CN105036852A - Method for producing macroelement water-soluble fertilizer by using industrial grade monoammonium phosphate mother liquor - Google Patents
Method for producing macroelement water-soluble fertilizer by using industrial grade monoammonium phosphate mother liquor Download PDFInfo
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Abstract
A method for producing macroelement water-soluble fertilizer by using industrial grade monoammonium phosphate mother liquor comprises: adding a urea solution or an ammonium nitrate solution, a potassium fertilizer, trace elements and a chelating agent into the industrial grade monoammonium phosphate mother liquor; and chelating, filtering, concentrating and drying the mixture to obtain the macroelement water-soluble fertilizer . The method provided by the invention is free of three-waste discharge in the whole course, so that gradient utilization and comprehensive utilization of resources are realized, the production cost is lowered, the economical benefit is improved, and moreover, compared to a fertilizer produced by a physical mixing method, the macroelement water-soluble fertilizer is high in purity, good in appearance and low in cost, and market popularization and agricultural application are favorably facilitated.
Description
Technical field
The invention belongs to technical field of fertilizers, be specifically related to utilize industrial grade monoammonium phosphate mother liquor to produce the method for macroelement water-soluble fertilizer.
Background technology
Water-soluble fertilizer refers to polyelement composite fertilizer that can be completely water-soluble, after water dissolution or dilution, may be used for solid or the liquid fertilizer of the purposes such as fertigation, leaf dressing.Because water-soluble fertilizer can be dissolved in the water completely, therefore more easily absorbed by crops, instant, high without residue, specific absorption, instant effect, to use convenient etc. be the remarkable advantage of water-soluble fertilizer, and by being applied to the industrialized agricultures such as spray, drip irrigation, can realize water-fertilizer integral." the Integration of Water into Fertilizer instruction " that the Ministry of Agriculture prints and distributes for 2013 is pointed out, promotes the total area reach more than 8,000 ten thousand mu to the Integration of Water into Fertilizer in 2015.
The production method of current domestic water-soluble fertilizer is mainly physics mixture method, carries out simple physics mixture by raw materials such as industrial grade monoammonium phosphate, potassium sulfate, potassium primary phosphates.Adopt this method to produce water-soluble fertilizer and have two problems: one is, cause because raw materials cost is high water-soluble fertilizer price high, peasant holds and dares not accept, and limits the promotion and application of water-soluble fertilizer significantly; Two are, the problems such as deliquescence, caking, flatulence, impurity is too much easily appear in the water-soluble fertilizer that this method is produced.Compared with physics mixture method, the water-soluble fertilizer outward appearance that chemical synthesis is produced is good, and Functionality, quality and appealing design, existing Patents is reported.Chinese patent CN103011122B discloses a kind of method of Wet-process Phosphoric Acid Production water-soluble phosphoric acid potassium ammonium, the method in a wet process phosphoric acid is raw material, monoammonium phosphate solution is obtained through desulfurization, defluorinate, ammonia neutralization, monoammonium phosphate clear liquid and Repone K carry out replacement(metathesis)reaction, crystallization obtains potassium-ammonium phosphate, and mother liquor is obtained chloro water-soluble fertilizer after evaporation, drying.Chinese patent CN102633551B discloses a kind of method that agricultural fertilizer produces macroelement water-soluble fertilizer, the method comprises the following steps: 1, potassium primary phosphate or agricultural potassium sulfate are mixed with saturated solution, filtration obtains clear liquid, then in saturated clear liquid, urea is added, obtained crystal phosphoric acid potassium dihydrogen or potassium sulfate after crystallisation by cooling, centrifuging; 2, dissolve agricultural monoammonium phosphate with the mother liquor from potassium primary phosphate or potassium sulfate, add ammoniacal liquor reaction, filter obtain monoammonium phosphate clear liquid; 3, monoammonium phosphate clear liquid, crystal phosphoric acid potassium dihydrogen or potassium sulfate, urea, saltpetre and trace element are added water-soluble fertilizer reactor, isothermal reaction is carried out spraying dry after half an hour and is obtained macroelement water-soluble fertilizer.
The technique of current domestic preparing industrial grade monoammonium phosphate from wet-process phosphoric acid is generally: phosphoric acid by wet process is through in desulfurization, defluorinate, ammonia and removal of impurities, obtain purer monoammonium phosphate solution after filtration, and monoammonium phosphate solution is again through concentrated, crystallisation by cooling, centrifuging, dry obtained industrial grade monoammonium phosphate.Two kinds of methods are generally had: one is to the process of mother liquor, after desulfurization, retrieval system mixes with phosphoric acid, or desulfurization again after retrieval system mixes with phosphoric acid, but need additionally introduce the sweetening agent such as barium carbonate, phosphate ore pulp, add production cost, and too much calcium ion can be introduced when using phosphate ore pulp, produce secondary calcium phosphate in ammonifying process, cause product water insolubles to exceed standard.Two are, directly mother liquor are delivered to phosphate fertilizer plant for the production of agricultural monoammonium phosphate, because the impurity in the mother liquor after refining is little, send to and produce that agricultural monoammonium phosphate causes manually undoubtedly, the waste of resource and the energy.A kind of method of Wet-process Phosphoric Acid Production monoammonium phosphate coproduction N-P binary compound fertilizer is disclosed in patent 201210329385.
Summary of the invention
The object of the invention is to recycle industrial grade monoammonium phosphate mother liquor, a kind of method utilizing industrial grade monoammonium phosphate mother liquor to produce macroelement water-soluble fertilizer is provided, can be effectively cost-saving, increase the benefit.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: utilize industrial grade monoammonium phosphate mother liquor to produce the method for macroelement water-soluble fertilizer, concrete steps are:
1) according to the macroelement water-soluble fertilizer of required preparation and the regulation according to NY1107-2010 standard, in industrial grade monoammonium phosphate mother liquor, urea soln, potash fertilizer, medium trace element and sequestrant is added; Then pH value to 4.5 ~ 5.0 passing into ammonia or add ammoniacal liquor regulator solution are reacted, and control temperature of reaction 70 ~ 90 DEG C, stir simultaneously, filtered while hot after reaction 30 ~ 60min;
2) step 1) gained filtrate concentrates, and when being 25 ~ 35% to water content massfraction, carries out spraying dry, obtains macroelement water-soluble fertilizer.
Further, the temperature of the urea soln in step 1) is 90 ~ 105 DEG C, mass concentration is 68 ~ 75%.
Urea soln in step 1) adopts ammonium nitrate solution to substitute, and its temperature is 110 ~ 125 DEG C, mass concentration is 85 ~ 90%.Concrete alternative amount proportioning needed for fertilizer is determined, uses ammonium nitrate solution just can not use urea soln.Described urea soln or ammonium nitrate solution all directly from urea plant or ammonium nitrate production device, can make full use of its heat, energy efficient.
Potash fertilizer described in step 1) is the combination of one or more in agricultural potassium chloride, agricultural potassium sulfate, Agricultural Potassium Nitrate and agricultural potassium primary phosphate.
Medium trace element described in step 1) is the combination of one or more in nitrocalcite, magnesium sulfate, water glass, ferrous sulfate, manganous sulfate, copper sulfate, zinc sulfate, ammonium molybdate, boric acid etc.
Sequestrant described in step 1) is the combination of one or more in ammonium polyphosphate, ethylenediamine tetraacetic acid (EDTA), citric acid, amino acid, humic acid, few chitose, glucose saccharic acid etc.
When adding medium trace element and sequestrant in step 1), the mol ratio of the medium trace element total content in its sequestrant addition and solution is 1 ~ 3 ﹕ 1.
Filter residue use water after filtering in step 1) rinses, and the filter residue after flushing and the water containing available phosphorus composition are all delivered in the production equipment of agricultural monoammonium phosphate and recycled.
When stirring in step 1), control mixing speed 400 ~ 800r/min.
It is fixing in order to what prevent soil to medium trace element that the present invention uses the object of chelating technology mainly, improves the utilization ratio of crop medium trace element.By the chelating condition that controls to be suitable for if temperature, pH and stir speed (S.S.) etc. are to obtain satisfactory macroelement water-soluble fertilizer.
Concentrated and spraying dry to be carried out to mother liquor in method provided by the invention, add other raw material before this, the intermediate product in other workshop can be utilized as urea soln or ammonium nitrate solution.
The method utilizing industrial grade monoammonium phosphate mother liquor to produce macroelement water-soluble fertilizer provided by the invention, has following beneficial effect:
1, with industrial grade monoammonium phosphate mother liquor for raw material, the macroelement water-soluble fertilizer of production high added value, instead of purer mother liquor is delivered to agricultural monoammonium phosphate device for the production of low value-added agricultural monoammonium phosphate, achieve the cascade utilization of resource, and take full advantage of the heat of urea soln or ammonium nitrate solution, reduce steam consumption;
2, present method is by adding medium trace element and sequestrant synthesis chelating medium trace element in the solution, instead of adds commercial high price chelating medium trace element, has both improve the utilization ratio of medium trace element, and has again reduced production cost;
3, present method can use agricultural fertilizer raw material to produce macroelement water-soluble fertilizer, and in dissolving, chelating, chemical reaction between raw material can carry out completely, avoids the problem such as the product caused due to the chemical reaction between raw material caking, flatulence often occurred in physics mixture method.
Embodiment
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to the scope of embodiment statement.
Industrial grade monoammonium phosphate mother liquor involved in following examples obtains when adopting phosphoric acid by wet process to prepare industrial grade monoammonium phosphate, and concrete steps are:
1) be 20 ~ 28%P by mass concentration
2o
5dilute phosphoric acid carry out concentrating and impurity removing, add sinking agent sedimentation removal of impurities after being concentrated into 46 ~ 48% again, the phosphoric acid after removal of impurities is diluted to 20 ~ 28% with process water again;
2) dilution phosphoric acid pump step 1) obtained is to ammoniation reactor, and logical ammonia once neutralizes, control degree of neutralization 1.01 ~ 1.04, temperature of reaction 105 ~ 115 DEG C, once and slip after filtering pump to Two-step neutralization groove;
3) in Two-step neutralization groove, add diluted acid and complete Two-step neutralization, control Two-step neutralization slip pH value 4.4 ~ 4.6, Two-step neutralization slip after filtering pump to two imitates concentration evaporator;
4) after slip economic benefits and social benefits are concentrated into relative density 1.34 ~ 1.38, pump is to crystallizer tank crystallisation by cooling, magma is through centrifuging, the crystal obtained obtains industrial grade monoammonium phosphate after vibra fluidized bed drying, and centrifuge mother liquor is the primary industry level monoammonium phosphate mother liquor in the application.
Sinking agent used is polyacrylamide or the similar additive with identical function, and addition is with 1 of volume basis ~ 5 ‰.The diluted acid added is the concentration after diluting with process water in step 1) is 20 ~ 28% dilute phosphoric acids.
The phosphoric acid by wet process produced with low-grade phosphate ore, for raw material, adopts concentrating and impurity removing and sedimentation removal of impurities to obtain pre-treatment phosphoric acid, and cost is low and technical process simple compared with interpolation compound impurity removing technology, can in phosphorus compound fertilizer enterprise large-scale promotion; And adopting concentration and settlement pre-treatment, Two-step neutralization and secondary concentration, technical process is simple, and technic index controls reliable, stable, convenient, and product quality is high, and output capacity is high.
The industrial grade monoammonium phosphate mother liquor of gained is ammonium sulfate and the monoammonium phosphate solution of water content 60% ~ 65%, and butt npk nutrient content is 13.5-53.5-0.
Embodiment 1:
1) the industrial grade monoammonium phosphate mother liquor 1071.4kg of water content 65% is got, then the urea soln 214.3kg of water content 30%, saltpetre 380.0kg, cupric sulfate pentahydrate 3.0kg, iron vitriol 10.0kg, three water manganous sulfate 7.0kg, Zinc Sulphate Heptahydrate 3.0kg, four water ammonium molybdate 1.0kg, magnesium sulfate heptahydrate 20.0kg, EDTA52.0kg is added, then pH value to 4.5 ~ 5.0 passing into ammonia or add ammoniacal liquor regulator solution are reacted, control temperature of reaction 70 ~ 90 DEG C, stir, filtered while hot after reaction 30min simultaneously;
2) step 1) gained filtrate concentrates, and when being 25% to water content massfraction, carries out spraying dry, obtains 1000.0kg macroelement water-soluble fertilizer, wherein containing 17.0%N, 20.0%P
2o
5, 17.0%K
2o, 0.075%Cu, 0.2%Fe, 0.2%Mn, 0.07%Zn, 0.05%Mo.
Embodiment 2:
1) the industrial grade monoammonium phosphate mother liquor 1400kg of water content 60% is got, then the ammonium nitrate solution 177.8kg of water content 10%, potassium sulfate 185.0kg, cupric sulfate pentahydrate 3.0kg, iron vitriol 10.0kg, three water manganous sulfate 7.0kg, Zinc Sulphate Heptahydrate 3.0kg, four water ammonium molybdate 1.0kg, magnesium sulfate heptahydrate 20.0kg, EDTA52.0kg is added, then pH value to 4.5 ~ 5.0 passing into ammonia or add ammoniacal liquor regulator solution are reacted, control temperature of reaction 70 ~ 90 DEG C, stir, filtered while hot after reaction 60min simultaneously;
2) step 1) gained filtrate concentrates, and when being 25% to water content massfraction, carries out spraying dry, obtains 1000.0kg macroelement water-soluble fertilizer, wherein containing 13.2%N, 30.0%P
2o
5, 9.3%K
2o, 0.075%Cu, 0.2%Fe, 0.2%Mn, 0.07%Zn, 0.05%Mo.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. utilize industrial grade monoammonium phosphate mother liquor to produce the method for macroelement water-soluble fertilizer, it is characterized in that, concrete steps are:
1) according to the macroelement water-soluble fertilizer of required preparation and the regulation according to NY1107-2010 standard, in industrial grade monoammonium phosphate mother liquor, urea soln, potash fertilizer, medium trace element and sequestrant is added; Then pH value to 4.5 ~ 5.0 passing into ammonia or add ammoniacal liquor regulator solution are reacted, and control temperature of reaction 70 ~ 90 DEG C, stir simultaneously, filtered while hot after reaction 30 ~ 60min;
2) step 1) gained filtrate concentrates, and when being 25 ~ 35% to water content massfraction, carries out spraying dry, obtains macroelement water-soluble fertilizer.
2. method according to claim 1, is characterized in that: the temperature of the urea soln in step 1) is 90 ~ 105 DEG C, mass concentration is 68 ~ 75%.
3. method according to claim 1, is characterized in that: the urea soln in step 1) adopts ammonium nitrate solution to substitute, and its temperature is 110 ~ 125 DEG C, mass concentration is 85 ~ 90%.
4. method according to claim 1, is characterized in that: the potash fertilizer described in step 1) is the combination of one or more in agricultural potassium chloride, agricultural potassium sulfate, Agricultural Potassium Nitrate and agricultural potassium primary phosphate.
5. method according to claim 1, is characterized in that: the medium trace element described in step 1) is the combination of one or more in nitrocalcite, magnesium sulfate, water glass, ferrous sulfate, manganous sulfate, copper sulfate, zinc sulfate, ammonium molybdate, boric acid etc.
6. method according to claim 1, is characterized in that: the sequestrant described in step 1) is the combination of one or more in ammonium polyphosphate, ethylenediamine tetraacetic acid (EDTA), citric acid, amino acid, humic acid, few chitose, glucose saccharic acid etc.
7. method according to claim 1, is characterized in that: when adding medium trace element and sequestrant in step 1), and the mol ratio of the medium trace element total content in its sequestrant addition and solution is 1 ~ 3 ﹕ 1.
8. method according to claim 1, is characterized in that: when stirring in step 1), controls mixing speed 400 ~ 800r/min.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106335888A (en) * | 2016-08-23 | 2017-01-18 | 湖北中孚化工集团有限公司 | Method and device for synthesis of ammonium polyphosphate from industrial monoammonium crystallization mother liquor |
| CN106916003A (en) * | 2015-12-28 | 2017-07-04 | 江苏绿方园生物科技有限公司 | Amount type Macroelement water-soluble suspension liquid fertilizer and preparation method in organic-inorganic |
| CN106977282A (en) * | 2017-04-06 | 2017-07-25 | 安徽康坶国际化肥股份有限公司 | A kind of insect pest a great number of elements water-soluble fertilizer |
| CN107285813A (en) * | 2016-04-11 | 2017-10-24 | 湖北南轻法麦克斯作物营养有限公司 | A kind of method that use rock phosphate in powder produces Water soluble fertilizer |
| CN109020695A (en) * | 2018-08-30 | 2018-12-18 | 安徽六国化工股份有限公司 | A kind of N P and K TE compound fertilizer preparation process |
| 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 |
| CN111592386A (en) * | 2020-06-10 | 2020-08-28 | 河南中之州植保有限公司 | Preparation method of chelated rare earth |
| CN112938923A (en) * | 2020-12-28 | 2021-06-11 | 瓮福（集团）有限责任公司 | Preparation method of nutrient-controllable ammonium polyphosphate |
| 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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| CN104446968A (en) * | 2014-11-27 | 2015-03-25 | 湖北三宁化工股份有限公司 | Water-soluble high-concentration organic-inorganic compound fertilizer for trickle and sprinkling irrigation and preparation method thereof |
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Patent Citations (2)
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| CN102863267A (en) * | 2012-09-08 | 2013-01-09 | 湖北三宁化工股份有限公司 | Method for producing monoammonium phosphate and coproducing N-P binary compound fertilizer by using wet-process phosphoric acid |
| CN104446968A (en) * | 2014-11-27 | 2015-03-25 | 湖北三宁化工股份有限公司 | Water-soluble high-concentration organic-inorganic compound fertilizer for trickle and sprinkling irrigation and preparation method thereof |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106916003A (en) * | 2015-12-28 | 2017-07-04 | 江苏绿方园生物科技有限公司 | Amount type Macroelement water-soluble suspension liquid fertilizer and preparation method in organic-inorganic |
| CN107285813A (en) * | 2016-04-11 | 2017-10-24 | 湖北南轻法麦克斯作物营养有限公司 | A kind of method that use rock phosphate in powder produces Water soluble fertilizer |
| CN106335888A (en) * | 2016-08-23 | 2017-01-18 | 湖北中孚化工集团有限公司 | Method and device for synthesis of ammonium polyphosphate from industrial monoammonium crystallization mother liquor |
| CN106977282A (en) * | 2017-04-06 | 2017-07-25 | 安徽康坶国际化肥股份有限公司 | A kind of insect pest a great number of elements water-soluble fertilizer |
| CN109020695A (en) * | 2018-08-30 | 2018-12-18 | 安徽六国化工股份有限公司 | A kind of N P and K TE compound fertilizer preparation process |
| 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 |
| CN111592386A (en) * | 2020-06-10 | 2020-08-28 | 河南中之州植保有限公司 | Preparation method of chelated rare earth |
| CN112938923A (en) * | 2020-12-28 | 2021-06-11 | 瓮福（集团）有限责任公司 | Preparation method of nutrient-controllable ammonium polyphosphate |
| WO2022142862A1 (en) * | 2020-12-28 | 2022-07-07 | 瓮福（集团）有限责任公司 | Method for preparing nutrient-controllable ammonium polyphosphate |
| 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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