CN106588128A - Method for producing large-particle ammonium sulfate - Google Patents
Method for producing large-particle ammonium sulfate Download PDFInfo
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- CN106588128A CN106588128A CN201611115585.7A CN201611115585A CN106588128A CN 106588128 A CN106588128 A CN 106588128A CN 201611115585 A CN201611115585 A CN 201611115585A CN 106588128 A CN106588128 A CN 106588128A
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- ammonium sulfate
- ammonia
- particle
- slurry
- phosphoric acid
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
Abstract
A method for producing large-particle ammonium sulfate comprises the following steps: step 1, mixing slag slurry produced in a process of wet phosphoric acid production of industrial phosphoric acid with sulfuric acid and a tail washed liquid according to the ratio of (0.5-3):10:(0.1-3) to form a mixed acid; step 2, adding ammonia gas or liquid ammonia or ammonia water to the mixed acid, and carrying out a neutralization reaction to obtain an ammonium sulfate slurry; step 3, sending the ammonium sulfate slurry into a granulator, granulating, and drying; step 4, sieving and grading the large-particle ammonium sulfate obtained by granulation; step 5, treating the finished product ammonium sulfate particles having the particle size of 2-4.5 mm and obtained from sieving, to obtain a finished product, and packaging; and step 6, carrying out circulating water washing of sieved dust-containing tail gas, adding sulfuric acid to the washed water according to the ratio of (4-5):1 and mixing into a dilute sulfuric acid, washing the granulated ammonia-containing tail gas, and thus obtaining a tail washed liquid containing sulfuric acid and ammonium sulfate after washing the ammonia-containing tail gas with the dilute sulfuric acid, wherein the tail washed liquid is used for preparing the mixed acid.
Description
Technical field
The present invention relates to chemical production technical field, and in particular to adopt Wet-process Phosphoric Acid Production industrial phosphoric acid process to a kind of
The slurry of middle generation coordinates the production method of gas washing in SA production large-particle ammonium sulfate.
Background technology
Being agriculturally a kind of good sulfur-containing nitrogen fertilizer, sulfur is the middle amount nutrient needed for crop to ammonium sulfate, sulfur-bearing
Fertilizer not only improve crop yield, crop quality can also be improved, in the state such as the U.S., Japan large usage quantity.Sulfur on market
The most lenticular ammonium sulfate higher for purity of sour ammonium, diameter ammonium sulfate in below 1mm and single is difficult to make again
Grain obtains large-particle ammonium sulfate.In agriculture highly-mechanized today, the ammonium sulfate of small crystalss shape does not reach the requirement of mechanization.
So be typically only capable to as raw material, for producing compound fertilizer, it is impossible to single administration.
Its cost of the technique of Wet-process Phosphoric Acid Production industrial monoammonium phosphate well below Traditional Method production technology, it is at present basic
All replace Traditional Methods, but its shortcoming is exactly to need supporting agriculture MAP Plant or compound fertilizer facility to digest production
During produce mother solution and slurry.Mother solution nutrient content is high, is directly used in the agriculture MAP of production or compound fertilizer will not be right
An agriculture ammonium or compound fertilizer nutrient are impacted, but impurity content is high in slurry, and viscosity is strong, for producing an agriculture ammonium or multiple
If Hefei, the ginseng amount of converting is big to be easily caused an agriculture ammonium and compound fertilizer nutrient is unqualified.
The content of the invention
The technical problem to be solved is to provide a kind of large-particle ammonium sulfate and production method, being capable of effectively utilizes
The characteristics of slurry produced during Wet-process Phosphoric Acid Production industrial monoammonium phosphate has viscosity strong, as production bulky grain sulfur
The binding agent of sour ammonium, solves the problems, such as that simple ammonium sulfate pelletize is difficult, and the nitrogen and phosphorus remained in slurry is effectively utilized again.
To solve above-mentioned technical problem, the technical solution adopted in the present invention is:N content is in a kind of large-particle ammonium sulfate
It is 1 ~ 3% that 19 ~ 20%, S content is 22 ~ 23%, P2O5 contents, and water content is 1 ~ 2%, granularity 2 ~ 4.5mm >=90%, intensity >=40N.
A kind of production method of large-particle ammonium sulfate includes following steps:
Step 1:During the slurry produced during Wet-process Phosphoric Acid Production industrial phosphoric acid or Wet-process Phosphoric Acid Production industrial phosphoric acid
The solid slag that filter pressing is produced, slurry presses 0.5 ~ 3 with sulphuric acid, tail washing liquid:10:The mixing of 0.1 ~ 3 ratio is made into nitration mixture;
Step 2:Step 1 gained nitration mixture is added into gas ammonia or liquefied ammonia or ammonia, reaction is neutralized, pH value 3.0 ~ 6.0 is controlled, is obtained
To ammonium sulfate slurry;
Step 3:Step 2 gained ammonium sulfate slurry is sent into into the masterbatch in comminutor, with comminutor carries out pelletize, drying, obtains
Large-particle ammonium sulfate;
Step 4:The grain ammonium sulfate that step 3 is obtained is sieved, and granule of the particle diameter less than 2mm returns comminutor as masterbatch,
Particle diameter is more than the comminutor of return after crushing of 4.5mm as masterbatch, while directly oarse-grained sulphuric acid is filled into in comminutor
Crystalline ammonium is used as masterbatch;
Step 5:The finished product sulfuric acid ammonium granule of the 2 ~ 4.5mm of particle diameter for obtaining will be sieved in step 4, the post processing after obtains bulky grain
Ammonium sulfate;
Step 6:The dust-containing tail gas sieved in step 3 are washed with water circulation, and washings press 4 ~ 5:1 adds sulphuric acid to convert into dilute sulfuric acid, dilute
Sulphuric acid is washed to the ammonia-containing exhaust of pelletize, is obtained the tail containing sulphuric acid and ammonium sulfate after dilute sulfuric acid washing ammonia-containing exhaust and is washed
Liquid, return to step 1, for configuring nitration mixture.
Further, the slurry described in step 1 is the slurry produced during Wet-process Phosphoric Acid Production industrial phosphoric acid, or
Be during Wet-process Phosphoric Acid Production industrial phosphoric acid filter pressing produce solid slag, wherein Fe2O3%+Al2O3%+MgO% contents be 10 ~
30%, described sulfuric acid concentration is 50 ~ 99%.
Further, the ammonium sulfate pelletize described in step 3 be slurryspraying granulation technique, pelletize built-in temperature≤200
℃。
Further, the dilute sulfuric acid concentration that washing ammonia-containing exhaust is matched somebody with somebody in step 6 is 10 ~ 30%.
A kind of production method of large-particle ammonium sulfate that the present invention is provided, has the beneficial effect that:
1st, the slurry produced during effectively utilizes Wet-process Phosphoric Acid Production industrial monoammonium phosphate, while solving simple ammonium sulfate
The difficult problem of pelletize.
2nd, process conditions are easy to control, easy to operate, good product quality, and the element such as nitrogen, phosphorus in slurry enters bulky grain sulfur
In sour ammonium product, efficent use of resources is produced without garbage.
Description of the drawings
With reference to the accompanying drawings and examples the invention will be further described:
Fig. 1 is the process chart of the inventive method.
Specific embodiment
Embodiment one
As shown in figure 1, a kind of production method of large-particle ammonium sulfate, the method is comprised the following steps:
Step 1:During the slurry produced during Wet-process Phosphoric Acid Production industrial phosphoric acid or Wet-process Phosphoric Acid Production industrial phosphoric acid
The solid slag that filter pressing is produced, with sulphuric acid, tail washing liquid 1 is pressed:10:The mixing of 1 ratio is made into nitration mixture;
Step 2:Step 1 gained nitration mixture is added into gas ammonia, reaction is neutralized, pH value 3.0 is controlled, ammonium sulfate slurry is obtained;
Step 3:Step 2 gained ammonium sulfate slurry is sent into into the masterbatch in comminutor, with comminutor carries out pelletize, drying, pelletize
Built-in temperature controls 160 ~ 180 DEG C, obtains large-particle ammonium sulfate;
Step 4:The large-particle ammonium sulfate that step 3 is obtained is sieved, granule of the particle diameter less than 2mm returns comminutor as mother
Material, particle diameter is more than the comminutor of return after crushing of 4.5mm as masterbatch, while directly oarse-grained sulfur is filled into in comminutor
Sour crystalline ammonium is used as masterbatch;
Step 5:It is post-treated by the finished product sulfuric acid ammonium granule of the 2 ~ 4.5mm of particle diameter for obtaining that sieves in step 4(Cooling, peplos,
Classification)Obtain finished product to be packed;
Step 6:After the dust-containing tail gas of screening are washed with water circulation, washings add sulphuric acid to convert into 20% dilute sulfuric acid, and dilute sulfuric acid is to making
The ammonia-containing exhaust of grain is washed, and after dilute sulfuric acid washing ammonia-containing exhaust the tail washing liquid containing sulphuric acid and ammonium sulfate is obtained, and returns step
Rapid 1, for configuring nitration mixture;
In step 1, Fe in slurry used2O3%+Al2O3%+MgO%≈17%(Fluctuate 10 or so, quality percentage
Than), slurry aqueous 55%(Mass percent).
In step 1, the mass concentration of sulphuric acid used is 50%.
In step 6, after tail washing liquid 1.20 ~ 1.25g/ml of density, start to take out the nitration mixture in configuration step 1, slurry,
Sulphuric acid, tail washing liquid by volume 1:10:1 ratio matches somebody with somebody nitration mixture.
Obtained large-particle ammonium sulfate, it is 1.5% for 22.8%, P2O5 contents that N content is 18.5%, S contents, water content
For 1.1%, granularity 2 ~ 4.5mm >=90%, intensity >=40N.
Embodiment two
As shown in figure 1, a kind of production method of large-particle ammonium sulfate, the method is comprised the following steps:
Step 1:The slurry that will be produced during Wet-process Phosphoric Acid Production industrial phosphoric acid, with sulphuric acid, tail washing liquid 1 is pressed:10:0.6 ratio
Example mixing is made into nitration mixture;
Step 2:Step 1 gained nitration mixture is added into gas ammonia, reaction is neutralized, pH value 4.0 is controlled, ammonium sulfate slurry is obtained;
Step 3:Step 2 gained ammonium sulfate slurry is sent into into the masterbatch in comminutor, with comminutor carries out pelletize, drying, pelletize
Built-in temperature controls 180 ~ 200 DEG C, obtains large-particle ammonium sulfate;
Step 4:The large-particle ammonium sulfate that step 3 is obtained is sieved, granule of the particle diameter less than 2mm returns comminutor as mother
Material, particle diameter is more than the comminutor of return after crushing of 4.5mm as masterbatch, while directly oarse-grained sulfur is filled into in comminutor
Sour crystalline ammonium is used as masterbatch;
Step 5:The finished product sulfuric acid ammonium granule of the 2 ~ 4.5mm of particle diameter for obtaining that sieves in step 4, Jing are subsequently further processed(Drop
Temperature, peplos, classification)Obtain finished product to be packed;
Step 6:After the dust-containing tail gas of screening are washed with water circulation, washings add sulphuric acid to convert into 20% dilute sulfuric acid, and pelletize is contained
Ammonia tail gas is washed, and the tail washing liquid containing sulphuric acid and ammonium sulfate is obtained after dilute sulfuric acid washing ammonia-containing exhaust, and return to step 1 is used
In configuration nitration mixture;
In step 1, Fe in slurry used2O3%+Al2O3%+MgO%≈17%(Fluctuate 1 15 or so, quality percentage
Than), slurry aqueous 55%(Mass percent).
In step 1, the mass concentration of sulphuric acid used is 60%.
In step 6, after tail washing liquid 1.20 ~ 1.25g/ml of density, start to take out the nitration mixture in configuration step 1.
Obtained large-particle ammonium sulfate, it is 1.4% for 22.6%, P2O5 contents that N content is 19.0%, S contents, water content
For 1.3%, granularity 2 ~ 4.5mm >=90%, intensity >=40N.
Embodiment three
As shown in figure 1, a kind of production method of large-particle ammonium sulfate, the method is comprised the following steps:
Step 1:The slurry that will be produced during Wet-process Phosphoric Acid Production industrial phosphoric acid, with sulphuric acid, tail washing liquid 0.8 is pressed:10:1 ratio
Example mixing is made into nitration mixture;
Step 2:Step 1 gained nitration mixture is added into gas ammonia, reaction is neutralized, pH value 5.0 is controlled, ammonium sulfate slurry is obtained;
Step 3:Step 2 gained ammonium sulfate slurry is sent into into the masterbatch in comminutor, with comminutor carries out pelletize, drying, pelletize
Built-in temperature controls 180 ~ 200 DEG C, obtains large-particle ammonium sulfate;
Step 4:The large-particle ammonium sulfate that step 3 is obtained carried out sieve classification, and granule of the particle diameter less than 2mm returns comminutor and make
For masterbatch, particle diameter is more than the comminutor of return after crushing of 4.5mm as masterbatch, while directly filling into bulky grain in comminutor
Ammonium sulfate crystallization as masterbatch;
Step 5:It is post-treated by the finished product sulfuric acid ammonium granule of the 2 ~ 4.5mm of particle diameter for obtaining that sieves in step 4(Cooling, peplos,
Classification)Obtain finished product to be packed;
Step 6:After the dust-containing tail gas of screening are washed with water circulation, washings add sulphuric acid to convert into 20% dilute sulfuric acid, and dilute sulfuric acid is to making
The ammonia-containing exhaust of grain is washed, and after dilute sulfuric acid washing ammonia-containing exhaust the tail washing liquid containing sulphuric acid and ammonium sulfate is obtained, and returns step
Rapid 1, for configuring nitration mixture;
In step 1, Fe in slurry used2O3%+Al2O3%+MgO%≈17%(Mass percent), slurry aqueous 55%(Quality percentage
Than).
In step 1, the mass concentration of sulphuric acid used is 70%.
In step 6, after tail washing liquid 1.20 ~ 1.25g/ml of density, start to take out the nitration mixture in configuration step 1, slurry,
Sulphuric acid, tail washing liquid by volume 1:10:1 ratio matches somebody with somebody nitration mixture.
Obtained large-particle ammonium sulfate, it is 1.4% for 22.4%, P2O5 contents that N content is 19.6%, S contents, water content
For 1.6%, granularity 2 ~ 4.5mm >=90%, intensity >=40N.
Example IV
As shown in figure 1, a kind of production method of large-particle ammonium sulfate, the method is comprised the following steps:
Step 1:The slurry that will be produced during Wet-process Phosphoric Acid Production industrial phosphoric acid, with sulphuric acid, tail washing liquid 1 is pressed:10:2 ratio
Mixing is made into nitration mixture;
Step 2:Step 1 gained nitration mixture is added into gas ammonia, reaction is neutralized, pH value 6.0 is controlled, ammonium sulfate slurry is obtained;
Step 3:Step 2 gained ammonium sulfate slurry is sent into into the masterbatch in comminutor, with comminutor carries out pelletize, drying, pelletize
Built-in temperature controls 160 ~ 180 DEG C, obtains large-particle ammonium sulfate;
Step 4:The large-particle ammonium sulfate that step 3 is obtained carried out sieve classification, and granule of the particle diameter less than 2mm returns comminutor and make
For masterbatch, particle diameter is more than the comminutor of return after crushing of 4.5mm as masterbatch, while directly filling into bulky grain in comminutor
Ammonium sulfate crystallization as masterbatch;
Step 5:The finished product sulfuric acid ammonium granule of the 2 ~ 4.5mm of particle diameter for obtaining that sieves in step 4, Jing are subsequently further processed(Drop
Temperature, peplos, classification)Obtain finished product to be packed;
Step 6:After the dust-containing tail gas of screening are washed with water circulation, washings add sulphuric acid to convert into 20% dilute sulfuric acid, and pelletize is contained
Ammonia tail gas is washed, and the tail washing liquid containing sulphuric acid and ammonium sulfate is obtained after dilute sulfuric acid washing ammonia-containing exhaust, and return to step 1 is used
In configuration nitration mixture;
In step 1, Fe in slurry used2O3%+Al2O3%+MgO%≈17%(Mass percent), slurry aqueous 55%(Quality percentage
Than).
In step 1, the mass concentration of sulphuric acid used is 60%.
In step 6, after tail washing liquid 1.20 ~ 1.25g/ml of density, start to take out the nitration mixture in configuration step 1, slurry,
Sulphuric acid, tail washing liquid by volume 1:10:1 ratio matches somebody with somebody nitration mixture.
Obtained large-particle ammonium sulfate, it is 1.6% for 22.0%, P2O5 contents that N content is 19.8%, S contents, water content
For 2.0%, granularity 2 ~ 4.5mm >=90%, intensity >=40N.
The present invention is implemented and is not restricted to the described embodiments, as long as employing method of the present invention design and technology
The improvement of the various unsubstantialities that scheme is carried out, or it is not improved by the present invention design and technical scheme directly apply other fields
Close, within protection scope of the present invention.
Claims (5)
1. a kind of large-particle ammonium sulfate, it is characterised in that:In the large-particle ammonium sulfate N content be 19 ~ 20%, S contents be 22 ~
23%, P2O5 content is 1 ~ 3%, and water content is 1 ~ 2%, granularity 2 ~ 4.5mm >=90%, intensity >=40N.
2. a kind of production method of large-particle ammonium sulfate, it is characterised in that:Method is comprised the following steps:
Step 1:During the slurry produced during Wet-process Phosphoric Acid Production industrial phosphoric acid or Wet-process Phosphoric Acid Production industrial phosphoric acid
The solid slag that filter pressing is produced, with sulphuric acid, tail washing liquid 0.5 ~ 3 is pressed:10:The mixing of 0.1 ~ 3 ratio is made into nitration mixture;
Step 2:Step 1 gained nitration mixture is added into gas ammonia or liquefied ammonia or ammonia, reaction is neutralized, pH value 3.0 ~ 6.0 is controlled, is obtained
To ammonium sulfate slurry;
Step 3:Step 2 gained ammonium sulfate slurry is sent into into the masterbatch in comminutor, with comminutor carries out pelletize, drying, obtains
Large-particle ammonium sulfate;
Step 4:The grain ammonium sulfate that step 3 is obtained is sieved, and granule of the particle diameter less than 2mm returns comminutor as masterbatch,
Particle diameter is more than the comminutor of return after crushing of 4.5mm as masterbatch, while directly oarse-grained sulphuric acid is filled into in comminutor
Crystalline ammonium is used as masterbatch;
Step 5:The finished product sulfuric acid ammonium granule of the 2 ~ 4.5mm of particle diameter for obtaining will be sieved in step 4, the post processing after obtains bulky grain
Ammonium sulfate;
Step 6:The dust-containing tail gas sieved in step 3 are washed with water circulation, and washings press 4 ~ 5:1 adds sulphuric acid to convert into dilute sulfuric acid, dilute
Sulphuric acid is washed to the ammonia-containing exhaust of pelletize, is obtained the tail containing sulphuric acid and ammonium sulfate after dilute sulfuric acid washing ammonia-containing exhaust and is washed
Liquid, return to step 1, for configuring nitration mixture.
3. the production method of a kind of large-particle ammonium sulfate according to claim 2, it is characterised in that:Described in step 1
Slurry is the slurry produced during Wet-process Phosphoric Acid Production industrial phosphoric acid, or is pressed during Wet-process Phosphoric Acid Production industrial phosphoric acid
The solid slag that filter is produced, wherein Fe2O3%+Al2O3%+MgO% contents are 10 ~ 30%, and described sulfuric acid concentration is 50 ~ 99%.
4. the production method of a kind of large-particle ammonium sulfate according to claim 2, it is characterised in that:Described in step 3
Ammonium sulfate pelletize be slurryspraying granulation technique, pelletize built-in temperature≤200 DEG C.
5. the production method of a kind of large-particle ammonium sulfate according to claim 2, it is characterised in that:Washing in step 6 contains
The dilute sulfuric acid concentration that ammonia tail gas is matched somebody with somebody is 10 ~ 30%.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112403391A (en) * | 2020-10-16 | 2021-02-26 | 湖北三宁化工股份有限公司 | Binder for producing large-particle ammonium sulfate and preparation method thereof |
CN114180994A (en) * | 2021-12-29 | 2022-03-15 | 连云港钧格环境科技有限公司 | Production process and equipment for large-particle ammonium sulfate product |
CN114735720A (en) * | 2022-04-25 | 2022-07-12 | 云南云天化云峰化工有限公司 | Method and system for producing granular ammonium sulfate by drum granulation through circulating neutralization method |
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CN101648713A (en) * | 2009-07-23 | 2010-02-17 | 瓮福(集团)有限责任公司 | Method for producing granular ammonium sulfate |
CN103626528A (en) * | 2013-11-28 | 2014-03-12 | 瓮福(集团)有限责任公司 | Method for producing granular ammonium sulphate by using phosphorus-containing wastewater |
CN104418626A (en) * | 2013-08-26 | 2015-03-18 | 山东聊城鲁西化工第五化肥有限公司 | Method for producing sulfur-based composite fertilizer by using monoammonium phosphate instead of phosphoric acid |
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2016
- 2016-12-07 CN CN201611115585.7A patent/CN106588128B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101648713A (en) * | 2009-07-23 | 2010-02-17 | 瓮福(集团)有限责任公司 | Method for producing granular ammonium sulfate |
CN104418626A (en) * | 2013-08-26 | 2015-03-18 | 山东聊城鲁西化工第五化肥有限公司 | Method for producing sulfur-based composite fertilizer by using monoammonium phosphate instead of phosphoric acid |
CN103626528A (en) * | 2013-11-28 | 2014-03-12 | 瓮福(集团)有限责任公司 | Method for producing granular ammonium sulphate by using phosphorus-containing wastewater |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112403391A (en) * | 2020-10-16 | 2021-02-26 | 湖北三宁化工股份有限公司 | Binder for producing large-particle ammonium sulfate and preparation method thereof |
CN114180994A (en) * | 2021-12-29 | 2022-03-15 | 连云港钧格环境科技有限公司 | Production process and equipment for large-particle ammonium sulfate product |
CN114735720A (en) * | 2022-04-25 | 2022-07-12 | 云南云天化云峰化工有限公司 | Method and system for producing granular ammonium sulfate by drum granulation through circulating neutralization method |
CN114735720B (en) * | 2022-04-25 | 2023-08-18 | 云南云天化云峰化工有限公司 | Method and system for producing granular ammonium sulfate by rotary drum granulation through cyclic neutralization method |
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