CN104310333B - A kind of production method preparing ammonium dihydrogen phosphate by-product corn fertilizer - Google Patents
A kind of production method preparing ammonium dihydrogen phosphate by-product corn fertilizer Download PDFInfo
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- CN104310333B CN104310333B CN201410477909.6A CN201410477909A CN104310333B CN 104310333 B CN104310333 B CN 104310333B CN 201410477909 A CN201410477909 A CN 201410477909A CN 104310333 B CN104310333 B CN 104310333B
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- TUNRTDCVNJKJTI-YFKPBYRVSA-N CC(C)(C1)[C@H]1[NH+](NC)[O-] Chemical compound CC(C)(C1)[C@H]1[NH+](NC)[O-] TUNRTDCVNJKJTI-YFKPBYRVSA-N 0.000 description 1
- MNIGTWMJIVEYII-NICGVCSZSA-N CC(C)COCC(C(CC1)C2C1[C@@H](C)C2)OC1CC1 Chemical compound CC(C)COCC(C(CC1)C2C1[C@@H](C)C2)OC1CC1 MNIGTWMJIVEYII-NICGVCSZSA-N 0.000 description 1
Abstract
The present invention relates to chemical technology field, a kind of production method preparing ammonium dihydrogen phosphate by-product corn 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 corn fertilizer produced is good, in filtrate, add formaldehyde simultaneously make a kind of controlled-releasing compounding fertilizer, this corn fertilizer produced disclosure satisfy that the nutritional need in each period in growth cycle, substantially increase corn 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 corn fertilizer
Method.
Background technology
Corn is Chinese first generalized grain crop and important feed resource, is also that the grain that whole world total output is the highest is made
Thing, corn contains substantial amounts of isomalto-oligosaccharide, and it is the most excellent in prebiotics, and prebiotics is the grain of probio, right
The probio breeding of human body has close relationship, thus gut flora is reached poised state so that intestinal health.Corn
Metabolizable energy is 14.06MJ/kg, and high person, up to 15.06MJ/kg, is the highest in cereals feed, possibly together with in a large number in corn
Magnesium, magnesium can be strengthened intestinal wall wriggling, promote the excretion of body waste.
The improvement of corn quality at present increasingly receives publicity with the raising of yield, and the use of agrochemical is beautiful in China
Rice occupies very important status in producing, and owing to there are some irrational factors during using, does not only result in fertilizer
Plant recovery of nutrient reduces, and makes the ecological environment including soil environment suffer serious destruction.Big according to China
The result of the test of amount confirms, N, P, K ratio of the current chemical fertilizer of China and soil nutrient supply situation and the crop absorption to nutrient
Situation is not in tune.Present Fertilizer Market mainly based on scattered fertilizer variety the most molten, instant, fast, exacerbates the wave of fertilizer
Take and the loss of nutrient, must could meet the crop whole puberty demand to nutrient by repeatedly topdressing on producing, this
Not only take a lot of work, increase fertilising cost, and topdress, top application fertilizer nutrient loss amount big, hence it is evident that reduce fertilizer efficiency, it is difficult to play fertilizer
Yield increasing effect, how to prepare one and not only can improve soil property, increase soil fertility, nutriment enriches, nutrient
Release is coordinated persistently, and fertilizer nutrient utilization ratio is high, and single fertilization becomes without the corn special-purpose fertilizer topdressed or topdress less
It is presently required and solves the technical problem that.
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 notable increasing both production and income, the amount of changing optimizes many excellent effects such as quality, resistant to lodging, disease and insect resistance, preventing and treating early ageing, and
There is the malnourished effect overcoming the plant growth later stage aging absorbability of root system to decline and to cause, belong to novel high density phosphorus
Potassium Was Used compound fertilizer, is efficient compound fertilizer agriculturally.Current domestic a lot of fertilizer producers are all producing ammonium dihydrogen phosphate
Composite 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, unsuitable conduct
Being widely popularized, therefore, Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate product becomes main method, wet process phosphoric acid for preparing ammonium dihydrogen phosphate
Basic step 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 done
Waste water is discharged, and had both wasted resource, and can cause again the waste of resource, and 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 component content of traditional corn special fertilizer and the absorbing state of corn are ground
Study carefully, effectively inquire into out from the filtrate of Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate, produce corn 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.
Summary of the invention
For solving above-mentioned technical problem, the invention provides a kind of production preparing ammonium dihydrogen phosphate by-product corn fertilizer
Method, by unique process production design, improve the purity of ammonium dihydrogen phosphate, make full use of wet process phosphoric acid for preparing phosphoric acid simultaneously
Phosphoamide, NH in the filtrate of ammonium dihydrogen4 +、H2PO4 -、HPO4 2-、PO4 3-Deng material, the corn producing out applicable corn growth is special
Fertile.
The present invention is achieved by the following technical programs.
A kind of production method preparing ammonium dihydrogen phosphate by-product corn fertilizer, comprises the following steps
(1) phosphoric acid of wet-method is used to be (1.3-1.6) with phosphoamide according to mol ratio: 1 mixes, and with programming rate
It is that 5 DEG C/min is warming up to 160 DEG C from 95 DEG C, stirring reaction 4-5h, isolated intermediate；
(2) using this intermediate again is 1:(1.1-1.3 with ammonia according to mol ratio) mix, during mixing, first by the middle of this
Body is soluble in water, is passed through ammonia the most again in solution, and the reaction time is 2h, after reaction terminates, it is thus achieved that nitrogenous, the material of phosphorus, potassium
Slurry, and the slip of nitrogenous, phosphorus, potassium is placed in cooler crystallizer cools to 30 DEG C, carry out crystallizing filtration treatment, make filtrate cold
But in 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 solution and phosphoric acid solution, adjust nitrogen, phosphorus, potassium content and pH value in filtrate, work as filtrate
In pH value be 3.5-4.0, nitrogen component content is 20-25%, phosphorus composition content is 4-10%, potassium component content is 10-15%
Time, stop adding potassium hydroxide solution and phosphoric acid solution；
(4) solution of step (3) adds formalin, during big 6-8 the atmospheric pressure of solution Quick-pressing, with 20-30Pa/
The speed of min increases pressure, keeps constant when reaching 10-12 atmospheric pressure, when being rapidly heated to 80-100 DEG C, with 2-5 DEG C/
The ramp of min, keeps constant when reaching 120 DEG C, keeps 1-2h when pressure and temperature all arrive peak, obtains
Suspension emulsion A,
(5) the most again in suspension emulsion A add trace element, obtain suspension emulsion B, described trace element be iron,
One or more in boron, arsenic, manganese, copper, cobalt, molybdenum, then corn fertilizer is made in recrystallization, granulation and drying.
Described potassium hydroxide solution concentration is 20-25%.
The concentration of described phosphoric acid solution is at 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.
Further, suspension emulsion B carrying out crystallisation step and is down to 30-35 DEG C for cooling pressurized treatment, temperature, pressure increases
To 6-8 atmospheric pressure, obtain crystal, dry finally by granulation and obtain corn fertilizer.
Described corn fertilizer is the Chemical Mixed Fertilizer of compound state, wherein the content of nitrogen component be 18-21%, phosphorus composition content
It is 8-13% for 4-7%, potassium component content.
The Chemical Mixed Fertilizer of described compound state contains in its composition containing following N P and K compound state structural formula:Wherein, the dotted line between carbon atom and oxygen atom represents existence coordination between C atom and O atom
Key, and containWithCan
Controlled Release Fertilizer.
In the present invention, by phosphoamide and phosphoric acid at 95 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.WithWhenIon 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 to contain in solution simultaneously
Substantial amounts of dihydrogen phosphate, when adding ammoniacal liquor, dihydrogen phosphate and ammoniacal liquor react generation ammonium dihydrogen phosphate, and are tied by cooling
Partial crystallization goes out；Then in filtrate, potassium hydroxide solution is added, when potassium content excess, it will with the ammonium root in intermediate-ion
Ionic reaction, further makes intermediate-ion chelate intoIntermediate-ion, and with
Positive charge, and then when solution participates in other electronegative ions or compound, it will form compound salt with this ion,
Nutritional labeling in the abundantest product.
Meanwhile, meanwhile, phosphoamide is at pH in the case of the acidity of 3.5-4.0, and phosphoamide can react with formalin, generates
Urea aldehyde series of productsOr
The most longer chemical chain,Reaction can be continued with phosphoamide and formaldehyde raw in the case of acidity
BecomeSimultaneously
Continue to react with phosphoamide and formaldehyde in the case of acidity,OrDeng urea aldehyde series of products after fertilising, through microorganism
Under effect, 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 ruptured 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 days,
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:
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 NH4·H2PO4In other crystal, entered cooling simultaneously and separated out
Possibly together with substantial amounts of phosphoamide, H in filtrate after phosphoamide crystal2PO4 -、HPO4 2-、PO4 3-Utilize Deng not operatively, the present invention
The temperature of wet process phosphoric acid for preparing ammonium dihydrogen phosphate is regulated to 80-160 DEG C, and heats up from 95 DEG C to 160 DEG C with the speed of 5 DEG C/min
In the environment of react, not only make the ammonium dihydrogen phosphate product purity of precipitation reach more than 98%, in filtrate add Strong oxdiative potassium
After solution, filtrate also generatesCation, to filtrate crystallisation separate out generate change
When conjunction state Chemical Mixed Fertilizer goes out finished product, it is ensured that compound state Chemical Mixed Fertilizer goes out in finished productMiddle from
Son and dihydrogen phosphate, and between C and O, form coordinate bond, this intermediate-ion can chelate shape with centering element compound
Become multielement intermediate-ion, and then can continue to the compound electronegative with other or ion formation chelate, improve multiple
Constituent content in salt, and then the nutrient content in the double salt that this ion exists can be adjusted, meanwhile, this chelate can be carried out again
Hydrolysis and by crop, and then effectively for a long time can provide fertilizer efficiency for crop, meanwhile, combine in the solution that this ion is existed first
The mensuration of cellulose content, and then adjust each constituent content when double salt is formed, dry and obtain compound state double salt composite fertilizer, its absorptivity
Fabulous, reduce corn planting cost and improve corn quality；
2. phosphoamide composition containing part in filtrate, adds formalin, in acid condition and certain pressure intensity and temperature
Under degree, generateOr
Deng urea aldehyde series composite fertilizer, this corn fertilizer can be made to reach the effect of realizing controlled-release；
3. by effective uptake of n-p-k element is examined by the constituent content in corn fertilizer and corn
Cls analysis, and the constituent content in production process is adjusted and arranges in pairs or groups so that being combined of the compound state prepared
The fertile demand that can meet crop to greatest extent, and reduce in composite heat transfer because of element mismatch, the cost caused
Too high, further avoid too much element to put among soil, cause 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 +, tied by cooling
Crystalline substance, generates NH4 H2PO4,, when filtrate adds excessive and appropriate potassium ion, unnecessary potassium ion and (CO5PN2H8)+From
Son reaction, and displace part NH4 +So that containing (CO in solution5PNH4K)+Double salt ion, and analyzed by detection and control
The content of N, P, K element in solution processed, can be prepared by containing N, P, the compound state composite fertilizer of K element at heat drying.
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 ammoniacal liquor react generation ammonium dihydrogen phosphate, and in succession reach saturated；Work as precipitation
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 in the case of being 3.5-4.0 acidity in pH value, and temperature is 55-75 DEG C can produce one
Lower reaction:
Reaction equation five
Reaction equation six
Generate urea aldehyde series of productsOr
The most longer chemical chain,Reaction can be continued with phosphoamide and formaldehyde in the case of acidity
Generate OrDeng urea aldehyde series of products after fertilising, through the work of microorganism
Under with, 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 ruptured the longest, produces
The time of raw fertilizer efficiency can discharge after a certain time, can reach the effect of sustained release generally,The release fertilizer efficiency time be 0-40 days,
The release fertilizer efficiency time be 40-80 days.
Noun illustrates:
Urea phosphate (Ureaphosphate, 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
A kind of production method preparing ammonium dihydrogen phosphate by-product corn fertilizer that the present invention provides, comprises the following steps
1) phosphoric acid using wet-method is that 1.3:1 mixes with phosphoamide according to mol ratio, and with programming rate be 5 DEG C/
Min is warming up to 160 DEG C from 95 DEG C, stirring reaction 5h, isolated intermediate；
2) using this intermediate again is that 1:1.1 mixes with ammonia according to mol ratio, during mixing, first this intermediate is dissolved in water
In, in solution, it being passed through ammonia the most again, the reaction time is 2h, after reaction terminates, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and will contain
Nitrogen, phosphorus, the slip of potassium are placed in cooler crystallizer and cool to 30 DEG C, carry out crystallizing filtration treatment, make filtrate at cooler crystallizer
Middle circulation crystallization process, it is thus achieved that filter cake be ammonium dihydrogen phosphate product, detection filtrate in component content；
3) add, filtrate, the potassium hydroxide solution and the phosphoric acid solution of 20% that concentration is 25%, adjust nitrogen in filtrate, phosphorus,
Potassium content and pH value, when in filtrate, pH value is 4.0, the content of nitrogen component is 25%, phosphorus composition content is 4%, potassium component content
When being 15%, stop adding potassium hydroxide solution and phosphoric acid solution；
4) adding formalin in the solution of step (3), the concentration of described formalin is 35%, and formaldehyde is with molten
The mol ratio of the phosphoamide contained in liquid is 1.5:4, during big 6 atmospheric pressure of solution Quick-pressing, increases with the speed of 30Pa/min
Add pressure, keep constant when reaching 10 atmospheric pressure, when being rapidly heated to 80 DEG C, with the ramp of 5 DEG C/min, when reaching
Keep constant when 120 DEG C, keep 2h when pressure and temperature all arrive peak, obtain suspension emulsion A,
5) the most again in suspension emulsion A add trace element, obtain suspension emulsion B, described trace element be iron,
One or more in boron, arsenic, manganese, copper, cobalt, molybdenum, then corn fertilizer is made in recrystallization, granulation and drying.
Entering detection, the purity of ammonium dihydrogen phosphate is more than 98%, and the corn fertilizer obtained containsThe potassium phosphate composite fertilizer of root and、Chemical Mixed Fertilizer, wherein the content of nitrogen component be 21%, phosphorus
Component content is 4%, potassium component content is 13%.
Embodiment two
A kind of production method preparing ammonium dihydrogen phosphate by-product corn fertilizer that the present invention provides, comprises the following steps
(1) phosphoric acid using wet-method is that 1.6:1 mixes with phosphoamide according to mol ratio, and with programming rate be 5 DEG C/
Min is warming up to 160 DEG C from 95 DEG C, stirring reaction 4h, isolated intermediate；
(2) using this intermediate again is that 1:1.3 mixes with ammonia according to mol ratio, during mixing, is first dissolved in by this intermediate
In water, being passed through ammonia the most again in solution, the reaction time is 1h, after reaction terminates, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and will
Slip nitrogenous, phosphorus, potassium is placed in cooler crystallizer and cools to 35 DEG C, carries out crystallizing filtration treatment, makes filtrate at crystallisation by cooling
In device circulation crystallization process, it is thus achieved that filter cake be ammonium dihydrogen phosphate product, detection filtrate in component content；
(3) add, filtrate, the potassium hydroxide solution and the phosphoric acid solution of 25% that concentration is 20%, adjust nitrogen in filtrate, phosphorus,
Potassium content and pH value, when in filtrate, pH value is 3.5, the content of nitrogen component is 20%, phosphorus composition content is 10%, potassium component content
When being 10%, stop adding potassium hydroxide solution, aqua calcis and phosphoric acid solution；
(4) in the solution of step (3) add formalin, the concentration of described formalin is 35%, and formaldehyde with
The mol ratio of the phosphoamide contained in solution is 0.5:4, during big 8 atmospheric pressure of solution Quick-pressing, with the speed of 30Pa/min
Increase pressure, keep constant when reaching 12 atmospheric pressure, when being rapidly heated to 100 DEG C, with the ramp of 5 DEG C/min, when
Reach to keep constant when 120 DEG C, keep 2h when pressure and temperature all arrive peak, obtain suspension emulsion A,
(5) the most again in suspension emulsion A add trace element, obtain suspension emulsion B, described trace element be iron,
One or more in boron, arsenic, manganese, copper, cobalt, molybdenum, then corn fertilizer is made in recrystallization, granulation and drying.
Entering detection, the purity of ammonium dihydrogen phosphate is more than 98%, and the corn fertilizer obtained containsThe potassium phosphate composite fertilizer of root and、Chemical Mixed Fertilizer, wherein the content of nitrogen component be 18%, phosphorus
Component content is 7%, potassium component content is 8%.
Embodiment three
A kind of production method preparing ammonium dihydrogen phosphate by-product corn fertilizer that the present invention provides, comprises the following steps
(1) phosphoric acid using wet-method is that 1.5:1 mixes with phosphoamide according to mol ratio, and with programming rate be 5 DEG C/
Min is warming up to 160 DEG C from 95 DEG C, stirring reaction 4h, isolated intermediate；
(2) using this intermediate again is that 1:1.2 mixes with ammonia according to mol ratio, during mixing, is first dissolved in by this intermediate
In water, being passed through ammonia the most again in solution, the reaction time is 1.5h, after reaction terminates, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and
The slip of nitrogenous, phosphorus, potassium is placed in cooler crystallizer and cools to 33 DEG C, carry out crystallizing filtration treatment, make filtrate at cooling knot
In brilliant device, circulation crystallization processes, it is thus achieved that filter cake be ammonium dihydrogen phosphate product, the component content in detection filtrate；
(3) add, filtrate, potassium hydroxide solution and the phosphoric acid solution of 23% that concentration is 23%, adjust nitrogen in filtrate,
Phosphorus, potassium content and pH value, when in filtrate, pH value is 3.8, the content of nitrogen component is 23%, phosphorus composition content is 7%, potassium composition contains
When amount is 13%, stop adding potassium hydroxide solution and phosphoric acid solution；
(4) adding formalin in the solution of step (3), the concentration of described formalin is 30-35%, and formaldehyde
It is 1.0:4 with the mol ratio of the phosphoamide contained in solution, during big 7 atmospheric pressure of solution Quick-pressing, with the speed of 25Pa/min
Rate increases pressure, keeps constant when reaching 10-12 atmospheric pressure, when being rapidly heated to 80-100 DEG C, with the speed of 4 DEG C/min
Heat up, keep constant when reaching 120 DEG C, keep 1.5h when pressure and temperature all arrive peak, obtain suspension emulsion A,
(5) the most again in suspension emulsion A add trace element, obtain suspension emulsion B, described trace element be iron,
One or more in boron, arsenic, manganese, copper, cobalt, molybdenum, then corn fertilizer is made in recrystallization, granulation and drying.
Entering detection, the purity of ammonium dihydrogen phosphate is more than 98%, and the corn fertilizer obtained containsThe potassium phosphate composite fertilizer of root and、Chemical Mixed Fertilizer, wherein the content of nitrogen component be 20%, phosphorus
Component content is 6%, potassium component content is 10%.
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
Using the corn fertilizer of above-described embodiment making as the most direct corn fertilizing to result of fertilizer, and make training
Corn seedling is cultivated by nutrient solution, the yield of statistics corn, and Solution culture method, after 30 days, detects N, P, K therein and divides content,
And the growing way situation of corn seedling.
Control group 1-3
Fertile as fertilizer using common N, P, K mixing, wherein N, P, K component content in this mixing fertilizer is respectively at embodiment
One is identical to N, P, K component content in embodiment three, and fertilising is planted in the production to corn respectively, and makes nutrient solution to corn
Seedling is cultivated, and the yield of statistics corn, Solution culture method, after 30 days, detects N, P, K component content therein.
By being the contrast of experimental group and control group, the yield height 300-500kg/ mu of the yield increased group of experimental group,
In cultivating seedling, N, P, K residual condition in the nutrient solution in experimental group is 34%, 41%, 27% respectively simultaneously, far away
Less than N, P, K residual content in the nutrient solution in control group.
Claims (5)
1. prepare a production method for ammonium dihydrogen phosphate by-product corn fertilizer, comprise the following steps
(1) phosphoric acid of wet-method is used to be (1.3～1.6) with phosphoamide according to mol ratio: 1 mixes, and with programming rate for 5
DEG C/min is warming up to 160 DEG C from 95 DEG C, stirring reaction 4～5h, isolated intermediate；
(2) using this intermediate again is 1:(1.1～1.3 with ammonia according to mol ratio) mix, during mixing, first by molten for this intermediate
Yu Shuizhong, is passed through ammonia the most again in solution, and the reaction time is 2h, after reaction terminates, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and
The slip of nitrogenous, phosphorus, potassium is placed in cooler crystallizer and cools to 30 DEG C, carry out crystallizing filtration treatment, make filtrate at cooling knot
In brilliant device, circulation crystallization processes, it is thus achieved that filter cake be ammonium dihydrogen phosphate product, the component content in detection filtrate；
(3) in filtrate, add potassium hydroxide solution and phosphoric acid solution, adjust nitrogen, phosphorus, potassium content and pH value in filtrate, work as filtrate
In pH value be 3.5～4.0, nitrogen component content be 20～25%, phosphorus composition content be 4～10%, potassium component content be 10～
When 15%, stop adding potassium hydroxide solution and phosphoric acid solution；
(4) solution of step (3) adds formalin, during solution Quick-pressing to 6～8 atmospheric pressure, with 20～30Pa/
The speed of min increases pressure, keeps constant when reaching 10～12 atmospheric pressure, when being rapidly heated to 80～100 DEG C, with 2～5
DEG C/ramp of min, keep constant when reaching 120 DEG C, keep 1～2h when pressure and temperature all arrive peak,
To suspension emulsion A,
(5) the most again in suspension emulsion A add trace element, obtain suspension emulsion B, described trace element be iron, boron,
One or more in arsenic, manganese, copper, cobalt, molybdenum, then corn fertilizer is made in recrystallization, granulation and drying；
Described corn fertilizer is the Chemical Mixed Fertilizer of compound state, wherein the content of nitrogen component be 18-21%, phosphorus composition content be 4-
7%, potassium component content is 8-13%；
The Chemical Mixed Fertilizer of described compound state contains following N P and K compound state structural formula:Its
In, the dotted line between carbon atom and oxygen atom represents and there is coordinate bond between C atom and O atom, and containsWithCan
Controlled Release Fertilizer.
Prepare the production method of ammonium dihydrogen phosphate by-product corn fertilizer the most as claimed in claim 1, it is characterised in that: described
Potassium hydroxide solution concentration be 20～25%.
Prepare the production method of ammonium dihydrogen phosphate by-product corn fertilizer the most as claimed in claim 1, it is characterised in that: described
The concentration of phosphoric acid solution 20～25%.
Prepare the production method of ammonium dihydrogen phosphate by-product corn 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 corn fertilizer the most as claimed in claim 1, it is characterised in that: suspend
Emulsion B carries out crystallisation step and is down to 30～35 DEG C for cooling pressurized treatment, temperature, and pressure increases to 6～8 atmospheric pressure, obtains crystalline substance
Body, dries finally by granulation and obtains corn fertilizer.
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|---|---|---|---|---|
| CN1343186A (en) * | 1999-03-18 | 2002-04-03 | Oms投资公司 | 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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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1343186A (en) * | 1999-03-18 | 2002-04-03 | Oms投资公司 | 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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