CN112403391A - Binder for producing large-particle ammonium sulfate and preparation method thereof - Google Patents

Binder for producing large-particle ammonium sulfate and preparation method thereof Download PDF

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Publication number
CN112403391A
CN112403391A CN202011112143.3A CN202011112143A CN112403391A CN 112403391 A CN112403391 A CN 112403391A CN 202011112143 A CN202011112143 A CN 202011112143A CN 112403391 A CN112403391 A CN 112403391A
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China
Prior art keywords
ammonium sulfate
binder
slurry
monoammonium phosphate
stirring
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CN202011112143.3A
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Chinese (zh)
Inventor
李万清
方超
肖林波
窦德军
刘燕琴
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Hubei Sanning Chemical Co Ltd
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Hubei Sanning Chemical Co Ltd
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Priority to CN202011112143.3A priority Critical patent/CN112403391A/en
Publication of CN112403391A publication Critical patent/CN112403391A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/28Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic using special binding agents

Abstract

The invention discloses a preparation method of a binder for producing large-particle ammonium sulfate, which mainly comprises industrial monoammonium phosphate slag slurry, magnesium sulfate heptahydrate, polyacrylamide and sodium carboxymethylcellulose, and is mainly used for binding powdery ammonium sulfate into large-particle ammonium sulfate with the average particle size of 1.8-4.2 mm. Mixing and stirring industrial monoammonium phosphate neutralized slag slurry, water and magnesium sulfate heptahydrate uniformly, and simultaneously heating to 55-80 ℃; adding polyacrylamide into the materials, stirring, and reacting for 20-60min under heat preservation; ) Adding sodium carboxymethylcellulose, stirring to emulsify binder, cooling to room temperature to obtain milky viscous homogeneous liquid with viscosity of 40-70 mps.

Description

Binder for producing large-particle ammonium sulfate and preparation method thereof
Technical Field
The invention relates to a preparation method of a binder for producing large-particle ammonium sulfate, which mainly acts on binding powdery ammonium sulfate into large-particle ammonium sulfate with the average particle size of 1.8-4.2 mm.
Background
Along with the change from traditional agriculture to modern agriculture in China, the granulated fertilizer is widely favored by customers, is much higher than the fertilizer in the traditional form, and meanwhile, due to the sharp increase of the caprolactam capacity in China, the powdery ammonium sulfate as a byproduct of caprolactam is seriously excessive in capacity and serious in loss, and if the powdery ammonium sulfate with excessive capacity is produced into large-particle ammonium sulfate with good economic value, huge economic benefit is generated.
Currently, in the existing patent technologies, CN200910102609.9 applied in 2009 by queenson in Guizhou discloses a method for producing ammonium sulfate by using an organic-inorganic binder, but the method cannot be widely popularized; CN201310725079.X, applied in 2013, of Songbaoan university at Guizhou, discloses a composite binder for granulating an organic-inorganic compound fertilizer, but the binder uses a large amount of organic matters, so that the dissolution of large-particle ammonium sulfate is not facilitated; CN201780065167.8, israeli, filed in 2017, discloses a fertilizer granulation binder, but is not specialized for granulation of large-particle ammonium sulfate.
At present, the granulation rate of ammonium sulfate granules of 1.8mm to 2.0mm is 17% or less, the granulation rate of ammonium sulfate granules of 2.0mm to 2.5mm is 14% or less, the granulation rate of ammonium sulfate granules of 2.5mm to 3.5mm is 34% or less, and the granulation rate of ammonium sulfate granules of 3.5mm to 4.2mm is less than 5%.
At present, the production binder sold in the market has limited granulation effect and higher price, so the special binder for large-particle ammonium sulfate, which is environment-friendly, has great economic benefit and good granulation effect, is urgently needed to meet the market environment requirement.
Disclosure of Invention
The invention aims to provide a preparation method of a binder for producing large-particle ammonium sulfate, which mainly comprises industrial monoammonium phosphate slag slurry, magnesium sulfate heptahydrate, polyacrylamide and sodium carboxymethylcellulose, and is mainly used for binding powdery ammonium sulfate into large-particle ammonium sulfate with the average particle size of 1.8-4.2 mm.
The object of the invention is achieved by the following embodiments:
a process for preparing the adhesive used to prepare large-particle ammonium sulfate includes such steps as neutralizing the dregs slurry of industrial monoammonium phosphate (70-90%), magnesium sulfate heptahydrate (1-10%), polyacrylamide (1-5%), carboxymethylcellulose sodium (0.1-0.5%) and water (rest). The main function is to bond the powdery ammonium sulfate into large-particle ammonium sulfate with the average particle size of 1.8mm-4.2 mm.
The main component of the binder is neutralized slag slurry of industrial monoammonium phosphate.
Industrial monoammonium phosphateThe component of the neutralized slurry is P2O5 30-35%、N 7-8%、Fe2O3 1-2%、Al2O3 3-5%、MgO 6-8%、Ca 0.5-2%、Si 4-8%、F 5-9%。
The pH =6-7 of magnesium sulfate heptahydrate in the binder can adjust the pH of industrial monoammonium phosphate neutralized slag slurry to make the pH of the binder neutral, and the magnesium sulfate heptahydrate is used as a curing agent to accelerate the forming process of the ammonium sulfate particles.
Polyacrylamide in the binder is used as a polymerization agent, so that industrial monoammonium phosphate neutralized slurry and other additives are easier to aggregate, the binder is more uniform, and the phenomena of binder layering and the like are avoided.
The sodium carboxymethyl cellulose in the binder is used as a modifier to emulsify the binder and further thicken the binder.
The dosage of the binder is 0.1-2% of the mass of the powdery ammonium sulfate.
The average particle size of the large-particle ammonium sulfate produced by the binder is 1.8-4.2mm, the granulation rate is 50-80%, and the average compressive resistance of the large-particle ammonium sulfate is not less than 10N.
The preparation method of the adhesive comprises the following steps: (1) taking 70-90% of industrial monoammonium phosphate neutralized slag slurry, a certain mass of water and 1-10 parts of magnesium sulfate heptahydrate, mixing and stirring uniformly, and simultaneously heating to 55-80 ℃.
(2) And (2) adding 1-5% of polyacrylamide into the material obtained in the step (1), stirring, and carrying out heat preservation reaction for 20-60 min.
(3) And (3) adding 0.1-0.5% of sodium carboxymethylcellulose into the step (2), stirring to emulsify the binder, cooling to normal temperature to obtain milky viscous homogeneous liquid with the viscosity of 40-70mps (rotary viscometer), wherein the effective time is more than or equal to 100 days.
The invention is characterized in that:
(1) the main raw material of the adhesive is industrial monoammonium phosphate neutralized slag slurry, the influence on the nutrients of large-particle ammonium sulfate is small, and the adhesive is low in production cost, good in stability and non-toxic.
(2) The binder is used as a special binder for producing large-particle ammonium sulfate, the average particle size of the produced large-particle ammonium sulfate is 1.8-4.2mm, the granulation rate is 50-80%, and the average compressive resistance of the large-particle ammonium sulfate is not less than 10N.
Detailed Description
The following further describes embodiments of the present invention with reference to examples.
The preparation method of the adhesive comprises the following steps:
(1) and (3) taking industrial monoammonium phosphate neutralized slag slurry, water and magnesium sulfate heptahydrate, mixing and stirring uniformly, and simultaneously heating to 55-80 ℃.
(2) And (2) adding polyacrylamide into the material obtained in the step (1), stirring, and carrying out heat preservation reaction for 20-60 min.
(3) And (3) adding sodium carboxymethylcellulose into the step (2), stirring to emulsify the binder, cooling to normal temperature to obtain milky viscous homogeneous liquid with the viscosity of 40-70mps (rotational viscometer), and the effective time of more than or equal to 100 days.
The component of the neutralized slurry of industrial monoammonium phosphate is P2O5 32%±0.5%、N 7.3%±0.1%、Fe2O3 1.5%±0.1%、Al2O3 4.2%±0.1%、MgO 7.2%±0.2%、Ca 1.3%±0.1%、Si 6.3%±0.1%、F 8.5%±0.1%。
Example 1:
70kg of industrial monoammonium phosphate residue slurry, 5kg of magnesium sulfate heptahydrate, 3kg of polyacrylamide, 0.2kg of sodium carboxymethylcellulose and 21.8kg of water are mixed according to the steps to prepare the binder, and the viscosity is 50 mps. Taking 10 kg of powdery ammonium sulfate, adding a binder according to 1.2% of the mass of the ammonium sulfate, mixing the materials into slurry, uniformly mixing the slurry and the slurry, uniformly adding the slurry into a granulator, and controlling the proportion and the process operation parameters to obtain a qualified large-particle ammonium sulfate product, wherein the nutrient content of the ammonium sulfate (calculated as N + S) is 44.59% (N-20.81%, S-23.78%) and the average particle size of the product is 2.8mm, the granulation rate is 67.4%, and the average pressure resistance is 12N. In a warehouse with the annual average relative humidity of 60% and the temperature of 25-35 ℃, the breakage rate of the stockpiling for 3 months is 1.6%, and the caking phenomenon is avoided.
Example 2:
75kg of industrial monoammonium phosphate residue slurry, 5kg of magnesium sulfate heptahydrate, 3kg of polyacrylamide, 0.2kg of sodium carboxymethylcellulose and 16.8kg of water are mixed according to the steps to prepare the binder, and the viscosity is 52 mps. Taking 10 kg of powdery ammonium sulfate, adding a binder according to 1.2% of the mass of the ammonium sulfate, mixing the materials into slurry, uniformly mixing the slurry and the slurry, uniformly adding the slurry into a granulator, and controlling the proportion and the process operation parameters to obtain a qualified large-particle ammonium sulfate product, wherein the nutrient content of the ammonium sulfate (calculated as N + S) is 44.64% (N-20.83%, S-23.81%) of the product, the average particle size is 3.1mm, the granulation rate is 76.6%, and the average pressure resistance is 13N. In a warehouse with the annual average relative humidity of 60% and the temperature of 25-35 ℃, the breakage rate of the stockpiling for 3 months is 1.1%, and the caking phenomenon is avoided.
Example 3:
80kg of industrial monoammonium phosphate residue slurry, 5kg of magnesium sulfate heptahydrate, 3kg of polyacrylamide, 0.2kg of sodium carboxymethylcellulose and 11.8kg of water are mixed according to the steps to prepare the binder, and the viscosity is 63 mps. Taking 10 kg of powdery ammonium sulfate, adding a binder according to 1.2% of the mass of the ammonium sulfate, mixing the materials into slurry, uniformly mixing the slurry and the slurry, uniformly adding the slurry into a granulator, and controlling the proportion and the process operation parameters to obtain a qualified large-particle ammonium sulfate product, wherein the nutrient content of the ammonium sulfate (calculated as N + S) is 44.64% (N-20.87%, S-23.77%) and the average particle size of the product is 3.7mm, the granulation rate is 75.5%, and the average pressure resistance is 15N. In a warehouse with the annual average relative humidity of 60% and the temperature of 25-35 ℃, the breakage rate of the stockpiling for 3 months is 0%, and no caking phenomenon exists.
Example 4:
90kg of industrial monoammonium phosphate residue slurry, 5kg of magnesium sulfate heptahydrate, 3kg of polyacrylamide, 0.2kg of sodium carboxymethylcellulose and 1.8kg of water are mixed according to the steps to prepare the binder, and the viscosity is 68 mps. Taking 10 kg of powdery ammonium sulfate, adding a binder according to 1.2% of the mass of the ammonium sulfate, mixing the materials into slurry, uniformly mixing the slurry and the slurry, uniformly adding the slurry into a granulator, and controlling the proportion and the process operation parameters to obtain a qualified large-particle ammonium sulfate product, wherein the nutrient content of the ammonium sulfate (calculated as N + S) is 44.65% (N-21.27%, S-23.38%) and the average particle size of the product is 3.3mm, the granulation rate is 72.7%, and the average pressure resistance is 13N. In a warehouse with the annual average relative humidity of 60% and the temperature of 25-35 ℃, the breakage rate of the stockpiling for 3 months is 0%, and no caking phenomenon exists.
Example 5:
65kg of industrial monoammonium phosphate residue slurry, 5kg of magnesium sulfate heptahydrate, 3kg of polyacrylamide, 0.2kg of sodium carboxymethylcellulose and 26.8kg of water are mixed according to the steps to prepare the binder, and the viscosity is 50 mps. Taking 10 kg of powdery ammonium sulfate, adding a binder according to 1.2% of the mass of the ammonium sulfate, mixing the materials into slurry, uniformly mixing the slurry and the slurry, uniformly adding the slurry into a granulator, and controlling the proportion and the process operation parameters to obtain a qualified large-particle ammonium sulfate product, wherein the nutrient content of the ammonium sulfate (calculated as N + S) is 44.59% (N-20.81%, S-23.78%) and the average particle size of the product is 3.4mm, the granulation rate is 60.4%, and the average pressure resistance is 12N. In a warehouse with the annual average relative humidity of 60% and the temperature of 25-35 ℃, the breakage rate of the stockpiling for 3 months is 9.7%, and the caking phenomenon is avoided.
Example 6:
55kg of industrial monoammonium phosphate slag slurry, 5kg of magnesium sulfate heptahydrate, 3kg of polyacrylamide, 0.2kg of sodium carboxymethylcellulose and 36.8kg of water are mixed according to the steps to prepare the binder, and the viscosity is 46 mps. Taking 10 kg of powdery ammonium sulfate, adding a binder according to 1.2% of the mass of the ammonium sulfate, mixing the materials into slurry, uniformly mixing the slurry and the slurry, uniformly adding the slurry into a granulator, and controlling the proportion and the process operation parameters to obtain a qualified large-particle ammonium sulfate product, wherein the ammonium sulfate nutrient (calculated by N + S) is 44.64% (N-20.83%, S-23.81%) of the product with the average particle size of 3.1mm, the granulation rate is 45.3%, and the average pressure resistance is 9N. In a warehouse with the annual average relative humidity of 60% and the temperature of 25-35 ℃, the breakage rate of the stockpiling for 3 months is 12.3%, and the caking phenomenon of about 6.5% occurs.
Example 7:
50kg of industrial monoammonium phosphate slag slurry, 5kg of magnesium sulfate heptahydrate, 3kg of polyacrylamide, 0.2kg of sodium carboxymethylcellulose and 41.8kg of water are mixed according to the steps to prepare the binder, and the viscosity is 42 mps. Taking 10 kg of powdery ammonium sulfate, adding a binder according to 1.2% of the mass of the ammonium sulfate, mixing the materials into slurry, uniformly mixing the slurry and the slurry, uniformly adding the slurry into a granulator, and controlling the proportion and the process operation parameters to obtain a qualified large-particle ammonium sulfate product, wherein the nutrient content of the ammonium sulfate (calculated as N + S) is 44.64% (N-20.87%, S-23.77%) of the product, the average particle size is 3.7mm, the granulation rate is 33.4%, and the average pressure resistance is 7N. In a warehouse with the annual average relative humidity of 60% and the temperature of 25-35 ℃, the breakage rate of the stockpiling for 3 months is 22.5%, and the caking phenomenon of about 18.5% occurs.
Example 8:
80kg of industrial monoammonium phosphate residue slurry, 5kg of magnesium sulfate heptahydrate and 15kg of water are mixed according to the steps to prepare the binder, and the viscosity is 55 mps. Taking 10 kg of powdery ammonium sulfate, adding a binder according to 1.2% of the mass of the ammonium sulfate, mixing the materials into slurry, uniformly mixing the slurry and the slurry, uniformly adding the slurry into a granulator, and controlling the proportion and the technological operation parameters to obtain a qualified large-particle ammonium sulfate product, wherein the nutrient content of the ammonium sulfate (calculated as N + S) is 44.76% (N-20.89%, S-23.87%) and the average particle size of the product is 2.9mm, the granulation rate is 71.1%, and the average pressure resistance is 12N. In a warehouse with the annual average relative humidity of 60% and the temperature of 25-35 ℃, the breakage rate of the stockpiling for 3 months is 0.7%, and the caking phenomenon is avoided.
Example 9:
80kg of industrial monoammonium phosphate residue slurry, 5kg of polyacrylamide, 0.5kg of sodium carboxymethylcellulose and 14.5kg of water are mixed according to the steps to prepare the binder with the viscosity of 65 mps. Taking 10 kg of powdery ammonium sulfate, adding a binder according to 1.2% of the mass of the ammonium sulfate, mixing the materials into slurry, uniformly mixing the slurry and the slurry, uniformly adding the slurry into a granulator, and controlling the proportion and the process operation parameters to obtain a qualified large-particle ammonium sulfate product, wherein the nutrient content of the ammonium sulfate (calculated as N + S) is 44.66% (N-20.84%, S-23.82%) and the average particle size of the product is 2.9mm, the granulation rate is 70.08%, and the average pressure resistance is 12N. In a warehouse with the annual average relative humidity of 60% and the temperature of 25-35 ℃, the breakage rate of the stockpiling for 3 months is 0.5%, and the caking phenomenon is avoided.
Example 10:
taking 10 kg of powdery ammonium sulfate, adding 1.2 percent of the mass of the ammonium sulfate into industrial monoammonium phosphate to neutralize the slag slurry, wherein the viscosity of the industrial monoammonium phosphate neutralized slag slurry is 55 mps. The materials are adjusted into slurry, the slurry is evenly added into a granulator after being evenly mixed, the qualified large-particle ammonium sulfate product is prepared by controlling the proportion and the technological operation parameters, the ammonium sulfate nutrient (calculated by N + S) is 44.4 percent (N-20.71 percent, S-23.69 percent), the average particle size of the product is 3.0mm, the granulation rate is 62.18 percent, and the average pressure resistance is 12N. In a warehouse with the annual average relative humidity of 60% and the temperature of 25-35 ℃, the breakage rate of the stockpiling for 3 months is 20.8%, and the caking phenomenon is 18%.

Claims (4)

1. The binder for producing large-particle ammonium sulfate is characterized by comprising 70-90% of neutralized slag slurry of industrial monoammonium phosphate, 1-10% of magnesium sulfate heptahydrate, 1-5% of polyacrylamide, 0.1-0.5% of sodium carboxymethylcellulose and the balance of water.
2. The binder for producing large-particle ammonium sulfate according to claim 1, wherein the component of the neutralized slurry of industrial monoammonium phosphate is P2O5 30-35%、N 7-8%、Fe2O3 1-2%、Al2O3 3-5%、MgO 6-8%、Ca 0.5-2%、Si 4-8%、F 5-9%。
3. The binder for producing large ammonium sulfate particles as claimed in claim 1, wherein the magnesium sulfate heptahydrate in the binder has a pH of 6 to 7.
4. The method for preparing a binder for producing large ammonium sulfate particles according to any one of claims 1 to 3, wherein the method for preparing the binder comprises: (1) mixing and stirring industrial monoammonium phosphate neutralized slag slurry, water and magnesium sulfate heptahydrate uniformly, and simultaneously heating to 55-80 ℃;
(2) adding polyacrylamide into the material obtained in the step (1), stirring, and carrying out heat preservation reaction for 20-60 min;
(3) and (3) adding sodium carboxymethylcellulose into the step (2), stirring to emulsify the binder, and cooling to normal temperature to obtain the binder with the viscosity of 40-70 mps.
CN202011112143.3A 2020-10-16 2020-10-16 Binder for producing large-particle ammonium sulfate and preparation method thereof Pending CN112403391A (en)

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Citations (8)

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Publication number Priority date Publication date Assignee Title
US5078779A (en) * 1988-12-01 1992-01-07 Martin Marietta Magnesia Specialties Inc. Binder for the granulation of fertilizers such as ammonium sulfate
CN101570455A (en) * 2009-06-05 2009-11-04 瓮福(集团)有限责任公司 Method for preparing particle ammonium sulfate product by organic-inorganic binder
CN101575222A (en) * 2009-06-05 2009-11-11 瓮福(集团)有限责任公司 Method for producing ammonium sulphate grain products by using inorganic caking agent
CN102674931A (en) * 2012-05-16 2012-09-19 瓮福(集团)有限责任公司 Method for co-producing ammonium sulfate phosphate fertilizer by using powder monoammonium phosphate production device
CN105272766A (en) * 2015-11-26 2016-01-27 北京清迈华清控股(集团)有限公司 Method for producing novel saline-alkaline restoration fertilizer by utilizing high-silicon iron tailings and product
CN106588128A (en) * 2016-12-07 2017-04-26 湖北三宁化工股份有限公司 Method for producing large-particle ammonium sulfate
CN109704863A (en) * 2019-02-18 2019-05-03 湖北三宁化工股份有限公司 A kind of bulky grain sulfur-containing nitrogen fertilizer and preparation method thereof
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5078779A (en) * 1988-12-01 1992-01-07 Martin Marietta Magnesia Specialties Inc. Binder for the granulation of fertilizers such as ammonium sulfate
CN101570455A (en) * 2009-06-05 2009-11-04 瓮福(集团)有限责任公司 Method for preparing particle ammonium sulfate product by organic-inorganic binder
CN101575222A (en) * 2009-06-05 2009-11-11 瓮福(集团)有限责任公司 Method for producing ammonium sulphate grain products by using inorganic caking agent
CN102674931A (en) * 2012-05-16 2012-09-19 瓮福(集团)有限责任公司 Method for co-producing ammonium sulfate phosphate fertilizer by using powder monoammonium phosphate production device
CN105272766A (en) * 2015-11-26 2016-01-27 北京清迈华清控股(集团)有限公司 Method for producing novel saline-alkaline restoration fertilizer by utilizing high-silicon iron tailings and product
CN106588128A (en) * 2016-12-07 2017-04-26 湖北三宁化工股份有限公司 Method for producing large-particle ammonium sulfate
CN109704863A (en) * 2019-02-18 2019-05-03 湖北三宁化工股份有限公司 A kind of bulky grain sulfur-containing nitrogen fertilizer and preparation method thereof
CN110218116A (en) * 2019-06-18 2019-09-10 北京尧之龙科技发展有限公司 A kind of granular compound fertilizer adhesive for granulating and preparation method thereof

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