CN103936510B - Slow-release fertilizer of a kind of applicable water-fertilizer integral and preparation method thereof - Google Patents

Slow-release fertilizer of a kind of applicable water-fertilizer integral and preparation method thereof Download PDF

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CN103936510B
CN103936510B CN201410156597.9A CN201410156597A CN103936510B CN 103936510 B CN103936510 B CN 103936510B CN 201410156597 A CN201410156597 A CN 201410156597A CN 103936510 B CN103936510 B CN 103936510B
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water
fertilizer
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emulsion
soluble
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CN103936510A (en
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陈庆
张芝媛
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Shandong Chingshang Chemical Industrial Co ltd
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Chengdu New Keli Chemical Science Co Ltd
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Abstract

A kind of slow-release fertilizer of applicable water-fertilizer integral.This slow-release fertilizer take chemical fertilizer as core, and slow soluble polymer is the Nano capsule slow-release fertilizer of wall material composition, and this slow-release fertilizer can be dispersed in water and form colloidal solution and the fertilizer reaching sustained-release and controlled release object.Invention further provides the preparation method of this slow-release fertilizer, the capsule material of this slow-release fertilizer is the rear polymerization reaction take place of slow soluble polymer mixing by oppositely charged, and coated core, add linking agent solidification, filtration drying, namely obtains Nano capsule slow-release fertilizer.This slow-release fertilizer can be dispersed in water, and forms colloidal solution, can irrigate together with water; And capsule material is slow soluble polymer, can slowly be dissolved in soil, reach the object of controlled release, and can not cause the secondary pollution of soil.

Description

Slow-release fertilizer of a kind of applicable water-fertilizer integral and preparation method thereof
Technical field
The invention belongs to the fertilizer field of farm crop, more precisely relate to a kind of slow release fertilizer with water-fertilizer integral that is applicable to.
Background technology
Along with the continuous increase of China's population, grain demand is also increasing, and greatly developing agricultural is important measures.Chemical fertilizer plays a part more and more important in agricultural, and it is large that present chemical fertilizer in use mainly exists amount of application, and utilization ratio is low, and pollutes this two large problems to soil.China's water resources lacks, and agricultural water consumption is large, and dry season, lack of water was one of important factor hindering China's agricultural development.So, solution chemical fertilizer utilization ratio, soil pollution have become one of important content of research chemical fertilizer with saving agricultural water problem.China's water resources famine, accounts for 61.9% of total water consumption by the water yield with agricultural, annual agricultural water breach is very large, and drought and water shortage has become one of key constraints threatening grain security, restriction agricultural sustainable development.Under this urgent form, China's agricultural development direction need be changed the intensive style of making rational use of resources into and be produced, and the Integration of Water into Fertilizer is the inevitable choice of modern agricultural development.Therefore, research can be applicable to water-fertilizer integral, improves chemical fertilizer utilization ratio, and reduce fertilizer amount, the chemical fertilizer alleviating environmental pressure is current emphasis.
These two aspect problems of current solution be new type chemical fertilizer---Water soluble fertilizer and slowly-releasing Controlled Release Fertilizer.Water soluble fertilizer can be dissolved in water, reaches fertilising object with water in irrigating, and is applicable to modern agriculture, but Water soluble fertilizer release rate is fast, and plant is limited to the absorption of nutrient within a certain period of time, result in the waste of Water soluble fertilizer, reduces utilization ratio; Sustained-release and controlled release fertilizer can discharge fertilizer slowly, and rate of release and the plant growing cycle of its fertilizer nutrient adapt, and utilization ratio is high, and saves manpower, decreases the time.But sustained-release and controlled release fertilizer is larger particles, current fertilization mode is artificial or mechanical system, fails to be dissolved in water, reaches the object of fertilising, waste manpower and time with water in can not irrigating.
It take nano material as polymer emulsion coated slow release fertilizer of carrier and preparation method thereof that China Patent Publication No. CN102180731A discloses a kind of.The program is for raw material with hydroxyethyl methylacrylate, vinyl cyanide and starch, adopt microemulsified and high-shear technology, prepare the heterogeneous mixed polymers of nano level hydroxyethyl methylacrylate-vinyl cyanide-starch, as water-maintaining slowly/controlled releasing fertilizer coating cementing agent and organic-inorganic complex fertilizer adhesive for granulating.This slow-release fertilizer has just used nano material as its coated fertilizer, and the particle of fertilizer is all larger, and in water, solvability is very poor, though reach the object of slowly-releasing, but is not suitable for the application of water-fertilizer integral.
China Patent Publication No. CN101717301A discloses a kind of capsule type microbial fertilizer and preparation method.The program is using biological bacteria as core, is carried out micro encapsulation, but wherein gained wets, the particle diameter of dry capsule is respectively 2.40-3.50mm and 0.8-1.5mm.Though this microorganism fertilizer is encapsulated by fertilizer, reach the effect of slowly-releasing, but its preparation method is mixed with fertilizer by monomer capsule material, capsule material is made to carry out absorption fully to fertilizer coated, and particle diameter is larger, can not be effectively dispersed in water and form aqueous suspensions, have larger limitation to the application of water-fertilizer integral.
China Patent Publication No. CN102731222A discloses a kind of slow controlled release compound fertilizer and preparation method thereof.The program is that various fertilizer is carried out micro encapsulation, and then is mixed and carry out granulation, because particle is large, poorly soluble in water, is still not suitable for the application of water-fertilizer integral.
According to above-mentioned, the current slow-release fertilizer particle of China is all larger, though can reach the object of Controlled release, is not suitable for modern agriculture water-fertilizer integral, wastes a large amount of manpower and time in fertilising process, increase the consumption of water.Therefore, in order to adapt to the development of modern agriculture, needing exploitation to be further suitable for water-fertilizer integral, the new-type fertilizer of sustained-release and controlled release can be reached again.
Summary of the invention
In order to solve above-mentioned deficiency and defect, the present invention proposes a kind of slow-release fertilizer of applicable water-fertilizer integral.This fertilizer is that Nano capsule is fertile, and granularity is little, is dissolved in water and can forms colloidal solution, can irrigate with water; And adopt microcapsule to carry out coated, the object of Controlled release can be reached, single fertilization, the fertile water-saving of time and labour saving province; Capsule material used in this fertilizer is the material of water-soluble, and after slowly dissolving in soil, fertilizer slowly releases, and reaches slow release effect, and production technique is simple.
Present invention further proposes a kind of preparation method of slow-release fertilizer of applicable water-fertilizer integral.This preparation method utilizes two kinds with after the slow soluble polymer mixing of opposite charges, by the pH value of regulation system, reduces the solubleness of capsule material, make it that aggregation occur, parcel core, then add solidifying agent and be cured, filtration drying, obtains Nano capsule slow-release fertilizer.This slow-release fertilizer is coated by delaying soluble polymer, and is nano particle size, can be quickly dispersed in water, forms colloidal solution, in being manured into soil together with water.Along with the slow dissolving of slow soluble polymer, fertilizer slow releasing, reaches the object of sustained-release and controlled release.
The slow-release fertilizer of a kind of applicable water-fertilizer integral of the present invention, is characterized in that, this slow-release fertilizer is made up of core and capsule material, wherein core is one or more mixtures in following chemical fertilizer: urea, potassium primary phosphate, primary ammonium phosphate, phosphoric acid one hydrogen ammonia, potassium sulfate, Repone K; Wherein capsule material is the mixture of positively charged polymkeric substance and electronegative soluble polymer.
Positively charged water-soluble polymkeric substance described above is one or more following mixtures: polyallyl quaternary ammonium salt, chitosan, gum arabic, cationic starch, cationic polyacrylamide, cationic polyvinyl base pyrrolidone, polyvinylamine, poly-2-vinyl imidazol quinoline, Modified cationic water-soluble poly aminoresin, cation water-soluble epoxy resin, polyethylene imine based, polyamine epichlorohydrin resin, heavy presses-epichlorohydrin resin, isobutyl alkyl ethyl ester, wherein add in positive charge water-soluble polymkeric substance liquid state with positive charge water-soluble amount of polymers 10% ~ 20% containing the 30% hydroxyalkyl starch aqueous solution, carry out emulsification, obtain positively charged water-soluble polymer micro-emulsion.
Electronegative water-soluble polymkeric substance described above is one or more following mixtures: gelatin, casein food grade, xanthan gum, hyaluronic acid, carboxymethyl cellulose, carboxymethyl starch, water soluble oxidized starch, phosphate ester starch, anionic polyacrylamide, negatively charged ion Polyvinylpyrolidone (PVP), polymaleic anhydride, negatively charged ion opens Pu Shi resin, Witco 1298 Soft Acid, sodium laurylsulfonate, sodium cetanesulfonate, anionic water soluble polyurethane resin, wherein add in negative charge water-soluble polymkeric substance liquid state with negative charge water-soluble polymkeric substance 10% ~ 20% containing the 30% hydroxyalkyl starch aqueous solution, carry out emulsification, obtain electronegative water-soluble polymer micro-emulsion.
The slow-release fertilizer of a kind of applicable water-fertilizer integral of the present invention, is characterized in that the preparation method of this slow-release fertilizer comprises the following steps:
(1), chemical fertilizer and water are dissolved in the ratio of 1:1 ~ 10, add the polyol non-ionic tensio-active agent of 3% ~ 10% of fertilizer amount again, lifting stirrer is at a high speed utilized to be mixed into emulsion, setting speed is 800r/min ~ 1200r/min, send into again in high pressure homogenizer and carry out high-pressure homogeneous twice, make emulsion reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), gained chemical fertilizer micro emulsion A micro emulsion in step (1) is sent into and is elevated at a high speed in stirrer, add step positively charged water-soluble polymer micro-emulsion to be more in proportion uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add a certain proportion of electronegative water-soluble polymer micro-emulsion again, wherein additional proportion is A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative soluble polymer microemulsion=1 ~ 2:1 ~ 2:1 ~ 2, pH adjusting agent adjust ph is utilized to be 3.8 ~ 5.0, design temperature is 25 DEG C ~ 35 DEG C, high-speed stirring, there is aggregation upon mixing in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, form Nano capsule,
(3), in the Nano capsule adding the solidifying agent gained in step (2) at a high speed lifting stirrer accounting for A micro emulsion 2% ~ 10%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule is shaping, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring, static 10 ~ 20min;
(4), gained Nano capsule mixed solution clear water in step (3) is washed twice, remove unreacted polymkeric substance and unnecessary solidifying agent, with pH adjusting agent adjust ph to 6.5 ~ 7.0, utilize centrifuge to filter, spraying dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral.
Polyol non-ionic tensio-active agent described in above-mentioned steps (1) is one or more following mixtures: sorbitol ester, tween, polyvinyl alcohol, sucrose fatty ester, diethanolamine fatty acid ester, stearyl methacrylate.
In above-mentioned steps (1), chemical fertilizer is dissolved in water, forms solution, then add the emulsifying agent of 5% ~ 20%, carry out homogeneous by high pressure homogenizer.Because capsule material is slow soluble materials, can be dissolved in water, and chemical fertilizer also can be dissolved in water and ionizes out zwitterion, carry out reaction with the capsule material with positive and negative charge to condense, therefore, in order to prevent the reaction of chemical fertilizer and capsule material, ensure fertilizer efficiency, chemical fertilizer need be dissolved in organic solvent, keep the stability of chemical fertilizer ion; Moreover the present invention makes Nano capsule slow-release fertilizer, but the globule size of capsule is determined by the emulsifying stage particle diameter of liquid, therefore by high pressure homogenizer, make chemical fertilizer become microemulsion, size is even, ensure that follow-up capsule size is at below 50nm, and embedding rate can reach more than 90%.
The positively charged water-soluble polymer micro-emulsion added in above-mentioned steps (2) and the treatment process of electronegative water-soluble polymer micro-emulsion are, by positively charged and water-soluble polymkeric substance that is negative charge, add the tensio-active agent 30% hydroxyalkyl starch aqueous solution of 10% ~ 20% respectively, again by high pressure homogenizer, be also ensure that capsule material can form nano level microemulsion.Wherein microemulsion is nano level, ensures follow-up capsule grain diameter; Add tensio-active agent simultaneously, the activity of polymkeric substance can be improved, the polymkeric substance with electric charge fully can be reacted, increase operation rate.
Solidifying agent described above is one or more following mixtures: methacrylic acid imidazolidyl ketone hydroxyl ethyl ester, glutaraldehyde, Virahol, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2 isopropyl imidazole, diethyl amino propylamine, Triethylenetetramine (TETA), dimethylaminopropylamine.
PH adjusting agent described above is acid-base modifier, and wherein acidity regulator is: citric acid, oxalic acid, tartrate; Alkalinity regulator is sodium hydroxide solution.
First chemical fertilizer micro emulsion A micro emulsion is fully mixed with positively charged water-soluble polymer micro-emulsion in above-mentioned steps (2), then add electronegative water-soluble polymer micro-emulsion.Because A micro emulsion fully mixes with positively charged water-soluble polymer micro-emulsion, positively charged water-soluble polymer micro-emulsion is evenly distributed on around A micro emulsion, after adding electronegative water-soluble polymer micro-emulsion, after positively charged water-soluble polymer micro-emulsion mixes with electronegative water-soluble polymer micro-emulsion, positive and negative charge combines, there is aggregation, coated core; Adjust ph again, reduces the solubleness of wall material, makes it separate out on core, forms capsule; Add solidifying agent, capsule is solidified, strengthen capsule equipment structure, reach good intensity, not cracky, redeposition is separated out, and washing, filtration drying, can obtain Nano capsule slow-release fertilizer.
High pressure homogenizer described in above-mentioned steps (1) is electromechanical type convection current high pressure homogenizer, two fluid channels, left and right are provided with in homogeneous chamber, utilize distinctive Y-shaped structure, the material convection current that high-pressure solution high speed is moved, from colliding, is ground into nanometer micro emulsion.
High speed lifting stirrer described in above-mentioned steps (1) (2) (3) is two guide pillar hydraulic lifting stirrers.Hydraulic lifting stirrer, utilizes motor to carry out speed governing, and material, under the high-speed rotation effect of blade, acutely stirs up and down in container, produces percussion and shearing with blade, makes aggregate disruption reach rapid dispersion, intimate mixing.Filter type in above-mentioned steps (6) is centrifuging, adopts electric centrifuge, utilizes centrifugal force, carry out solid-liquid separation, obtain required Nano capsule solid.
The present invention with the slow-release fertilizer of water-fertilizer integral, is characterized in that by chemical fertilizer by abundant microemulsified at a kind of being applicable to, then micro encapsulation, becomes Nano capsule.The slow-release fertilizer of current China is mainly coat fertilizer, also has and fertilizer is made into microcapsule, but coat fertilizer and Microcapsule fertilizer particle all larger, irrigate easy blocking pipe together with water.But Nano capsule and microcapsule are except the difference of size, also different in capsule material, dispersiveness etc.Microcapsules Size is general larger, be dispersed in water as suspension liquid, precipitation is produced as dealt with improperly, be easy to blocking pipe, and Nano capsule particle diameter is nanometer, is dispersed in water as colloidal solution, plant membrane can be penetrated, enter in vegetable cell and tissue, slow releasing in the tissue, Promoting plant growth.
The outstanding feature of the slow-release fertilizer of a kind of applicable water-fertilizer integral of the present invention and preparation method thereof is:
1, the water-soluble of chemical fertilizer and slowly-releasing control-release function combine by the present invention, utilize water miscible polymkeric substance as capsule material, coated chemical fertilizer, and along with the slow dissolving of capsule material, fertilizer efficiency slow releasing, reaches the object of sustained-release and controlled release.By chemical fertilizer microemulsified, the reaction of recycling positive and negative charge polymer agglomerates, parcel chemical fertilizer, can make chemical fertilizer capsule reach nano level, be dispersed in water, and forms colloidal solution, irrigates, not blocking pipe together with water, is applicable to the modern agriculture of water-fertilizer integral.
2, the capsule material used in the present invention is slow molten polymkeric substance, is dispersed in soil and can effectively slowly dissolves, and the material after water-soluble can not cause secondary pollution to soil.
3, the chemical fertilizer in the present invention, can need to carry out any proportioning according to crop, according to the growth rhythm of crop different times, provide nutrition, promotes plant growth, improves the utilization ratio of fertilizer, can use again together with water, time saving and energy saving water-saving saving of labor.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but should not be construed as scope authority of the present invention and be only limitted to following example.
embodiment 1
A slow-release fertilizer for applicable water-fertilizer integral, it is composed as follows:
Core: urea
Capsule material: positively charged water-soluble polymkeric substance: chitosan
Electronegative water-soluble polymkeric substance: hyaluronic acid
The pre-treatment of capsule material:
(1), in the liquid chitosan of positive charge water-soluble polymkeric substance add the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains positively charged polymer micro-emulsion, stand-by;
(2), in the liquid hyaluronic acid of negative charge water-soluble polymkeric substance add the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains electronegative polymer micro-emulsion, stand-by;
A preparation method for the slow-release fertilizer of applicable water-fertilizer integral, its preparation methods steps is as follows:
(1), urea and water are dissolved in the ratio of 1:2, add the polyol non-ionic surface active agent tween-60 accounting for chemical fertilizer 5% again, lifting stirrer is mixed into emulsion at a high speed, setting speed is 800r/min ~ 1200r/min, is mixed into emulsion, then send into carry out in high pressure homogenizer high-pressure homogeneous, emulsion is made to reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), gained urea micro emulsion A micro emulsion in step (1) is sent into and is elevated at a high speed in stirrer, add step positively charged water-soluble polymer shell glycan microemulsion to be more in proportion uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add a certain proportion of electronegative polymer hyaluronic acid micro emulsion again, wherein additional proportion is A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative soluble polymer microemulsion=2:1:1, pH adjusting agent adjust ph is utilized to be 4.5 ~ 5.0, design temperature is 25 DEG C ~ 35 DEG C, high-speed stirring, setting speed is 1200r/min ~ 1400r/min, there is aggregation upon mixing in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, form Nano capsule,
(3), in the Nano capsule adding the solidifying agent glutaraldehyde gained in step (2) at a high speed lifting stirrer accounting for A micro emulsion 5%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule is shaping, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring, static 10 ~ 20min;
(4), gained Nano capsule mixed solution clear water in step (3) is washed twice, remove unreacted polymkeric substance and unnecessary solidifying agent, with pH adjusting agent adjust ph to 6.5 ~ 7.0, utilize centrifuge to filter, spraying dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral.
By urea leaching test, the slow-release fertilizer nutrients release of a kind of applicable water-fertilizer integral of the present invention is as following table:
Fertilization time Fertilizer efficiency leaching yield Capsule material dissolution rate
24h 3% 1%
30d 65% 50%
60d 96% 80%
90d Completely dissolve Completely dissolve
embodiment 2
A slow-release fertilizer for applicable water-fertilizer integral, it is composed as follows:
Core: urea, potassium primary phosphate, and ratio is urea: potassium primary phosphate=2:1
Capsule material: positively charged water-soluble polymkeric substance: quaternary ammonium starch ethers
Electronegative water-soluble polymkeric substance: anionic starch
The pre-treatment of capsule material:
(1), in the liquid quaternary ammonium starch ethers of positive charge water-soluble polymkeric substance add the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains positively charged polymer micro-emulsion, stand-by;
(2), in the liquid anionic starch of negative charge water-soluble polymkeric substance add the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains electronegative polymer micro-emulsion, stand-by;
A preparation method for the slow-release fertilizer of applicable water-fertilizer integral, its preparation methods steps is as follows:
(1), by the mixture of urea and potassium primary phosphate, dissolve with the ratio of water in 1:4, add the polyol non-ionic tensio-active agent sucrose fatty ester of chemical fertilizer amount 5% again, lifting stirrer is mixed into emulsion at a high speed, and setting speed is 800r/min ~ 1200r/min, be mixed into emulsion, send into again and carry out high-pressure homogeneous in high pressure homogenizer, make emulsion reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), gained urea in step (1) and potassium primary phosphate mixing micro emulsion A micro emulsion being sent into is elevated at a high speed in stirrer, add positively charged water-soluble polymeric quartenary ammonium starch ethers micro emulsion to be more in proportion uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add a certain proportion of electronegative water-soluble polymer anion Sumstar 190 micro emulsion again, wherein additional proportion is A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative soluble polymer microemulsion=1:2:2, pH adjusting agent adjust ph is utilized to be 4.0 ~ 4.5, design temperature is 25 DEG C ~ 35 DEG C, high-speed stirring, setting speed is 1200r/min ~ 1400r/min, there is aggregation upon mixing in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, form Nano capsule,
(3), in the Nano capsule adding the solidifying agent glutaraldehyde gained in step (2) at a high speed lifting stirrer accounting for A micro emulsion 8%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule is shaping, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring, static 10 ~ 20min;
(4), gained Nano capsule mixed solution clear water in step (3) is washed twice, remove unreacted polymkeric substance and unnecessary solidifying agent, with pH adjusting agent adjust ph to 6.5 ~ 7.0, utilize centrifuge to filter, spraying dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral.
By chemical fertilizer leaching test, the slow-release fertilizer nutrients release of a kind of applicable water-fertilizer integral of the present invention is as following table:
Fertilization time Fertilizer efficiency leaching yield Capsule material dissolution rate
24h 1% 0.5%
30d 57.5% 40%
60d 95% 85%
90d Completely dissolve Completely dissolve
embodiment 3
A slow-release fertilizer for applicable water-fertilizer integral, it is composed as follows:
Core: phosphoric acid one hydrogen ammonia
Capsule material: positively charged water-soluble polymkeric substance: cationic polyurethane resin
Electronegative water-soluble polymkeric substance: carboxymethyl starch
The pre-treatment of capsule material:
(1), in the liquid cationic polyurethane resin of positive charge water-soluble polymkeric substance add the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains positively charged polymer micro-emulsion, stand-by;
(2), in the liquid carboxymethyl starch of negative charge water-soluble polymkeric substance add the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains electronegative polymer micro-emulsion, stand-by;
A preparation method for the slow-release fertilizer of applicable water-fertilizer integral, its preparation methods steps is as follows:
(1), phosphoric acid one hydrogen ammonia and water are dissolved in the ratio of 1:1, add the polyol non-ionic tensio-active agent stearyl methacrylate accounting for chemical fertilizer 8% again, lifting stirrer is mixed into emulsion at a high speed, setting speed is 800r/min ~ 1200r/min, is mixed into emulsion, then send into carry out in high pressure homogenizer high-pressure homogeneous, emulsion is made to reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), gained phosphoric acid one hydrogen ammonia micro emulsion A micro emulsion in step (1) is sent into and is elevated at a high speed in stirrer, add positively charged water-soluble polymer cation urethane resin micro emulsion to be more in proportion uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add a certain proportion of electronegative water-soluble polymer carboxymethyl starch micro emulsion again, wherein additional proportion is A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative soluble polymer microemulsion=2:1:1, pH adjusting agent adjust ph is utilized to be 4.0 ~ 4.5, design temperature is 25 DEG C ~ 35 DEG C, high-speed stirring, setting speed is 1200r/min ~ 1400r/min, there is aggregation upon mixing in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, form Nano capsule,
(3), in the Nano capsule adding the solidifying agent 2 isopropyl imidazole gained in step (2) at a high speed lifting stirrer accounting for A micro emulsion 4%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule is shaping, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring, static 10 ~ 20min;
(4), gained Nano capsule mixed solution clear water in step (3) is washed twice, remove unreacted polymkeric substance and unnecessary solidifying agent, with pH adjusting agent adjust ph to 6.5 ~ 7.0, utilize centrifuge to filter, spraying dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral.
By chemical fertilizer leaching test, the slow-release fertilizer nutrients release of a kind of applicable water-fertilizer integral of the present invention is as following table:
Fertilization time Fertilizer efficiency leaching yield Capsule material dissolution rate
24h 2% 1%
30d 60% 45%
60d 95% 80%
90d Completely dissolve Completely dissolve
embodiment 4
A slow-release fertilizer for applicable water-fertilizer integral, it is composed as follows:
Core: urea, ammonium hydrogen phosphate, and ratio is urea: ammonium hydrogen phosphate=1:1
Capsule material: positively charged water-soluble polymkeric substance: cationic polyvinylpyrrolidone
Electronegative water-soluble polymkeric substance: phosphate ester starch
The pre-treatment of capsule material:
(1), in the liquid cationic polyvinylpyrrolidone of positive charge water-soluble polymkeric substance add the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains positively charged polymer micro-emulsion, stand-by;
(2), in the liquid phosphate ester starch of negative charge water-soluble polymkeric substance add the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains electronegative polymer micro-emulsion, stand-by;
A preparation method for the slow-release fertilizer of applicable water-fertilizer integral, its preparation methods steps is as follows:
(1), by the mixture of urea and potassium primary phosphate, dissolve with the ratio of water in 1:4, add the polyol non-ionic tensio-active agent diethanolamine fatty acid ester of chemical fertilizer amount 5% again, lifting stirrer is mixed into emulsion at a high speed, and setting speed is 800r/min ~ 1200r/min, be mixed into emulsion, send into again and carry out high-pressure homogeneous in high pressure homogenizer, make emulsion reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), gained urea micro emulsion A micro emulsion in step (1) is sent into and is elevated at a high speed in stirrer, add positively charged water-soluble polymer cation polyvinylpyrrolidone micro emulsion to be more in proportion uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add a certain proportion of electronegative polymeric phosphoric acid ester starch micro emulsion again, wherein additional proportion is A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative soluble polymer microemulsion=1:1:1, pH adjusting agent adjust ph is utilized to be 4.0 ~ 4.5, design temperature is 25 DEG C ~ 35 DEG C, high-speed stirring, setting speed is 1200r/min ~ 1400r/min, there is aggregation upon mixing in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, form Nano capsule,
(3), in the Nano capsule adding the solidifying agent glutaraldehyde gained in step (2) at a high speed lifting stirrer accounting for A micro emulsion 15%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule is shaping, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring, static 10 ~ 20min;
(4), gained Nano capsule mixed solution clear water in step (3) is washed twice, remove unreacted polymkeric substance and unnecessary solidifying agent, with pH adjusting agent adjust ph to 6.5 ~ 7.0, utilize centrifuge to filter, spraying dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral.
By chemical fertilizer leaching test, the slow-release fertilizer nutrients release of a kind of applicable water-fertilizer integral of the present invention is as following table:
Fertilization time Fertilizer efficiency leaching yield Capsule material dissolution rate
24h 3% 0.5%
30d 63% 45%
60d 94% 85%
90d Completely dissolve Completely dissolve
embodiment 5
A slow-release fertilizer for applicable water-fertilizer integral, it is composed as follows:
Core: urea, primary ammonium phosphate, potassium sulfate, and ratio is urea: primary ammonium phosphate: potassium sulfate=2:2:1
Capsule material: positively charged water-soluble polymkeric substance: gum arabic
Electronegative water-soluble polymkeric substance: xanthan gum
The pre-treatment of capsule material:
(1), in the liquid gum arabic of positive charge water-soluble polymkeric substance add the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains positively charged polymer micro-emulsion, stand-by;
(2), in the liquid xanthan gum of negative charge water-soluble polymkeric substance add the 30% hydroxyalkyl starch aqueous solution, add-on is 10%, by high pressure homogenizing twice, obtains electronegative polymer micro-emulsion, stand-by;
A preparation method for the slow-release fertilizer of applicable water-fertilizer integral, its preparation methods steps is as follows:
(1), by urea, the mixture of primary ammonium phosphate and potassium sulfate, dissolves with the ratio of water in 1:5, then adds the polyol non-ionic tensio-active agent sorbitol ester accounting for chemical fertilizer 6%, lifting stirrer is mixed into emulsion at a high speed, setting speed is 800r/min ~ 1200r/min, is mixed into emulsion, then send into carry out in high pressure homogenizer high-pressure homogeneous, emulsion is made to reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), by gained urea in step (1), primary ammonium phosphate, potassium sulfate mixing micro emulsion A micro emulsion is sent into and is elevated at a high speed in stirrer, add positively charged polymkeric substance gum arabic micro emulsion to be more in proportion uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add a certain proportion of electronegative polymkeric substance xanthan gum micro emulsion again, wherein additional proportion is A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative soluble polymer microemulsion=2:1:1, pH adjusting agent adjust ph is utilized to be 4.0 ~ 4.5, design temperature is 25 DEG C ~ 35 DEG C, high-speed stirring, setting speed is 1200r/min ~ 1400r/min, there is aggregation upon mixing in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, form Nano capsule,
(3), in the Nano capsule adding the solidifying agent Virahol gained in step (2) at a high speed lifting stirrer accounting for A micro emulsion 15%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule is shaping, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring, static 10 ~ 20min;
(4), gained Nano capsule mixed solution clear water in step (3) is washed twice, remove unreacted polymkeric substance and unnecessary solidifying agent, with pH adjusting agent adjust ph to 6.5 ~ 7.0, utilize centrifuge to filter, spraying dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral.
By chemical fertilizer leaching test, the slow-release fertilizer nutrients release of a kind of applicable water-fertilizer integral of the present invention is as following table:
Fertilization time Fertilizer efficiency leaching yield Capsule material dissolution rate
24h 3% 2%
30d 70% 58%
60d 98% 87%
90d Completely dissolve Completely dissolve
In above example, the fertilizer release in 30 days of each fertilizer all≤75%, meets slow-release fertilizer standard.

Claims (2)

1. a slow-release fertilizer for applicable water-fertilizer integral, is characterized in that: this slow-release fertilizer is made up of core and capsule material, and wherein core is one or more mixtures in following chemical fertilizer: urea, potassium primary phosphate, primary ammonium phosphate, ammonium hydrogen phosphate, potassium sulfate, Repone K; Wherein capsule material is the mixture of positively charged water-soluble polymkeric substance and electronegative water-soluble polymkeric substance; Prepare by the following method and obtain:
(1), chemical fertilizer and water are dissolved in the ratio of 1:1 ~ 10, add the polyol non-ionic tensio-active agent of 3% ~ 10% of fertilizer amount again, lifting stirrer is at a high speed utilized to be mixed into emulsion, setting speed is 800r/min ~ 1200r/min, send into again in high pressure homogenizer and carry out high-pressure homogeneous twice, make emulsion reach nano level, become chemical fertilizer microemulsion, be set as A micro emulsion, stand-by;
(2), gained chemical fertilizer micro emulsion A in step (1) is sent in high speed lifting stirrer, add positively charged water-soluble polymer micro-emulsion to be uniformly mixed, setting mixing speed is 1200r/min ~ 1400r/min, churning time is 5min ~ 15min, add electronegative water-soluble polymer micro-emulsion again, pH adjusting agent adjust ph is utilized to be 3.8 ~ 5.0, design temperature is 25 DEG C ~ 35 DEG C, high-speed stirring, there is aggregation upon mixing in the polymkeric substance of oppositely charged, coated chemical fertilizer microemulsion, forms Nano capsule; Wherein additional proportion is: A micro emulsion: positively charged water-soluble polymer micro-emulsion: electronegative water-soluble polymer micro-emulsion=1 ~ 2:1 ~ 2:1 ~ 2;
(3), add again in the Nano capsule of the solidifying agent gained in step (2) at a high speed lifting stirrer accounting for A micro emulsion 2% ~ 10%, continue to keep high-speed stirring, Nano capsule is solidified, guarantee Nano capsule is shaping, mixing speed is 1200r/min ~ 1400r/min, churning time 5 ~ 15min, stops stirring, leaves standstill 10 ~ 20min;
(4), gained Nano capsule mixed solution clear water in step (3) is washed twice, remove unreacted polymkeric substance and unnecessary solidifying agent, with pH adjusting agent adjust ph to 6.5 ~ 7.0, utilize centrifuge to filter, spraying dry, can obtain a kind of slow-release fertilizer of applicable water-fertilizer integral;
Described positively charged water-soluble polymkeric substance is one or more following mixtures: polyallyl quaternary ammonium salt, sodium alginate, chitosan, gum arabic, cationic starch, cationic polyacrylamide, cationic polyvinyl base pyrrolidone, polyvinylamine, poly-2-vinyl imidazol quinoline, Modified cationic water-soluble poly aminoresin, cation water-soluble epoxy resin, polyethylene imine based, polyamine epichlorohydrin resin, heavy polyamine-epichlorohydrin resin, isobutyl alkyl ethyl ester; What in positively charged water-soluble polymkeric substance liquid state, wherein add 10% ~ 20% of positively charged water-soluble amount of polymers contains the 30% hydroxyalkyl starch aqueous solution, carries out emulsification, obtains positively charged water-soluble polymer micro-emulsion;
Described electronegative water-soluble polymkeric substance is one or more following mixtures: gelatin, casein food grade, xanthan gum, hyaluronic acid, carboxymethyl cellulose, carboxymethyl starch, water soluble oxidized starch, phosphate ester starch, anionic polyacrylamide, negatively charged ion Polyvinylpyrolidone (PVP), polymaleic anhydride, negatively charged ion opens Pu Shi resin, anionic water soluble polyurethane resin; What in electronegative water-soluble polymkeric substance liquid state, wherein add 10% ~ 20% of electronegative water-soluble polymkeric substance contains the 30% hydroxyalkyl starch aqueous solution, carries out emulsification, obtains electronegative water-soluble polymer micro-emulsion;
Polyol non-ionic tensio-active agent described in step (1) is one or more following mixtures: sorbitol ester, tween, polyvinyl alcohol, sucrose fatty ester, diethanolamine fatty acid ester, stearyl methacrylate;
Step (2) and the pH adjusting agent described in step (4) are acid-base modifier, and wherein acidity regulator is: citric acid, oxalic acid, tartrate; Alkalinity regulator is sodium hydroxide solution;
Solidifying agent described in step (3) is one or more following mixtures: methacrylic acid imidazolidyl ketone hydroxyl ethyl ester, glutaraldehyde, Virahol, 2-ethyl-4-methylimidazole, 2-phenylimidazole, 2 isopropyl imidazole, diethyl amino propylamine, Triethylenetetramine (TETA), dimethylaminopropylamine.
2. the slow-release fertilizer of a kind of applicable water-fertilizer integral according to claim 1, it is characterized in that: wherein the high pressure homogenizer described in step (1) is electromechanical type convection current high pressure homogenizer, two fluid channels, left and right are provided with in homogeneous chamber, utilize distinctive Y-shaped structure, the material convection current that high-pressure solution high speed is moved, from colliding, is ground into nanometer micro emulsion.
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