CN103130205B - The method of the water-soluble ammonium phosphate sulfate of a kind of manufacture level monoammonium phosphate co-production - Google Patents
The method of the water-soluble ammonium phosphate sulfate of a kind of manufacture level monoammonium phosphate co-production Download PDFInfo
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- CN103130205B CN103130205B CN201310076353.5A CN201310076353A CN103130205B CN 103130205 B CN103130205 B CN 103130205B CN 201310076353 A CN201310076353 A CN 201310076353A CN 103130205 B CN103130205 B CN 103130205B
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Abstract
The present invention relates to the method for the water-soluble ammonium phosphate sulfate of a kind of manufacture level monoammonium phosphate co-production, its step is as follows: A, get the agricultural phosphorus ammonium of total nutrient 60%, be dissolved in water by 1.5 times of its quality, add the pH value to 4.2 of bicarbonate of ammonia or ammoniacal liquor adjustment slip again, react and carry out press filtration after 30 minutes; B, press filtration gained phosphorus ammonium clear liquid is carried out concentrating under reduced pressure, then the phosphor ammonium slurry concentrated is delivered to crystallizer tank carries out crystallisation by cooling, then obtained industrial grade monoammonium phosphate product after centrifugation, drying; C, be heated to 85 DEG C by mother liquid obtained for centrifugation, regulate pH value to 4.5-5.0, constant temperature carried out press filtration after 20 minutes, and clear liquid send spray drying system to be drying to obtain pulverulent water-soluble ammonium phosphate sulfate after normal pressure is concentrated.The present invention produces desired raw material wide material sources, cheap and easy to get, and technique is simple, with short production cycle, three-waste free discharge, and energy consumption is low, and the mother liquor produced in production process does not need supporting fertilizer system to digest, thus reduces production cost.
Description
Technical field
The invention belongs to industrial grade monoammonium phosphate production field, relate to a kind of production method using agricultural monoammonium phosphate and diammonium phosphate, bicarbonate of ammonia or the water-soluble ammonium phosphate sulfate of ammoniacal liquor manufacture level monoammonium phosphate co-production.
Background technology
The purposes of industrial grade monoammonium phosphate is comparatively extensive, and be mainly used as ABC powder extinguishing agent, ammonium polyphosphate flame retardant and drip irrigation and spray fertile main raw material, be also used in the industries such as medicine, food, paper, timber in addition, its market outlook are very good.Water-soluble ammonium phosphate sulfate can be directly used in and drip a sprinkler irrigation fertilization, also can be used as the raw materials for production of water soluble fertilizer, and along with the continuous popularization of national water-saving agriculture and water-fertilizer integral, Water soluble fertilizer market will progressively expand, and water-soluble ammonium phosphate sulfate market demand will constantly increase.In prior art, phosphoric acid is that the technology of raw material production industrial grade monoammonium phosphate becomes main flow in a wet process, and a large amount of mother liquors that the method produces must pass through fertilizer system recoveries, the common fertilizer that production added value is extremely low.Patent report is there is no at present about with the production method of the water-soluble ammonium phosphate sulfate of agricultural phosphorus ammonium manufacture level monoammonium phosphate co-production.
Summary of the invention
The object of the invention is the defect for existing industrial grade monoammonium phosphate technology, thering is provided a kind of is the novel technique route of the water-soluble ammonium phosphate sulfate of raw material production high-quality industrial grade monoammonium phosphate co-production with agricultural phosphorus ammonium, is intended at utmost to reduce the production cost of industrial grade monoammonium phosphate and improves its economic benefit.
To achieve these goals, the present invention by the following technical solutions, the steps include:
A, get the agricultural phosphorus ammonium of a certain amount of total nutrient 60%, be dissolved in water by 1.5 times of its quality, control temperature 85 DEG C, dissolved after 15 minutes, add the pH value to 4.2 of amount of ammonium bicarbonate or ammoniacal liquor adjustment slip again, react, after 30 minutes, slurry pipeline transport is carried out press filtration to plate-and-frame filter press.
B, press filtration gained phosphorus ammonium clear liquid is delivered to vacuum concentration system carries out concentrating under reduced pressure, heating is stopped to during density 1.36-1.38g/ml, again the phosphor ammonium slurry concentrated is delivered to crystallizer tank and carries out crystallisation by cooling, cooling terminal temperature controls at 35-40 DEG C, then obtained industrial grade monoammonium phosphate product after centrifugation, drying.Gained filter residue about 65 DEG C hot water wash, and wash water returns to steps A for dissolved phosphorus ammonium, and filter residue sells separately as slag fertilizer.
C, be heated to 85 DEG C by mother liquid obtained for centrifugation, regulate pH value to 4.5-5.0, slip is delivered to plate-and-frame filter press and is carried out press filtration by constant temperature after 20 minutes, filter residue mixes as slag fertile with step B gained filter residue, clear liquid, when normal pressure is concentrated into about density 1.50g/ml, send spray drying system to be drying to obtain pulverulent water-soluble ammonium phosphate sulfate.
The invention has the advantages that: produce desired raw material wide material sources, cheap and easy to get, technique is simple, with short production cycle, three-waste free discharge, energy consumption is low, the mother liquor produced in production process does not need supporting fertilizer system to digest, but be directly used for the water-soluble ammonium phosphate sulfate of production high added value, thus reduce production cost, significant economic benefit can be obtained.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention
Embodiment
Below in conjunction with embodiment, the present invention will be further described, and following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment one:
1, with 60% agricultural monoammonium phosphate and 25% ammoniacal liquor for raw material production industrial grade monoammonium phosphate and water-soluble ammonium phosphate sulfate, the monoammonium phosphate 1000g getting total nutrient 60% 1500g that adds water is mixed with the ammonium phosphate solution of 85 DEG C, mixes the pH value to 4.2 adding 60g ammoniacal liquor regulator solution after 15 minutes;
2, react after 30 minutes and filter, obtain clear liquid 2045g, after filter residue 1000g water washing, filter to obtain filter residue 228.6g, washing lotion 1065.4 g.Clear liquid, filter residue and wash water composition are as follows: P in clear liquid
2o
5content is 20.5%, and N content is 4.6%; P in filter residue
2o
5content is 21.3%, and N content is 4.1%, H
2o content is 30.6%; P in washing lotion
2o
5content is 2.5%, and N content is 0.5%.By clear liquid concentrating under reduced pressure, when density reaches 1.38g/ml, stop heating, then crystallisation by cooling, obtains mother liquor 630.5 g through centrifugation after temperature is down to 35 DEG C, and centrifugation gained crystal obtains industrial grade monoammonium phosphate product 450.5 g after drying.P in analysed preparation
2o
5content is 61.2%, and N content is 11.9%, and water-insoluble is 0.04%, H
2o content is 0.1%;
3, mother liquid obtained for centrifugation 630.5g is heated to 85 DEG C, adjusts its pH value to 4.8 with 5g ammoniacal liquor, react filtered while hot after 20 minutes, obtain slag 7.8g, clear liquid obtains water-soluble ammonium phosphate sulfate 315.2 g through concentrated post-drying.Slag and water-soluble ammonium phosphate sulfate composition as follows: P in slag
2o
5content is 23.3%, and N content is 5.1%, H
2o content is 36.5%; P in water-soluble ammonium phosphate sulfate
2o
5content is 44.6%, and N content is 12.8%, and water-insoluble is 0.1%, H
2o content is 1.2%.
Embodiment two:
1, get the monoammonium phosphate 1000g of total nutrient 60%, add washing lotion 1065.4g in embodiment one, separately add the ammonium phosphate solution that water 500g is mixed with 85 DEG C, mix the pH value to 4.2 adding 58g ammoniacal liquor regulator solution after 15 minutes;
2, react after 30 minutes and filter, obtain clear liquid 2115g, after filter residue 1000g water washing, filter to obtain filter residue 232.4g, washing lotion 1078.2 g.Clear liquid, filter residue and wash water composition are as follows: P in clear liquid
2o
5content is 21.1%, and N content is 4.7%; P in filter residue
2o
5content is 20.7%, and N content is 4.1%, H
2o content is 31.4%; P in washing lotion
2o
5content is 2.6%, and N content is 0.5%.By clear liquid concentrating under reduced pressure, when density reaches 1.38g/ml, stop heating, then crystallisation by cooling, obtains mother liquor 643.6 g through centrifugation after temperature is down to 35 DEG C, and centrifugation gained crystal obtains industrial grade monoammonium phosphate product 490.8 g after drying.P in analysed preparation
2o
5content is 61.1%, and N content is 12.0%, and water-insoluble is 0.06%, H
2o content is 0.1%;
3, mother liquid obtained for centrifugation 643.6g is heated to 85 DEG C, adjusts its pH value to 4.8 with 6g ammoniacal liquor, react filtered while hot after 20 minutes, obtain slag 9.2g, clear liquid obtains water-soluble ammonium phosphate sulfate 321.8 g through concentrated post-drying.Slag and water-soluble ammonium phosphate sulfate composition as follows: P in slag
2o
5content is 24.1%, and N content is 5.1%, H
2o content is 35.2%; P in water-soluble ammonium phosphate sulfate
2o
5content is 44.5%, and N content is 12.7%, and water-insoluble is 0.1%, H
2o content is 1.2%.
Embodiment three:
1, get the monoammonium phosphate 1000g of total nutrient 60%, add washing lotion 1078.2g in embodiment two, separately add the ammonium phosphate solution that water 500g is mixed with 85 DEG C, mix the pH value to 4.2 adding 58g ammoniacal liquor regulator solution after 15 minutes;
2, react after 30 minutes and filter, obtain clear liquid 2121.6g, after filter residue 1000g water washing, filter to obtain filter residue 231.5g, washing lotion 1072.3 g.Clear liquid, filter residue and wash water composition are as follows: P in clear liquid
2o
5content is 21.2%, and N content is 4.7%; P in filter residue
2o
5content is 20.9%, and N content is 4.1%, H
2o content is 30.2%; P in washing lotion
2o
5content is 2.6%, and N content is 0.5%.By clear liquid concentrating under reduced pressure, when density reaches 1.35g/ml, stop heating, then crystallisation by cooling, obtains mother liquor 862.3 g through centrifugation after temperature is down to 35 DEG C, and centrifugation gained crystal obtains industrial grade monoammonium phosphate product 412.6 g after drying.P in analysed preparation
2o
5content is 61.3%, and N content is 12.0%, and water-insoluble is 0.02%, H
2o content is 0.1%;
3, mother liquid obtained for centrifugation 862.3g is heated to 85 DEG C, adjusts its pH value to 4.8 with 6g ammoniacal liquor, react filtered while hot after 20 minutes, obtain slag 8.6g, clear liquid obtains water-soluble ammonium phosphate sulfate 402.4g through concentrated post-drying.Slag and water-soluble ammonium phosphate sulfate composition as follows: P in slag
2o
5content is 23.6%, and N content is 5.1%, H
2o content is 34.5%; P in water-soluble ammonium phosphate sulfate
2o
5content is 48.8%, and N content is 12.3%, and water-insoluble is 0.1%, H
2o content is 1.2%.
Claims (1)
1. a method for the water-soluble ammonium phosphate sulfate of manufacture level monoammonium phosphate co-production, its step is as follows:
A, get the agricultural phosphorus ammonium of total nutrient 60%, be dissolved in water by 1.5 times of its quality, control temperature 85 DEG C, dissolved after 15 minutes, add the pH value to 4.2 of bicarbonate of ammonia or ammoniacal liquor adjustment slip again, react, after 30 minutes, slurry pipeline transport is carried out press filtration to plate-and-frame filter press;
B, press filtration gained phosphorus ammonium clear liquid is delivered to vacuum concentration system carries out concentrating under reduced pressure, heating is stopped to during density 1.36-1.38g/mL, again the phosphor ammonium slurry concentrated is delivered to crystallizer tank and carries out crystallisation by cooling, cooling terminal temperature controls at 35-40 DEG C, then obtained industrial grade monoammonium phosphate product after centrifugation, drying, gained filter residue 65 DEG C of hot water wash, and wash water returns to steps A for dissolved phosphorus ammonium, and filter residue is fertile as slag;
C, be heated to 85 DEG C by mother liquid obtained for centrifugation, adjust ph is to 4.5-5.0, slip is delivered to plate-and-frame filter press and is carried out press filtration by constant temperature after 20 minutes, filter residue mixes as slag fertile with step B gained filter residue, clear liquid is concentrated into density 1.50g/mL through normal pressure, send spray drying system to be drying to obtain pulverulent water-soluble ammonium phosphate sulfate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106629644B (en) * | 2017-01-14 | 2018-11-09 | 湖南省正源储能材料与器件研究所 | A method of producing industrial level-one and LITHIUM BATTERY monoammonium phosphate with chemical fertilizer grade monoammonium phosphate |
| CN106831139A (en) * | 2017-02-22 | 2017-06-13 | 武汉中东磷业科技有限公司 | A kind of method that slurry-spraying pelletizing produces nitrogen nitre sulfenyl water-flush compound fertilizer high |
| KR101935820B1 (en) * | 2017-08-28 | 2019-01-07 | 세종화학 (주) | Method for manufacturing high purity ammonium dihydrogenphosphate using ammonium phosphate waste solutions |
| CN107746044B (en) * | 2017-12-06 | 2020-01-24 | 上海新增鼎工业科技有限公司 | Method for producing industrial grade monoammonium phosphate from agricultural monoammonium phosphate |
| CN109574735A (en) * | 2018-12-20 | 2019-04-05 | 四川大学 | The processing and MAP coproduction of phosphorus ammonium mother liquor are containing the technique of middle microelement APP |
| CN109384208A (en) * | 2018-12-20 | 2019-02-26 | 湖北六国化工股份有限公司 | A kind of the step application method and system of phosphor ammonium slurry |
| CN115231971A (en) * | 2021-04-23 | 2022-10-25 | 嘉施利（荆州）化肥有限公司 | Preparation process of agricultural zinc-containing fully water-soluble monoammonium phosphate |
| CN116588908A (en) * | 2023-05-19 | 2023-08-15 | 曲靖市德方纳米科技有限公司 | Method for preparing battery-grade ammonium dihydrogen phosphate by using phosphate fertilizer and its application |
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| CN102515923A (en) * | 2011-12-28 | 2012-06-27 | 四川宏达股份有限公司 | Drip irrigation-grade ammonium phosphate sulfate composite fertilizer and preparation process thereof |
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| JPS54102300A (en) * | 1978-01-31 | 1979-08-11 | Chisso Corp | Production of industrial grade ammonium phosphate |
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