CN104291287B - A kind of production method preparing ammonium dihydrogen phosphate by-product wax gourd special fertilizer - Google Patents
A kind of production method preparing ammonium dihydrogen phosphate by-product wax gourd special fertilizer Download PDFInfo
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Abstract
The present invention relates to chemical technology field, a kind of production method preparing ammonium dihydrogen phosphate by-product wax gourd special fertilizer, it is changed by the coefficients such as the temperature of ammonium dihydrogen phosphate being prepared by phosphoric acid by wet process, improve the purity of ammonium dihydrogen phosphate product, can produce containing N simultaneously, P, the Chemical Mixed Fertilizer of K compound state, it is possible not only to improve the purity of ammonium dihydrogen phosphate, the absorptivity of this wax gourd special fertilizer produced is good, in filtrate, add formaldehyde simultaneously make a kind of controlled-releasing compounding fertilizer, this wax gourd special fertilizer produced disclosure satisfy that the nutritional need in each period in growth cycle, substantially increase wax gourd yield, it it is efficient Chemical Mixed Fertilizer.
Description
Technical field
The present invention relates to chemical technology field, particularly relate to a kind of production preparing ammonium dihydrogen phosphate by-product wax gourd special fertilizer
Method.
Background technology
Wax gourd is the fruit of Curcurbitaceae herbaceous plant wax gourd.Its shape such as pillow, originates in China, is on common people's dining table in summer
Common food.Wax gourd is planted edible very early by people.The record of wax gourd just it is related to, referred to as in Shennong's Herbal
" water sesame ".All there is cultivation China various places, pluck at the beginning of late summer, autumn during fruit maturation.Slightly sweet flavor, cold nature.This product contains albumen, sugar
Class, carrotene, multivitamin, crude fibre and calcium, phosphorus, iron, and potassium salts content is high, sodium salt content is low.Clearing heat and detoxicating, Li Shui
Dissolving phlegm, relieving restlessness are quenched the thirst, clearing damp relieving summer-heat.Cough for ambition dysphoria with smothery sensation, difficult urination, lung carbuncle breathe heavily, cirrhotic ascites, hypertension etc..
Being the composite fertilizer of N, P, K generally for the fertilization mode of wax gourd, wax gourd as a kind of in patent of invention is special strengthens fertilizer
Formula and preparation method (CN201110438756.0), it is mainly with phosphoamide, ammonium sulfate, calcium superphosphate, potassium nitrate, heavily mistake
Calcium phosphate and additive mix；It is that inserts produces wax gourd Chemical Mixed Fertilizer that patent of invention one ardealite processes medical stone
Formula (CN201110424502.3), it is to be mixed by inserts, phosphoamide, a sour ammonium, potassium chloride.This mixing is fertile
Shortcoming be N, P, K element absorbability bad, it was reported that phosphoamide, the plant absorption utilization rate of carbon ammonium be: 20% 1
46%, the plant absorption utilization rate of phosphate fertilizer (two ammoniums, an ammonium, coarse whiting) is: 10% one 25%, and the plant absorption of common potash fertilizer utilizes
Rate is: 35% one 60%, and Long-Time Service can make soil aggregate be destroyed, and easily causes soil compaction, soil property hardening, thus
Affect the decline of the growth of crops, quality, cause vicious circle.Though fertilizer is rich in organic simultaneously
Matter, but nutrients release is slow, causes crops to absorb slowly, fertilizer efficiency is low, does not reaches effectively between various available nutrients
Balance, due to the fertilizer formula not science of crops, the yield causing crops is the highest, and quality also can not get improving.
Ammonium dihydrogen phosphate, is widely used in the work of the almost all types such as all types of industrial crops, grain, melon fruits and vegetables
Thing, has many excellent effects such as notable increasing both production and income, the amount of changing optimization quality.Current domestic a lot of fertilizer producers are all producing phosphorus
Acid dihydride ammonium compound fertilizer, it mainly includes that thermal phosphoric acid and phosphoric acid by wet process produce ammonium dihydrogen phosphate, and thermal phosphoric acid cost is relatively big,
Should not be as being widely popularized, therefore, Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate product becomes main method, wet process phosphoric acid for preparing phosphorus
The basic step of acid dihydride ammonium is as follows:
Reaction equation one:
CO(NH2)2+H3PO4=CO (NH2)2.H3PO4
Reaction equation two
CO(NH2)2.H3PO4+NH3=NH4.H2PO4+CO(NH2)2
After whole reaction terminates, for there is any change, simultaneously because phosphoamide solubility is the highest, at 20 DEG C in phosphoamide
Time, its solubility is that 85g/100ml (refers to " phosphate fertilizer and composite fertilizer " volume 20 the 6th phase solubility of chemical fertilizer and compound
Fertile production technology), the rising of the solubility with temperature of phosphoamide simultaneously and increase, so the phosphoamide contained in filtrate is passing through
After cooling crystal separates out, possibly together with a large amount of undecomposed phosphoamides, NH in filtrate4 +、H2PO4 ~、HPO4 2～、PO4 3～If, directly
Doing waste water to discharge, both wasted resource, and can cause again the waste of resource, the dipotassium hydrogen phosphate product purity being simultaneously manufactured is the highest.
During Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate, the purity of ammonium dihydrogen phosphate is the highest, possibly together with greatly in filtrate
Measure undecomposed phosphoamide, NH4 +、H2PO4 ~、HPO4 2～、PO4 3～Deng material, the researcher of the present invention is from substantial amounts of prior art literary composition
Offer and exploration for many years and research, and the tradition component content of wax gourd special fertilizer and the absorbing state of wax gourd are ground
Study carefully, effectively inquire into out from the filtrate of Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate, produce wax gourd special fertilizer, solve phosphoric acid by wet process raw
Produce the problems such as active ingredient cannot utilize in the filtrate of ammonium dihydrogen phosphate, at home in fertilizer production, have no report.
During Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate, the purity of ammonium dihydrogen phosphate is the highest, possibly together with greatly in filtrate
Measure undecomposed phosphoamide, H2PO4 ~、HPO4 2～、PO4 3～Deng material, the researcher of the present invention from substantial amounts of prior art literature with
And exploration for many years and research, and the tradition component content of wax gourd special fertilizer and the absorbing state of wax gourd are studied, have
Inquire into out to effect from the filtrate of Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate, produce wax gourd special fertilizer, solve Wet-process Phosphoric Acid Production phosphoric acid
In the filtrate of ammonium dihydrogen, active ingredient such as cannot utilize at the problem, at home in fertilizer production, has no report.
Summary of the invention
For solving above-mentioned technical problem, the invention provides a kind of production preparing ammonium dihydrogen phosphate by-product wax gourd special fertilizer
Method, by unique process production design, improves the purity of ammonium dihydrogen phosphate, makes full use of wet process phosphoric acid for preparing di(2-ethylhexyl)phosphate simultaneously
Phosphoamide, H in the filtrate of hydrogen ammonium2PO4 ~、HPO4 2～、PO4 3～Deng material, produce out the wax gourd special fertilizer of applicable wax gourd growth.
The present invention is achieved by the following technical programs.
A kind of production method preparing ammonium dihydrogen phosphate by-product wax gourd special fertilizer that the present invention provides, it is characterised in that comprise
Following steps:
(1) phosphoric acid using phosphoric acid by wet process to prepare is (1.1～1.6) with phosphoamide according to mol ratio: 1 mixes, and to rise
Temperature speed is that 5～8 DEG C/min is warming up to 160 DEG C from 90 DEG C, stirring reaction 4～5h, isolated intermediate；
(2) being then dissolved in phosphoric acid solution by intermediate, the pH of regulation solution, 3～3.5, is passed through ammonia in solution,
Ammonia and intermediate be (1.1～1.4) according to mol ratio: 1, and stirring reaction 2～3h, after reaction terminates, it is thus achieved that slip, and by
Slip is placed in cooler crystallizer and cools to 25～30 DEG C, carries out crystallizing filtration treatment, makes filtrate circulate in cooler crystallizer
Crystallization treatment, it is thus achieved that filter cake be ammonium dihydrogen phosphate product, detection filtrate in component content；
(3) at filtrate hydro-oxidation potassium, calcium hydroxide and phosphoric acid solution, when the pH of solution is 3.3～4.0, and nitrogen component contains
Amount be 30～35%, phosphorus composition content be 10～14%, potassium component content is 15～the component content of 20%, calcium is 6～10%
Time, in filtrate, add formalin, temperature is risen to 65～75 DEG C, stirring reaction 2～4h；
(4) the most again in solution add trace element, be cooled to 20～25 DEG C, separate out compound state Chemical Mixed Fertilizer crude product,
Wax gourd special fertilizer is made through granulation and drying.
The concentration of described potassium hydroxide solution is 30～35%.
Described step (2) and the concentration of the phosphoric acid solution of step (3) are 17～20%.
The concentration of described aqua calcis is 20～25%.
The concentration of described formalin is 30～35%, and the mol ratio of the phosphoamide contained in formaldehyde and solution is
(0.5～1.5): 4.
Described trace element is Fe2 +Chelate, H3BO3In one or more mixtures.
N, P, K, Ca component content of the Chemical Mixed Fertilizer crude product of described compound state be respectively 25～30%, 8～12%, 13～
17%, 6～9%.
The Chemical Mixed Fertilizer of described compound state contains following N P and K compound state structural formula:
Wherein, the dotted line between carbon atom and oxygen atom represents and there is coordinate bond between C atom and O atom, and contains Can
Controlled Release Fertilizer.
In the present invention, by phosphoamide and phosphoric acid at 90 DEG C, and in the environment of being warming up to 160 DEG C with the speed of 5 DEG C/min
Reaction, generates urea phosphate, and being stepped up along with temperature, and then makes the coordinate bond dialysis between urea phosphate form two kinds
Ion like material, be exactly i.e.WhenIon is in phosphoric acid environment
In, it will close with phosphoric acid, and then carry out ionic polymerization under the temperature environment when urea phosphate coordinate bond dialysis so thatIon generates with phosphoric acidIntermediate-ion, makes in solution containing big simultaneously
The dihydrogen phosphate of amount, when adding potassium ion compound, dihydrogen phosphate and potassium ion react generation ammonium dihydrogen phosphate, and phase
Continue and reach saturated；When potassium content excess, it will react with the ammonium radical ion in intermediate-ion, further make middle from
Son chelates intoIntermediate-ion, and with positive charge, and then when solution participates in other
When electronegative ion or compound, it will form compound salt with this ion, the nutrition in the abundantest product becomes
Point.
Meanwhile, meanwhile, phosphoamide is at pH in the case of the acidity of 3.3～4.0, and phosphoamide can react with formalin, raw
Become urea aldehyde series of products
The most longer chemical chain,Reaction can be continued with phosphoamide and formaldehyde raw in the case of acidity
BecomeSimultaneously?
Continue in the case of acidity to react with phosphoamide and formaldehyde, Deng urea aldehyde series of products after fertilising, through micro-life
Under the effect of thing, can discharge N, the C element being easily absorbed by plants, the chain length of its urea aldehyde is the longest, and chain needs the time of fracture
The longest, the time producing fertilizer efficiency can discharge after a certain time, can reach the effect of sustained release generally,The release fertilizer efficiency time be 0～40 day,
The release fertilizer efficiency time be 40～80 days.
The beneficial effects of the present invention is: compared with prior art, there is following characteristics in the present invention:
1. rich in carbon amide solution in the filtrate of conventional wet lay phosphoric acid ammonium dihydrogen phosphate, phosphoamide mutually synthermal
Under solubility relatively large, isolated phosphoamide crystal is rich in KH2PO4In other crystal, entered cooling simultaneously and separated out phosphinylidyne
Possibly together with substantial amounts of phosphoamide, H in filtrate after amine crystal2PO4 ~、HPO4 2～、PO4 3～Utilizing Deng not operatively, the present invention is by wet
The temperature of method phosphoric acid ammonium dihydrogen phosphate regulates to 90～160 DEG C, and heats up from 90 DEG C to 160 DEG C with the speed of 5～8 DEG C/min
In the environment of react, not only make the ammonium dihydrogen phosphate product purity of precipitation reach more than 98%, filtrate also generateCation, to filtrate crystallisation separate out generate compound state Chemical Mixed Fertilizer go out finished product time, protect
Demonstrate,prove compound state Chemical Mixed Fertilizer to go out in finished productIntermediate-ion and dihydrogen phosphate, and at C and O
Between formed coordinate bond, this intermediate-ion can with centering element compound chelating formed multielement intermediate-ion, Jin Erneng
Enough continuation forms chelate with other electronegative compounds or ion, improves constituent content in double salt, and then can adjust
Nutrient content in the double salt that this ion whole exists, meanwhile, this chelate can be hydrolyzed again and by crop, and then can have
The long-term of effect provides fertilizer efficiency for crop, meanwhile, in conjunction with the mensuration of constituent content in the solution that there is this ion, and then adjusts multiple
Each constituent content when salt is formed, dries and obtains compound state double salt composite fertilizer, and by avoiding the addition of chlorine element so that chemical combination
While the product quality of state double salt composite fertilizer disclosure satisfy that the requirement of wax gourd nutritional labeling, it is to avoid wax gourd is brought by fertilizer
Infringement, reduces wax gourd planting cost and improves wax gourd yield；
2. containing phosphoamide composition partly in filtrate, add formalin, acid condition, generate Deng
Urea aldehyde series composite fertilizer, can make this wax gourd special fertilizer reach the effect of realizing controlled-release；
3. by effective uptake of N P and K calcium constituent is carried out by the constituent content in wax gourd special fertilizer and wax gourd
Detection is analyzed, and is adjusted the constituent content in production process and arranges in pairs or groups so that answering of the compound state prepared
Hefei can meet the demand of crop to greatest extent, and reduces in composite heat transfer because of element mismatch, the one-tenth caused
This is too high, further avoids too much element to put among soil, causes the solidification of composite fertilizer to pollute environment.
Detailed description of the invention
Below in conjunction with specific embodiment, the concrete technical scheme of the present invention is described in detail.
Principle illustrates:
The present invention carries out research and discussion by the mechanism reacting phosphoric acid and phosphoamide, and combines prior art literature
Solution arrives, and phosphoric acid and phosphoamide react generation urea phosphate, and its molecular formula is: CO (NH2)2.H3PO4, in the environment of higher temperature,
Chemical bond meeting dialysis between H and O in phosphoric acid, hydrogen ion is combined with phosphoamide and forms the ionic state containing positive charge so that
Urea phosphate forms the ion double salt that a kind of positive and negative charge attracts mutually, its mechanism structural response following expression: CO (NH2)2.H3PO4
→(H2PO4)-.(H2NCONH3)+
Further, urea phosphate ion double salt phosphoric acid exist in the environment of, (H therein2NCONH3)+Cation and phosphorus
Acid is close, forms the intermediate-ion of C → O coordinate bond, is (CO5PN2H8)+, and then make in urea phosphate intermediate containing a large amount of
(H2PO4) -(CO5PN2H8)+Ion, when adding ammonia in solution, ammonia can react generation NH with acid4 +, by cooling
Crystallization, generates NH4 H2PO4, when adding excessive and appropriate potassium ion in filtrate, dihydrogen phosphate is formed with potassium ion
Ammonium dihydrogen phosphate crystal is precipitated, unnecessary potassium ion and (CO5PN2H8)+Ionic reaction, and displace part NH4 +So that molten
Containing (CO in liquid5PNH4K)+Double salt ion, and analyzed and control the content of N in solution, P, K element by detection, in heating
It is dried and can be prepared by containing N, P, the compound state composite fertilizer of K element.
Its concrete reaction principle will carry out further instruction by following reaction structure formula and reaction mechanism:
Reaction equation one:
CO(NH2)2+H3PO4→CO(NH2)2.H3PO4
Reaction equation two:
Reaction equation three:
Wherein, the dotted line between carbon atom and oxygen atom represents and there is coordinate bond between C atom and O atom.
When adding ammoniacal liquor, dihydrogen phosphate and potassium ion react generation ammonium dihydrogen phosphate, and in succession reach saturated；Work as analysis
Go out NH4.H2PO4After crystal, containing substantial amounts of in filtrateRoot, to adding hydroxide in filtrate
Potassium solution, when potassium content excess, it will react with the ammonium radical ion in intermediate-ion.
Reaction equation four:
Wherein, the dotted line between carbon atom and oxygen atom represents and there is coordinate bond between C atom and O atom.
In the present invention, phosphoamide and formaldehyde are under being 3.3～4.0 alkaline case in pH value, can produce following reaction:
Reaction equation five
Reaction equation six
Generate urea aldehyde series of products
The most longer chemical chain,Reaction can be continued with phosphoamide and formaldehyde in the case of acidity
GenerateSimultaneously
Continue to react with phosphoamide and formaldehyde in the case of acidity, Deng urea aldehyde series of products after fertilising, through micro-life
Under the effect of thing, can discharge N, the C element being easily absorbed by plants, the chain length of its urea aldehyde is the longest, and chain needs the time of fracture
The longest, the time producing fertilizer efficiency can discharge after a certain time, can reach the effect of sustained release generally,The release fertilizer efficiency time be 0～40 day,
The release fertilizer efficiency time be 40～80 days.
Noun illustrates:
Urea phosphate (Urea phosphate, UP), No. CAS is 4861～19～2, and molecular formula is CH7N2O5P, is represented by
CO(NH2)2·H3PO4:
Being a kind of fine chemical product being widely used in the fields such as animal husbandry, industry, agricultural, its solid is white crystals
Or crystalline powder, soluble in water and alcohol, insoluble in ethers, toluene and carbon tetrachloride, the aqueous solution is acidity, starts point time melted
Solve and release carbon dioxide and ammonia.
Embodiment one
The present embodiment provides a kind of production method preparing ammonium dihydrogen phosphate by-product wax gourd special fertilizer, it is characterised in that comprise
Following steps:
(1) phosphoric acid using phosphoric acid by wet process to prepare is that 1.6:1 mixes with phosphoamide according to mol ratio, and with programming rate is
8 DEG C/min is warming up to 160 DEG C from 90 DEG C, stirring reaction 4h, isolated intermediate；
(2) being then dissolved in phosphoric acid solution by intermediate, the concentration of phosphoric acid solution is 17%, regulation solution pH 3.5,
Being passed through ammonia in solution, ammonia and intermediate are 1.1:1 according to mol ratio, and stirring reaction 3h, after reaction terminates, it is thus achieved that material
Slurry, and slip is placed in cooler crystallizer cools to 25 DEG C, carry out crystallizing filtration treatment, make filtrate follow in cooler crystallizer
Ring crystallization treatment, it is thus achieved that filter cake be ammonium dihydrogen phosphate product, detection filtrate in component content；
(3) at filtrate hydro-oxidation potassium, calcium hydroxide and phosphoric acid solution, for regulating pH value and N, P, K, Ca of solution
Content, the concentration of described potassium hydroxide solution is 35%, the concentration of phosphoric acid solution 17%, the concentration of aqua calcis
It is 25%；When the pH of solution is 3.3, nitrogen component content is 30%, phosphorus composition content is 14%, potassium component content is 15%, calcium
Component content when being 10%, in filtrate, add formalin, the concentration of formalin is 30%, and formaldehyde with in solution
The mol ratio of the phosphoamide contained is 0.5:4, and temperature rises to 65 DEG C, stirring reaction 2h；
(4) in solution, Fe is added the most again2 +Chelate, H3BO3Deng trace element, it is cooled to 20 DEG C, separates out chemical combination
The Chemical Mixed Fertilizer crude product of state, when N, P, K, Ca component content in Chemical Mixed Fertilizer crude product compound state being detected is respectively N, P, K, Ca
Point content is respectively 25%, 12%, 13%, 9% time, stop crystallization；
(5) the Chemical Mixed Fertilizer crude product of above-mentioned compound state makes wax gourd special fertilizer through granulation and drying.
Through detection, the purity of the ammonium dihydrogen phosphate product made is more than 98%；The wax gourd special fertilizer made
In containing N P and K compound state structural formula:Wherein, the dotted line between carbon atom and oxygen atom
Represent and there is coordinate bond between C atom and O atom, and contain Realizing controlled-release fertile.
Embodiment two
The present embodiment provides a kind of production method preparing ammonium dihydrogen phosphate by-product wax gourd special fertilizer, it is characterised in that comprise
Following steps:
(1) phosphoric acid using phosphoric acid by wet process to prepare is that 1.1:1 mixes with phosphoamide according to mol ratio, and with programming rate is
5 DEG C/min is warming up to 160 DEG C from 90 DEG C, stirring reaction 5h, isolated intermediate；
(2) being then dissolved in phosphoric acid solution by intermediate, the concentration of phosphoric acid solution is 20%, regulation solution pH 3, to
Being passed through ammonia in solution, ammonia and intermediate are 1.4:1 according to mol ratio, and stirring reaction 2h, after reaction terminates, it is thus achieved that material
Slurry, and slip is placed in cooler crystallizer cools to 30 DEG C, carry out crystallizing filtration treatment, make filtrate follow in cooler crystallizer
Ring crystallization treatment, it is thus achieved that filter cake be ammonium dihydrogen phosphate product, detection filtrate in component content；
(3) at filtrate hydro-oxidation potassium, calcium hydroxide and phosphoric acid solution, for regulating the pH value of solution and N, P, K, Ca
Content, the concentration of described potassium hydroxide solution is 30%, and the concentration of phosphoric acid solution is 20%, and the concentration of aqua calcis is
20%；When the pH of solution is 4.0, nitrogen component content is 35%, phosphorus composition content is 10%, potassium component content is 20%, calcium
When component content is 6%, adding formalin in filtrate, the concentration of formalin is 35%, and formaldehyde contains in solution
The mol ratio of some phosphoamides is 1.5:4, and temperature rises to 75 DEG C, stirring reaction 4h；
(4) in solution, Fe is added the most again2 +Chelate, H3BO3Deng trace element, it is cooled to 20 DEG C, separates out chemical combination
The Chemical Mixed Fertilizer crude product of state, when N, P, K, Ca component content in Chemical Mixed Fertilizer crude product compound state being detected be respectively 30%, 8%,
17%, 6% time, stop crystallization；
(5) the Chemical Mixed Fertilizer crude product of above-mentioned compound state makes wax gourd special fertilizer through granulation and drying.
Through detection, the purity of the ammonium dihydrogen phosphate product made is more than 98%；The wax gourd special fertilizer made contains
N P and K compound state structural formula:Wherein, the dotted line between carbon atom and oxygen atom represents
There is coordinate bond between C atom and O atom, and contain Realizing controlled-release fertile.
Embodiment three
The present embodiment provides a kind of production method preparing ammonium dihydrogen phosphate by-product wax gourd special fertilizer, it is characterised in that comprise
Following steps:
(1) phosphoric acid using phosphoric acid by wet process to prepare is that 1.4:1 mixes with phosphoamide according to mol ratio, and with programming rate is
6 DEG C/min is warming up to 160 DEG C from 90 DEG C, stirring reaction 4.5h, isolated intermediate；
(2) being then dissolved in phosphoric acid solution by intermediate, the concentration of phosphoric acid solution is 18%, regulation solution pH 3.2,
Being passed through ammonia in solution, ammonia and intermediate are 1.3:1 according to mol ratio, and stirring reaction 2.5h, after reaction terminates, it is thus achieved that
Slip, and slip is placed in cooler crystallizer cools to 27 DEG C, carry out crystallizing filtration treatment, make filtrate in cooler crystallizer
Circulation crystallization process, it is thus achieved that filter cake be ammonium dihydrogen phosphate product, detection filtrate in component content；
(3) at filtrate hydro-oxidation potassium, calcium hydroxide and phosphoric acid solution, for regulating the pH value of solution and N, P, K, Ca
Content, the concentration of described potassium hydroxide solution is 32%, and the concentration of phosphoric acid solution is 19%, and the concentration of aqua calcis is
23%；When the pH of solution is 3.7, nitrogen component content is 33%, phosphorus composition content is 12%, potassium component content is 17%, calcium
When component content is 8%, adding formalin in filtrate, the concentration of formalin is 33%, and formaldehyde contains in solution
The mol ratio of some phosphoamides is 1:4, and temperature rises to 70 DEG C, stirring reaction 3h；
(4) in solution, Fe is added the most again2 +Chelate, H3BO3Deng trace element, it is cooled to 23 DEG C, separates out chemical combination
The Chemical Mixed Fertilizer crude product of state, when N, P, K, Ca component content in Chemical Mixed Fertilizer crude product compound state being detected be respectively 27%, 10%,
16%, 7% time, stop crystallization；
(5) the Chemical Mixed Fertilizer crude product of above-mentioned compound state makes wax gourd special fertilizer through granulation and drying.
Through detection, the purity of the ammonium dihydrogen phosphate product made is more than 98%；The wax gourd special fertilizer made
In containing N P and K compound state structural formula:Wherein, the dotted line between carbon atom and oxygen atom
Represent and there is coordinate bond between C atom and O atom, and contain Realizing controlled-release fertile.
In order to well prove the beneficial effect of patent of the present invention, the present invention also provides for following experimental example:
Experimental group 1～3
As fertilizer using the wax gourd special fertilizer that above-described embodiment makes directly the wax gourd of result is applied fertilizer and makes training respectively
Wax gourd seedling is cultivated by nutrient solution.The yield of statistics wax gourd, after Solution culture method 30, detects N, P, K, Ca composition therein and contains
Amount, and the growing way situation of wax gourd seedling.
Control group 1～3
Fertile as fertilizer using common N, P, K, Ca mixing, wherein N, P, K, Ca component content in this mixing fertilizer respectively at
Embodiment one is identical to N, P, K, Ca component content in embodiment three, the most directly applies fertilizer the wax gourd of result, and makes training
Wax gourd seedling is cultivated by nutrient solution.The yield of statistics wax gourd, after Solution culture method 30, detects N, P, K, Ca composition therein and contains
Amount, and the growing way situation of wax gourd seedling.
By being the contrast of experimental group and control group, the yield high 3000～4000kg/ of the yield increased group of experimental group
Mu, in cultivating seedling, the seedling height of experimental group is than control group high 30～50cm, simultaneously in the nutrient solution in experimental group
N, P, K, Ca residual condition is the 72% of control group, 51%, 42%, 39% respectively.
Claims (8)
1. the production method preparing ammonium dihydrogen phosphate by-product wax gourd special fertilizer, it is characterised in that comprise the steps of
(1) phosphoric acid using phosphoric acid by wet process to prepare is (1.1～1.6) with phosphoamide according to mol ratio: 1 mixes, and with the speed that heats up
Degree is that 5～8 DEG C/min is warming up to 160 DEG C from 90 DEG C, stirring reaction 4～5h, isolated intermediate；
(2) being then dissolved in phosphoric acid solution by intermediate, the pH of regulation solution, 3～3.5, is passed through ammonia, ammonia in solution
Being (1.1～1.4) with intermediate according to mol ratio: 1, stirring reaction 2～3h, after reaction terminates, it is thus achieved that slip, and by slip
It is placed in cooler crystallizer and cools to 25～30 DEG C, carry out crystallizing filtration treatment, make filtrate circulation crystallization in cooler crystallizer
Process, it is thus achieved that filter cake be ammonium dihydrogen phosphate product, detection filtrate in component content；
(3) at filtrate hydro-oxidation potassium, calcium hydroxide and phosphoric acid solution, when the pH of solution is 3.3～4.0, and nitrogen component content is
30～35%, phosphorus composition content be 10～14%, potassium component content be 15～time the component content of 20%, calcium is 6～10%, to
Filtrate adds formalin, temperature is risen to 65～75 DEG C, stirring reaction 2～4h；
(4) in solution, add trace element the most again, be cooled to 20～25 DEG C, separate out the Chemical Mixed Fertilizer crude product of compound state, process
Wax gourd special fertilizer is made in granulation and drying.
Prepare the production method of ammonium dihydrogen phosphate by-product wax gourd special fertilizer the most as claimed in claim 1, it is characterised in that: described
The concentration of potassium hydroxide solution be 30～35%.
Prepare the production method of ammonium dihydrogen phosphate by-product wax gourd special fertilizer the most as claimed in claim 1, it is characterised in that: described
Step (2) and the concentration of phosphoric acid solution of step (3) 17～20%.
Prepare the production method of ammonium dihydrogen phosphate by-product wax gourd special fertilizer the most as claimed in claim 1, it is characterised in that: hydrogen-oxygen
The concentration changing calcium solution is 20～25%.
Prepare the production method of ammonium dihydrogen phosphate by-product wax gourd special fertilizer the most as claimed in claim 1, it is characterised in that: described
The concentration of formalin be 30～35%, and the mol ratio of the phosphoamide contained in formaldehyde and solution is (0.5～1.5):
4。
Prepare the production method of ammonium dihydrogen phosphate by-product wax gourd special fertilizer the most as claimed in claim 1, it is characterised in that: described
Trace element be Fe2 +Chelate, H3BO3In one or more mixtures.
Prepare the production method of ammonium dihydrogen phosphate by-product wax gourd special fertilizer the most as claimed in claim 1, it is characterised in that: described
N, P, K, Ca component content of the Chemical Mixed Fertilizer crude product of compound state is respectively 25～30%, 8～12%, 13～17%, 6～9%.
Prepare the production method of ammonium dihydrogen phosphate by-product wax gourd special fertilizer the most as claimed in claim 7, it is characterised in that: described
The Chemical Mixed Fertilizer of compound state contain following N P and K compound state structural formula:Wherein, carbon atom
And the dotted line between oxygen atom represents and there is coordinate bond between C atom and O atom, and contain Can
Controlled Release Fertilizer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410478068.0A CN104291287B (en) | 2014-09-19 | 2014-09-19 | A kind of production method preparing ammonium dihydrogen phosphate by-product wax gourd special fertilizer |
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| CN201410478068.0A CN104291287B (en) | 2014-09-19 | 2014-09-19 | A kind of production method preparing ammonium dihydrogen phosphate by-product wax gourd special fertilizer |
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| CN104291287A CN104291287A (en) | 2015-01-21 |
| CN104291287B true CN104291287B (en) | 2016-09-07 |
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