CN113493364A - Preparation method of ammonium sulfate containing urea aldehyde slow-release nitrogen component - Google Patents

Preparation method of ammonium sulfate containing urea aldehyde slow-release nitrogen component Download PDF

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Publication number
CN113493364A
CN113493364A CN202010196044.1A CN202010196044A CN113493364A CN 113493364 A CN113493364 A CN 113493364A CN 202010196044 A CN202010196044 A CN 202010196044A CN 113493364 A CN113493364 A CN 113493364A
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CN
China
Prior art keywords
ammonium sulfate
particles
preparation
urea
formalin
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Pending
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CN202010196044.1A
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Chinese (zh)
Inventor
曹贤高
杨永宁
孙思鹏
胥学辉
罗涛波
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Summit Fertilizer Qingdao Co ltd
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Summit Fertilizer Qingdao Co ltd
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Priority to CN202010196044.1A priority Critical patent/CN113493364A/en
Publication of CN113493364A publication Critical patent/CN113493364A/en
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C3/00Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor

Abstract

The invention belongs to the technical field of agricultural fertilizers, and particularly relates to a preparation method of ammonium sulfate containing urea aldehyde slow-release nitrogen components, which comprises the following steps: adding a proper amount of urea, formalin and water into a reaction kettle for mixing, heating under the condition of stirring for addition reaction after mixing, and generating a hydroxyurea solution; carrying out condensation reaction on the hydroxyurea solution under an acidic condition, then spraying the solution into a rotary drum granulator, adding a powdery ammonium sulfate raw material, mixing and granulating to obtain round particles; drying and cooling the ammonium sulfate round particles, and then screening, and selecting 2-4 mm particles to obtain the ammonium sulfate particles containing the slow-release components. The preparation method takes powdery ammonium sulfate as a main body, and utilizes the hydroxyurea-formaldehyde to participate in ammonium sulfate granulation, so that the produced finished product has high particle strength, smooth appearance and uniform particle size, and the quality of the ammonium sulfate particles can be obviously improved.

Description

Preparation method of ammonium sulfate containing urea aldehyde slow-release nitrogen component
Technical Field
The invention belongs to the technical field of agricultural fertilizers, and particularly relates to a preparation method of ammonium sulfate containing urea aldehyde slow-release nitrogen components.
Background
Ammonium sulfate is an excellent nitrogen fertilizer, has high nitrogen utilization rate and quick fertilizer effect, is suitable for general soil and crops, can make branches and leaves grow vigorously, improve fruit quality and yield, enhance the resistance of the crops to disasters, and can be used as a base fertilizer, an additional fertilizer and a seed fertilizer. Most of domestic ammonium sulfate products are powdery ammonium sulfate, are byproducts of coking and other industries, and are generally white or slightly yellow fine grains.
With the development of agricultural mechanization, the defects of powdery ammonium sulfate are gradually exposed, hardening is a defect which needs to be solved urgently, and one of the ways to solve the problem is to realize granulation of fertilizers. A few foreign manufacturers use a specific method to produce high-strength and high-nutrient granular ammonium sulfate products, and due to the confidential production process, only a certain enterprise can produce the ammonium sulfate products abroad. The domestic granular ammonium sulfate is mainly extruded granules, the extruded ammonium sulfate is only a single ammonium nitrogen component, the granular strength of the product is low, the product is easy to pulverize, the granules are irregular and not round, the granule size is not uniform, the hardening is easy, and a large peculiar smell is easy to generate in a matched BB fertilizer, so that the smooth proceeding of agricultural production and mechanical fertilization is limited.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a preparation method of ammonium sulfate containing urea-formaldehyde slow-release nitrogen components.
The technical scheme of the invention is as follows:
a preparation method of ammonium sulfate containing urea aldehyde slow-release nitrogen components comprises the following steps:
(1) adding urea, formalin and water into a reaction kettle for mixing, wherein the adding amount of the raw materials is as follows: 40-200 kg/t of urea, 10-60 kg/t of formalin and 10-60 kg/t of water; heating the mixed raw materials to 40-95 ℃ under the condition of stirring, and carrying out addition reaction for 20-200 min to generate a hydroxyurea solution;
(2) carrying out condensation reaction on a hydroxyurea solution under an acidic condition, then spraying the solution into a rotary drum granulator, setting the granulation temperature to be 30-50 ℃, adding 400-900 kg/t of powdery ammonium sulfate raw material, mixing and granulating, carrying out condensation reaction again under the rotation action of the rotary drum, and setting the steam pressure to be 0.2-0.5 MPa as auxiliary steam to solidify the reaction product into round particles with different sizes;
in the formula raw materials, the ratio of the powdery ammonium sulfate reaches 40-90%.
Effect of stable supply and temperature of hydroxyurea solution on production in granulation: if the stable supply and temperature (30-50 ℃) of the hydroxyurea and the pH control are not good, the ammonium sulfate material is hardly granulated, and the material is obviously granulated under the condition of controlling the stable supply of the hydroxyurea and the granulation temperature, which is beneficial to the stable and continuous production.
Because the granulating property of water is poor and the moisture of finished product particles is influenced, the direct use of water for granulating is avoided in the granulating process.
(3) And (3) drying the ammonium sulfate round particles at a drying air temperature of 80-200 ℃ until the moisture content of the material is less than or equal to 1.0%, cooling, screening, and selecting 2-4 mm particles to obtain the ammonium sulfate particles containing the slow-release components.
After ammonium sulfate granule material carried drying equipment, reduce moisture through 80 ~ 200 ℃ dry air stoving, dry air is through dust collecting equipment and light oxygen deodorization equipment, and the atmosphere can not cause the influence to the environment in the exhaust. And (3) feeding the dried material into cooling and screening equipment, screening out 2-4 mm particles to obtain qualified finished product particles, performing anti-caking treatment, and conveying the finished product particles to a finished product storage tank for storage, packaging and warehousing. Wherein the screened particles with the particle size of more than 4mm and less than 2mm are crushed and then returned to the granulator for secondary granulation utilization.
Controlling the drying temperature of the materials: the production is carried out in a humid weather, materials are easy to accumulate in the drying equipment to a certain extent, the material flowability is poor, and the current of the drying equipment is high; therefore, a certain drying air drying temperature needs to be stably controlled, the production efficiency is favorably improved, and the drying production is influenced by overhigh or overlow temperature, so that secondary granulation is not favorably realized.
Urea formalin reaction formula
NH2-CO-NH2+HCHO→NH2-CO-NH-CH2-NH-CO-NH2
The reaction process is as follows:
1) addition reaction
NH2-CO-NH2+HCHO→NH2-CO-NH-CH2-OH
2) Condensation reaction
NH2-CO-NH-CH2-OH+NH2-CO-NH2→NH2-CO-NH-CH2-NH-CO-NH2+H2O。
Further, the adding amount of the raw materials in the step (1) is as follows: 80-160 kg/t of urea, 20-40 kg/t of formalin and 20-40 kg/t of water.
Further, the adding amount of the raw materials in the step (1) is as follows: 120kg/t of urea, 30kg/t of formalin and 30kg/t of water.
Furthermore, the nitrogen content of the ammonium sulfate particle containing the slow-release component prepared by the preparation method is 20.5-26.0%, and the ammonium sulfate particle containing the slow-release component comprises 1.0-2.0% of urea formaldehyde slow-release nitrogen, 3.0-9.0% of urea nitrogen and 9.0-18.0% of ammonium nitrogen.
Furthermore, potassium fulvate, magnesium oxide, zinc sulfate and boric acid can also be added in the preparation process; the potassium fulvate is mineral potassium fulvate.
Further, an anti-caking agent is added into the prepared ammonium sulfate granules containing the slow-release components for anti-caking treatment. The added anti-caking agent can improve the moisture absorption resistance and the anti-caking performance of the granular ammonium sulfate product and improve the overall performance of the granular ammonium sulfate product.
Further, the concentration of the formalin is 35-40%.
Furthermore, the powdery ammonium sulfate raw material is from coking industry and other industrial byproducts, and is one or two of coking grade ammonium sulfate in steel plants or triple effect evaporation byproduct ammonium sulfate.
The invention has the beneficial effects that:
(1) the invention takes the powdery ammonium sulfate as a main raw material, and adopts the hydroxyurea-formaldehyde to participate in ammonium sulfate granulation, thereby improving the balling rate of the product and improving the production efficiency by more than 50 percent; the ammonium sulfate containing the sustained-release components obtained by production has high particle strength, smooth appearance and uniform particle size, and can obviously improve the quality of the ammonium sulfate particles. In addition, the method mainly uses the medium-low grade ammonium sulfate as a main nitrogen source, can fully utilize industrial and other industrial byproducts such as coking and the like, has low production cost, is suitable for large-scale production, and has remarkable economic benefit.
(2) Compared with the ammonium sulfate which is pelletized by extrusion and only has a single ammonium nitrogen component, the invention can increase the urea nitrogen and the urea-formaldehyde nitrogen on the basis of the single ammonium nitrogen of the ammonium sulfate, expand the application range of the ammonium sulfate, facilitate fertilization, prolong the release time of nitrogen, improve the utilization rate of fertilizer, and add other medium and trace elements and various synergists required by crops according to the needs.
Detailed Description
The technical solutions of the present invention will be described in detail and fully with reference to the following specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
For a further understanding of the present invention, reference will now be made in detail to the following examples.
Example 1
A preparation method of ammonium sulfate containing urea aldehyde slow-release nitrogen components comprises the following steps:
and sequentially conveying 120kg/t of urea, 30kg/t of formalin and 30kg/t of water into a reaction kettle, mixing and heating to 40-95 ℃ in the reaction kettle under the condition of motor stirring, and carrying out addition reaction for 50-80min to generate a hydroxyurea solution. Carrying out condensation reaction on the generated hydroxyurea solution under an acidic condition, conveying the solution to a spray head through a pipeline, spraying the solution into a rotary drum granulator through the spray head, adding 700kg/t of powdery ammonium sulfate raw material and mineral source potassium fulvate into the rotary drum granulator, mixing and granulating, and carrying out condensation reaction again under the rotation of the rotary drum and the auxiliary action of steam to solidify reaction products into round particles with different sizes; conveying the ammonium sulfate round particles into a drying device, drying by drying air at 80-200 ℃ to reduce moisture, then conveying into a cooling and screening device, screening and selecting particles with the size of 2-4 mm to obtain qualified finished product particles, adding an anti-caking agent, carrying out anti-caking treatment, conveying into a finished product storage tank, storing, packaging and warehousing.
Example 2
A preparation method of ammonium sulfate containing urea aldehyde slow-release nitrogen components comprises the following steps:
and sequentially conveying 40kg/t of urea, 10kg/t of formalin and 10kg/t of water into a reaction kettle, mixing and heating to 40-95 ℃ in the reaction kettle under the condition of motor stirring, and carrying out addition reaction for 20-60 min to generate a hydroxyurea solution. Carrying out condensation reaction on the generated hydroxyurea solution under an acidic condition, conveying the solution to a spray head through a pipeline, spraying the solution into a rotary drum granulator through the spray head, adding 900kg/t of powdery ammonium sulfate raw material, mineral potassium fulvate and medium and trace elements such as magnesium oxide, zinc sulfate and boric acid into the rotary drum granulator, mixing and granulating, and carrying out condensation reaction again under the rotation of the rotary drum and the auxiliary action of steam to solidify reaction products into round particles with different sizes; conveying the ammonium sulfate round particles into a drying device, drying by drying air at 80-200 ℃ to reduce moisture, then conveying into a cooling and screening device, screening and selecting particles with the size of 2-4 mm to obtain qualified finished product particles, adding an anti-caking agent, carrying out anti-caking treatment, conveying into a finished product storage tank, storing, packaging and warehousing.
Example 3
A preparation method of ammonium sulfate containing urea aldehyde slow-release nitrogen components comprises the following steps:
sequentially conveying 200kg/t of urea, 60kg/t of formalin and 60kg/t of water into a reaction kettle, mixing and heating to 40-95 ℃ in the reaction kettle under the condition of motor stirring, and carrying out addition reaction for 100-200min to generate a hydroxyurea solution. Carrying out condensation reaction on the generated hydroxyurea solution under an acidic condition, conveying the solution to a spray head through a pipeline, spraying the solution into a rotary drum granulator through the spray head, adding 500kg/t of powdery ammonium sulfate raw material, mineral potassium fulvate and medium and trace elements such as magnesium oxide, zinc sulfate and boric acid into the rotary drum granulator, mixing and granulating, and carrying out condensation reaction again under the rotation of the rotary drum and the auxiliary action of steam to solidify reaction products into round particles with different sizes; conveying the ammonium sulfate round particles into a drying device, drying by drying air at 80-200 ℃ to reduce moisture, then conveying into a cooling and screening device, screening and selecting particles with the size of 2-4 mm to obtain qualified finished product particles, adding an anti-caking agent, carrying out anti-caking treatment, conveying into a finished product storage tank, storing, packaging and warehousing.
Example 4
A preparation method of ammonium sulfate containing urea aldehyde slow-release nitrogen components comprises the following steps:
and sequentially conveying 80kg/t of urea, 20kg/t of formalin and 20kg/t of water into a reaction kettle, mixing and heating to 40-95 ℃ in the reaction kettle under the condition of motor stirring, and carrying out addition reaction for 40-70min to generate a hydroxyurea solution. Carrying out condensation reaction on the generated hydroxyurea solution under an acidic condition, conveying the solution to a spray head through a pipeline, spraying the solution into a rotary drum granulator through the spray head, adding 800kg/t of powdery ammonium sulfate raw material into the rotary drum granulator, mixing and granulating, and carrying out condensation reaction again under the rotation of the rotary drum and the auxiliary action of steam to solidify reaction products into round particles with different sizes; conveying the ammonium sulfate round particles into a drying device, drying by drying air at 80-200 ℃ to reduce moisture, then conveying into a cooling and screening device, screening and selecting particles with the size of 2-4 mm to obtain qualified finished product particles, adding an anti-caking agent, carrying out anti-caking treatment, conveying into a finished product storage tank, storing, packaging and warehousing.
Example 5
A preparation method of ammonium sulfate containing urea aldehyde slow-release nitrogen components comprises the following steps:
and sequentially conveying 160kg/t of urea, 40kg/t of formalin and 40kg/t of water into a reaction kettle, mixing and heating the urea, the formalin and the water in the reaction kettle to 40-95 ℃ under the condition of motor stirring, and carrying out addition reaction for 80-120min to obtain a hydroxyurea solution. Carrying out condensation reaction on the generated hydroxyurea solution under an acidic condition, conveying the solution to a spray head through a pipeline, spraying the solution into a rotary drum granulator through the spray head, adding 600kg/t of powdery ammonium sulfate raw material and mineral source potassium fulvate into the rotary drum granulator, mixing and granulating, and carrying out condensation reaction again under the rotation of the rotary drum and the auxiliary action of steam to solidify reaction products into round particles with different sizes; conveying the ammonium sulfate round particles into a drying device, drying by drying air at 80-200 ℃ to reduce moisture, then conveying into a cooling and screening device, screening and selecting particles with the size of 2-4 mm to obtain qualified finished product particles, adding an anti-caking agent, carrying out anti-caking treatment, conveying into a finished product storage tank, storing, packaging and warehousing.
Test examples
The determination is carried out according to each experimental method in national standard GB/T535-:
sample (I) Appearance of the product N% H2O% Particle size Hardness of Colour(s)
Ammonium sulfate granules obtained in example 1 Spherical shape 22.64 1.0 96% 20N Coffee, yellow
Extruded ammonium sulfate granules Irregular shape 20.5 1.2 50% 6.4N Light yellow
The above description is only for the preferred embodiment of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements and the like made within the scope of the present invention should be included in the patent protection scope of the present invention.

Claims (8)

1. A preparation method of ammonium sulfate containing urea aldehyde slow-release nitrogen components is characterized by comprising the following steps:
(1) adding urea, formalin and water into a reaction kettle for mixing, wherein the adding amount of the raw materials is as follows: 40-200 kg/t of urea, 10-60 kg/t of formalin and 10-60 kg/t of water; heating the mixed raw materials to 40-95 ℃ under the condition of stirring, and carrying out addition reaction for 20-200 min to generate a hydroxyurea solution;
(2) carrying out condensation reaction on a hydroxyurea solution under an acidic condition, then spraying the solution into a rotary drum granulator, setting the granulation temperature to be 30-50 ℃, adding 400-900 kg/t of powdery ammonium sulfate raw material, mixing and granulating, carrying out condensation reaction again under the rotation action of the rotary drum, and setting the steam pressure to be 0.2-0.5 MPa as auxiliary steam to solidify the reaction product into round particles with different sizes;
(3) and (3) drying the ammonium sulfate round particles at a drying air temperature of 80-200 ℃ until the moisture content of the material is less than or equal to 1.0%, cooling, screening, and selecting 2-4 mm particles to obtain the ammonium sulfate particles containing the slow-release components.
2. The preparation method according to claim 1, wherein the raw materials in the step (1) are added in the following amounts: 80-160 kg/t of urea, 20-40 kg/t of formalin and 20-40 kg/t of water.
3. The preparation method according to claim 2, wherein the raw materials in the step (1) are added in the following amounts: 120kg/t of urea, 30kg/t of formalin and 30kg/t of water.
4. The preparation method of claim 1, wherein potassium fulvate, magnesium oxide, zinc sulfate and boric acid can be added during the preparation process.
5. The method according to claim 4, wherein the potassium fulvate is mineral potassium fulvate.
6. The method according to claim 1, wherein the ammonium sulfate granules containing the sustained-release component are prepared by adding an anti-caking agent to carry out an anti-caking treatment.
7. The method according to claim 1, wherein the concentration of formalin is 35 to 40%.
8. The method of claim 1, wherein the powdered ammonium sulfate feedstock is derived from coking and other industrial by-products.
CN202010196044.1A 2020-03-19 2020-03-19 Preparation method of ammonium sulfate containing urea aldehyde slow-release nitrogen component Pending CN113493364A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1307756A (en) * 1970-08-12 1973-02-21 Mitsubishi Gas Chemical Co Urea-containing granular fertilizers and process for producing the same
AU2003203753A1 (en) * 2002-04-16 2003-10-30 de Vreeze, Christiaan Mr A fertiliser
AU2004229098A1 (en) * 1998-04-17 2004-12-09 Airborne Industrial Minerals Inc. Fertilizer granulation method
CN1740119A (en) * 2004-08-23 2006-03-01 徐耀武 Production process of composite sulfur-base large grain urea
CN101913965A (en) * 2010-07-23 2010-12-15 山东谷丰源化肥有限公司 Urea formaldehyde sustained-release fertilizer and preparation method thereof
CN102503590A (en) * 2011-10-27 2012-06-20 山西师范大学 Production process for ammonium sulfate granules
CN103011982A (en) * 2012-12-29 2013-04-03 山东金正大生态工程股份有限公司 Industrial production method and device of urea-formaldehyde slow-release compound fertilizer

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1307756A (en) * 1970-08-12 1973-02-21 Mitsubishi Gas Chemical Co Urea-containing granular fertilizers and process for producing the same
AU2004229098A1 (en) * 1998-04-17 2004-12-09 Airborne Industrial Minerals Inc. Fertilizer granulation method
AU2003203753A1 (en) * 2002-04-16 2003-10-30 de Vreeze, Christiaan Mr A fertiliser
CN1740119A (en) * 2004-08-23 2006-03-01 徐耀武 Production process of composite sulfur-base large grain urea
CN101913965A (en) * 2010-07-23 2010-12-15 山东谷丰源化肥有限公司 Urea formaldehyde sustained-release fertilizer and preparation method thereof
CN102503590A (en) * 2011-10-27 2012-06-20 山西师范大学 Production process for ammonium sulfate granules
CN103011982A (en) * 2012-12-29 2013-04-03 山东金正大生态工程股份有限公司 Industrial production method and device of urea-formaldehyde slow-release compound fertilizer

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Application publication date: 20211012