It measures higher；Therefore it is feasible for selecting dosage is citric acid soluble phosphorus fertilizer amount 10%~40%.
Reaction temperature in the present invention is 60 DEG C~90 DEG C, and temperature is beyond the ammonia state contained in 60~90 DEG C of citrate acid soluble phosphatic fertilizers
Nitrogen easily escapes, and condensation reaction can occur for the urea state nitrogen that ureasulfuric acid is brought into；Therefore it is feasible for selecting reaction temperature to be 60 DEG C~90 DEG C
's.
Mixed reaction time of the invention, selects 50~90min to be convenient for cured later and curing；When can also make reaction
Between reach 4.5~6.5h, water-soluble phosphorus content tends towards stability at this time, so as to shorten process flow.
Solidify in the present invention, cure, be the reaction under low temperature, moisture evaporation is few, the material after hybrid reaction through 60~
120min is curable；It carries out stirring curing after solidification, water-soluble phosphorus tends to be steady in 1~3 day material.
The mass ratio of urea and sulfuric acid is 0.92~2.2: 1 in ureasulfuric acid of the present invention；When lower than 0.92: 1, though Chinese holly
Soluble phosphorus conversion ratio improves, but free acid content increases, and solid-liquor separation occur in simultaneous reactions；And the increasing of sulfuric acid amount makes to react
Passivation is generated, conversion ratio is caused to decline；Higher than 2.2: 1, the conversion ratio of Chinese holly Soluble phosphorus is not high, and material viscosity increases.Therefore choosing urine
It is feasible that the mass ratio of element and sulfuric acid, which is 0.92~2.2: 1,.
Ureasulfuric acid of the present invention is kept for 80~90 DEG C in configuration temperature, and main purpose is to solidify ureasulfuric acid not；It is super
80~90 DEG C out, condensation reaction can occur for urea state nitrogen；Therefore it is feasible that temperature, which is 80~90 DEG C,.
It is mixed using ureasulfuric acid with citrate acid soluble phosphatic fertilizer in the present invention, the hydrogen ion, acid ion after ureasulfuric acid dissociation make Chinese holly
Dissolubility phosphorus is converted into water-soluble phosphorus, and urea is complexed with water-soluble phosphorus again, obtains the water-soluble phosphorus of complex status.
Citrate acid soluble phosphatic fertilizer of the present invention is in ammonia and to clean in Wet-process Phosphoric Acid Production water soluble composite fertilizer production process
Filter residue, the citrate acid soluble phosphatic fertilizer filter residue that for example ammonia neutralizes in water-soluble 66% monoammonium phosphate production process.
The invention has the following advantages:
1, the part citric acid soluble phosphorus in citrate acid soluble phosphatic fertilizer is converted water-soluble phosphorus by the present invention, and can be stabilized；Because of sulphur
The amidonitrogen brought into sour urea is in complex status, reduces the loss of nitrogen, nitrogen content effectively improves.
2, the present invention handles citrate acid soluble phosphatic fertilizer using ureasulfuric acid, can simplify process flow, is not adding unclassified stores
In the case of, there are water-soluble phosphorus and water in citrate acid soluble phosphatic fertilizer and is effectively mentioned than (water has than referring to the ratio between water-soluble phosphorus and available phosphorus)
Height can be used as the raw material of formula fertilizer or nitrogen-phosphorus-potassium compound fertilizer.
3, present invention process is simple, at low cost, strong operability, will not generate reluctant waste in the process, right
It is environmental-friendly.
Specific embodiment
Following embodiment be only be further illustrate examples made by the present invention, be not limited to the present invention.It is right
Various forms of modifications and variations can be made on the basis of the present invention for the those of ordinary skill of same domain.It is all
Obvious modifications and variations amplified on concept of the invention etc., all should protection scope of the present invention it
Column.
Embodiment 1:
S1: weighing 100 grams of ureasulfuric acids (urea: sulfuric acid=2.2:1) addition, 1000 grams of citrate acid soluble phosphatic fertilizers, (water-soluble phosphorus occupies effect
The ratio of phosphorus be 25%) in, hybrid reaction 50min, obtains material A at 60 DEG C；
S2: material A solidifies 60min, obtains material B at 50 DEG C；
S3: material B at 45 DEG C, cure 1 day, obtain compound fertilizer's head product, the ratio that water-soluble phosphorus accounts for available phosphorus is
65.83%.
Embodiment 2:
S1: weighing 300 grams of ureasulfuric acids (urea: sulfuric acid=1.22:1) addition, 1000 grams of citrate acid soluble phosphatic fertilizers, (water-soluble phosphorus occupies
Imitate phosphorus ratio be 30%) in, hybrid reaction 70min, obtains material A at 75 DEG C；
S2: material A solidifies 90min, obtains material B at 55 DEG C；
S3: material B at 50 DEG C, cure 2 days, obtain compound fertilizer's head product, the ratio that water-soluble phosphorus accounts for available phosphorus is
84.81%.
Embodiment 3:
S1: weighing 400 grams of ureasulfuric acids (urea: sulfuric acid=0.92:1) addition, 1000 grams of citrate acid soluble phosphatic fertilizers, (water-soluble phosphorus occupies
Imitate phosphorus ratio be 40%) in, hybrid reaction 90min, obtains material A at 90 DEG C；
S2: material A solidifies 120min, obtains material B at 60 DEG C；
S3: material B at 55 DEG C, cure 3 days, obtain compound fertilizer's head product, the ratio that water-soluble phosphorus accounts for available phosphorus is
74.54%.
Embodiment 4:
Weighing 100 grams of ureasulfuric acids (urea: sulfuric acid=2.2:1) addition, 1000 grams of citrate acid soluble phosphatic fertilizers, (water-soluble phosphorus accounts for available phosphorus
Ratio be 30%) in, hybrid reaction 4.5h at 60 DEG C obtains compound fertilizer's head product, and the ratio that water-soluble phosphorus accounts for available phosphorus is
68.42%.
Embodiment 5:
Weighing 300 grams of ureasulfuric acids (urea: sulfuric acid=1.22:1) addition, 1000 grams of citrate acid soluble phosphatic fertilizers, (water-soluble phosphorus accounts for available phosphorus
Ratio be 40%) in, hybrid reaction 5.5h at 75 DEG C obtains compound fertilizer's head product, and the ratio that water-soluble phosphorus accounts for available phosphorus is
83.42%.
Embodiment 6:
Weigh 400 grams of ureasulfuric acids (urea: sulfuric acid=0.92:1) be added 1000 grams of citrate acid soluble phosphatic fertilizers in (water-soluble phosphorus occupies effect
25%) ratio of phosphorus is that hybrid reaction 6.5h at 90 DEG C obtains compound fertilizer's head product, and the ratio that water-soluble phosphorus accounts for available phosphorus is
75.06%.
Comparative example 1:
It will be first added in the filter residue of the Chinese holly Soluble phosphorus containing 1000g (it is 40% that water-soluble phosphorus, which accounts for the ratio of available phosphorus) and contain 100g sulphur
The aqueous solution of acid, 200g nitric acid, adds the work of 10.0g mixed by 5 parts of neopelexes and 1 part of ammonium nitrate
Agent, priming reaction 2.0h at 88 DEG C；100g yeast source Organic Ingredients is added, is uniformly mixed, obtains stable water-soluble phosphorus material
Slurry, the ratio that water-soluble phosphorus accounts for available phosphorus is 49.16%.
Comparative example 2:
It will be first added in the filter residue of the Chinese holly Soluble phosphorus containing 1000g (it is 25% that water-soluble phosphorus, which accounts for the ratio of available phosphorus) and contain 100g sulphur
The aqueous solution of acid, 100g nitric acid, adds the work of 20.0g mixed by 6 parts of neopelexes and 1 part of ammonium nitrate
Agent, priming reaction 2.0h at 85 DEG C；50.0g yeast source Organic Ingredients is added, is uniformly mixed, obtains stable water-soluble phosphorus material
Slurry, the ratio that water-soluble phosphorus accounts for available phosphorus is 31.21%.
Comparative example 3:
It will be first added in the filter residue of the Chinese holly Soluble phosphorus containing 1000g (it is 30% that water-soluble phosphorus, which accounts for the ratio of available phosphorus) and contain 100g sulphur
The aqueous solution of acid, 200g nitric acid, adds the work of 5.0g mixed by 4 parts of neopelexes and 1 part of ammonium nitrate
Agent, priming reaction 2.5h at 90 DEG C；200g yeast source Organic Ingredients is added, is uniformly mixed, obtains stable water-soluble phosphorus material
Slurry, the ratio that water-soluble phosphorus accounts for available phosphorus is 36.90%.
The data of above-described embodiment and comparative example are unified as (wherein water has the ratio than accounting for available phosphorus for water-soluble phosphorus to following table
Example):
By Examples 1 to 6 it is found that water after being handled with method of the invention citrate acid soluble phosphatic fertilizer, in final material
Have than reaching 65~85%；The citrate acid soluble phosphatic fertilizer handled by comparative example method, water-soluble phosphorus content is improved in final material,
But water has than relatively low.
The present invention can also have other various embodiments, without deviating from the spirit and substance of the present invention, be familiar with this
The technical staff in field can make various corresponding changes and modifications according to the present invention, but these corresponding changes and modifications are all answered
It belongs to the protection scope of the claims of the invention.
Claims (8)
1. a kind of production method for improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer, which comprises the steps of:
(1) it hybrid reaction: by 10%~40% that ureasulfuric acid dosage is citric acid soluble phosphorus fertilizer amount, is added in citrate acid soluble phosphatic fertilizer, mixing
60~90 DEG C of reaction temperature, 50~90min of hybrid reaction obtains material A；
(2) solidify: material A solidifies 60~120min, obtains material B at 50~60 DEG C；
(3) cure: material B is cured 1~3 day at 45~55 DEG C, and compound fertilizer's head product is made.
2. the production method according to claim 1 for improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer, which is characterized in that described
The mass ratio of solid urea and sulfuric acid is 0.92~2.2: 1 in ureasulfuric acid, and temperature when configuring ureasulfuric acid remains 80~90 DEG C.
3. the production method according to claim 1 for improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer, which is characterized in that described
It is 25%~40% that water-soluble phosphorus, which accounts for the ratio of available phosphorus, in citrate acid soluble phosphatic fertilizer.
4. the production method according to claim 1 for improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer, which is characterized in that (1)
In step, compound fertilizer's head product is directly made in 4.5~6.5h of hybrid reaction.
5. the production method according to claim 1 or 4 for improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer, which is characterized in that system
It is 65%~85% that water-soluble phosphorus, which accounts for the ratio of available phosphorus, in the compound fertilizer's head product obtained.
6. the production method according to claim 1 or 4 for improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer, which is characterized in that sulphur
Sour urea dosage is the 20%~30% of citric acid soluble phosphorus fertilizer amount.
7. the production method according to claim 2 for improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer, which is characterized in that described
The mass ratio of solid urea and sulfuric acid is 1.07~1.38: 1 in ureasulfuric acid.
8. the production method according to claim 1 for improving the water-soluble phosphorus content of citrate acid soluble phosphatic fertilizer, which is characterized in that (1)
In step, hybrid reaction temperature is 70~80 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110357670A (en) * | 2019-07-04 | 2019-10-22 | 湖北祥云(集团)化工股份有限公司 | A method of compound fertilizer containing ammonium polyphosphate is prepared using industrial monoammonium phosphate slag |
| CN114349572A (en) * | 2022-01-19 | 2022-04-15 | 云南云天化股份有限公司 | Method for producing compound fertilizer containing polymerized phosphorus by using citric soluble phosphorus slag |
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| CN110357670A (en) * | 2019-07-04 | 2019-10-22 | 湖北祥云(集团)化工股份有限公司 | A method of compound fertilizer containing ammonium polyphosphate is prepared using industrial monoammonium phosphate slag |
| CN114349572A (en) * | 2022-01-19 | 2022-04-15 | 云南云天化股份有限公司 | Method for producing compound fertilizer containing polymerized phosphorus by using citric soluble phosphorus slag |
| CN114349572B (en) * | 2022-01-19 | 2022-12-30 | 云南云天化股份有限公司 | Method for producing compound fertilizer containing polymerized phosphorus by using citric soluble phosphorus slag |
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