CN104445123B - A kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer - Google Patents
A kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer Download PDFInfo
- Publication number
- CN104445123B CN104445123B CN201410479119.1A CN201410479119A CN104445123B CN 104445123 B CN104445123 B CN 104445123B CN 201410479119 A CN201410479119 A CN 201410479119A CN 104445123 B CN104445123 B CN 104445123B
- Authority
- CN
- China
- Prior art keywords
- solution
- radix ipomoeae
- potassium
- fertilizer
- dihydrogen phosphate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The present invention relates to chemical technology field, a kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer, coefficient is waited to be changed by phosphoric acid by wet process is prepared the warm of potassium dihydrogen phosphate, improve the purity of potassium dihydrogen phosphate product, can produce containing N simultaneously, P, the Chemical Mixed Fertilizer of K compound state, and in filtrate, add formaldehyde make a kind of controlled-releasing compounding fertilizer, improve the purity of potassium dihydrogen phosphate, the absorbance of this Radix Ipomoeae special fertilizer produced is good, this Radix Ipomoeae special fertilizer simultaneously produced disclosure satisfy that the nutritional need in each period in Radix Ipomoeae growth cycle, substantially increase Radix Ipomoeae 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 potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer
Method.
Background technology
Potassium 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 senilism, 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 phosphorus potassium complex fertilizer agriculturally.Current domestic a lot of fertilizer producers are all producing di(2-ethylhexyl)phosphate
Hydrogen K composite fertilizer, its production method mainly have neutralisation, extraction, ion exchange, double decomposition, direct method, crystallization process and
Electrolysis etc., wherein double decomposition includes that thermal phosphoric acid and phosphoric acid by wet process produce potassium dihydrogen phosphate, and thermal phosphoric acid cost is relatively big,
Should not be as being widely popularized, therefore, Wet-process Phosphoric Acid Production potassium dihydrogen phosphate product becomes main method, wet process phosphoric acid for preparing phosphorus
The basic step of acid is as follows:
Reaction equation one:
CO(NH2)2+H3PO4=CO (NH2)2.H3PO4
Reaction equation two
CO(NH2)2.H3PO4+ KOH=KH2PO4+H2O+CO(NH2)2
Reacting at 40～80 DEG C in whole reaction, there is not any change in substantial amounts of phosphoamide after the completion of reaction, with
Time due to phosphoamide dissolubility the highest, when 20 DEG C, its dissolubility is that 85g/100ml (refers to " phosphate fertilizer and compound fertilizer " volume 20
6th phase solubility of chemical fertilizer and Compound fertilizer production technology), the rising of the solubility with temperature of phosphoamide simultaneously and increase
Greatly, so the phosphoamide contained in filtrate by cooling crystal separate out after, in filtrate possibly together with a large amount of undecomposed phosphoamides,
K+、H2PO4 -、HPO4 2-、PO4 3-If directly doing waste water and discharge, both having wasted resource, the waste of resource, meanwhile, analysis can be caused again
The purity of the potassium dihydrogen phosphate crystal gone out is the highest.
Radix Ipomoeae rich in proteins, starch, pectin, cellulose, aminoacid, vitamin and several mineral materials, have " long-lived food
Product " reputation.Sugar content reaches 15%-20%.There are the effects such as anticancer, cardioprotection, prevention emphysema, diabetes, fat-reducing.According to grinding
Study carefully, often produce 1000 kilograms of fresh potatos, need from soil, absorb available nitrogen 3.5 kilograms, phosphorus pentoxide 1.8 kilograms, potassium 5 public affairs
Jin.Traditional Radix Ipomoeae fertilising is all to use poultry manure, and the patent of invention such as Patent No. CN201310506237.2 is " a kind of red
Potato slag chicken manure fertilizer and preparation method thereof " and the patent of invention one of Patent No. CN201210566294.5 utilize sweet potato waste
The primary raw material of the method preparing chicken manure fertilizer is exactly sweet potato waste and chicken manure, and its major defect is: N, P, the K in poultry manure without
Method determines, the yield of Radix Ipomoeae cannot be maintained at one well in the range of；And use the fertilizer such as plant ash, such as Patent No.
The patent of invention of the CN201210142052.3 formula fertilizer of Radix Ipomoeae high yield " a kind of allow ", primary raw material is Fructus Jujubae wood timber, Fructus Pruni wood wood
Material, peach wood timber, weedtree timber is sintered into ash respectively, and its advantage is that P, K content is high, but the content of N is less, and Radix Ipomoeae is in growth
Early stage, it is impossible to seal woods soon, in some arid areas, seals woods overlong time, and soil moisture runs off fast, can cause Radix Ipomoeae yield
Low；Also using the mixing fertilizer of nitrogen, phosphorus, potassium, the patent of invention such as Patent No. CN200910227408.1 is " a kind of for Radix Ipomoeae
Formula fertilizer ", it is mainly composed of phosphoamide, calcium superphosphate, calcium and magnesium phosphorus and potassium chloride, and its shortcoming is to mix fertile absorption not
It is good, it was reported that:
Phosphoamide, the plant absorption utilization rate of carbon ammonium be: 20% one 46%；
The plant absorption utilization rate of phosphate fertilizer (diammonium, an ammonium, triple superphosphate) is: 10% one 25%；
The plant absorption utilization rate of common potash fertilizer is: 45% one 60%.
Unabsorbed mixing fertilizer, easily causes soil compaction, the release of this fertilizer simultaneously and lose too fast, and early stage can cause
The overgrowing of sweet potato vine, the later stage is due to Radix Ipomoeae overgrowing and soaks because of rainwater or fertilizer self decomposes, cause nutrition in soil without
The needs of method supply Radix Ipomoeae, cause yield extremely low.
During Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, the purity of potassium dihydrogen phosphate is the highest, possibly together with greatly in filtrate
Measure undecomposed phosphoamide, K+、H2PO4 -、HPO4 2-、PO4 3-Deng material, the researcher of the present invention is from substantial amounts of prior art literature
And exploration for many years and research, and the tradition component content of Radix Ipomoeae special fertilizer and the absorbing state of Radix Ipomoeae are studied,
Effectively inquire into out from the filtrate of Wet-process Phosphoric Acid Production potassium dihydrogen phosphate, produce Radix Ipomoeae special fertilizer, solve Wet-process Phosphoric Acid Production phosphorus
In the filtrate of acid dihydride potassium, effective ingredient such as cannot utilize at the problem, at home in fertilizer production, has no report.
Summary of the invention
For above technical problem, the invention provides a kind of producer preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer
Method, by unique process production design, improves the purity of potassium dihydrogen phosphate, makes full use of wet process phosphoric acid for preparing biphosphate simultaneously
Phosphoamide, K in the filtrate of potassium+、H2PO4 -、HPO4 2-、PO4 3-Deng material, produce out the Radix Ipomoeae special fertilizer of applicable Radix Ipomoeae growth.
The present invention is achieved by the following technical solutions:
The invention provides a kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer, mainly include following step
Rapid:
1) use phosphoric acid to be (1.2-1.6) with phosphoamide according to mol ratio: 1 mixes, and with programming rate be 5 DEG C/min from
80 DEG C are warming up to 150 DEG C, stirring reaction 4-5h, isolated intermediate；Use again this intermediate and alkaline potassium salt according to mole
Ratio is 1:(1.1-1.3) mixing, regulation pH value is 8.5-9.5, 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 40～45 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 potassium dihydrogen phosphate product, the phosphoamide in detection filtrate, K+、H2PO4 -Contain
Amount；
2) in filtrate, formalin is added, according to being (0.8～0.9) with the mol ratio of phosphoamide that contains in solution: 1
Mixing, becomes with the nitrogen with potassium hydroxide solution with phosphoric acid solution regulation solution of phosphoric acid solution regulation solution with potassium hydroxide solution
The content divided is 15-25%, phosphorus composition content is 1.5-4.5%, potassium component content is that 8-14%, pH are 8.5～9.0., then
Mixed liquor is put in retort, pressure is increased to 8～10 atmospheric pressure, be rapidly heated 85 DEG C time, with 5～6 DEG C/min
Ramp, when reaching 120 DEG C, keep 2～3h；
3) by step 2) solution that obtains is divided into two parts,
The solution fast cooling taking a deal to 60 DEG C and is depressurized under normal pressure stand, named solution A,
The solution taking a deal is put in a retort, when atmospheric pressure is quickly ramped up to 2 atmospheric pressure, with 50～100Pa/
The speed of min increases atmospheric pressure, simultaneously temperature from 85 DEG C with the ramp of 1～2 DEG C/min, when reaching 3 atmospheric pressure, temperature
When reaching 95 DEG C, keep 0.5～1h, named solution B；
4) by step 3) solution A that obtains, it is cooled to 60～65 DEG C after B mixing, and add a certain amount of H2SO4Solution, adjusts
The scope of joint pH to 7.0～7.4, adds a small amount of CaSO4, add MgSO4、Fe2+Chelate, H3BO3In at least one
Kind, stand 0.5～1h, obtain solution C；
5) by step 4) in the solution C that obtains be cooled to 20～25 DEG C, carry out crystallizing filtration treatment, obtain substantial amounts ofThe potassium phosphate of root and a small amount of The compound state Chemical Mixed Fertilizer of urea aldehyde go out finished product；
6) pelletize is dried, in this step, first by step 5) mixture that separates out is fabricated to a diameter of 0.2～0.4cm
Granule, be subsequently placed in temperature be 60～65 DEG C, flow velocity be 3～4m/s ammonia environment in dry.
Further, step 2) in the potassium hydroxide solution concentration that adds be 35～40%, described
The concentration of phosphoric acid solution be 20～25%.
Further, described step 4) sulfuric acid solution concentration be 5～15%.
Further, when compound state compound fertilizer just product nitrogen component content be 16～20%, phosphorus becomes
Point content be 3～5%, potassium component content stop crystallization when being 11-16%.
Further, described Radix Ipomoeae special fertilizer is the Chemical Mixed Fertilizer of compound state.
In the present invention, by phosphoamide and phosphoric acid at 80 DEG C, and in the environment of being warming up to 150 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 potassium 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, phosphoamide, can react with formalin at pH under 8.5～9.0 alkaline case, generatesDeng urea aldehyde series of products,It is difficult to preserve under alkaline case Deng urea aldehyde series of products, therefore
This needs the pH value with sulfuric acid solution regulation solution when 7.0～7.4, separates out the time preserved longer.SimultaneouslyDeng 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 slow release.
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 potassium dihydrogen phosphate making, phosphoamide mutually synthermal
Under dissolubility relatively large, isolated phosphoamide crystal is rich in KH2PO4In other crystal, entered cooling simultaneously and separated out phosphinylidyne
In filtrate after amine crystal possibly together with substantial amounts of phosphoamide, K+、H2PO4 -、HPO4 2-、PO4 3-Utilize Deng not operatively, the present invention
The temperature of phosphoric acid by wet process potassium dihydrogen phosphate making is regulated to 80～150 DEG C, and heats up from 80 DEG C to 150 with the speed of 5 DEG C/min
React in the environment of DEG C, not only make the potassium dihydrogen phosphate product purity of precipitation reach more than 98%, filtrate also generatesCation, 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 C Yu O it
Between form coordinate bond, this intermediate-ion can form multielement intermediate-ion with centering element compound chelating, and then can
Continue to form chelate with other electronegative compounds or ion, improve constituent content in double salt, and then can adjust
Nutrient content in the double salt that this ion exists, meanwhile, this chelate can be hydrolyzed again and by crop, and then can be effective
Long-term for crop provide fertilizer efficiency, meanwhile, ins conjunction with the mensuration of constituent content in the solution that this ion is existed, so adjustment double salt
Each constituent content during formation, dries and obtains compound state double salt compound fertilizer, and by avoiding the addition of chlorine element so that compound state
While the product quality of double salt compound fertilizer disclosure satisfy that the requirement of sweet potato nutrient composition, it is to avoid the damage that Radix Ipomoeae is brought by fertilizer
Evil, reduces Radix Ipomoeae planting cost and improves Radix Ipomoeae quality；
2. phosphoamide composition containing part in filtrate, adds formalin, in alkalescence condition and certain pressure intensity and temperature
Under degree, generateDeng urea aldehyde series compound fertilizer, this can be made red
Potato special fertilizer reaches the effect of realizing controlled-release；
3., during granulating and drying, be passed through the ammonia that flow velocity is certain, can absorbed nitrogen element further, after fertilising
Can quickly be absorbed by plants, ensure that the supply of Radix Ipomoeae early stage nutrition further；
4. this Radix Ipomoeae special fertilizer has the advantages that absorbance is good, realizing controlled-release formula is good, for the plantation of Radix Ipomoeae, average product
Increase by 700～1000kg/ mus.
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, hydrion 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 excessive and appropriate potassium ion, dihydrogen phosphate is formed with potassium ion
Potassium 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 compound 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.
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 8.5～9.0 alkaline case at pH value, can produce and react:
Reaction equation five
Reaction equation six
GenerateDeng urea aldehyde series of products,It is difficult to preserve under alkaline case Deng urea aldehyde series of products, therefore
This needs the pH value with sulfuric acid solution regulation solution when 7.0～7.4, separates out the time preserved longer.SimultaneouslyDeng 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 slow release.
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, aqueous solution is acidity, starts point time melted
Solve and release carbon dioxide and ammonia.Embodiment one
A kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer, mainly comprises the steps that
1) using phosphoric acid is that 1.2:1 mixes with phosphoamide according to mol ratio, and is that 5 DEG C/min rises from 80 DEG C with programming rate
Temperature is to 150 DEG C, and 5h, isolated intermediate are reacted in stirring；Using this intermediate and alkaline potassium salt again is 1:1.1 according to mol ratio
Mixing, regulation pH value is 9.5, after reaction terminates, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and is placed in cold by the slip of nitrogenous, phosphorus, potassium
Crystallizer but cools to 40 DEG C, carries out crystallizing filtration treatment, make filtrate circulation crystallization in cooler crystallizer process, it is thus achieved that
Filter cake is potassium dihydrogen phosphate product, the component content in detection filtrate；
2) in filtrate, add formalin, according to being that 0.9:1 mixes with the mol ratio of the phosphoamide contained in solution, use
The pH of potassium hydroxide solution and phosphoric acid solution regulation solution 8.5, when detect in solution the content of nitrogen component be 15-25%,
When phosphorus composition content is 1.5-4.5%, potassium component content is 8-14%, then mixed liquor is put in retort, pressure is increased
Big to 8 atmospheric pressure, be rapidly heated 85 DEG C time, with the ramp of 5 DEG C/min, when reaching 120 DEG C, keep 3h, described
Potassium hydroxide solution concentration be 35%, the concentration of described phosphoric acid solution is 25%；
3) by step 2) solution that obtains is divided into two parts,
The solution fast cooling taking a deal to 60 DEG C and is depressurized under normal pressure stand, named solution A,
The solution taking a deal is put in a retort, when atmospheric pressure is quickly ramped up to 2 atmospheric pressure, with the speed of 50Pa/min
Rate increases atmospheric pressure, and temperature is from 85 DEG C with the ramp of 2 DEG C/min simultaneously, and when reaching 3 atmospheric pressure, temperature reaches 95 DEG C
Time, keep 1h, named solution B；
4) by step 3) solution A that obtains, it is cooled to 65 DEG C after B mixing, and add a certain amount of H2SO4Solution, regulates pH
To the scope of 7.0, add a small amount of CaSO4, add MgSO4、Fe2+Chelate, H3BO3In one at least, stand 1h,
Obtaining solution C, described sulfuric acid solution concentration is 5%；
5) by step 4) in the solution C that obtains be cooled to 20～25 DEG C, carry out crystallizing filtration treatment, obtain substantial amounts ofThe potassium phosphate of root, and a small amount of Deng the compound state compound fertilizer just finished product of urea aldehyde, when compound state compound fertilizer just product nitrogen composition
When content is 16%, phosphorus composition content is 5%, potassium component content is 16%, stop crystallization.
6) pelletize is dried, in this step, first by step 5) mixture that separates out is fabricated to a diameter of 0.2～0.4cm
Granule, be subsequently placed in temperature be 60～65 DEG C, flow velocity be 3m/s ammonia environment in dry, make Radix Ipomoeae special fertilizer, described
Radix Ipomoeae special fertilizer is the Chemical Mixed Fertilizer of compound state.
Embodiment two
A kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer, mainly comprises the steps that
1) using phosphoric acid is that 1.6:1 mixes with phosphoamide according to mol ratio, and is that 5 DEG C/min rises from 80 DEG C with programming rate
Temperature is to 150 DEG C, and 4h, isolated intermediate are reacted in stirring；Using this intermediate and alkaline potassium salt again is 1:1.3 according to mol ratio
Mixing, regulation pH value is 9.5, after reaction terminates, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and is placed in cold by the slip of nitrogenous, phosphorus, potassium
Crystallizer but cools to 45 DEG C, carries out crystallizing filtration treatment, make filtrate circulation crystallization in cooler crystallizer process, it is thus achieved that
Filter cake is potassium dihydrogen phosphate product, the component content in detection filtrate；
2) in filtrate, add formalin, according to being that 0.8:1 mixes with the mol ratio of the phosphoamide contained in solution, use
The pH of potassium hydroxide solution and phosphoric acid solution regulation solution 9.0, when detect in solution the content of nitrogen component be 15-25%,
When phosphorus composition content is 1.5-4.5%, potassium component content is 8-14%, then mixed liquor is put in retort, pressure is increased
Big to 8 atmospheric pressure, be rapidly heated 85 DEG C time, with the ramp of 5 DEG C/min, when reaching 120 DEG C, keep 3h, described
Potassium hydroxide solution concentration be 35～40%, the concentration of described phosphoric acid solution is 20～25%；
3) by step 2) solution that obtains is divided into two parts,
The solution fast cooling taking a deal to 60 DEG C and is depressurized under normal pressure stand, named solution A,
The solution taking a deal is put in a retort, when atmospheric pressure is quickly ramped up to 2 atmospheric pressure, with 100Pa/min's
Speed increases atmospheric pressure, and temperature is from 85 DEG C with the ramp of 2 DEG C/min simultaneously, and when reaching 3 atmospheric pressure, temperature reaches 95 DEG C
Time, keep 1h, named solution B；
4) by step 3) solution A that obtains, it is cooled to 65 DEG C after B mixing, and add a certain amount of H2SO4Solution, regulates pH
To the scope of 7.0～7.4, add a small amount of CaSO4, add MgSO4、Fe2+Chelate, H3BO3In one at least, quiet
Setting to 0 .5h, obtain solution C, described sulfuric acid solution concentration is 15%；
5) by step 4) in the solution C that obtains be cooled to 20～25 DEG C, carry out crystallizing filtration treatment, obtain substantial amounts ofThe potassium phosphate of root, and a small amount of Deng the compound state compound fertilizer just finished product of urea aldehyde, when compound state compound fertilizer just product nitrogen composition
When content is 20%, phosphorus composition content is 3%, potassium component content is 16%, stop crystallization.
6) pelletize is dried, in this step, first by step 5) mixture that separates out is fabricated to a diameter of 0.2～0.4cm
Granule, be subsequently placed in temperature be 60～65 DEG C, flow velocity be 3m/s ammonia environment in dry, make Radix Ipomoeae special fertilizer, described
Radix Ipomoeae special fertilizer is the Chemical Mixed Fertilizer of compound state.
Embodiment three
A kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer, mainly comprises the steps that
1) using phosphoric acid is that 1.4:1 mixes with phosphoamide according to mol ratio, and is that 5 DEG C/min rises from 80 DEG C with programming rate
Temperature is to 150 DEG C, and 4.5h, isolated intermediate are reacted in stirring；Using this intermediate and alkaline potassium salt again is 1 according to mol ratio:
1.2 mixing, regulation pH value is 8.5-9.5, after reaction terminates, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and by nitrogenous, phosphorus, the material of potassium
Slurry is placed in cooler crystallizer and cools to 43 DEG C, carries out crystallizing filtration treatment, makes filtrate at circulation crystallization in cooler crystallizer
Reason, it is thus achieved that filter cake be potassium dihydrogen phosphate product, detection filtrate in component content；
2) in filtrate, formalin is added, according to being that 0.84:1 mixes with the mol ratio of the phosphoamide contained in solution,
With the pH of potassium hydroxide solution and phosphoric acid solution regulation solution 8.6, when detecting that in solution, the content of nitrogen component is 15-
25%, phosphorus composition content is 1.5-4.5%, potassium component content is when being 8-14%, then puts in retort by mixed liquor, will pressure
Increase to by force 9 atmospheric pressure, be rapidly heated 85 DEG C time, with the ramp of 5～6 DEG C/min, when reaching 120 DEG C, keep 2
～3h, described potassium hydroxide solution concentration is 36%, and the concentration of described phosphoric acid solution is 23%；
3) by step 2) solution that obtains is divided into two parts,
The solution fast cooling taking a deal to 60 DEG C and is depressurized under normal pressure stand, named solution A,
The solution taking a deal is put in a retort, when atmospheric pressure is quickly ramped up to 2 atmospheric pressure, with the speed of 80Pa/min
Rate increases atmospheric pressure, and temperature is from 85 DEG C with the ramp of 1 DEG C/min simultaneously, and when reaching 3 atmospheric pressure, temperature reaches 95 DEG C
Time, keep 0.5～1h, named solution B；
4) by step 3) solution A that obtains, it is cooled to 62 DEG C after B mixing, and add a certain amount of H2SO4Solution, regulates pH
To the scope of 7.2, add a small amount of CaSO4, add MgSO4、Fe2+Chelate, H3BO3In one at least, stand 1h,
Obtaining solution C, described sulfuric acid solution concentration is 10%；
5) by step 4) in the solution C that obtains be cooled to 20～25 DEG C, carry out crystallizing filtration treatment, obtain substantial amounts ofThe potassium phosphate of root, and a small amount of Deng the compound state compound fertilizer just finished product of urea aldehyde, when compound state compound fertilizer just product nitrogen composition
When content is 19%, phosphorus composition content is 5%, potassium component content is 14%, stop crystallization.
6) pelletize is dried, in this step, first by step 5) mixture that separates out is fabricated to a diameter of 0.2～0.4cm
Granule, be subsequently placed in temperature be 60～65 DEG C, flow velocity be 3.3m/s ammonia environment in dry, make Radix Ipomoeae special fertilizer, described
Radix Ipomoeae special fertilizer be the Chemical Mixed Fertilizer of compound state.
In order to preferably prove the beneficial effect that the present invention embodies, the present embodiment also provides for following experimental example:
Experimental example one
Fertile as Radix Ipomoeae plantation fertilizer using common N, P, K mixing, nitrogen component content is 19%, phosphorus composition content is 5%, becomes
Dividing content is 14%, makes culture fluid, carries out soilless culture plantation Radix Ipomoeae, and by the adjustment of prior art, culture fluid can be very
Good plantation Radix Ipomoeae, named A1
Experimental example two is to test example four
The Radix Ipomoeae special fertilizer made with embodiment one to embodiment tripartite's method respectively makes culture fluid, carries out soilless culture kind
Planting Radix Ipomoeae, by the adjustment of prior art, culture fluid can be good at planting Radix Ipomoeae, named A2, A3, A4.
Above-mentioned experimental example carries out cultivating Radix Ipomoeae after 20 days, and in detection culture fluid, the content of N, P, K, observes the life of Radix Ipomoeae simultaneously
Long situation.As shown in the table:
The production method of the Radix Ipomoeae special fertilizer that the above-mentioned experimental example surface present invention provides, its absorbance is more fertile than general mixing
Good, there is the effect that absorbance is good.
Experimental example five
Fertile as Radix Ipomoeae plantation fertilizer using common N, P, K mixing, nitrogen component content is 19%, phosphorus composition content is 5%, potassium
Component content is 14%, plants 10 mu of Radix Ipomoeae, applies fertilizer moderate, when Radix Ipomoeae maturation, randomly selects the Radix Ipomoeae yield of 1 mu as right
Ratio, yield is respectively designated as B1
Experimental example six is to experimental example 12
Special with the potassium dihydrogen phosphate by-product Radix Ipomoeae that a kind of production method of embodiment hereof one to embodiment six statement produces
Fertile with the plantation that fertilizer is Radix Ipomoeae, plant 10 mu of Radix Ipomoeae, apply fertilizer moderate, when Radix Ipomoeae maturation, the Radix Ipomoeae yield randomly selecting 1 mu is made
For contrast, yield is respectively designated as B2, B3, B4, B5, B6, B7.
Statistics result above, such as following table:
Table 2: the yield of each experimental example
By result above it can be seen that in Radix Ipomoeae planting process, use the Radix Ipomoeae special fertilizer that the method makes, its yield
Increase by 700～1200kg/ mus, substantially increase the yield of Radix Ipomoeae.
Above-described embodiment, only for technology design and the feature of the explanation present invention, its objective is to allow and is familiar with the skill of this technical field
Art personnel will appreciate that present disclosure and implement according to this, can not limit the scope of the invention with this.
Claims (4)
1. prepare a production method for potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer, mainly comprise the steps that
1) phosphoric acid is used to be (1.2-1.6) with phosphoamide according to mol ratio: 1 mixes, and is that 5 DEG C/min is from 80 DEG C with programming rate
It is warming up to 150 DEG C, stirring reaction 4-5h, isolated intermediate；This intermediate is used with alkaline potassium salt according to mol ratio to be again
1:(1.1-1.3) mixing, regulation pH value is 8.5-9.5, react terminate after, it is thus achieved that nitrogenous, the slip of phosphorus, potassium, and by nitrogenous,
Phosphorus, the slip of potassium are placed in cooler crystallizer and cool to 40～45 DEG C, carry out crystallizing filtration treatment, make filtrate at cooler crystallizer
Middle circulation crystallization process, it is thus achieved that filter cake be potassium dihydrogen phosphate product, detection filtrate in component content；
2) in filtrate, formalin is added, according to being (0.8～0.9) with the mol ratio of phosphoamide that contains in solution: 1 mixes
Closing, the content of the nitrogen component regulating solution with potassium hydroxide solution and phosphoric acid solution is 15-25%, phosphorus composition content is 1.5-
4.5%, potassium component content be 8-14%, pH 8.5～9.0, then mixed liquor is put in retort, pressure is increased to 8
～10 atmospheric pressure, be rapidly heated 85 DEG C time, with the ramp of 5～6 DEG C/min, when reaching 120 DEG C, keep 2～3h；
3) by step 2) solution that obtains is divided into two parts；
The solution fast cooling taking a deal to 60 DEG C and is depressurized under normal pressure stand, named solution A,
The solution taking a deal is put in a retort, when atmospheric pressure is quickly ramped up to 2 atmospheric pressure, with 50～100Pa/min
Speed increases atmospheric pressure, and temperature is from 85 DEG C with the ramp of 1～2 DEG C/min simultaneously, reaches when reaching 3 atmospheric pressure, temperature
When 95 DEG C, keep 0.5～1h, named solution B；
4) by step 3) solution A that obtains, it is cooled to 60～65 DEG C after B mixing, and add a certain amount of H2SO4Solution, regulates pH
To the scope of 7.0～7.4, add a small amount of CaSO4, add MgSO4、Fe2+Chelate, H3BO3In one at least, quiet
Set to 0 .5～1h, obtain solution C；
5) by step 4) in the solution C that obtains be cooled to 20～25 DEG C, carry out crystallizing filtration treatment, obtain substantial amounts ofThe potassium phosphate of root, and a small amount of The compound state compound fertilizer just finished product of urea aldehyde；
6) pelletize is dried, in this step, first by step 5) mixture that separates out is fabricated to the granule of a diameter of 0.2～0.4cm,
Be subsequently placed in temperature be 60～65 DEG C, flow velocity be 3～4m/s ammonia environment in dry, make Radix Ipomoeae special fertilizer.
A kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer, it is characterised in that:
Step 2) in add potassium hydroxide solution concentration be 35～40%, the concentration of described phosphoric acid solution is 20～25%.
A kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer, it is characterised in that:
Described step 4) sulfuric acid solution concentration be 5～15%.
A kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer, it is characterised in that:
When compound state compound fertilizer just product nitrogen component content be 16～20%, phosphorus composition content be 3～5%, potassium component content be 11-
When 16%, stop crystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410479119.1A CN104445123B (en) | 2014-09-19 | 2014-09-19 | A kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410479119.1A CN104445123B (en) | 2014-09-19 | 2014-09-19 | A kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104445123A CN104445123A (en) | 2015-03-25 |
| CN104445123B true CN104445123B (en) | 2016-12-07 |
Family
ID=52891987
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410479119.1A Expired - Fee Related CN104445123B (en) | 2014-09-19 | 2014-09-19 | A kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104445123B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110182776B (en) * | 2019-07-05 | 2021-08-03 | 郑州机械研究所有限公司 | Method for recycling smelting smoke dust of copper-phosphorus brazing filler metal |
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 |
| CN101811899A (en) * | 2009-12-10 | 2010-08-25 | 吴鲁智 | Special formulated fertilizer for sweet potatoes |
| CN103803518A (en) * | 2014-01-24 | 2014-05-21 | 贵阳中化开磷化肥有限公司 | Method for preparing monopotassium phosphate by using wet-process phosphoric acid |
-
2014
- 2014-09-19 CN CN201410479119.1A patent/CN104445123B/en not_active Expired - Fee Related
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 |
| CN101811899A (en) * | 2009-12-10 | 2010-08-25 | 吴鲁智 | Special formulated fertilizer for sweet potatoes |
| CN103803518A (en) * | 2014-01-24 | 2014-05-21 | 贵阳中化开磷化肥有限公司 | Method for preparing monopotassium phosphate by using wet-process phosphoric acid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104445123A (en) | 2015-03-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104445123B (en) | A kind of production method preparing potassium dihydrogen phosphate by-product Radix Ipomoeae special fertilizer | |
| CN104326455B (en) | A kind of production method preparing potassium dihydrogen phosphate by-product Chinese yew special fertilizer | |
| CN104310344B (en) | A kind of production method preparing potassium dihydrogen phosphate by-product Fructus Pruni salicinae special fertilizer | |
| CN104386660B (en) | A kind of production method preparing ammonium dihydrogen phosphate by-product fertilizer special for watermelon | |
| CN104291287B (en) | A kind of production method preparing ammonium dihydrogen phosphate by-product wax gourd special fertilizer | |
| CN104310329B (en) | A kind of production method preparing ammonium dihydrogen phosphate by-product Fructus Kaki special fertilizer | |
| CN104326457B (en) | A kind of production method preparing dikalium phosphate by-product clube tree special fertilizer | |
| CN104291304B (en) | A kind of production method preparing calcium hydrogen phosphate by-product calabash special fertilizer | |
| CN104326462B (en) | A kind of production method preparing calcium dihydrogen phosphate by-product red bean special fertilizer | |
| CN104326447B (en) | A kind of production method preparing ammonium dihydrogen phosphate by-product special-purpose fertilizer for green cucumber | |
| CN104310356B (en) | Production method of monopotassium phosphate with by-product welsh onion special fertilizer | |
| CN104291301B (en) | A kind of production method preparing dikalium phosphate by-product osmanthus fragrans special fertilizer | |
| CN104310361B (en) | A kind of production method preparing biphosphate calcium oxide by-product tree peony special fertilizer | |
| CN104310333B (en) | A kind of production method preparing ammonium dihydrogen phosphate by-product corn fertilizer | |
| CN104326454B (en) | A kind of production method preparing sodium dihydrogen phosphate by-product special fertilizer of Eucommia ulmoides | |
| CN104326448B (en) | A kind of production method preparing ammonium dihydrogen phosphate by-product sugarcane special-purpose fertilizer | |
| CN104326463B (en) | A kind of production method preparing dalcium biphosphate by-product paddy rice-dedicated fertilizer | |
| CN104310357B (en) | A kind of production method preparing potassium dihydrogen phosphate by-product Chinese cassia tree special fertilizer | |
| CN104291300A (en) | Production method for preparing potassium dihydrogen phosphate and by-producing special fertilizer for gingko seedlings | |
| CN104326453B (en) | A kind of production method preparing ammonium dihydrogen phosphate by-product chive special fertilizer | |
| CN104310345B (en) | Method for preparing potassium dihydrogen phosphate and preparing special fertilizer for hawthorn fruits as byproduct | |
| CN104326461B (en) | A kind of production method preparing dalcium biphosphate by-product Semen sojae atricolor special fertilizer | |
| CN104310359B (en) | A kind of production method preparing calcium dihydrogen phosphate by-product Chinese sorghum special fertilizer | |
| CN104310336B (en) | A kind of production method for preparing ammonium dihydrogen phosphate by-product ginger special fertilizer | |
| CN104310347B (en) | A kind of production method preparing potassium dihydrogen phosphate by-product chrysanthemum special fertilizer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20160919 Address after: No. 237 Jinyang City Kailin Lake District Road 550009 Guizhou city of Guiyang Province Applicant after: Phosphorylcholine group limited-liability company is opened in Guizhou Applicant after: Guizhou Ke Xinhua smelting company limited Applicant after: Guizhou University Address before: 550000 Huaxi District, Guizhou, Guiyang Applicant before: Guizhou University Applicant before: Zhonghuakai Phosphorous Chemical Fertilizer Co., Ltd., Guiyang Applicant before: Guizhou Ke Xinhua smelting company limited |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20161014 Address after: 550000 Huaxi District, Guizhou, Guiyang Applicant after: Guizhou University Applicant after: Phosphorylcholine group limited-liability company is opened in Guizhou Applicant after: Guizhou Ke Xinhua smelting company limited Address before: No. 237 Jinyang City Kailin Lake District Road 550009 Guizhou city of Guiyang Province Applicant before: Phosphorylcholine group limited-liability company is opened in Guizhou Applicant before: Guizhou Ke Xinhua smelting company limited Applicant before: Guizhou University |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20161207 Termination date: 20200919 |