CN103130205A - Method for producing industrial monoammonium phosphate and coproducing water-soluble ammonium sulfate phosphate - Google Patents
Method for producing industrial monoammonium phosphate and coproducing water-soluble ammonium sulfate phosphate Download PDFInfo
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- CN103130205A CN103130205A CN2013100763535A CN201310076353A CN103130205A CN 103130205 A CN103130205 A CN 103130205A CN 2013100763535 A CN2013100763535 A CN 2013100763535A CN 201310076353 A CN201310076353 A CN 201310076353A CN 103130205 A CN103130205 A CN 103130205A
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- 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
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- IHBBREPROWBPRG-UHFFFAOYSA-N pentaazanium;phosphate;sulfate Chemical compound [NH4+].[NH4+].[NH4+].[NH4+].[NH4+].[O-]P([O-])([O-])=O.[O-]S([O-])(=O)=O IHBBREPROWBPRG-UHFFFAOYSA-N 0.000 title abstract 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 235000015097 nutrients Nutrition 0.000 claims abstract description 6
- 239000002002 slurry Substances 0.000 claims abstract description 6
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 4
- 238000001694 spray drying Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims 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 claims description 20
- 238000005119 centrifugation Methods 0.000 claims description 13
- 239000002893 slag Substances 0.000 claims description 13
- QLULGSLAHXLKSR-UHFFFAOYSA-N azane;phosphane Chemical compound N.P QLULGSLAHXLKSR-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 abstract description 8
- 239000002994 raw material Substances 0.000 abstract description 8
- 239000004254 Ammonium phosphate Substances 0.000 abstract description 7
- 229910000148 ammonium phosphate Inorganic materials 0.000 abstract description 7
- 235000019289 ammonium phosphates Nutrition 0.000 abstract description 7
- 239000003337 fertilizer Substances 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 abstract description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 abstract description 2
- 239000001099 ammonium carbonate Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000011085 pressure filtration Methods 0.000 abstract 3
- 239000010413 mother solution Substances 0.000 abstract 2
- 238000000926 separation method Methods 0.000 abstract 2
- 239000000243 solution Substances 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 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
- 239000012452 mother liquor Substances 0.000 description 4
- 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
- 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
- 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
- 230000002950 deficient 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
- 239000000463 material 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 invention relates to a method for producing industrial monoammonium phosphate and coproducing water-soluble ammonium sulfate phosphate, which comprises the following steps: A. taking agricultural ammonium phosphate accounting for 60% of the total nutrients, dissolving the agricultural ammonium phosphate in 1.5 times by mass of water, adding ammonium bicarbonate or ammonia water to regulate the pH value of the slurry to 4.2, reacting for 30 minutes, and carrying out pressure filtration; B. concentrating the ammonium phosphate clear solution obtained by pressure filtration under reduced pressure, delivering the concentrated ammonium phosphate slurry to a crystallization tank, cooling to crystallize, carrying out centrifugal separation, and drying to obtain an industrial monoammonium phosphate product; and C. heating the mother solution obtained by centrifugal separation to 85 DEG C, regulating the pH value to 4.5-5.0, keeping the temperature for 20 minutes, carrying out pressure filtration, concentrating the clear solution under atmospheric pressure, delivering to a spray drying system, and drying to obtain the powdery water-soluble ammonium sulfate phosphate. The invention has the advantages of wide raw material sources, cheap and accessible raw materials, simple technique, short production cycle, no discharge of three wastes, and low energy consumption, and the mother solution generated in the production process does not need to be digested by a matched fertilizer system, thereby lowering the production cost.
Description
Technical field
The invention belongs to the industrial grade monoammonium phosphate production field, relate to a kind of production method of using agricultural monoammonium phosphate and diammonium phosphate, bicarbonate of ammonia or ammoniacal liquor manufacture level monoammonium phosphate and the water-soluble ammonium phosphate sulfate of coproduction.
Background technology
The purposes of industrial grade monoammonium phosphate is comparatively extensive, mainly sprays fertile main raw material as ABC powder extinguishing agent, ammonium polyphosphate flame retardant and drip irrigation, also is used in addition the industries such as medicine, food, paper, timber, and its market outlook are very good.Water-soluble ammonium phosphate sulfate can be directly used in and drip 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 fertile market will progressively enlarge, and water-soluble ammonium phosphate sulfate market demand will constantly increase.In prior art, the technology take phosphoric acid by wet process as the raw material production industrial grade monoammonium phosphate has become main flow, and a large amount of mother liquors that the method produces must pass through fertilizer system recoveries, the common fertilizer that the production added value is extremely low.At present there is no patent report about the production method with agricultural phosphorus ammonium manufacture level monoammonium phosphate and the water-soluble ammonium phosphate sulfate of coproduction.
Summary of the invention
The objective of the invention is the defective for existing industrial grade monoammonium phosphate technology, it is the novel technique route of the high-quality industrial grade monoammonium phosphate of raw material production and the water-soluble ammonium phosphate sulfate of coproduction that the agricultural phosphorus ammonium of a kind of use is provided, and is intended at utmost reduce the production cost of industrial grade monoammonium phosphate and improves its economic benefit.
To achieve these goals, the present invention the steps include: by the following technical solutions
A, get the agricultural phosphorus ammonium of a certain amount of total nutrient 60%, 1.5 times by its quality are dissolved in water, and control 85 ℃ of temperature, dissolve after 15 minutes, add again amount of ammonium bicarbonate or ammoniacal liquor to regulate the pH value to 4.2 of slip, react and after 30 minutes, slurry pipeline transport to plate-and-frame filter press is carried out press filtration.
B, press filtration gained phosphorus ammonium clear liquid is delivered to vacuum concentration system carries out concentrating under reduced pressure, stopped heating during to density 1.36-1.38g/ml, the phosphor ammonium slurry that will concentrate again is delivered to crystallizer tank and carries out crystallisation by cooling, cooling terminal temperature is controlled at 35-40 ℃, then makes the industrial grade monoammonium phosphate product after centrifugation, drying.The gained filter residue washs with 65 ℃ of left and right hot water, and wash water returns to steps A and is used for the dissolved phosphorus ammonium, and filter residue sells separately as slag fertilizer.
C, be heated to 85 ℃ with centrifugation is mother liquid obtained, regulate pH value to 4.5-5.0, constant temperature after 20 minutes is delivered to slip plate-and-frame filter press and is carried out press filtration, filter residue mixes as slag fertile with step B gained filter residue, when clear liquid is concentrated into density 1.50g/ml left and right through normal pressure, send spray drying system to be drying to obtain the pulverulent water-soluble ammonium phosphate sulfate.
The invention has the advantages that: produce the 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 that produces in production process does not need supporting fertilizer system to digest, but directly be used for the water-soluble ammonium phosphate sulfate of production high added value, thus reduce production costs, can obtain significant economic benefit.
Description of drawings
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, take 60% agricultural monoammonium phosphate and 25% ammoniacal liquor as raw material production industrial grade monoammonium phosphate and water-soluble ammonium phosphate sulfate, the monoammonium phosphate 1000g that gets total nutrient 60% adds the ammonium phosphate solution that water 1500g is mixed with 85 ℃, mixes and adds the pH value to 4.2 of 60g ammoniacal liquor regulator solution after 15 minutes;
2, reaction was filtered after 30 minutes, obtained clear liquid 2045g, and filter residue filters to get filter residue 228.6g, washing lotion 1065.4 g after with the 1000g water washing.Clear liquid, filter residue and wash water composition are as follows: P in clear liquid
2O
5Content is that 20.5%, N content is 4.6%; P in filter residue
2O
5Content is that 21.3%, N content is 4.1%, H
2O content is 30.6%; P in washing lotion
2O
5Content is that 2.5%, N content is 0.5%.With the clear liquid concentrating under reduced pressure, stopped heating when density reaches 1.38g/ml, crystallisation by cooling then, temperature is down to 35 ℃ and is got mother liquor 630.5 g by centrifugation, centrifugation gained crystal after drying industrial grade monoammonium phosphate product 450.5 g.P in analysed preparation
2O
5Content is that 61.2%, N content is 11.9%, and water-insoluble is 0.04%, H
2O content is 0.1%;
3, the mother liquid obtained 630.5g of centrifugation is heated to 85 ℃, transfers its pH value to 4.8 with 5g ammoniacal liquor, react filtered while hot after 20 minutes, get slag 7.8g, clear liquid gets water-soluble ammonium phosphate sulfate 315.2 g through concentrated post-drying.Slag and water-soluble ammonium phosphate sulfate composition are as follows: P in slag
2O
5Content is that 23.3%, N content is 5.1%, H
2O content is 36.5%; P in water-soluble ammonium phosphate sulfate
2O
5Content is that 44.6%, 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 entry 500g is mixed with 85 ℃, mix and add the pH value to 4.2 of 58g ammoniacal liquor regulator solution after 15 minutes;
2, reaction was filtered after 30 minutes, obtained clear liquid 2115g, and filter residue filters to get filter residue 232.4g, washing lotion 1078.2 g after with the 1000g water washing.Clear liquid, filter residue and wash water composition are as follows: P in clear liquid
2O
5Content is that 21.1%, N content is 4.7%; P in filter residue
2O
5Content is that 20.7%, N content is 4.1%, H
2O content is 31.4%; P in washing lotion
2O
5Content is that 2.6%, N content is 0.5%.With the clear liquid concentrating under reduced pressure, stopped heating when density reaches 1.38g/ml, crystallisation by cooling then, temperature is down to 35 ℃ and is got mother liquor 643.6 g by centrifugation, centrifugation gained crystal after drying industrial grade monoammonium phosphate product 490.8 g.P in analysed preparation
2O
5Content is that 61.1%, N content is 12.0%, and water-insoluble is 0.06%, H
2O content is 0.1%;
3, the mother liquid obtained 643.6g of centrifugation is heated to 85 ℃, transfers its pH value to 4.8 with 6g ammoniacal liquor, react filtered while hot after 20 minutes, get slag 9.2g, clear liquid gets water-soluble ammonium phosphate sulfate 321.8 g through concentrated post-drying.Slag and water-soluble ammonium phosphate sulfate composition are as follows: P in slag
2O
5Content is that 24.1%, N content is 5.1%, H
2O content is 35.2%; P in water-soluble ammonium phosphate sulfate
2O
5Content is that 44.5%, 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 entry 500g is mixed with 85 ℃, mix and add the pH value to 4.2 of 58g ammoniacal liquor regulator solution after 15 minutes;
2, reaction was filtered after 30 minutes, obtained clear liquid 2121.6g, and filter residue filters to get filter residue 231.5g, washing lotion 1072.3 g after with the 1000g water washing.Clear liquid, filter residue and wash water composition are as follows: P in clear liquid
2O
5Content is that 21.2%, N content is 4.7%; P in filter residue
2O
5Content is that 20.9%, N content is 4.1%, H
2O content is 30.2%; P in washing lotion
2O
5Content is that 2.6%, N content is 0.5%.With the clear liquid concentrating under reduced pressure, stopped heating when density reaches 1.35g/ml, crystallisation by cooling then, temperature is down to 35 ℃ and is got mother liquor 862.3 g by centrifugation, centrifugation gained crystal after drying industrial grade monoammonium phosphate product 412.6 g.P in analysed preparation
2O
5Content is that 61.3%, N content is 12.0%, and water-insoluble is 0.02%, H
2O content is 0.1%;
3, the mother liquid obtained 862.3g of centrifugation is heated to 85 ℃, transfers its pH value to 4.8 with 6g ammoniacal liquor, react filtered while hot after 20 minutes, get slag 8.6g, clear liquid gets water-soluble ammonium phosphate sulfate 402.4g through concentrated post-drying.Slag and water-soluble ammonium phosphate sulfate composition are as follows: P in slag
2O
5Content is that 23.6%, N content is 5.1%, H
2O content is 34.5%; P in water-soluble ammonium phosphate sulfate
2O
5Content is that 48.8%, N content is 12.3%, and water-insoluble is 0.1%, H
2O content is 1.2%.
Claims (1)
1. the method for a manufacture level monoammonium phosphate and the water-soluble ammonium phosphate sulfate of coproduction, 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 85 ℃ of temperature, dissolve after 15 minutes, then add the pH value to 4.2 of bicarbonate of ammonia or ammoniacal liquor adjusting slip, react and after 30 minutes, slurry pipeline transport to plate-and-frame filter press is carried out press filtration;
B, press filtration gained phosphorus ammonium clear liquid is delivered to vacuum concentration system carries out concentrating under reduced pressure, stopped heating during to density 1.36-1.38g/ml, the phosphor ammonium slurry that will concentrate again is delivered to crystallizer tank and carries out crystallisation by cooling, cooling terminal temperature is controlled at 35-40 ℃, then make the industrial grade monoammonium phosphate product after centrifugation, drying, the gained filter residue washs with 65 ℃ of left and right hot water, and wash water returns to steps A and is used for the dissolved phosphorus ammonium, and filter residue is fertile as slag;
C, be heated to 85 ℃ with centrifugation is mother liquid obtained, regulate pH value to 4.5-5.0, constant temperature after 20 minutes is delivered to slip plate-and-frame filter press and is carried out press filtration, filter residue mixes as slag fertile with step B gained filter residue, when clear liquid is concentrated into density 1.50g/ml left and right through normal pressure, send spray drying system to be drying to obtain the pulverulent water-soluble ammonium phosphate sulfate.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629644A (en) * | 2017-01-14 | 2017-05-10 | 湖南省正源储能材料与器件研究所 | Method for producing industrial first-stage and battery-stage monoammonium phosphate by using fertilizer-stage 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 |
| CN107746044A (en) * | 2017-12-06 | 2018-03-02 | 上海新增鼎工业科技有限公司 | A kind of method for producing industrial grade monoammonium phosphate with agricultural MAP |
| 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 |
| WO2019045130A1 (en) * | 2017-08-28 | 2019-03-07 | 세종화학 주식회사 | Method for preparing high-purity ammonium dihydrogen phosphate using ammonium phosphate waste liquid |
| 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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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106629644A (en) * | 2017-01-14 | 2017-05-10 | 湖南省正源储能材料与器件研究所 | Method for producing industrial first-stage and battery-stage monoammonium phosphate by using fertilizer-stage monoammonium phosphate |
| 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 |
| WO2019045130A1 (en) * | 2017-08-28 | 2019-03-07 | 세종화학 주식회사 | Method for preparing high-purity ammonium dihydrogen phosphate using ammonium phosphate waste liquid |
| CN107746044A (en) * | 2017-12-06 | 2018-03-02 | 上海新增鼎工业科技有限公司 | A kind of method for producing industrial grade monoammonium phosphate with agricultural MAP |
| 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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|---|---|
| CN103130205B (en) | 2015-09-30 |
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