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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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 29
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 title claims abstract description 24
- 235000019837 monoammonium phosphate Nutrition 0.000 title claims abstract description 24
- 239000006012 monoammonium phosphate Substances 0.000 title claims abstract description 24
- KNQKRMVYLDOGCT-UHFFFAOYSA-N ammonium phosphate sulfate Chemical compound [NH4+].[NH4+].OP(O)([O-])=O.OS([O-])(=O)=O KNQKRMVYLDOGCT-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000005119 centrifugation Methods 0.000 claims abstract description 15
- QLULGSLAHXLKSR-UHFFFAOYSA-N azane;phosphane Chemical compound N.P QLULGSLAHXLKSR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 6
- 235000015097 nutrients Nutrition 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims abstract description 5
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 4
- 238000001694 spray drying Methods 0.000 claims abstract description 3
- 239000002893 slag Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000003337 fertilizer Substances 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000012452 mother liquor Substances 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 18
- 238000005406 washing Methods 0.000 description 11
- 239000006210 lotion Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 4
- 239000004254 Ammonium phosphate Substances 0.000 description 3
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 3
- 235000019289 ammonium phosphates Nutrition 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000002262 irrigation Effects 0.000 description 2
- 238000003973 irrigation Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- 239000004114 Ammonium polyphosphate Substances 0.000 description 1
- 239000005696 Diammonium phosphate Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 1
- 229920001276 ammonium polyphosphate Polymers 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 1
- 235000019838 diammonium phosphate Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000004720 fertilization Effects 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
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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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| 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 |
| 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 |
| 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 |
| 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 |
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| JPS54102300A (en) * | 1978-01-31 | 1979-08-11 | Chisso Corp | Production of industrial grade ammonium phosphate |
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