CN104326454B - A kind of production method preparing sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides - Google Patents
A kind of production method preparing sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides Download PDFInfo
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- dihydrogen phosphate
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Abstract
The present invention relates to chemical technology field, a kind of production method preparing sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides, it is changed by the coefficients such as the temperature of sodium dihydrogen phosphate being prepared by phosphoric acid by wet process, improve the purity of sodium 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 sodium dihydrogen phosphate, the absorptivity of this special fertilizer of Eucommia ulmoides produced is good, in filtrate, add formaldehyde simultaneously make a kind of controlled-releasing compounding fertilizer, this special fertilizer of Eucommia ulmoides produced disclosure satisfy that the nutritional need in each period in growth cycle, substantially increase bark of eucommia 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 sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides
Method.
Background technology
The bark of eucommia (Eucommia ulmoides Oliver) is Chinese famous and precious tonic herb.Taste is sweet, warm in nature.Return liver, kidney, stomach
Warp.Effect tonifies the liver and kidney, strengthens muscles and bones, coordinating Chong and Conception Vessels, solid through antiabortive.The pain in waist and lower extremities or aching and limp unable that treatment kidney-yang deficiency causes.
Born of the same parents' tire that liver-qi invasion causes is solid, and scrotum is wet the disease such as itches.The fertilising of the tradition bark of eucommia is all to use fertilizer to mix with chemical mixing fertilizer
Closing and use, its absorptivity is the highest.
Sodium dihydrogen phosphate (Sodium Dihydrogen Phosphate), colourless iris crystallizes, slightly hygroscopicity.Easily
It is dissolved in water, under certain ph value, by sodium carbonate and phosphatase reaction or by disodium hydrogen phosphate and a certain proportion of phosphatase reaction system
Easily must lump in humid air.Seal and preserve.Acid-base value regulating.Processing for boiler water, plating, process hides, baking powder, fuel help
Agent, washing agent, the thorough conjunction of mica, acid slow agent etc., be also to produce calgon and the raw material of polycondensation hydrochlorate.It mainly makes bag
Include thermal phosphoric acid and phosphoric acid by wet process produces sodium dihydrogen phosphate, and thermal phosphoric acid cost is relatively big, should not be as being widely popularized, therefore,
Wet-process Phosphoric Acid Production sodium dihydrogen phosphate product becomes main method, and the basic step of wet process phosphoric acid for preparing sodium dihydrogen phosphate is such as
Under:
Reaction equation one:
CO(NH2)2+H3PO4=CO (NH2)2.H3PO4
Reaction equation two
CO(NH2)2.H3PO4+ NaOH=NaH2PO4+CO(NH2)2+H2O
After whole reaction terminates, for there is any change, simultaneously because phosphoamide solubility is the highest, 20 in phosphoamide
DEG C time, its solubility is that 85g/100ml (refers to " phosphate fertilizer and composite fertilizer " volume 20 the 6th phase solubility of chemical fertilizer with multiple
Complex fertilizer production technology), the rising of the solubility with temperature of phosphoamide simultaneously and increase, so the phosphoamide contained in filtrate is logical
After crossing the precipitation of cooling crystal, possibly together with a large amount of undecomposed phosphoamides, NH in filtrate4 +、H2PO4 ~、HPO4 2～、PO4 3～If, directly
Connecing and do waste water 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 sodium dihydrogen phosphate, the purity of sodium 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 maize special fertilizer and the absorbing state of maize are ground
Study carefully, effectively inquire into out from the filtrate of Wet-process Phosphoric Acid Production sodium dihydrogen phosphate, produce maize special fertilizer, solve phosphoric acid by wet process raw
Produce the problems such as active ingredient cannot utilize in the filtrate of sodium 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 sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides
Method, by unique process production design, improves the purity of sodium dihydrogen phosphate, makes full use of wet process phosphoric acid for preparing di(2-ethylhexyl)phosphate simultaneously
Phosphoamide, NH in the filtrate of hydrogen sodium4 +、H2PO4 ~、HPO4 2～、PO4 3～Deng material, the bark of eucommia producing out applicable Growth of Eucommia ulmoides is special
Fertile.
The present invention is achieved by the following technical programs.
A kind of production method preparing sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides, 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 the speed that heats up
Degree is that 5 DEG C/min is warming up to 160 DEG C from 95 DEG C, stirring reaction 4～5h, isolated intermediate；
(2) intermediate is put in sodium hydroxide solution stirring reaction, and the mol ratio of intermediate and NaOH is
1.2～1.4:1, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and the slip of nitrogenous, phosphorus, potassium is placed in cooler crystallizer cools to 30
DEG C, carry out crystallize filtration treatment, make filtrate in cooler crystallizer circulation crystallization process, it is thus achieved that filter cake be sodium dihydrogen phosphate produce
Product, the component content in detection filtrate；
(3) add potassium hydroxide solution and phosphoric acid solution filtrate, adjust nitrogen, phosphorus, potassium content and pH value in filtrate, work as filter
PH value in liquid is 3.5～4.0, nitrogen component content be 20～25%, phosphorus composition content be 10～15%, potassium component content be 12
～when 18%, stop adding potassium hydroxide solution and phosphoric acid solution；
(4) solution of step (3) adds formalin, during big 6～8 atmospheric pressure of solution Quick-pressing, with 20～
The speed of 30Pa/min increases pressure, keeps constant when reaching 10～12 atmospheric pressure, when being rapidly heated to 80～100 DEG C,
With the ramp of 2～5 DEG C/min, keep constant when reaching 120 DEG C, keep 1 when pressure and temperature all arrive peak
～2h, 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 special fertilizer of Eucommia ulmoides is made in recrystallization, granulation and drying.
The concentration of described sodium hydroxide solution is 20～25%, and described potassium hydroxide solution concentration is 20～25%,
The concentration of described phosphoric acid solution is 20～25%.
The concentration of described formalin is 30～35%, and the mol ratio of formaldehyde and phosphoamide is (0.5～1.5):
4。
Described suspension 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, obtain crystal, dry finally by granulation and obtain special fertilizer of Eucommia ulmoides.
Described special fertilizer of Eucommia ulmoides is the Chemical Mixed Fertilizer of compound state, wherein the content of nitrogen component be 18-21%, phosphorus composition content
It is 11-14% for 10-12%, potassium component content.
The Chemical Mixed Fertilizer of described compound state contains following N P and K compound state structural formula:Wherein, carbon
Dotted line between atom and oxygen atom represents and there is coordinate bond between C atom and O atom, and contains
WithRealizing controlled-release fertile.
In the present invention, by urea and phosphoric acid at 95 DEG C and anti-in the environment of being warming up to 160 DEG C with the speed of 5 DEG C/min
Should, generate urea phosphate, and being stepped up along with temperature, and then make the coordinate bond dialysis between urea phosphate and formed two kinds from
Sub-shape material, be exactly i.e.WhenIon is in phosphoric acid environment,
Will be 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 sodium hydroxide solution, dihydrogen phosphate and sodium ion react generation sodium dihydrogen phosphate, and phase
Continue and reach saturated；When adding potassium ion and excess, it will react, in further making with the ammonium radical ion in intermediate-ion
Between ion chelating becomeIntermediate-ion, and with positive charge, and then when solution participates in
Battalion when other electronegative ions or compound, it will form compound salt with this ion, in the abundantest product
Form point.
Meanwhile, meanwhile, urea 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 products The most longer chemical chain,
In the case of acidity, reaction can be continued with phosphoamide and formaldehyde to generateSimultaneouslyContinue to react with phosphoamide and formaldehyde in the case of acidity, Deng urea aldehyde series of products after fertilising, under the effect of microorganism, can discharge
The N that is easily absorbed by plants, C element, the chain length of its urea aldehyde is the longest, and chain needs time of fracture the longest, produces the time of fertilizer efficiency
Can discharge after a certain time, the effect of sustained release can be reached generally,Release
Putting the fertilizer efficiency time is 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:
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 sodium 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 sodium dihydrogen phosphate is regulated to 80～160 DEG C, and heats up from 95 DEG C to 160 with the speed of 5 DEG C/min
React in the environment of DEG C, not only make the sodium dihydrogen phosphate product purity of precipitation reach more than 98%, to filtrate adds hydroxide
After potassium 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 productIntermediate-ion and
Dihydrogen phosphate, and between C and O, form coordinate bond, this intermediate-ion can be formed many with centering element compound chelating
Element intermediate-ion, and then can continue to the compound electronegative with other or ion formation chelate, improve in double salt
Constituent content, and then the nutrient content in the double salt that this ion exists can be adjusted, meanwhile, this chelate can be hydrolyzed again
And by crop, and then effectively can provide fertilizer efficiency for crop for a long time, contain in conjunction with element in the solution that this ion is existed meanwhile
The mensuration of amount, and then adjust each constituent content when double salt is formed, dry and obtain compound state double salt composite fertilizer, its absorptivity pole
Good, reduce bark of eucommia planting cost and improve bark of eucommia quality；
2. phosphoamide composition containing part in filtrate, adds formalin, in acid condition and certain pressure intensity and temperature
Under degree, generate Deng urea aldehyde series
Composite fertilizer, can make this special fertilizer of Eucommia ulmoides reach the effect of realizing controlled-release；
3. by effective uptake of n-p-k element is examined by the constituent content in special fertilizer of Eucommia ulmoides and the bark of eucommia
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 urea and forms the ionic state containing positive charge so that phosphorus
Acid urea 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 NaOH in solution, NaOH can react with acid, by cooling
Crystallization, generates NaH2PO4, when filtrate adds excessive and appropriate potassium ion, potassium ion and (CO5PN2H8)+Ion is anti-
Should, and displace part NH4 +So that containing (CO in solution5PNH4K)+Double salt ion, and analyzed by detection and control molten
The content of N, P, K element in liquid, 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 NaOH, dihydrogen phosphate and sodium ion react generation sodium dihydrogen phosphate, and in succession reach saturated；Work as analysis
Go out NaH2PO4After crystal, containing substantial amounts of in filtrateRoot, to adding potassium hydroxide in filtrate
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, urea and formaldehyde are in the case of being 3.5～4.0 acidity in pH value, can produce and react:
Reaction equation five
Reaction equation six
Generate urea aldehyde series of products
The most longer chemical chain,In the case of acidity, reaction can be continued with phosphoamide and formaldehyde to generate 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,Release
Putting the fertilizer efficiency time is 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
A kind of production method preparing sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides that the present invention provides, comprises the following steps:
(1) be that 1.3:1 mix with phosphoamide according to mol ratio with the phosphoric acid of wet-method, 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) it is stirring reaction in 20% sodium hydroxide solution that intermediate is put into concentration, and intermediate and NaOH
Mol ratio be 1.2:1, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and the slip of nitrogenous, phosphorus, potassium is placed in cooler crystallizer cooling
To 30 DEG C, carry out crystallize filtration treatment, make filtrate in cooler crystallizer circulation crystallization process, it is thus achieved that filter cake be biphosphate
Sodium product, the component content in detection filtrate；
(3) add, filtrate, the potassium hydroxide solution and the phosphoric acid solution of 20% that concentration is 20%, 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 10%, potassium component content
When being 18%, stop adding potassium hydroxide solution, aqua calcis and phosphoric acid solution；
(4) adding formalin in the solution of step (3), the concentration of described formalin is 30～35%, and first
Aldehyde is 1.5:4 with the mol ratio of phosphoamide, during big 6 atmospheric pressure of solution Quick-pressing, increases pressure with the speed of 30Pa/min,
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 120 DEG C
Keep constant, 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 special fertilizer of Eucommia ulmoides is made in recrystallization, granulation and drying.
Entering detection, the purity of sodium dihydrogen phosphate is more than 98%, and the special fertilizer of Eucommia ulmoides obtained contains
The potassium phosphate composite fertilizer of root and Multiple
Complex fertilizer, wherein the content of nitrogen component be 21%, phosphorus composition content be 10%, potassium component content be 14%.
Embodiment two
A kind of production method preparing sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides 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) it is stirring reaction in 25% sodium hydroxide solution that intermediate is put into concentration, and intermediate and NaOH
Mol ratio be 1.4:1, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and the slip of nitrogenous, phosphorus, potassium is placed in cooler crystallizer cooling
To 35 DEG C, carry out crystallize filtration treatment, make filtrate in cooler crystallizer circulation crystallization process, it is thus achieved that filter cake be biphosphate
Sodium product, the component content in detection filtrate；
(3) add, filtrate, the potassium hydroxide solution and the phosphoric acid solution of 25% that concentration is 25%, 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 15%, potassium component content
When being 12%, 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 first
Aldehyde is 0.5:4 with the mol ratio of phosphoamide, during big 8 atmospheric pressure of solution Quick-pressing, increases pressure with the speed of 20Pa/min,
Keep constant when reaching 12 atmospheric pressure, when being rapidly heated to 100 DEG C, with the ramp of 5 DEG C/min, when reaching 120 DEG C
Time keep constant, when pressure and temperature all arrive peak keep 2h, 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 special fertilizer of Eucommia ulmoides is made in recrystallization, granulation and drying.
Entering detection, the purity of sodium dihydrogen phosphate is more than 98%, and the special fertilizer of Eucommia ulmoides obtained contains
The potassium phosphate composite fertilizer of root and Chemical Mixed Fertilizer, wherein
The content of nitrogen component is 18%, phosphorus composition content is 12%, potassium component content is 11%.
Embodiment three
A kind of production method preparing sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides 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) intermediate is put in sodium hydroxide solution stirring reaction, and the mol ratio of intermediate and NaOH is
1.3:1, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and the slip of nitrogenous, phosphorus, potassium is placed in cooler crystallizer cools to 33 DEG C, enter
Row crystallization filtration treatment, make filtrate in cooler crystallizer circulation crystallization process, it is thus achieved that filter cake be sodium dihydrogen phosphate product, inspection
Survey the component content in filtrate；
(3) add, filtrate, the phosphoric acid solution of potassium hydroxide solution 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 12%, 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 30～35%, and first
Aldehyde is 1.0:4 with the mol ratio of phosphoamide, during big 7 atmospheric pressure of solution Quick-pressing, increases pressure with the speed of 25Pa/min,
Keep constant when reaching 10～12 atmospheric pressure, when being rapidly heated to 80～100 DEG C, with the ramp of 4 DEG C/min, when reaching
Keep constant during to 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 special fertilizer of Eucommia ulmoides is made in recrystallization, granulation and drying.
Entering detection, the purity of sodium dihydrogen phosphate is more than 98%, and the special fertilizer of Eucommia ulmoides obtained contains
The potassium phosphate composite fertilizer of root and Chemical Mixed Fertilizer, wherein
The content of nitrogen component is 20%, phosphorus composition content is 11%, potassium component content is 12%.
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
The most directly the bark of eucommia of result is applied fertilizer as fertilizer using the special fertilizer of Eucommia ulmoides that above-described embodiment makes, and make training
Bark of eucommia seedling is cultivated by nutrient solution, the yield of the statistics bark of eucommia, after Solution culture method 30, detects N, P, K therein and divides content, with
And the growing way situation of bark of eucommia 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 the bark of eucommia respectively, and makes nutrient solution to the bark of eucommia
Seedling is cultivated, the yield of the statistics bark of eucommia, after Solution culture method 30, detects N, P, K component content therein.
By being the contrast of experimental group and control group, the yield high 200 of the yield increased group of experimental group～300kg/ mu,
In cultivating seedling, N, P, K residual condition in the nutrient solution in experimental group is 41%, 31%, 27% respectively simultaneously, far away
Less than N, P, K residual content in the nutrient solution in control group.
Claims (6)
1. prepare a production method for sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides, 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) intermediate is put into stirring reaction in sodium hydroxide solution, and the mol ratio of intermediate and NaOH is (1.2
～1.4): 1, 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
Cool to 30 DEG C, carry out crystallize filtration treatment, make filtrate in cooler crystallizer circulation crystallization process, it is thus achieved that filter cake be phosphoric acid
Sodium dihydrogen product, the component content in detection filtrate；
(3) add potassium hydroxide solution and phosphoric acid solution filtrate, adjust nitrogen, phosphorus, potassium content and pH value in filtrate, when in filtrate
PH value be 3.5～4.0, nitrogen component content be 20～25%, phosphorus composition content be 10～15%, potassium component content be 12～
When 18%, stop adding potassium hydroxide solution and phosphoric acid solution；
(4) solution of step (3) adds formalin, during big 6～8 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/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 special fertilizer of Eucommia ulmoides is made in recrystallization, granulation and drying.
Prepare the production method of sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides the most as claimed in claim 1, it is characterised in that: described
The concentration of sodium hydroxide solution be 20～25%, described potassium hydroxide solution concentration is 20～25%, and described phosphoric acid is molten
The concentration of liquid is 20～25%.
Prepare the production method of sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides 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 formaldehyde and phosphoamide is (0.5～1.5): 4.
Prepare the production method of sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides 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 special fertilizer of Eucommia ulmoides.
Prepare the production method of sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides the most as claimed in claim 1, it is characterised in that: described
The Chemical Mixed Fertilizer that special fertilizer of Eucommia ulmoides is compound state, wherein the content of nitrogen component be 18-21%, phosphorus composition content be 10-12%, potassium
Component content is 11-14%.
Prepare the production method of sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides the most as claimed in claim 5, 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 oxygen
Dotted line between atom represents and there is coordinate bond between C atom and O atom, and containsWithRealizing controlled-release fertile.
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| CN1060648A (en) * | 1990-10-08 | 1992-04-29 | 邢新华 | Polybasic fertilizer |
| US6254655B1 (en) * | 1999-03-18 | 2001-07-03 | Oms Investments, Inc. | Processes for preparing granular composite fertilizer compositions and products produced thereby |
| EP2766301A4 (en) * | 2011-10-13 | 2015-06-24 | Ekobalans Fenix Ab | Dewatering of phosphate precipitates |
| 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 |
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