CN104310341B - A kind of method for preparing ammonium dihydrogen phosphate by-product grapefruit special complex fertilizer - Google Patents
A kind of method for preparing ammonium dihydrogen phosphate by-product grapefruit special complex fertilizer Download PDFInfo
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- CN104310341B CN104310341B CN201410478887.5A CN201410478887A CN104310341B CN 104310341 B CN104310341 B CN 104310341B CN 201410478887 A CN201410478887 A CN 201410478887A CN 104310341 B CN104310341 B CN 104310341B
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Abstract
The invention discloses a kind of method for preparing ammonium dihydrogen phosphate by-product grapefruit special complex fertilizer, this method comprises the following steps：Raw material prepares, prepares ammonium dihydrogen phosphate, filtrate element addition, dries.Adjustment is processed to mother liquor caused by reaction while preparing the ammonium dihydrogen phosphate of high-purity by phosphoric acid and the reaction of urea and ammoniacal liquor, the composite fertilizer suitable for grapefruit growth is prepared into, reduces the waste of resource, there is the certain value of environmental protection and economic value.
Description
Technical field
The present invention relates to technical field of fertilizers, and in particular to one kind prepares ammonium dihydrogen phosphate by-product grapefruit special complex fertilizer
Method.
Background technology
Grapefruit, Rutaceae.Aiphyllium leaf is big and thick, and winged petiole is big, in heart-shaped.Hua great, normal fasciation is into raceme.
Fruit is big, circular, oblate or wealthy obovate, in faint yellow or orange when ripe.Pericarp is thick, has big oil droplet, is not easily stripped.Fruit
Meat white is red, and entitled shaddock, shaddock fruity sweet and sour palatability, autumn Mo is ripe, storage tolerance, seed list embryo.Fruit eat raw or
Processing, pericarp can preserved fruit processed.The extractable aromatic oil of flower, leaf, pericarp, and the shaddock of high-quality be unable to do without good fertilizer, shaddock
The main nutrient elements that subtree absorbs is nitrogen, phosphorus, potassium, calcium, magnesium etc., but in common fertilizer N P and K utilization rate it is very low, typically
Nitrogen use efficiency is 20%-40% in composite fertilizer, and phosphorus only has 20% or so, and potassium is up to more than 30%.It follows that this season profit of phosphorus
Minimum with rate, nitrogen, the utilization rate of potassium are suitable.There is loss of elements height in common fertilizer, Soil Environmental Pollution is big, and cost height etc. is asked
Topic, so for the difference of crop, the specificity of composite fertilizer has great importance.
There is the technology of preparing of mixing composite fertilizer currently for crops, but not in Patents file and open text
Offer and find for the different by the research to element needed for crop of variety of crops, the compound state that element is arranged in pairs or groups
The technical scheme of composite fertilizer is present, and is also preparing the skill of ammonium dihydrogen phosphate byproduct in process grapefruit special complex fertilizer without discovery
Art scheme occurs.
Therefore, the present inventor by largely study and put into practice from needed for grapefruit element collocation based on, improve phosphoric acid
Whole production technology and ginseng are adjusted to the absorptivity of required element for crop while preparing the purity of ammonium dihydrogen phosphate product
Number by-product goes out the special efficient composite fertilizer suitable for grapefruit.
The content of the invention
In order to solve the above technical problems, the invention provides a kind of loss of elements is few, environmental pollution is low, element collocation is closed
Reason, the grapefruit that by-product can make grapefruit sufficiently absorb element while ammonium dihydrogen phosphate product purity is improved are special
With the preparation method of composite fertilizer.
The present invention is achieved by the following technical programs：
A kind of method for preparing ammonium dihydrogen phosphate by-product grapefruit special complex fertilizer, this method comprise the following steps：
A, prepared by raw material：It is first 2 in molar ratio by phosphoric acid and urea:1.4~1.6 ratio mixing, phosphoric acid concentration 70
~74%, it is that 6 DEG C/min rises to 90-120 DEG C, stirring reaction 28min by programming rate, slurry, isolated urea phosphate is made；
B, ammonium dihydrogen phosphate is prepared：Ammoniacal liquor is slowly added into the slurry containing urea phosphate and controls pH value as 3.2~3.6 simultaneously
It is sufficiently stirred to obtain the slurry containing nitrogen, phosphorus, slurry is through being cooled to 24 DEG C, filtering, isolated di(2-ethylhexyl)phosphate in cooling crystallization machine
Hydrogen ammonium；
C, filtrate element is added：Potassium element and the micro- chemical combination needed for grapefruit are added into isolated filtrate
Thing obtains the mother liquor of grapefruit special complex fertilizer；
D, drying：Mother liquor is placed in drying machine, temperature control is at 38 DEG C, and after drying 24min, it is 4% to control water content
Obtain grapefruit special fertilizer.
The reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid in the step a, and phosphoric acid and urea are massaged
You are than being 2:1.4 ratio mixing, the concentration of phosphoric acid is 72%.
Trace element compound is calcium, the chelate of magnesium in the step c, nitrogen member in the mother liquor of grapefruit special complex fertilizer
The content of element is 15.7%, phosphorus pentoxide 7.6%, potassium element 8.2%, calcium constituent 4.5%, magnesium elements 4.3%.
In the step d nitrogen element content of grapefruit special complex fertilizer be 15.4%, calcium element content 3.8%, magnesium
The content of element is 4.1%, the content of phosphorus pentoxide is 7.3%, the content of potassium element is 8.1%.
Grapefruit special complex fertilizer is compound state chemical mixed fertilizer in the step d.
Contain following N P and K compound state structural formula in the step d in its composition of grapefruit special complex fertilizer：
Wherein, the dotted line between carbon atom and oxygen atom is represented between C atoms and O atom
Coordinate bond be present.
The beneficial effects of the present invention are：While the ammonium dihydrogen phosphate of high-purity being prepared by phosphoric acid and urea reaction
Remaining slurry can also be added by element, and the technique such as dry is prepared into the special complex fertilizer needed for grapefruit, and mother liquor obtains
Sufficient utilization, reduces cost, for the research of the constituent content needed for grapefruit and grapefruit to the absorptivity of element
And analysis, the requirement for meeting grapefruit of the compound state composite fertilizer prepared to the full extent, reduce the waste of element,
Avoid soil contamination problem caused by the residual of composite fertilizer.
Embodiment
Technical scheme is further described with reference to embodiments, but claimed scope is not limited to
In described.
Reaction principle explanation：
First by the adjustment to phosphoric acid and urea reaction parameter, urea phosphate is prepared, urea phosphate can continue to and phosphoric acid
React to form H2NCONH3 +And H2PO4 -, H2NCONH3 +In the environment of containing phosphoric acid, the shape when temperature is 85~120 DEG C
IntoIntermediate-ion and dihydrogen phosphate, after adding excessive ammonium ion, dihydrogen phosphate
Generation ammonium dihydrogen phosphate is reacted with ammonium ion to separate out, and is added the ammonium ion after potassium ion and in intermediate-ion and is reacted to be formedThen the chelate of calcium constituent and magnesium elements is added, compound state composite fertilizer is formed, through overdrying
Grapefruit special complex fertilizer is obtained after dry processing.The reaction equation of above-mentioned reaction principle is as follows：
Chemical equation one：
H2PO3+CO(NH2)2—CO(NH2)2·H3PO4
Chemical equation two：
CO(NH2)2·H3PO4—H2NCONH3 ++H2PO4 -
Chemical equation three：
H2PO4 -+NH4 +—NH4H2PO4
Chemical equation four：
Chemical equation five：
With reference to specific embodiment, the present invention is further elaborated.
Embodiment one
A, prepared by raw material：It is first 2 in molar ratio by phosphoric acid and urea:1.4 ratio mixing, phosphoric acid concentration 70%, is pressed
Programming rate is that 6 DEG C/min rises to 90 DEG C, stirring reaction 28min, is made slurry, isolated urea phosphate, phosphoric acid and urea
React the reaction for phosphoric acid solution and urea solid；
B, ammonium dihydrogen phosphate is prepared：Ammoniacal liquor is slowly added into the slurry containing urea phosphate controls pH value simultaneously abundant for 3.6
Stirring obtains the slurry containing nitrogen, phosphorus, and slurry is through being cooled to 24 DEG C, filtering, isolated ammonium dihydrogen phosphate in cooling crystallization machine；
C, filtrate element is added：Potassium element and the micro- chemical combination needed for grapefruit are added into isolated filtrate
Thing obtains the mother liquor of grapefruit special complex fertilizer, and trace element compound is calcium, the chelate of magnesium, grapefruit special complex fertilizer
In mother liquor the content of nitrogen be 15.7%, phosphorus pentoxide 7.6%, potassium element 8.2%, calcium constituent 4.5%, magnesium member
Element is 4.3%；
D, drying：Mother liquor is placed in drying machine, temperature control is at 38 DEG C, and after drying 24min, it is 4% to control water content
Obtain grapefruit special fertilizer, the nitrogen element content of grapefruit special complex fertilizer is 15.4%, calcium element content 3.8%, magnesium member
The content of element is 4.1%, the content of phosphorus pentoxide is 7.3%, the content of potassium element is 8.1%.
Embodiment two
A, prepared by raw material：It is first 2 in molar ratio by phosphoric acid and urea:1.5 ratio mixing, phosphoric acid concentration 71%, is pressed
Programming rate is that 6 DEG C/min rises to 95 DEG C, stirring reaction 28min, is made slurry, isolated urea phosphate, phosphoric acid and urea
React the reaction for phosphoric acid solution and urea solid；
B, ammonium dihydrogen phosphate is prepared：Ammoniacal liquor is slowly added into the slurry containing urea phosphate controls pH value simultaneously abundant for 3.5
Stirring obtains the slurry containing nitrogen, phosphorus, and slurry is through being cooled to 24 DEG C, filtering, isolated ammonium dihydrogen phosphate in cooling crystallization machine；
C, filtrate element is added：Potassium element and the micro- chemical combination needed for grapefruit are added into isolated filtrate
Thing obtains the mother liquor of grapefruit special complex fertilizer, and trace element compound is calcium, the chelate of magnesium, grapefruit special complex fertilizer
In mother liquor the content of nitrogen be 15.7%, phosphorus pentoxide 7.6%, potassium element 8.2%, calcium constituent 4.5%, magnesium member
Element is 4.3%；
D, drying：Mother liquor is placed in drying machine, temperature control is at 38 DEG C, and after drying 24min, it is 4% to control water content
Obtain grapefruit special fertilizer, the nitrogen element content of grapefruit special complex fertilizer is 15.4%, calcium element content 3.8%, magnesium member
The content of element is 4.1%, the content of phosphorus pentoxide is 7.3%, the content of potassium element is 8.1%.
Embodiment three
A, prepared by raw material：It is first 2 in molar ratio by phosphoric acid and urea:1.6 ratio mixing, phosphoric acid concentration 73%, is pressed
Programming rate is that 6 DEG C/min rises to 90-120 DEG C, stirring reaction 28min, and slurry, isolated urea phosphate, phosphoric acid and urine is made
The reaction of element is the reaction of phosphoric acid solution and urea solid；
B, ammonium dihydrogen phosphate is prepared：Ammoniacal liquor is slowly added into the slurry containing urea phosphate controls pH value simultaneously abundant for 3.4
Stirring obtains the slurry containing nitrogen, phosphorus, and slurry is through being cooled to 24 DEG C, filtering, isolated ammonium dihydrogen phosphate in cooling crystallization machine；
C, filtrate element is added：Potassium element and the micro- chemical combination needed for grapefruit are added into isolated filtrate
Thing obtains the mother liquor of grapefruit special complex fertilizer, and trace element compound is calcium, the chelate of magnesium, grapefruit special complex fertilizer
In mother liquor the content of nitrogen be 15.7%, phosphorus pentoxide 7.6%, potassium element 8.2%, calcium constituent 4.5%, magnesium member
Element is 4.3%；
D, drying：Mother liquor is placed in drying machine, temperature control is at 38 DEG C, and after drying 24min, it is 4% to control water content
Obtain grapefruit special fertilizer, the nitrogen element content of grapefruit special complex fertilizer is 15.4%, calcium element content 3.8%, magnesium member
The content of element is 4.1%, the content of phosphorus pentoxide is 7.3%, the content of potassium element is 8.1%.
Example IV
A, prepared by raw material：It is first 2 in molar ratio by phosphoric acid and urea:1.4 ratio mixing, phosphoric acid concentration 74%, is pressed
Programming rate is that 6 DEG C/min rises to 100 DEG C, stirring reaction 28min, is made slurry, isolated urea phosphate, phosphoric acid and urea
React the reaction for phosphoric acid solution and urea solid；
B, ammonium dihydrogen phosphate is prepared：Ammoniacal liquor is slowly added into the slurry containing urea phosphate controls pH value simultaneously abundant for 3.3
Stirring obtains the slurry containing nitrogen, phosphorus, and slurry is through being cooled to 24 DEG C, filtering, isolated ammonium dihydrogen phosphate in cooling crystallization machine；
C, filtrate element is added：Potassium element and the micro- chemical combination needed for grapefruit are added into isolated filtrate
Thing obtains the mother liquor of grapefruit special complex fertilizer, and trace element compound is calcium, the chelate of magnesium, grapefruit special complex fertilizer
In mother liquor the content of nitrogen be 15.7%, phosphorus pentoxide 7.6%, potassium element 8.2%, calcium constituent 4.5%, magnesium member
Element is 4.3%；
D, drying：Mother liquor is placed in drying machine, temperature control is at 38 DEG C, and after drying 24min, it is 4% to control water content
Obtain grapefruit special fertilizer, the nitrogen element content of grapefruit special complex fertilizer is 15.4%, calcium element content 3.8%, magnesium member
The content of element is 4.1%, the content of phosphorus pentoxide is 7.3%, the content of potassium element is 8.1%.
Embodiment five
A, prepared by raw material：It is first 2 in molar ratio by phosphoric acid and urea:1.4 ratio mixing, phosphoric acid concentration 74%, is pressed
Programming rate is that 6 DEG C/min rises to 105 DEG C, stirring reaction 28min, is made slurry, isolated urea phosphate, phosphoric acid and urea
React the reaction for phosphoric acid solution and urea solid；
B, ammonium dihydrogen phosphate is prepared：Ammoniacal liquor is slowly added into the slurry containing urea phosphate controls pH value simultaneously abundant for 3.3
Stirring obtains the slurry containing nitrogen, phosphorus, and slurry is through being cooled to 24 DEG C, filtering, isolated ammonium dihydrogen phosphate in cooling crystallization machine；
C, filtrate element is added：Potassium element and the micro- chemical combination needed for grapefruit are added into isolated filtrate
Thing obtains the mother liquor of grapefruit special complex fertilizer, and trace element compound is calcium, the chelate of magnesium, grapefruit special complex fertilizer
In mother liquor the content of nitrogen be 15.7%, phosphorus pentoxide 7.6%, potassium element 8.2%, calcium constituent 4.5%, magnesium member
Element is 4.3%；
D, drying：Mother liquor is placed in drying machine, temperature control is at 38 DEG C, and after drying 24min, it is 4% to control water content
Obtain grapefruit special fertilizer, the nitrogen element content of grapefruit special complex fertilizer is 15.4%, calcium element content 3.8%, magnesium member
The content of element is 4.1%, the content of phosphorus pentoxide is 7.3%, the content of potassium element is 8.1%.
Embodiment six
A, prepared by raw material：It is first 2 in molar ratio by phosphoric acid and urea:1.6 ratio mixing, phosphoric acid concentration 74%, is pressed
Programming rate is that 6 DEG C/min rises to 120 DEG C, stirring reaction 28min, is made slurry, isolated urea phosphate, phosphoric acid and urea
React the reaction for phosphoric acid solution and urea solid；
B, ammonium dihydrogen phosphate is prepared：Ammoniacal liquor is slowly added into the slurry containing urea phosphate controls pH value simultaneously abundant for 3.4
Stirring obtains the slurry containing nitrogen, phosphorus, and slurry is through being cooled to 24 DEG C, filtering, isolated ammonium dihydrogen phosphate in cooling crystallization machine；
C, filtrate element is added：Potassium element and the micro- chemical combination needed for grapefruit are added into isolated filtrate
Thing obtains the mother liquor of grapefruit special complex fertilizer, and trace element compound is calcium, the chelate of magnesium, grapefruit special complex fertilizer
In mother liquor the content of nitrogen be 15.7%, phosphorus pentoxide 7.6%, potassium element 8.2%, calcium constituent 4.5%, magnesium member
Element is 4.3%；
D, drying：Mother liquor is placed in drying machine, temperature control is at 38 DEG C, and after drying 24min, it is 4% to control water content
Obtain grapefruit special fertilizer, the nitrogen element content of grapefruit special complex fertilizer is 15.4%, calcium element content 3.8%, magnesium member
The content of element is 4.1%, the content of phosphorus pentoxide is 7.3%, the content of potassium element is 8.1%.
The product and technique effect of the present invention are further described with reference to specific experiment example.
Experimental example one
The embodiment of the present invention one, embodiment two, embodiment three, example IV, embodiment five, embodiment six, in prepare
Ammonium dihydrogen phosphate product detected by the standard of GB25569-2010, testing result is as shown in table 1：
The ammonium dihydrogen phosphate product purity detecting of the present invention of table 1
| Ammonium dihydrogen phosphate | Criterion of acceptability | Embodiment one | Embodiment two | Embodiment three | Example IV | Embodiment five | Embodiment six |
| Purity >=% | 96 | 98.3 | 98.5 | 98.3 | 98.1 | 98 | 98.2 |
| Moisture≤% | 0.5 | 0.39 | 0.41 | 0.42 | 0.4 | 0.43 | 0.41 |
As can be seen from Table 1, the ammonium dihydrogen phosphate that technical scheme is produced has not only reached qualified mark
Standard, and the purity of product is also higher, illustrates that this method prepares ammonium dihydrogen phosphate product and has significant progress.
Experimental example two
According to absorption of the grapefruit to constituent content and the growing state of grapefruit, to grapefruit special complex fertilizer and commonly
Composite fertilizer compares experiment.Using 9 grapefruits as subjects, respectively marked as A, B, C, D, E, F, G, H, I, to A, B, C tri-
The grapefruit of individual label applies common fertilizer, and embodiment is applied respectively to the grapefruit seedling of six labels such as D, E, F, G, H, I
First, grapefruit special fertilizer prepared in embodiment two, embodiment three, example IV, embodiment five, embodiment six, contrast
Experimental result is as shown in table 2：
Table 2 applies Common compound fertilizer and grapefruit special complex fertilizer to grapefruit element absorption rate to when to shaddock
Set the influence of growth
The grapefruit special complex fertilizer that as can be seen from the above table prepared by the present invention can sufficiently be absorbed by grapefruit, and
Nutrient needed for also rich in grapefruits such as Ca, Me, provides guarantee to the normal growth of grapefruit, improves grapefruit
Growing way, the yield of shaddock is added, so as to improve economic benefit.
Claims (3)
- A kind of 1. method for preparing ammonium dihydrogen phosphate by-product grapefruit special complex fertilizer, it is characterised in that this method includes following Step：A, prepared by raw material：It is first 2 in molar ratio by phosphoric acid and urea:1.4~1.6 ratio mixing, phosphoric acid concentration be 70~ 74%, it is that 6 DEG C/min rises to 90-120 DEG C, stirring reaction 28min by programming rate, slurry, isolated urea phosphate is made；B, ammonium dihydrogen phosphate is prepared：Ammoniacal liquor is slowly added into the slurry containing urea phosphate controls p H values to be 3.2~3.6 and fill Stirring is divided to obtain the slurry containing nitrogen, phosphorus, slurry is through being cooled to 24 DEG C, filtering, isolated biphosphate in cooling crystallization machine Ammonium；C, filtrate element is added：Potassium element is added into isolated filtrate and the trace element compound needed for grapefruit obtains To the mother liquor of grapefruit special complex fertilizer；D, drying：Mother liquor is placed in drying machine, temperature control is at 38 DEG C, after drying 24min, controls water content to be obtained for 4% Grapefruit special fertilizer；The reaction of phosphoric acid and urea is the reaction of phosphoric acid solution and urea solid in the step a, and phosphoric acid and urea are in molar ratio For 2:1.4 ratio mixing, the concentration of phosphoric acid is 72%；Trace element compound is calcium, the chelate of magnesium in the step c, nitrogen in the mother liquor of grapefruit special complex fertilizer Content is 15.7%, phosphorus pentoxide 7.6%, potassium element 8.2%, calcium constituent 4.5%, magnesium elements 4.3%；In the step d nitrogen element content of grapefruit special complex fertilizer be 15.4%, calcium element content 3.8%, magnesium elements Content be 4.1%, the content of phosphorus pentoxide is 7.3%, the content of potassium element is 8.1%.
- 2. the method according to claim 1 for preparing ammonium dihydrogen phosphate by-product grapefruit special complex fertilizer, it is characterised in that： Grapefruit special complex fertilizer is compound state chemical mixed fertilizer in the step d.
- 3. the method according to claim 1 for preparing ammonium dihydrogen phosphate by-product grapefruit special complex fertilizer, it is characterised in that： Contain following N P and K compound state structural formula in the step d in its composition of grapefruit special complex fertilizer：Wherein, the dotted line between carbon atom and oxygen atom represents to deposit between C atoms and O atom In coordinate bond.
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| CN201410478887.5A CN104310341B (en) | 2014-09-19 | 2014-09-19 | A kind of method for preparing ammonium dihydrogen phosphate by-product grapefruit special complex fertilizer |
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| US6254655B1 (en) * | 1999-03-18 | 2001-07-03 | Oms Investments, Inc. | Processes for preparing granular composite fertilizer compositions and products produced thereby |
| CN103787293A (en) * | 2014-01-24 | 2014-05-14 | 贵阳中化开磷化肥有限公司 | Method for preparing sodium dihydrogen phosphate by utilizing phosphoric acid by wet process |
| CN104016323A (en) * | 2014-05-20 | 2014-09-03 | 贵阳中化开磷化肥有限公司 | Production method for monoammonium phosphate |
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