Summary of the invention
For solving the problems of the technologies described above, the invention provides that a kind of loss of elements is few, environmental pollution is low, rationally, while improving primary ammonium phosphate product purity by-product can make eggplant element be carried out to the preparation method of the eggplant composite fertilizer special absorbed fully in element collocation.
The present invention is achieved by the following technical programs:
Prepare a method for primary ammonium phosphate by-product eggplant composite fertilizer special, the method comprises the following steps:
Prepared by a, raw material: the ratio being first 1.8 ~ 2.2:1.4 ~ 1.6 in molar ratio by phosphoric acid and urea mixes, and phosphoric acid concentration is 65 ~ 75%, is that 8 DEG C/min rises to 85 ~ 120 DEG C by heat-up rate, stirring reaction 20min, and obtained slip, is separated and obtains Ureaphil;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.4 ~ 3.7 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 18-24 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and eggplant obtains the mother liquor of eggplant composite fertilizer special;
D, drying: mother liquor is placed in drying machine, temperature controls at 33 ~ 36 DEG C, and after dry 25 ~ 30min, controlling water content is 3 ~ 5% obtain Fertilizer special for eggplant.
In described step a, the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid, and phosphoric acid and urea mix for the ratio of 2:1.5 in molar ratio, and the concentration of phosphoric acid is 70%.
Described step c medium trace element compound is the inner complex of calcium, magnesium, and in the mother liquor of eggplant composite fertilizer special, the content of nitrogen element is 15%, Vanadium Pentoxide in FLAKES is 3%, potassium element is 11%, calcium constituent is 5%, magnesium elements is 5%.
In described steps d, the nitrogen element content of eggplant composite fertilizer special is 15%, calcium element content is 4%, the content of magnesium elements is 4%, the content of Vanadium Pentoxide in FLAKES is 3%, the content of potassium element is 10%.
In described steps d, eggplant composite fertilizer special is chemical combination state Chemical Mixed Fertilizer.
Following N P and K chemical combination state structural formula is contained in its composition of eggplant composite fertilizer special in described steps d:
wherein, the dotted line between carbon atom and Sauerstoffatom represents to there is coordinate bond between C atom and O atom.
Beneficial effect of the present invention is: slip remaining while preparing highly purified primary ammonium phosphate by phosphoric acid and urea reaction can also be added by element, the techniques such as drying are prepared into the composite fertilizer special needed for eggplant, mother liquor is fully utilized, reduce cost, for the constituent content needed for eggplant and eggplant to the research and analysis of the specific absorption of element, the chemical combination state composite fertilizer requirement meeting eggplant to the full extent prepared, decrease the waste of element, avoid the residual soil contamination problem caused of composite fertilizer.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further described, but described in claimed scope is not limited to.
Reaction principle illustrates:
First by the adjustment to phosphoric acid and urea reaction parameter, prepare Ureaphil, Ureaphil can continue to react with phosphoric acid to form H
2nCONH
3 +and H
2pO
4 -, H
2nCONH
3 +containing under the environment of phosphoric acid, formed when temperature is 85 ~ 120 DEG C
intermediate-ion and dihydrogen phosphate, after adding excessive ammonium radical ion, dihydrogen phosphate and ammonium radical ion react and generate primary ammonium phosphate and separate out, and the ammonium radical ion reaction after adding potassium ion and in intermediate-ion is formed
then add the inner complex of calcium constituent and magnesium elements, form chemical combination state composite fertilizer, after drying treatment, namely obtain eggplant composite fertilizer special.The reaction equation of above-mentioned reaction principle is as follows:
Chemical equation one:
H
2PO
3+CO(NH
2)
2—CO(NH
2)
2·H
3PO
4
Chemical equation two:
CO(NH
2)
2·H
3PO
4—H
2NCONH
3 ++H
2PO
4 -
Chemical equation three:
H
2PO
4 -+NH
4 +—NH
4H
2PO
4
Chemical equation four:
Chemical equation five:
Below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment one
Prepared by a, raw material: the ratio being first 1.8:1.4 in molar ratio by phosphoric acid and urea mixes, phosphoric acid concentration is 65%, be that 8 DEG C/min rises to 85 DEG C by heat-up rate, stirring reaction 20min, obtained slip, separation obtains Ureaphil, and the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.6 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 18 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and eggplant obtains the mother liquor of eggplant composite fertilizer special, trace compound is the inner complex of calcium, magnesium, and in the mother liquor of eggplant composite fertilizer special, the content of nitrogen element is 15%, Vanadium Pentoxide in FLAKES is 3%, potassium element is 11%, calcium constituent is 5%, magnesium elements is 5%;
D, drying: mother liquor is placed in drying machine, temperature controls at 33 DEG C, after dry 25min, controlling water content is 5% obtain Fertilizer special for eggplant, and the nitrogen element content of eggplant composite fertilizer special is 15%, calcium element content is 4%, the content of magnesium elements is 4%, the content of Vanadium Pentoxide in FLAKES is 3%, the content of potassium element is 10%.
Embodiment two
Prepared by a, raw material: the ratio being first 1.8:1.5 in molar ratio by phosphoric acid and urea mixes, phosphoric acid concentration is 66%, be that 8 DEG C/min rises to 90 DEG C by heat-up rate, stirring reaction 20min, obtained slip, separation obtains Ureaphil, and the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.5 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 19 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and eggplant obtains the mother liquor of eggplant composite fertilizer special, trace compound is the inner complex of calcium, magnesium, and in the mother liquor of eggplant composite fertilizer special, the content of nitrogen element is 15%, Vanadium Pentoxide in FLAKES is 3%, potassium element is 11%, calcium constituent is 5%, magnesium elements is 5%;
D, drying: mother liquor is placed in drying machine, temperature controls at 34 DEG C, after dry 26min, controlling water content is 4.8% obtain Fertilizer special for eggplant, and the nitrogen element content of eggplant composite fertilizer special is 15%, calcium element content is 4%, the content of magnesium elements is 4%, the content of Vanadium Pentoxide in FLAKES is 3%, the content of potassium element is 10%.
Embodiment three
Prepared by a, raw material: the ratio being first 1.8:1.6 in molar ratio by phosphoric acid and urea mixes, phosphoric acid concentration is 68%, be that 8 DEG C/min rises to 95 DEG C by heat-up rate, stirring reaction 20min, obtained slip, separation obtains Ureaphil, and the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.6 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 20 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and eggplant obtains the mother liquor of eggplant composite fertilizer special, and trace compound is the inner complex of calcium, magnesium.In the mother liquor of described eggplant composite fertilizer special, the content of nitrogen element is 15%, Vanadium Pentoxide in FLAKES is 3%, potassium element is 11%, calcium constituent is 5%, magnesium elements is 5%;
D, drying: mother liquor is placed in drying machine, temperature controls at 35 DEG C, after dry 27min, controlling water content is 4.4% obtain Fertilizer special for eggplant, and the nitrogen element content of eggplant composite fertilizer special is 15%, calcium element content is 4%, the content of magnesium elements is 4%, the content of Vanadium Pentoxide in FLAKES is 3%, the content of potassium element is 10%.
Embodiment four
Prepared by a, raw material: the ratio being first 2.0:1.4 in molar ratio by phosphoric acid and urea mixes, phosphoric acid concentration is 69%, be that 8 DEG C/min rises to 98 DEG C by heat-up rate, stirring reaction 20min, obtained slip, separation obtains Ureaphil, and the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.4 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 21 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and eggplant obtains the mother liquor of eggplant composite fertilizer special, trace compound is the inner complex of calcium, magnesium, and in the mother liquor of eggplant composite fertilizer special, the content of nitrogen element is 15%, Vanadium Pentoxide in FLAKES is 3%, potassium element is 11%, calcium constituent is 5%, magnesium elements is 5%;
D, drying: mother liquor is placed in drying machine, temperature controls at 35 DEG C, after dry 28min, controlling water content is 4.1% obtain Fertilizer special for eggplant, and the nitrogen element content of eggplant composite fertilizer special is 15%, calcium element content is 4%, the content of magnesium elements is 4%, the content of Vanadium Pentoxide in FLAKES is 3%, the content of potassium element is 10%.
Embodiment five
Prepared by a, raw material: the ratio being first 2.0:1.5 in molar ratio by phosphoric acid and urea mixes, phosphoric acid concentration is 70%, be that 8 DEG C/min rises to 99 DEG C by heat-up rate, stirring reaction 20min, obtained slip, separation obtains Ureaphil, and the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.5 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 22 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and eggplant obtains the mother liquor of eggplant composite fertilizer special, trace compound is the inner complex of calcium, magnesium, and in the mother liquor of eggplant composite fertilizer special, the content of nitrogen element is 15%, Vanadium Pentoxide in FLAKES is 3%, potassium element is 11%, calcium constituent is 5%, magnesium elements is 5%;
D, drying: mother liquor is placed in drying machine, temperature controls at 35.5 DEG C, after dry 29min, controlling water content is 3.8% obtain Fertilizer special for eggplant, and the nitrogen element content of eggplant composite fertilizer special is 15%, calcium element content is 4%, the content of magnesium elements is 4%, the content of Vanadium Pentoxide in FLAKES is 3%, the content of potassium element is 10%.
Embodiment six
Prepared by a, raw material: the ratio being first 2.0:1.6 in molar ratio by phosphoric acid and urea mixes, phosphoric acid concentration is 73%, be that 8 DEG C/min rises to 110 DEG C by heat-up rate, stirring reaction 20min, obtained slip, separation obtains Ureaphil, and the reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid;
B, prepare primary ammonium phosphate: toward containing slowly adding ammoniacal liquor in the slip of Ureaphil to control pH value be 3.6 and fully stirring the slip obtained containing nitrogen, phosphorus, slip is cooled to 23 DEG C in cooling crystallization machine, filtration, separation obtain primary ammonium phosphate;
C, filtrate element add: in the filtrate that separation obtains, the trace compound added needed for potassium element and eggplant obtains the mother liquor of eggplant composite fertilizer special, trace compound is the inner complex of calcium, magnesium, and in the mother liquor of eggplant composite fertilizer special, the content of nitrogen element is 15%, Vanadium Pentoxide in FLAKES is 3%, potassium element is 11%, calcium constituent is 5%, magnesium elements is 5%;
D, drying: mother liquor is placed in drying machine, temperature controls at 36 DEG C, after dry 30min, controlling water content is 3.5% obtain Fertilizer special for eggplant, and the nitrogen element content of eggplant composite fertilizer special is 15%, calcium element content is 4%, the content of magnesium elements is 4%, the content of Vanadium Pentoxide in FLAKES is 3%, the content of potassium element is 10%.
Below in conjunction with specific experiment example, product of the present invention and technique effect are further described.
Experimental example one
The embodiment of the present invention one, embodiment two, embodiment three, embodiment four, embodiment five, embodiment six, in the primary ammonium phosphate product prepared detect by the standard of GB25569-2010, detected result is as shown in table 1:
Table 1 primary ammonium phosphate product purity of the present invention detects
Primary ammonium phosphate |
Criterion of acceptability |
Embodiment one |
Embodiment two |
Embodiment three |
Embodiment four |
Embodiment five |
Embodiment six |
Purity >=% |
96 |
98.2 |
98.6 |
98.1 |
98.3 |
98.2 |
98.3 |
Moisture≤% |
0.5 |
0.4 |
0.43 |
0.42 |
0.41 |
0.41 |
0.4 |
As can be seen from Table 1, the primary ammonium phosphate that technical scheme of the present invention is produced not only reaches criterion of acceptability, and the purity of product is also higher, illustrates that present method is prepared primary ammonium phosphate product and had significant progress.
Experimental example two
According to the absorption of eggplant to constituent content and the growing state of eggplant, test is compared to eggplant composite fertilizer special and Common compound fertilizer.With 9 eggplants for subjects, label is A, B, C, D, E, F, G, H, I, uses common fertilizer to the eggplant of A, B, C tri-labels respectively, use Fertilizer special for eggplant prepared in embodiment one, embodiment two, embodiment three, embodiment four, embodiment five, embodiment six respectively to the eggplant seedling of six labels such as D, E, F, G, H, I, contrast and experiment is as shown in table 2:
Table 2 use Common compound fertilizer and eggplant composite fertilizer special on eggplant element absorption rate on when on the impact that eggplant grows
The eggplant composite fertilizer special that as can be seen from the above table prepared by the present invention can be absorbed fully by eggplant, and the nutritive element be rich in needed for the eggplants such as Ca, Me, guarantee is provided to the normal growth of eggplant, is improving eggplant growing way, while prevention eggplant is ill, improve economic benefit.