CN114349572B - Method for producing compound fertilizer containing polymerized phosphorus by using citric soluble phosphorus slag - Google Patents
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Abstract
The invention discloses a method for producing a compound fertilizer containing polymerized phosphorus by utilizing citric soluble phosphorus slag, and relates to the technical field of compound fertilizer production containing polymerized phosphorus. Mixing citrate soluble phosphorus slag and phosphoric acid uniformly to prepare slag slurry with the solid content of 30-70 percent; adding urea into the slurry, heating to 80-130 ℃, stirring and reacting for 45-90 min to obtain neutralized slurry; adding a potassium source into the neutralized slurry, heating to 130-250 ℃, and carrying out synthetic reaction for 30-150 min to obtain a primary product containing the polymerized phosphorus compound fertilizer; and cooling and crushing the primary product, and granulating to obtain a granular finished product of the compound fertilizer containing the polymerized phosphorus. Water-soluble P in the obtained finished product 2 O 5 Occupied by effective P 2 O 5 More than 75% of the content, polymerizing P 2 O 5 Occupied by effective P 2 O 5 The content is more than 35 percent, and the pH value of the product is 6-8. The method has the advantages of simple process, strong operability, no waste generation in the process, environmental friendliness and provision of an effective way for efficiently recycling the citrate soluble phosphorus slag.
Description
Technical Field
The invention relates to the technical field of production of compound fertilizers containing polymerized phosphorus, in particular to a method for producing compound fertilizers containing polymerized phosphorus by utilizing citric acid soluble phosphorus slag.
Background
In the method for measuring phosphate fertilizer, phosphorus which is difficult to dissolve or slightly soluble in water but can be extracted by a neutral ammonium citrate solution or a solution with c (EDTA) =0.2mol/L is called citrate-soluble phosphorus. The citrate soluble phosphorus is directly applied to soil, needs weak acid secreted by crop roots and can be absorbed by plants after being dissolved, so that the citrate soluble phosphorus is low in utilization rate and poor in fertilizer effect and is not beneficial to agricultural application. In recent years, with the increasing demand of the market for high-quality compound fertilizers and water-soluble fertilizers, different byproducts are associated with the production process of the phosphorus compound fertilizer according to different production products. For example, in the production of industrial monoammonium phosphate, the phosphorus slag produced by filtering after wet-process phosphoric acid is neutralized by ammonia has the byproduct amount reaching more than half of the yield of the industrial monoammonium phosphate, and the effective phosphorus content of the part of the phosphorus slag is 25-35 percent, and the water-soluble phosphorus content is 5-15 percent; the phosphorus-potassium slag as the by-product in the extraction process for producing potassium dihydrogen phosphate contains 35-45% of available phosphorus, 5-10% of water-soluble phosphorus and 5-10% of potassium oxide. The phosphorus slag has high available phosphorus and low water-soluble phosphorus, the direct production of compound fertilizers can not meet the requirements of national quality standards, the phosphorus slag belongs to high citrate soluble phosphorus slag, the phosphorus content is high, the utilization value is very high, and the phosphorus slag contains medium and trace elements such as Fe, mg, ca, S, si and the like, but the phosphorus slag is difficult to be directly utilized in the existing production system. At present, the utilization of citrate soluble phosphorus slag becomes the bottleneck of enterprises in developing high-quality fertilizers.
Patent CN110372434A discloses a method for recovering nutrient elements from industrial monoammonium phosphate slag, which comprises the steps of adding water into raw material industrial ammonium slag for pulping, carrying out acidolysis by sulfuric acid, nitric acid or hydrochloric acid, neutralizing by urea, concentrating and drying to obtain a compound fertilizer containing thiourea. In order to ensure that the slurry can flow fully, a large amount of water is required to be added in the process to pulp the industrial ammonium slag, and the sulfuric acid, the nitric acid or the hydrochloric acid selected in the acidolysis process has strong activity, reacts violently with the slurry, can generate a large amount of reaction heat, and has high requirements on the high-temperature resistance and the corrosion resistance of equipment.
Patent CN110357670A discloses a method for preparing a compound fertilizer containing ammonium polyphosphate by using industrial monoammonium phosphate slag, which comprises the steps of adding water into the industrial ammonium slag as a raw material to prepare slurry, adding sulfuric acid to hydrolyze, neutralizing urea, adding a condensing agent to perform a condensation reaction, foaming, curing and crushing to obtain a binary fertilizer containing ammonium polyphosphate, and granulating with other compound fertilizers to obtain the compound fertilizer containing ammonium polyphosphate. In order to make the slurry flow sufficiently, a large amount of water is required to be added in the process to pulp the industrial ammonium slag, and high-concentration sulfuric acid is selected in the acidolysis process, reacts violently with the slurry, generates a large amount of reaction heat, and has high requirements on the high-temperature resistance and corrosion resistance of equipment. In the reaction process, a condensing agent is additionally added to complete the condensation reaction to obtain the binary fertilizer containing the ammonium polyphosphate, and other compound fertilizers are added according to the content of nitrogen and phosphorus to produce the compound fertilizer, so that the production process is complex.
Disclosure of Invention
The invention aims to provide a method for producing a compound fertilizer containing polymerized phosphorus by utilizing citric soluble phosphorus slag, which solves the problems of high requirement on equipment, complex process and large consumption of water resources in the prior art.
In order to solve the technical problem, the invention adopts the following technical scheme: a method for producing a compound fertilizer containing polymeric phosphorus by utilizing citrate soluble phosphorus slag is characterized by comprising the following steps:
s1, uniformly mixing citric soluble phosphorus slag and phosphoric acid to prepare slag slurry with the solid content of 30-70%.
S2, adding urea into the slurry, heating to 80-130 ℃, and stirring for reacting for 45-90 min to obtain neutralized slurry.
S3, adding a potassium source into the neutralized slurry, heating to 130-250 ℃, and carrying out synthetic reaction for 30-150 min to obtain a primary product of the compound fertilizer containing the polymeric phosphorus. The reaction temperature is lower than 130 ℃, P 2 O 5 Insufficient polymerization results in polymerization P in the system 2 O 5 The content is low; the reaction temperature is higher than 250 ℃, and a large amount of P with high polymerization degree appears 2 O 5 The product is applied to soil and has high polymerization degree P 2 O 5 Is difficult to be converted into orthophosphate which is easy to be absorbed by crops and is not good for fertilizer efficiency.
And S4, cooling and crushing the primary product, and granulating to obtain a granular finished product of the compound fertilizer containing the polymerized phosphorus.
The further technical proposal is that the citrate soluble phosphorus slag in the step S1 is monoammonium phosphate filter slag or potassium dihydrogen phosphate by-product phosphorus potassium slag, wherein the dry basis P 2 O 5 The content of the P is 25 to 50 percent, wherein the water-soluble P 2 O 5 Occupy effective P 2 O 5 15-40% of the content.
The further technical proposal is that the phosphoric acid in the step S1 is wet phosphoric acid or purified phosphoric acid raffinate acid, wherein P 2 O 5 The content is 20-50%.
A further technical scheme is that in the step S2, the urea is mixed according to the mol ratio of urea: p 2 O 5 And (5) metering and adding 1-4. Urea is a condensing agent for synthesis reaction and one of the sources of N nutrients in the fertilizer, and the urea addition is too low, so that the synthesis reaction is incomplete, and polymerized P in the system 2 O 5 The content is low; the addition of the urea is too high, and the urea is not added into the reactor,resulting in incomplete urea decomposition, low nitrogen recovery and other disadvantages.
The further technical scheme is that in the step S3, the addition amount of the potassium source is adjusted according to the nutrient structure of the finished compound fertilizer containing the polymerized phosphorus, and the potassium source is at least one of potassium sulfate, potassium chloride and potassium nitrate.
According to the structural requirement of the finished product nutrient of the compound fertilizer containing the polymerized phosphorus, at least one of zinc sulfate heptahydrate and borax is added while the potassium source is added in the step S3.
The further technical proposal is that the water-solubility P in the finished product of the compound fertilizer containing the polymerized phosphorus 2 O 5 Occupy effective P 2 O 5 More than 75% of the content, polymerizing P 2 O 5 Occupied by effective P 2 O 5 The content is more than 35 percent, and the pH value of the product is 6-8.
The reaction mechanism is as follows: phosphoric acid is mixed with citric soluble phosphorus slag, pulping is directly carried out on the premise of not consuming a large amount of water resources, the activity of the phosphoric acid is relatively weak in the acidolysis process, the reaction process is milder, the citric soluble phosphorus is activated and the phosphorus element is brought in, so that the phosphorus content in the finished product is greatly improved. Adding urea for neutralization, adding a potassium source, synthesizing a multi-element compound fertilizer by one step, and converting citrate soluble phosphorus into water soluble phosphorus and polymeric phosphorus to realize the high-efficiency utilization of citrate soluble phosphorus. The urea not only provides N nutrient, but also serves as a condensing agent, the high-temperature synthesized polymeric phosphorus has the function of chelating metal ions, and medium and trace elements such as insoluble iron, magnesium and the like in the phosphorus slag are converted into a soluble state capable of being absorbed by crops, so that the quality of the compound fertilizer is effectively improved.
Compared with the prior art, the invention has the beneficial effects that:
1. phosphoric acid is mixed with citric soluble phosphorus slag, direct pulping is carried out on the premise of not consuming a large amount of water resources, the phosphoric acid activity is relatively weak in the acidolysis process, the reaction process is milder, phosphorus elements are brought in while citric soluble phosphorus is activated, and the phosphorus content in a finished product is greatly improved.
2. According to the method, citric soluble phosphorus is converted into water soluble phosphorus and polymeric phosphorus through a high-temperature synthesis reaction, nutrients such as nitrogen, phosphorus and potassium in the citric soluble phosphorus slag are fully converted into fertilizer nutrients, and the high-efficiency utilization of the citric soluble phosphorus slag is realized.
3. The polymeric phosphorus obtained by the high-temperature synthesis reaction has a certain effect of chelating metal ions, can convert the middle and trace elements such as insoluble iron, magnesium and the like in the citrate soluble phosphorus slag into a soluble state which can be absorbed by crops, is beneficial to the efficient recycling of the citrate soluble phosphorus slag, and can effectively improve the quality of a compound fertilizer product.
4. The method directly obtains the compound fertilizer product, the phosphorus element is orthophosphate and polymeric phosphorus, after the fertilizer is applied, the orthophosphate can rapidly provide the phosphorus element for crops, and the polymeric phosphorus is slowly converted into the orthophosphate, so that the phosphorus element is not fixed by soil metal ions in the growth period of the crops, the phosphorus element can be supplied for the crops for a long time, and the effect of prolonging the fertilizer efficiency is achieved.
5. According to the invention, a potassium source is directly added from the synthesis step, potassium element directly participates in polymerization reaction to produce the ternary compound fertilizer containing ammonium polyphosphate, potassium polyphosphate and ammonium potassium polyphosphate, the ternary compound fertilizer is obtained by one-step synthesis, and the polymerized nitrogen, phosphorus and potassium are more beneficial to crop growth.
6. The method has the advantages of simple process, strong operability, no waste generation in the process, environmental friendliness and provision of an effective way for efficiently recycling the citrate soluble phosphorus slag.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Taking monoammonium phosphate filter residues, wherein dry base nutrients comprise N:6.96% of total P 2 O 5 :36.71%, effective P 2 O 5 :34.01%, water-soluble P 2 O 5 Occupied by effective P 2 O 5 The content is 29.21%; the phosphoric acid is wet-process phosphoric acid, P 2 O 5 ：25.12％。
Mixing 1200g of monoammonium phosphate filter residue and 800g of phosphoric acid in a mixing device to obtain a slag slurry with a solid content of 63.0%, adding 465g of urea into the slag slurry, heating to 120 ℃, carrying out neutralization reaction for 65min to obtain phosphorus slag neutralized slurry, transferring the phosphorus slag neutralized slurry to a high-temperature synthesizer, simultaneously adding 480g of potassium sulfate for synthesis reaction at the reaction temperature of 190 ℃ for 90min, cooling and crushing to obtain 2527g of compound fertilizer containing polymerized phosphorus, wherein the nutrient composition is as follows: n:9.97% of available P 2 O 5 :25.27% of water-soluble P 2 O 5 ：20.41％、K 2 O:9.49%, pH: 6.7, average degree of polymerization 4.52. Wherein the water solubility P 2 O 5 Occupied by effective P 2 O 5 80.77% of the content, polymerization P 2 O 5 Occupied by effective P 2 O 5 The content is 52.4 percent.
After the compound fertilizer is subjected to a drum granulation process, the granular polymerized phosphorus compound fertilizer with nitrogen, phosphorus and potassium nutrients of 10-25-10 and the grain size of 0.5-2.0 mm is obtained.
Example 2
Taking monoammonium phosphate filter residues, wherein dry base nutrients comprise N:6.96% of total P 2 O 5 :36.71%, effective P 2 O 5 :34.01%, water-soluble P 2 O 5 Occupy effective P 2 O 5 The content is 29.21%; phosphoric acid is the raffinate acid, P, which is the byproduct of wet-process phosphoric acid purification 2 O 5 ：45.61％。
Mixing 1100g of monoammonium phosphate filter residue and 900g of phosphoric acid in a mixing device to obtain slag slurry with the solid content of 58.5%, adding 720g of urea into the slag slurry, heating to 130 ℃, performing neutralization reaction for 50min to obtain phosphorus slag neutralized slurry, transferring the phosphorus slag neutralized slurry to a high-temperature synthesizer, simultaneously adding 240g of potassium nitrate to perform synthesis reaction, wherein the reaction temperature is 175 ℃, the reaction time is 120min, cooling and crushing to obtain 2360g of the phosphorus-containing compound fertilizer, and the nutrient composition is as follows: n:15.23% effective P 2 O 5 :33.29% of water-soluble P 2 O 5 ：28.28％、K 2 O:5.08%, pH 6.6, and average degree of polymerization 4.06. Wherein the water solubility P 2 O 5 Occupied by effective P 2 O 5 84.95% of the content, polymerization P 2 O 5 Occupied by effective P 2 O 5 47.6 percent of the content.
After the compound fertilizer is subjected to a disc granulation process, the granular phosphorus-potassium compound fertilizer with 15-33-5 of nitrogen-phosphorus-potassium nutrients and 0.5-2.0 mm of grain size is obtained.
Example 3
Taking monoammonium phosphate filter residues, wherein the dry basis nutrient comprises N:6.96% of total P 2 O 5 :28.82, effective P 2 O 5 :26.70% of water-soluble P 2 O 5 Occupied by effective P 2 O 5 The content is 24.34%; phosphoric acid is the raffinate acid, P, which is the byproduct of wet-process phosphoric acid purification 2 O 5 ：38.76％。
Mixing 600g of monoammonium phosphate filter residue with 1400g of phosphoric acid in a mixing device to obtain a slurry with a solid content of 36.3%, adding 770g of urea into the slurry, heating to 115 ℃, carrying out neutralization reaction for 60min to obtain phosphorus slag neutralized slurry, transferring the phosphorus slag neutralized slurry to a high-temperature synthesizer, simultaneously adding 480g of potassium chloride for synthesis reaction at 165 ℃ for 100min, cooling and crushing to obtain 2882g of the compound fertilizer containing polymerized phosphorus, wherein the nutrient composition is as follows: n:9.84% effective P 2 O 5 :24.42% water-soluble P 2 O 5 ：22.50％、K 2 O:9.99%, pH 6.9, and average degree of polymerization 4.06. Wherein the water solubility P 2 O 5 Occupied by effective P 2 O 5 92.12% of content, polymerization P 2 O 5 Occupied by effective P 2 O 5 The content is 53.22 percent.
After the compound fertilizer is subjected to a disc granulation process, the granular phosphorus-potassium compound fertilizer with 10-24-10 of nitrogen-phosphorus-potassium nutrients and 0.5-2.0 mm of grain size is obtained.
Example 4
Taking citrate soluble phosphorus slag (potassium dihydrogen phosphate byproduct phosphorus potassium slag) and dry base nutrient composition K 2 O:8.35% of total P 2 O 5 :40.65%, effective P 2 O 5 :40.39% of water-soluble P 2 O 5 Occupied by effective P 2 O 5 Content 32.08%; extraction residue produced by using phosphoric acid as by-product of wet-process purified phosphoric acidAcid, P 2 O 5 ：26.58％。
1300g of citrate soluble phosphorus slag and 700g of phosphoric acid are mixed in a mixing device to prepare slag slurry with the solid content of 67.9 percent, 800g of urea is added into the slag slurry, the temperature is raised to 120 ℃, neutralization reaction is carried out for 70min to obtain phosphorus slag neutralized slurry, the phosphorus slag neutralized slurry is transferred to a high-temperature synthesizer, 100g of zinc sulfate heptahydrate and 190g of borax are simultaneously added for synthesis reaction, the reaction temperature is 210 ℃, the reaction time is 50min, and 2528g of the compound fertilizer containing polymerized phosphorus is obtained after cooling and crushing, and the nutrient composition is as follows: n:11.82% effective P 2 O 5 :29.75% water-soluble P 2 O 5 ：24.89％、K 2 O:4.77%, zn:1%, B:1%, pH 7.3, and average degree of polymerization 3.90. Wherein the water solubility of P 2 O 5 Occupy effective P 2 O 5 83.66% of the content, polymerization P 2 O 5 Occupied by effective P 2 O 5 43.09 percent of the content.
After the compound fertilizer is subjected to a micro-fine particle extrusion granulation process, the granular polymerized phosphorus compound fertilizer with the nitrogen, phosphorus and potassium nutrients of 12-30-5+ TE and the particle size of 0.5-2.0 mm is obtained.
Example 5
Taking citrate soluble phosphorus slag (potassium dihydrogen phosphate byproduct phosphorus potassium slag) and dry base nutrient composition K 2 O:8.35% of total P 2 O 5 :40.65% of water-soluble P 2 O 5 Occupied by effective P 2 O 5 Content 32.08%; phosphoric acid is the raffinate acid, P, which is the byproduct of wet-process phosphoric acid purification 2 O 5 ：26.58％。
1340g of citrate soluble phosphorus slag and 660g of phosphoric acid are mixed in a mixing device to prepare slag slurry with the solid content of 69.2%, 920g of urea is added into the slag slurry, the temperature is raised to 100 ℃, neutralization reaction is carried out for 65min to obtain phosphorus slag neutralized slurry, the phosphorus slag neutralized slurry is transferred to a high-temperature synthesizer, 260g of potassium nitrate is added to carry out synthesis reaction at the same time, the reaction temperature is 200 ℃, the reaction time is 60min, 2375g of polymeric phosphorus-containing compound fertilizer is obtained after cooling and crushing, and the nutrient composition is as follows: n:15.23% effective P 2 O 5 :29.26% water-soluble P 2 O 5 ：23.29％、K 2 O：9.84 percent, pH value of 5.61 and average polymerization degree of 3.95. Wherein the water solubility of P 2 O 5 Occupied by effective P 2 O 5 79.6% of the content, polymerization P 2 O 5 Occupy effective P 2 O 5 44.20 percent of the content and the pH value is 6.5.
After the compound fertilizer is granulated by a fluidized bed, the granular polymeric phosphorus compound fertilizer with 15-30-10 of nitrogen, phosphorus and potassium nutrients and 0.5-2.0 m of grain diameter is obtained.
Example 6
Taking citrate soluble phosphorus slag (potassium dihydrogen phosphate byproduct phosphorus potassium slag) and dry base nutrient composition K 2 O:8.35% of total P 2 O 5 :40.65%, effective P 2 O 5 :40.39% water-soluble P 2 O 5 Occupy effective P 2 O 5 The content is 32.08%; phosphoric acid is the raffinate acid, P, by-product of wet purification of phosphoric acid 2 O 5 ：38.76％。
Mixing 800g of citrate soluble phosphorus slag and 1200g of phosphoric acid in a mixing device to prepare slag slurry with the solid content of 42.5%, adding 810g of urea into the slag slurry, heating to 125 ℃, performing neutralization reaction for 75min to obtain phosphorus slag neutralized slurry, transferring the phosphorus slag neutralized slurry to a high-temperature synthesizer, simultaneously adding 450g of potassium chloride, 140g of zinc sulfate heptahydrate and 140g of borax to perform synthesis reaction at the reaction temperature of 220 ℃, performing reaction for 70min, cooling and crushing to obtain 3095g of a composite fertilizer containing polymerized phosphorus, wherein the nutrient composition is as follows: n:10.28% effective P 2 O 5 :23.07% of water-soluble P 2 O 5 ：20.67％、K 2 O:10.88%, zn:1%, B:0.5%, pH 7.3, and average degree of polymerization 3.90. Wherein the water solubility P 2 O 5 Occupy effective P 2 O 5 89.61% of the content, 30-40% of the polymerization occupancy P 2 O 5 The content is 53.09%.
After the compound fertilizer is subjected to a micro-fine particle extrusion granulation process, the granular polymerized phosphorus compound fertilizer with nitrogen, phosphorus and potassium nutrients of 10-23-10+ TE and particle size of 0.5-2.0 mm is obtained.
While the invention has been described herein with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the scope of the disclosure.
Claims (6)
1. A method for producing a compound fertilizer containing polymeric phosphorus by utilizing citrate soluble phosphorus slag is characterized by comprising the following steps:
s1, uniformly mixing citric soluble phosphorus slag and phosphoric acid to prepare slag slurry with the solid content of 30-70%;
s2, adding urea into the slurry, heating to 100-130 ℃, and stirring for reacting for 45-90 min to obtain neutralized slurry; the urea is prepared by mixing the following components in molar ratio: p is 2 O 5 Metering and adding the mixture in a ratio of 1 to 4;
s3, adding a potassium source into the neutralized slurry, heating to 165-220 ℃, and carrying out synthetic reaction for 50-120 min to obtain a primary product containing the polymerized phosphorus compound fertilizer;
s4, cooling and crushing the primary product, and granulating to obtain a granular finished product of the compound fertilizer containing the polymerized phosphorus;
the citrate soluble phosphorus slag is potassium dihydrogen phosphate and byproduct phosphorus potassium slag, dry basis P 2 O 5 The content of the P is 25 to 50 percent, wherein the water-soluble P 2 O 5 Occupied by effective P 2 O 5 15-40% of the content of phosphoric acid, wherein the phosphoric acid is purified phosphoric acid raffinate acid, and P is 2 O 5 The content is 20-50%.
2. The method for producing the compound fertilizer containing the polymerized phosphorus by using the citric soluble phosphorus slag as claimed in claim 1, is characterized in that: and in the step S1, the citric soluble phosphorus slag is monoammonium phosphate filter residue.
3. The method for producing the compound fertilizer containing the polymerized phosphorus by using the citric soluble phosphorus slag as claimed in claim 1, is characterized in that: the phosphoric acid in step S1 is wet-process phosphoric acid.
4. The method for producing the compound fertilizer containing the polymerized phosphorus by using the citric soluble phosphorus slag as claimed in claim 1, is characterized in that: and S3, adjusting the adding amount of the potassium source according to the nutrient structure of the finished product of the compound fertilizer containing the required polymerized phosphorus, wherein the potassium source is at least one of potassium sulfate, potassium chloride and potassium nitrate.
5. The method for producing the compound fertilizer containing the polymerized phosphorus by utilizing the citric soluble phosphorus slag according to the claim 1, which is characterized in that: and according to the nutrient structure requirement of the finished product of the compound fertilizer containing the polymerized phosphorus, adding at least one of zinc sulfate heptahydrate and borax while adding the potassium source in the step S3.
6. The method for producing the compound fertilizer containing the polymerized phosphorus by utilizing the citric soluble phosphorus slag according to the claim 1, which is characterized in that: the water-soluble P in the finished product of the compound fertilizer containing the polymerized phosphorus 2 O 5 Occupy effective P 2 O 5 More than 75% of the content, polymerizing P 2 O 5 Occupied by effective P 2 O 5 The content is more than 35 percent, and the pH value of the product is 6-8.
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