CN104291292B - A kind of method preparing ammonium dihydrogen phosphate by-product blue berry composite fertilizer special - Google Patents

A kind of method preparing ammonium dihydrogen phosphate by-product blue berry composite fertilizer special Download PDF

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Publication number
CN104291292B
CN104291292B CN201410481995.8A CN201410481995A CN104291292B CN 104291292 B CN104291292 B CN 104291292B CN 201410481995 A CN201410481995 A CN 201410481995A CN 104291292 B CN104291292 B CN 104291292B
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blue berry
composite fertilizer
dihydrogen phosphate
ammonium dihydrogen
fertilizer special
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CN201410481995.8A
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CN104291292A (en
Inventor
陈肖虎
郑培俊
高贵龙
廖吉星
薛涛
熊刚
曾舒
廖川
黄芳
赵平原
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Guiyang Kailin Chemical Co Ltd
Guizhou University
Guizhou Kexin Chemical and Metallurgical Co Ltd
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Guiyang Kailin Chemical Co Ltd
Guizhou University
Guizhou Kexin Chemical and Metallurgical Co Ltd
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Abstract

The invention discloses a kind of method preparing ammonium dihydrogen phosphate by-product blue berry composite fertilizer special, the method comprises the following steps: raw material is prepared, prepares ammonium dihydrogen phosphate, the interpolation of filtrate element, is dried.Reacted the mother solution while preparing highly purified ammonium dihydrogen phosphate, reaction produced to be processed adjusting by phosphoric acid and carbamide and ammonia, be prepared as being suitable to the compound fertilizer of blue berry growth, decrease the waste of resource, there is certain value of environmental protection and economic worth.

Description

A kind of method preparing ammonium dihydrogen phosphate by-product blue berry composite fertilizer special
Technical field
The present invention relates to technical field of fertilizers, be specifically related to a kind of ammonium dihydrogen phosphate by-product blue berry composite fertilizer special prepared Method.
Background technology
Blue berry is shrub, and tree body size and morphological differences are notable.The height of tree, from 5m to 0.3m, is grown thickly for many years, and having evergreen also has Fallen leaves, single leaf alternate, Ye Quanyuan or have sawtooth.Corolla is often in urniform or bell-shaped.Petal base portion is combined, and outer rim 4 or 5 is split, white Or pink, stamen 8~10, it is shorter than style, by insecticide or anemophily, inflorescence mostly is raceme.Most kinds are ripe Shi Guoshi is black-and-blue, and some kinds are red;Fruit has spherical, oval, oblate or pyriform, and average fruit weight is about 0.5 ~between 2.5g.Sarcocarp is soft, many juices.Seed is tiny, can not affect mouthfeel time edible under eating with sarcocarp, and root system is many and fine Carefully, sturdy few, is distributed shallow, does not has root hair.The blue berry of high-quality be unable to do without good fertilizer, the Major Nutrient unit that blue berry absorbs Element is nitrogen, phosphorus, potassium, boron, magnesium etc., but in common fertilizer, the utilization rate of N P and K is the lowest, and in general compound fertilizer, nitrogen use efficiency is 20%-40%, phosphorus only has about 20%, and potassium is up to more than 30%.It follows that this season utilization rate of phosphorus is minimum, nitrogen, the profit of potassium Suitable by rate.It is high to there is loss of elements in common fertilizer, and Soil Environmental Pollution is big, high in cost of production problem, so for crop not With, the specificity of compound fertilizer has great importance.
The technology of preparing mixing compound fertilizer is also had currently for crops, but not at Patents file and open literary composition Offer the discovery difference for variety of crops by the research of element needed for crop, the compound state carrying out element arranging in pairs or groups The technical scheme of compound fertilizer exists, and does not the most find in the technology preparing ammonium dihydrogen phosphate byproduct in process blue berry composite fertilizer special Scheme occurs.
Therefore, by substantial amounts of research and practice, element collocation needed for blue berry is main to the present inventor, is improving phosphoric acid system For crop, the absorbance of required element is adjusted whole production technology and parameter while the purity of standby ammonium dihydrogen phosphate product By-product goes out to be applicable to the special efficient compound fertilizer of blue berry.
Summary of the invention
For solving above-mentioned technical problem, loss of elements is few, environmental pollution is low, element collocation is closed to the invention provides one Reason, the blue berry that by-product can make blue berry sufficiently absorb element while improving ammonium dihydrogen phosphate product purity are special multiple The preparation method in Hefei.
The present invention is achieved by the following technical programs:
A kind of method preparing ammonium dihydrogen phosphate by-product blue berry composite fertilizer special, the method comprises the following steps:
Prepared by a, raw material: first by phosphoric acid and carbamide, ratio for 1.8:1.1-1.4 mixes in molar ratio, and phosphoric acid concentration is 68-72%, is that 4 DEG C/min rises to 84-104 DEG C by programming rate, stirring reaction 30min, prepares slip, isolated phosphoric acid Urea;
B, prepare ammonium dihydrogen phosphate: be slowly added to ammonia in the slip containing urea phosphate controlling pH value is 3.3~3.6 also Be sufficiently stirred for obtaining containing nitrogen, the slip of phosphorus, the cooled crystallizer of slip is cooled to 25 DEG C, filter, isolated di(2-ethylhexyl)phosphate Hydrogen ammonium;
C, filtrate element add: add the trace compound needed for potassium element and blue berry in the filtrate of isolated Obtain the mother solution of blue berry composite fertilizer special;
D, it is dried: being placed in drying machine by mother solution, temperature controls at 32 DEG C, is dried after 30min, and controlling water content is 4% Obtain blueberry special fertilizer.
In described step a, phosphoric acid is massaged with the react reaction for phosphoric acid solution with urea solid, phosphoric acid and the carbamide of carbamide You mix than the ratio for 1.8:1.3, and the concentration of phosphoric acid is 71%.
In described step c, trace compound is the chelate of calcium, magnesium, nitrogen element in the mother solution of blue berry composite fertilizer special Content be 15.5%, phosphorus pentoxide be 7.5%, potassium element be 8.5%, calcium constituent be 4.2%, magnesium elements be 4.4%.
In described step d the nitrogen element content of blue berry composite fertilizer special be 15.2%, calcium element content be 4%, magnesium elements Content be 4.1%, the content of phosphorus pentoxide be 7.2%, the content of potassium element be 8.2%.
In described step d, blue berry composite fertilizer special is compound state Chemical Mixed Fertilizer.
Containing following N P and K compound state structural formula in its composition of blue berry composite fertilizer special in described step d:
Wherein, the dotted line between carbon atom and oxygen atom represent C atom and O atom it Between there is coordinate bond.
The beneficial effects of the present invention is: while preparing highly purified ammonium dihydrogen phosphate by phosphoric acid and urea reaction The techniques such as remaining slip can also be added by element, dry are prepared as the composite fertilizer special needed for blue berry, and mother solution obtains Sufficiently utilize, reduce cost, the research and analysis to the absorbance of element for the constituent content needed for blue berry and blue berry, The compound state compound fertilizer the prepared requirement meeting blue berry to the full extent, decrease the waste of element, it is to avoid multiple The soil contamination problem that the residual in Hefei causes.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme is further described, but claimed scope is not limited to In described.
Reaction principle illustrates:
First passing through the adjustment to phosphoric acid Yu urea reaction parameter, prepare urea phosphate, urea phosphate can continue to and phosphoric acid React formation H2NCONH3 +And H2PO4 -, H2NCONH3 +In the environment of containing phosphoric acid, the shape when temperature is 85~120 DEG C BecomeIntermediate-ion and dihydrogen phosphate, after adding the ammonium radical ion of excess, dihydrogen phosphate Reacting generation ammonium dihydrogen phosphate with ammonium radical ion to separate out, the ammonium radical ion reaction after adding potassium ion and in intermediate-ion is formedIt is subsequently adding the chelate of calcium constituent and magnesium elements, forms compound state compound fertilizer, through overdrying Blue berry composite fertilizer special is i.e. obtained after dry process.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:
Below in conjunction with specific embodiment, the present invention is further elaborated.
Embodiment one
Prepared by a, raw material: first by phosphoric acid and carbamide, ratio for 1.8:1.1 mixes in molar ratio, and phosphoric acid concentration is 68%, It is that 4 DEG C/min rises to 84 DEG C by programming rate, stirring reaction 30min, prepare slip, isolated urea phosphate, phosphoric acid and carbamide Reaction be phosphoric acid solution and urea solid reaction;
B, prepare ammonium dihydrogen phosphate: be slowly added to ammonia in the slip containing urea phosphate controlling pH value is 3.3 and fully Stirring obtain containing nitrogen, the slip of phosphorus, the cooled crystallizer of slip is cooled to 25 DEG C, filter, isolated ammonium dihydrogen phosphate;
C, filtrate element add: add the trace compound needed for potassium element and blue berry in the filtrate of isolated Obtaining the mother solution of blue berry composite fertilizer special, trace compound is the chelate of calcium, magnesium, in the mother solution of blue berry composite fertilizer special The content of nitrogen element is 15.5%, phosphorus pentoxide is 7.5%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.4%;
D, it is dried: being placed in drying machine by mother solution, temperature controls at 32 DEG C, is dried after 30min, and controlling water content is 4% Obtaining blueberry special fertilizer, the nitrogen element content of blue berry composite fertilizer special is 15.2%, calcium element content is 4%, the containing of magnesium elements Amount is 4.1%, the content of phosphorus pentoxide is 7.2%, the content of potassium element is 8.2%.
Embodiment two
Prepared by a, raw material: first by phosphoric acid and carbamide, ratio for 1.8:1.1 mixes in molar ratio, and phosphoric acid concentration is 69%, It is that 4 DEG C/min rises to 88 DEG C by programming rate, stirring reaction 30min, prepare slip, isolated urea phosphate, phosphoric acid and carbamide Reaction be phosphoric acid solution and urea solid reaction;
B, prepare ammonium dihydrogen phosphate: be slowly added to ammonia in the slip containing urea phosphate controlling pH value is 3.4 and fully Stirring obtain containing nitrogen, the slip of phosphorus, the cooled crystallizer of slip is cooled to 25 DEG C, filter, isolated ammonium dihydrogen phosphate;
C, filtrate element add: add the trace compound needed for potassium element and blue berry in the filtrate of isolated Obtaining the mother solution of blue berry composite fertilizer special, trace compound is the chelate of calcium, magnesium, in the mother solution of blue berry composite fertilizer special The content of nitrogen element is 15.5%, phosphorus pentoxide is 7.5%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.4%;
D, it is dried: being placed in drying machine by mother solution, temperature controls at 32 DEG C, is dried after 30min, and controlling water content is 4% Obtaining blueberry special fertilizer, the nitrogen element content of blue berry composite fertilizer special is 15.2%, calcium element content is 4%, the containing of magnesium elements Amount is 4.1%, the content of phosphorus pentoxide is 7.2%, the content of potassium element is 8.2%.
Embodiment three
Prepared by a, raw material: first by phosphoric acid and carbamide, ratio for 1.8:1.2 mixes in molar ratio, and phosphoric acid concentration is 70%, It is that 4 DEG C/min rises to 84 DEG C by programming rate, stirring reaction 30min, prepare slip, isolated urea phosphate, phosphoric acid and carbamide Reaction be phosphoric acid solution and urea solid reaction;
B, prepare ammonium dihydrogen phosphate: be slowly added to ammonia in the slip containing urea phosphate controlling pH value is 3.4 and fully Stirring obtain containing nitrogen, the slip of phosphorus, the cooled crystallizer of slip is cooled to 25 DEG C, filter, isolated ammonium dihydrogen phosphate;
C, filtrate element add: add the trace compound needed for potassium element and blue berry in the filtrate of isolated Obtaining the mother solution of blue berry composite fertilizer special, trace compound is the chelate of calcium, magnesium, in the mother solution of blue berry composite fertilizer special The content of nitrogen element is 15.5%, phosphorus pentoxide is 7.5%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.4%;
D, it is dried: being placed in drying machine by mother solution, temperature controls at 32 DEG C, is dried after 30min, and controlling water content is 4% Obtaining blueberry special fertilizer, the nitrogen element content of blue berry composite fertilizer special is 15.2%, calcium element content is 4%, the containing of magnesium elements Amount is 4.1%, the content of phosphorus pentoxide is 7.2%, the content of potassium element is 8.2%.
Embodiment four
Prepared by a, raw material: first by phosphoric acid and carbamide, ratio for 1.8:1.3 mixes in molar ratio, and phosphoric acid concentration is 71%, It is that 4 DEG C/min rises to 88 DEG C by programming rate, stirring reaction 30min, prepare slip, isolated urea phosphate, phosphoric acid and carbamide Reaction be phosphoric acid solution and urea solid reaction;
B, prepare ammonium dihydrogen phosphate: be slowly added to ammonia in the slip containing urea phosphate controlling pH value is 3.5 and fully Stirring obtain containing nitrogen, the slip of phosphorus, the cooled crystallizer of slip is cooled to 25 DEG C, filter, isolated ammonium dihydrogen phosphate;
C, filtrate element add: add the trace compound needed for potassium element and blue berry in the filtrate of isolated Obtaining the mother solution of blue berry composite fertilizer special, trace compound is the chelate of calcium, magnesium, in the mother solution of blue berry composite fertilizer special The content of nitrogen element is 15.5%, phosphorus pentoxide is 7.5%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.4%;
D, it is dried: being placed in drying machine by mother solution, temperature controls at 32 DEG C, is dried after 30min, and controlling water content is 4% Obtaining blueberry special fertilizer, the nitrogen element content of blue berry composite fertilizer special is 15.2%, calcium element content is 4%, the containing of magnesium elements Amount is 4.1%, the content of phosphorus pentoxide is 7.2%, the content of potassium element is 8.2%.
Embodiment five
Prepared by a, raw material: first by phosphoric acid and carbamide, ratio for 1.8:1.4 mixes in molar ratio, and phosphoric acid concentration is 71%, It is that 4 DEG C/min rises to 100 DEG C by programming rate, stirring reaction 30min, prepare slip, isolated urea phosphate, phosphoric acid and carbamide Reaction be phosphoric acid solution and urea solid reaction;
B, prepare ammonium dihydrogen phosphate: be slowly added to ammonia in the slip containing urea phosphate controlling pH value is 3.6 and fully Stirring obtain containing nitrogen, the slip of phosphorus, the cooled crystallizer of slip is cooled to 25 DEG C, filter, isolated ammonium dihydrogen phosphate;
C, filtrate element add: add the trace compound needed for potassium element and blue berry in the filtrate of isolated Obtaining the mother solution of blue berry composite fertilizer special, trace compound is the chelate of calcium, magnesium, in the mother solution of blue berry composite fertilizer special The content of nitrogen element is 15.5%, phosphorus pentoxide is 7.5%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.4%;
D, it is dried: being placed in drying machine by mother solution, temperature controls at 32 DEG C, is dried after 30min, and controlling water content is 4% Obtaining blueberry special fertilizer, the nitrogen element content of blue berry composite fertilizer special is 15.2%, calcium element content is 4%, the containing of magnesium elements Amount is 4.1%, the content of phosphorus pentoxide is 7.2%, the content of potassium element is 8.2%.
Embodiment six
Prepared by a, raw material: first by phosphoric acid and carbamide, ratio for 1.8:1.4 mixes in molar ratio, and phosphoric acid concentration is 72%, It is that 4 DEG C/min rises to 104 DEG C by programming rate, stirring reaction 30min, prepare slip, isolated urea phosphate, phosphoric acid and carbamide Reaction be phosphoric acid solution and urea solid reaction;
B, prepare ammonium dihydrogen phosphate: be slowly added to ammonia in the slip containing urea phosphate controlling pH value is 3.6 and fully Stirring obtain containing nitrogen, the slip of phosphorus, the cooled crystallizer of slip is cooled to 25 DEG C, filter, isolated ammonium dihydrogen phosphate;
C, filtrate element add: add the trace compound needed for potassium element and blue berry in the filtrate of isolated Obtaining the mother solution of blue berry composite fertilizer special, trace compound is the chelate of calcium, magnesium, in the mother solution of blue berry composite fertilizer special The content of nitrogen element is 15.5%, phosphorus pentoxide is 7.5%, potassium element is 8.5%, calcium constituent is 4.2%, magnesium elements is 4.4%;
D, it is dried: being placed in drying machine by mother solution, temperature controls at 32 DEG C, is dried after 30min, and controlling water content is 4% Obtaining blueberry special fertilizer, the nitrogen element content of blue berry composite fertilizer special is 15.2%, calcium element content is 4%, the containing of magnesium elements Amount is 4.1%, the content of phosphorus pentoxide is 7.2%, the content of potassium element is 8.2%.
Below in conjunction with specific experiment example, product and the technique effect of the present invention are further described.
Experimental example one
The embodiment of the present invention one, embodiment two, embodiment three, embodiment four, embodiment five, embodiment six, in prepare Ammonium dihydrogen phosphate product detect by the standard of GB25569 2010, testing result is as shown in table 1:
Table 1 ammonium dihydrogen phosphate of the present invention product purity detects
Ammonium dihydrogen phosphate Criterion of acceptability Embodiment one Embodiment two Embodiment three Embodiment four Embodiment five Embodiment six
Purity >=% 96 98.5 98.3 98.3 98.2 98.3 98.2
Moisture≤% 0.5 0.42 0.4 0.41 0.41 0.42 0.42
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 the highest, illustrates that this method is prepared ammonium dihydrogen phosphate product and had the most progressive.
Experimental example two
According to the blue berry absorption to constituent content and the growing state of blue berry, to blue berry composite fertilizer special and Common compound fertilizer Compare test.With 9 blue berry Seedlings as subjects, be numbered respectively A, B, C, D, E, F, G, H, I, to tri-labels of A, B, C Blue berry Seedling use common fertilizer, the blue berry Seedling of six labels such as D, E, F, G, H, I is used embodiment one, embodiment respectively Two, blueberry special fertilizer prepared in embodiment three, embodiment four, embodiment five, embodiment six, contrast and experiment such as table Shown in 2:
Table 2 use Common compound fertilizer and blue berry composite fertilizer special to blue berry element absorption rate to when to blue berry growth Impact
The blue berry composite fertilizer special that as can be seen from the above table prepared by the present invention sufficiently can be absorbed by blue berry, and also rich Containing the nutrient needed for the blue berries such as Ca, Me, the normal growth of blue berry is provided guarantee, improve the growing way of blue berry, increase The yield of blue berry, thus improve economic benefit.

Claims (6)

1. the method preparing ammonium dihydrogen phosphate by-product blue berry composite fertilizer special, it is characterised in that the method includes following step Rapid:
Prepared by a, raw material: first by phosphoric acid and carbamide, ratio for 1.8:1.1-1.4 mixes in molar ratio, and phosphoric acid concentration is 68- 72%, it is that 4 DEG C/min rises to 84-104 DEG C by programming rate, stirring reaction 30min, prepare slip, isolated urea phosphate;
B, prepare ammonium dihydrogen phosphate: be slowly added to ammonia in the slip containing urea phosphate controlling pH value is 3.3-3.6 fully Stirring obtain containing nitrogen, the slip of phosphorus, the cooled crystallizer of slip is cooled to 25 DEG C, filter, isolated ammonium dihydrogen phosphate;
C, filtrate element add: the trace compound needed for adding potassium element and blue berry in the filtrate of isolated obtains The mother solution of blue berry composite fertilizer special;
D, being dried: being placed in drying machine by mother solution, temperature controls at 32 DEG C, is dried after 30min, controlling water content is 4% to obtain Blueberry special fertilizer.
The method preparing ammonium dihydrogen phosphate by-product blue berry composite fertilizer special the most according to claim 1, it is characterised in that: institute Stating the reaction that in step a, the reaction of phosphoric acid and carbamide is phosphoric acid solution with urea solid, phosphoric acid and carbamide are 1.8 in molar ratio: The ratio mixing of 1.3, the concentration of phosphoric acid is 71%.
The method preparing ammonium dihydrogen phosphate by-product blue berry composite fertilizer special the most according to claim 1, it is characterised in that: institute Stating trace compound in step c is the chelate of calcium, magnesium, and in the mother solution of blue berry composite fertilizer special, the content of nitrogen element is 15.5%, phosphorus pentoxide be 7.5%, potassium element be 8.5%, calcium constituent be 4.2%, magnesium elements be 4.4%.
The method preparing ammonium dihydrogen phosphate by-product blue berry composite fertilizer special the most according to claim 1, it is characterised in that: institute State the nitrogen element content of blue berry composite fertilizer special in step d be 15.2%, calcium element content be 4%, the content of magnesium elements be 4.1%, the content of phosphorus pentoxide be 7.2%, the content of potassium element be 8.2%.
The method preparing ammonium dihydrogen phosphate by-product blue berry composite fertilizer special the most according to claim 1, it is characterised in that: institute Stating blue berry composite fertilizer special in step d is compound state Chemical Mixed Fertilizer.
The method preparing ammonium dihydrogen phosphate by-product blue berry composite fertilizer special the most according to claim 1, it is characterised in that: institute State and step d contain in its composition of blue berry composite fertilizer special following N P and K compound state structural formula:
Wherein, the dotted line between carbon atom and oxygen atom represents and deposits between C atom and O atom In coordinate bond.
CN201410481995.8A 2014-09-19 A kind of method preparing ammonium dihydrogen phosphate by-product blue berry composite fertilizer special Expired - Fee Related CN104291292B (en)

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CN104291292B true CN104291292B (en) 2017-01-04

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