CN100457694C - Biological biodegradable self-control slow-releasing fertilizer and preparation method thereof - Google Patents
Biological biodegradable self-control slow-releasing fertilizer and preparation method thereof Download PDFInfo
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- CN100457694C CN100457694C CNB2007100130999A CN200710013099A CN100457694C CN 100457694 C CN100457694 C CN 100457694C CN B2007100130999 A CNB2007100130999 A CN B2007100130999A CN 200710013099 A CN200710013099 A CN 200710013099A CN 100457694 C CN100457694 C CN 100457694C
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Abstract
The invention discloses a biodegradable self-controlling slow-release fertilizer which is produced by uniformly coating a layer of controlled-release layer of water soluble macromolecule polymer at the surface of the urea or complex fertilizer grain. The weight ratio of the complex fertilizer grain to macromolecule polymer is 0.3-0.4:9.7-9.6. The macromolecule polymer is produced in proportion of fibrin, oxidized starch, polyvinyl alcohol, polyurethane prepolyme, epoxide resin, epoxide resin solidified agent, cross linker, emolsifier, ignition primer, deionized water. The invention adopts glue and latex crosslinking with a biodegradable material to improve the controlled-release capability of the fertilizer and conquer the ''white pollution'', increase the usage ratio of nitrogen of 20-35%, and satisfy the crop need in a whole growth period.
Description
Technical field
The present invention relates to a kind of automatic control slow release fertilizer and preparation method thereof, relate in particular to a kind of with spraying one deck water-soluble high polymers material on urea or compound fertilizer granule surface as biological biodegradable self-control slow-releasing fertilizer of controlled release layer and preparation method thereof.
Background technology
Chemical fertilizer generally is extensive use of as conventional fertilizer in proportion of crop planting, and it is easy, remarkably productive to apply fertilizer, but exist a lot of problems in the use of chemical fertilizer, one of distinct issues are that nitrogen utilization efficiency is low, and the nitrogenous fertilizer that brings thus use the financial loss that caused and environmental pollution etc. in a large number.How to increase substantially chemical nitrogen fertilizer nitrogen utilization efficiency and the effect of giving full play to chemical fertilizer, be present development resource saving type, environmentally friendly, continue in the high-efficiency agriculture one of distinct issues, nearest agrotechnique development shows: the invention of release and release control fertilizer and production and being applied as on agricultural address this problem has opened up new thinking and valid approach comparatively.
The type of film-coated controlled release fertilizer mainly contains both at home and abroad at present: inorganics coated fertilizer and organic polymer coated fertilizer two big classes.
The inorganics coated fertilizer is domestic mainly to be as coated fertilizer (see for details Chinese patent 02126743.x, 03106547.3,200410024201.1,200610045310.0 etc.) with ground phosphate rock, fused(calcium magnesium)phosphate, talcum powder, terra alba, flyash, organic or inorganic matrix material, though these inorganic coated fertilizer low prices, make simple, but the nutrient controlled release properties is poor, nitrogen utilization efficiency is low, and applied once causes crop to have in the later stage taking off fertile phenomenon easily; Abroad mainly with TV.A comPany, the sulfur-coated urea (SCU) of USA exploitation is representative (US3295950), though its price is not high yet, but the problem that exists is the rate of release that 1. is difficult to strict its nutrient of control, because the sulphur clothing is more crisp, putamina can take place in the process that nutrient discharges to break, cause the interior nutrient of film all to discharge suddenly, claim " crushing release " again, tend to crop root is worked the mischief; 2. a large amount of sulphur shells by behind the microbiological degradation, easily cause soil acidification in soil; 3. sulfur-coated urea also exists the easy oxidation of sulphur coating, fragmentation, is unfavorable for the problem of carrying.
The organic polymer coated fertilizer can be divided into the film-coated controlled release fertilizer of two types of thermoplasticity and thermosetting resins again according to the character of organic polymer coated fertilizer.The release and release control fertilizer of thermoplastic resin membrane wrapping is representative with " Meister " of Japan, and thermohardening resin coated release and release control fertilizer is representative with " Osmocote " of the U.S. mainly.These film-coated controlled release fertilizer great majority are that solvent-applied is first with the coating resin dissolves, gradually mould material are uniformly sprayed the fertiliser granulates surface then in sulfuration bed coating tower and form.Though this technology can uniformly spray mould material the fertiliser granulates surface, its energy consumption height, solvent is difficult to whole recovery, easily causes the pollution of production plant and surrounding environment, and uses fluidized-bed process to be difficult to realize producing in enormous quantities; At home, the organic polymer coated fertilizer is representative with Chinese patent 2004100240497 described thermosetting epoxy resin film-coated controlled release fertilizers, the more above-mentioned organic polymer coated fertilizer of this patent has solved the coating process complexity, organic solvent is to production plant and surrounding environment pollution problems thereof, it is good to have the nutrient controlled release properties, the advantage that nitrogen utilization efficiency is high, shortcoming is the 1. biological non-degradable of coated fertilizer, cause " white pollution " easily, 2. production cost height, 3. the crop narrow range of Shi Yonging is only applicable to garden crop, the lawn, golf course and ornamental plant etc. are unfavorable for applying on food crop.
Given this, research and develop biodegradable, cost is low, be suitable on food crop, applying, technology is simple, controlled release properties good, solvent is nontoxic, be suitable for quick production in enormous quantities, and the controlled release coating that can be applied to urea and compound (mixing) fertilizer is simultaneously newly filled a prescription, novel process, will the sound development and the industrialization of China's release and release control fertilizer be of great importance.
Summary of the invention
At the deficiencies in the prior art, the problem to be solved in the present invention provides a kind of biological biodegradable self-control slow-releasing fertilizer and preparation method thereof.Characteristics biodegradable, that cost is lower, controlled release properties is good that slow release fertilizer provided by the invention has, and preparation technology is simple, solvent is nontoxic, be suitable for quick production in enormous quantities.
Biological biodegradable self-control slow-releasing fertilizer of the present invention, utilization is made in the controlled release layer of urea or the even spraying in compound fertilizer granule surface one deck high molecular weight water soluble polymer, and the weight ratio of described urea or compound fertilizer granule and high molecular polymer is 0.3～0.4: 9.7～9.6; Wherein, described urea is granular urea, and described compound fertilizer is the compound fertilizer of spray granulating type; Described high molecular weight water soluble polymer is made by the component of following weight proportion: Mierocrystalline cellulose: Sumstar 190: polyvinyl alcohol: polyurethane prepolymer: Resins, epoxy E44: epoxy curing agent T593: the linking agent N hydroxymethyl acrylamide: emulsifier tween 80: initiator potassium persulfate: deionized water is 22～35: 1～2: 4～8: 5～8: 6～18: 2～3: 1～2: 0.10～0.15: 0.001～0.002: 35～51.
Preferred 1.6～the 3.5mm of the median size of described urea or compound fertilizer.
Preferably, described Mierocrystalline cellulose is two kinds or three kinds in Walocel MT 20.000PV, soluble cotton, the carboxymethyl cellulose, and the mixed weight ratio between it is 1: 1 or 1: 1: 1.
Preferably, described polyvinyl alcohol mean polymerisation degree is 550～1800, and molecular weight is 27000～89000 dalton.
Further preferred, described polyvinyl alcohol mean polymerisation degree is 1700～1800, and molecular weight is 84000～89000 dalton.
Described polyurethane prepolymer is the dual-component aqueous polyurethane prepolymer, can be buied by market, as the polyurethane prepolymer of Zibo China day chemical industry company limited product; Also can make as follows:
With relative molecular weight is that 1000 210 polyethers, 98～112 weight parts are packed in the there-necked flask of 250ml, 100 ℃ of vacuum outgas 2h, loading onto fluid-tight stirs, the prolong that has drying tube, thermometer, dimethylol propionic acid 121～140 weight parts that adding was ground and the N-N-methyl-2-2-pyrrolidone N-solvent of 134～150 weight parts, after stirring, add tolylene diisocyanate (TDI, 65/35, technical grade) 278 weight parts, 80 ℃ of reaction 3h judge reaction end with the normal butane volumetry, add 50 weight part triethylamines and 80 weight part acetone solvents then in above-mentioned prepolymer, 50 ℃ of reaction 40min, cooling.The deionized water that adds 1034 weight parts in above-mentioned neutralized reaction product simultaneously with 8000～12000r/mim rotating speed violent stirring 30min, promptly gets polyurethane prepolymer.
The basic preparation method of biological biodegradable self-control slow-releasing fertilizer of the present invention is: adopt the latex ipn technology that materials such as Mierocrystalline cellulose, starch, polyvinyl alcohol, polyurethane prepolymer, Resins, epoxy (E44), epoxy curing agent, emulsifying agent is synthetic with the high molecular weight water soluble polymer emulsion of water as dispersion medium earlier, then it is uniformly sprayed urea or compound fertilizer granule surface, after heating, solidifying, make biological biodegradable self-control slow-releasing fertilizer.
The preparation method of biological biodegradable self-control slow-releasing fertilizer of the present invention, concrete steps are as follows:
(1) preparation of high molecular weight water soluble polymer coated fertilizer emulsion: each component that takes by weighing described high molecular weight water soluble polymer with above-mentioned weight proportion respectively, then Mierocrystalline cellulose, Sumstar 190, polyvinyl alcohol, polyurethane prepolymer, Resins, epoxy E44, epoxy curing agent T593, N hydroxymethyl acrylamide are poured in the container that fills tween 80 and deionized water, under 20 ℃～27 ℃, with 5000～12000r/mim rotating speed cutting emulsification, 0.4～0.6h, get emulsion; With the deionized water of reserving Potassium Persulphate is made into the solution that concentration is 1mg/ml simultaneously, as initiator; Transfer ph value of emulsion to 7.5; Getting the emulsion of 1/10 volume and the initiator solution of 1/5 volume adds in the four-hole bottle or in the reactor, feed nitrogen, be warming up to 75 ℃～80 ℃, behind the 20min, drip the above-mentioned remaining emulsion that is mixed with the residue initiator solution, drip in the 2h, continue reaction 3～3.5h afterwards, being able to Mierocrystalline cellulose is the high molecular weight water soluble polymer coated fertilizer emulsion of main ingredient;
(2) urea or compound fertilizer granule coating and curing: urea or compound fertilizer are poured in the heat drying rotary drum, rolled and be preheated to 60 ℃～80 ℃; Rotary drum is with 45～60 rev/mins of rollings then, and the high molecular weight water soluble polymer coated fertilizer emulsion that step (1) is made is delivered to two-fluid spray nozzle or jet head sets through pump or pressure-bearing form simultaneously, and with on the fertiliser granulates that sprays to after its atomizing in the rotary drum; Fertilizer in the rotary drum is heated to 80 ℃～100 ℃ simultaneously, is heating and curing, stop to continue to be heating and curing 5 minutes after the spraying, the lactous coated fertilizer is a completely solidified;
(3) sieve and the secondary coating: the coated fertilizer particle that step (2) obtains is crossed the 5mm sieve while hot; Simultaneously that the fertiliser granulates of particle diameter＞5mm is conventional broken, merge with the fertiliser granulates of particle diameter≤5mm, the spray procedure of common repeating step (2) is carried out the secondary coating, and lactous coated fertilizer consumption is to be principle at 0.3～0.4: 9.7～9.6 with the weight ratio of urea or compound fertilizer granule and high molecular polymer;
(4) screening and packing: the fertiliser granulates behind step (3) the secondary coating is crossed the 5mm sieve, the fertiliser granulates of particle diameter≤5mm behind the collection screen, cooling back packing is stored standby; Simultaneously that the fertiliser granulates of particle diameter＞5mm is conventional broken, with the fertiliser granulates merging of the described particle diameter≤5mm of step (3), carry out coating once more.
Among the preparation method of above-mentioned biological biodegradable self-control slow-releasing fertilizer: each component of the described high molecular weight water soluble polymer of step (1) is take weight proportion as cellulose: oxidized starch: polyvinyl alcohol: polyurethane prepolymer: epoxy resin E44: epoxy curing agent T593: crosslinking agent N hydroxymethyl acrylamide: emulsifier tween 80: initiator potassium persulfate: deionized water is 30～35: 1～2: 4～6: 5～8: 6～9: 2～3: 1～2: 0.10～0.15: 0.001～0.002: 35～51 when taking by weighing; 25 ℃ of of of conditions of Gained release and release control fertilizer product is under, and controlled nutrient-lapsed time is 60 ± 1 days.
Among the preparation method of above-mentioned biological biodegradable self-control slow-releasing fertilizer: each component of the described high molecular weight water soluble polymer of step (1) is take weight proportion as cellulose: oxidized starch: polyvinyl alcohol: polyurethane prepolymer: epoxy resin E44: epoxy curing agent T593: crosslinking agent N hydroxymethyl acrylamide: emulsifier tween 80: initiator potassium persulfate: deionized water is 25～29: 1～2: 4～6: 5～8: 12～15: 2～3: 1～2: 0.10～0.15: 0.001～0.002: 35～50 when taking by weighing; 25 ℃ of of of conditions of Gained release and release control fertilizer product is under, and controlled nutrient-lapsed time is 90 ± 2 days.
Among the preparation method of above-mentioned biological biodegradable self-control slow-releasing fertilizer: each component of the described high molecular weight water soluble polymer of step (1) is take weight proportion as cellulose: oxidized starch: polyvinyl alcohol: polyurethane prepolymer: epoxy resin E44: epoxy curing agent T593: crosslinking agent N hydroxymethyl acrylamide: emulsifier tween 80: initiator potassium persulfate: deionized water is 22～24: 1～2: 5～8: 5～8: 14～18: 2～3: 1～2: 0.10～0.15: 0.001～0.002: 35～50 when taking by weighing; 25 ℃ of of of conditions of Gained release and release control fertilizer product is under, and controlled nutrient-lapsed time is 120 ± 3 days.
Among the preparation method of above-mentioned biological biodegradable self-control slow-releasing fertilizer:
Each component of the described high molecular weight water soluble polymer of step (1) preferably under 25 ℃, with 8000r/mim rotating speed cutting emulsification 0.5h, gets emulsion.
The described urea of step (2) is granular urea, and described compound fertilizer is the compound fertilizer of spray granulating type; Preferred 1.6～the 2.8mm of the median size of described urea or compound fertilizer.
The present invention prepares coated fertilizer by selecting biodegradable material for use, thereby has guaranteed the degradability of fertilizer.Among the preparation method of the present invention, at first water is made into emulsion as dispersion medium with Mierocrystalline cellulose and carries out crosslinked, then with crosslinked Mierocrystalline cellulose emulsion as " seed ", add monomer (starch, polyvinyl alcohol, polyurethane prepolymer, Resins, epoxy, linking agent, solidifying agent and initiator) again, make monomer carry out polymerization and crosslinked, make the latex interpenetrating net polymer on " seed " latex granule surface.This polymkeric substance is sprayed to the surface of fertiliser granulates, and after being heating and curing, promptly having formed with the Mierocrystalline cellulose is skeleton, and the hypotonic material of superpolymer is the hydrophobic membrane of weighting material.Many micropores are arranged on this hydrophobic membrane, water in the soil enters fertilizer inside with the gasiform form by the micropore on the film, make the fertile wicking swelling that wets, the nutrient in the fertilizer will be under huge inside and outside concentration gradient by film on micropore enter in the soil, realize the effect of automatic control slow release fertilizer.
The size in the quantity of micropore and aperture becomes the controlled factor that nutrient discharges speed on the film, and the size in the quantity of micropore and aperture is subjected to the influence of mould material consumption and component, the present invention has effectively realized the controllability that nutrient discharges by regulating the consumption and the component of mould material.
Advantage of the present invention is, with the Mierocrystalline cellulose is that main ingredient is come the composite envelope material, guaranteed the degradability of coated fertilizer, the application of latex ipn technology, the controlled release properties and the nitrogen utilization efficiency of fertilizer self have been improved greatly, reduced the consumption of coated fertilizer, reduced cost, thereby the applicable crops scope is further enlarged.In addition, the present invention has also that preparation technology is simple, and solvent is nontoxic, be fit to fast, the advantage of scale operation, and single-dose application just can be satisfied the needs of crop whole growing to nutrient.
The made biological biodegradable self-control slow-releasing fertilizer of the present invention has good controlled release properties and degradation property and higher nitrogen utilization efficiency, comes effect of the present invention is described further with the data in table 1 and the table 2 below.
Table 1 polymkeric substance is formed the influence to mould material water-absorbent and water vapour permeability
Annotate: control 60 is meant can 60 days coated fertilizer of controlled release, other mould material and the like.
Table 2 polymkeric substance is formed the influence to nitrogen utilization efficiency and degradation rate
Annotate: test materials is a wheat, and the time of calculating the mould material degradation rate is 360 days.
In a word, the present invention has overcome the superpolymer coating because not biodegradable " white pollution " problem of bringing because mould material has mainly adopted biodegradable; In the preparation process of mould material, adopt the latex ipn technology, thereby improved the controlled release properties of fertilizer, reduced the mould material cost.Nutrient slowly discharges by the crop regulation of fertilizer requirement, and nitrogen utilization efficiency improves 20%～35%, and applied once can satisfy the crop needs in the time of infertility, and joint is fertile, and the saving of labor reduces environmental pollution, and application prospect is very wide.
Description of drawings
Fig. 1 is preparation technology's schema of biological biodegradable self-control slow-releasing fertilizer.
Embodiment
The present invention will be further described below in conjunction with embodiment, but be not limited only to this.
Raw materials used being described as follows among the embodiment:
Granular urea, Shandong Jin Funongnongization company limited, Shandong Zhucheng Liangfeng Chemical Co., Ltd. sell,
Mierocrystalline cellulose (Walocel MT 20.000PV, soluble cotton, carboxymethyl cellulose), sell the Zhongxiang Jinhanjiang Cellulose Co.,Ltd, Hubei,
Sumstar 190, Dezhou light moral starch chemical industry company limited sells,
Polyvinyl alcohol, lake, last Haikang chemical industry company limited sells,
Polyurethane prepolymer, Zibo China day chemical industry company limited sells,
Resins, epoxy E44, Shenzhen Jitian's chemical industry company limited sells,
Epoxy curing agent T593, Zhejiang Pingyang County stand Xiang tackiness agent factory, Shanghai should be good industry and trade company limited produce,
The linking agent N hydroxymethyl acrylamide, gloomy chemical industry company limited sells in Zibo.
Embodiment 1:
(1) preparation of high molecular weight water soluble polymer coated fertilizer emulsion: with the weight proportion is Mierocrystalline cellulose: Sumstar 190: polyvinyl alcohol: polyurethane prepolymer: Resins, epoxy E44: epoxy curing agent T593: linking agent N hydroxymethyl acrylamide: emulsifier tween 80: initiator potassium persulfate: deionized water is 35: 2: 6: 8: 9: 3: 2: 0.15: 0.002: 51 (units: restrain) take by weighing each component of described high molecular weight water soluble polymer respectively, then with Mierocrystalline cellulose (Walocel MT 20.000PV: soluble cotton: the mixed weight ratio between the carboxymethyl cellulose is 1: 1: 1), Sumstar 190, (mean polymerisation degree is 1700～1800 to polyvinyl alcohol, molecular weight is 84000～89000 dalton), polyurethane prepolymer, Resins, epoxy E44, epoxy curing agent T593, N hydroxymethyl acrylamide is poured in the container that fills tween 80 and deionized water, under 25 ℃, with 8000r/mim rotating speed cutting emulsification 0.5h, get emulsion; With the deionized water of reserving Potassium Persulphate is made into the solution that concentration is 1mg/ml simultaneously, as initiator; Transfer ph value of emulsion to 7.5; Getting the emulsion of 1/10 volume and the initiator solution of 1/5 volume adds in the reactor, feed nitrogen, be warming up to 80 ℃, behind the 20min, drip the above-mentioned remaining emulsion that is mixed with the residue initiator solution, drip in the 2h, continue reaction 3.5h afterwards, being able to Mierocrystalline cellulose is the high molecular weight water soluble polymer coated fertilizer emulsion of main ingredient;
(2) urea or compound fertilizer granule coating and curing: (median size 2～3mm) is poured in the heat drying rotary drum, rolls and is preheated to 60 ℃～80 ℃ with urea or compound fertilizer; Rotary drum is with 55 rev/mins of rollings then, and the high molecular weight water soluble polymer coated fertilizer emulsion that step (1) is made is delivered to two-fluid spray nozzle or jet head sets through pump or pressure-bearing form simultaneously, and with on the fertiliser granulates that sprays to after its atomizing in the rotary drum; Fertilizer in the rotary drum is heated to 90 ℃～100 ℃ simultaneously, is heating and curing, stop to continue to be heating and curing 5 minutes after the spraying, the lactous coated fertilizer is a completely solidified;
(3) sieve and the secondary coating: the coated fertilizer particle that step (2) obtains is crossed the 5mm sieve while hot; Simultaneously that the fertiliser granulates of particle diameter＞5mm is conventional broken, merge with the fertiliser granulates of particle diameter≤5mm, the spray procedure of common repeating step (2) is carried out the secondary coating, and lactous coated fertilizer consumption is to be principle at 0.3～0.4: 9.7～9.6 with the weight ratio of urea or compound fertilizer granule and high molecular polymer;
(4) screening and packing: the fertiliser granulates behind step (3) the secondary coating is crossed the 5mm sieve, the fertiliser granulates of particle diameter≤5mm behind the collection screen, cooling back packing is stored standby; Simultaneously that the fertiliser granulates of particle diameter＞5mm is conventional broken, with the fertiliser granulates merging of the described particle diameter≤5mm of step (3), carry out coating once more.
Gained release and release control fertilizer product is under 25 ℃ of conditions, and controlled nutrient discharges and is about 60 days.
Embodiment 2:
(1) preparation of high molecular weight water soluble polymer coated fertilizer emulsion: with the weight proportion is Mierocrystalline cellulose: Sumstar 190: polyvinyl alcohol: polyurethane prepolymer: Resins, epoxy E44: epoxy curing agent T593: linking agent N hydroxymethyl acrylamide: emulsifier tween 80: initiator potassium persulfate: deionized water is 28: 1.5: 5: 6: 14: 2.5: 1.5: 0.12: 0.0015: 50 (units: restrain) take by weighing each component of described high molecular weight water soluble polymer respectively, then with Mierocrystalline cellulose (Walocel MT 20.000PV: the mixed weight ratio between the carboxymethyl cellulose is 1: 1), Sumstar 190, (mean polymerisation degree is 550～650 to polyvinyl alcohol, molecular weight is 27000～32000 dalton), polyurethane prepolymer, Resins, epoxy E44, epoxy curing agent T593, N hydroxymethyl acrylamide is poured in the container that fills tween 80 and deionized water, under 24 ℃, with 9000r/mim rotating speed cutting emulsification 0.6h, get emulsion; With the deionized water of reserving Potassium Persulphate is made into the solution that concentration is 1mg/ml simultaneously, as initiator; Transfer ph value of emulsion to 7.5; Getting the emulsion of 1/10 volume and the initiator solution of 1/5 volume adds in the four-hole bottle or in the reactor, feed nitrogen, be warming up to 80 ℃, behind the 20min, drip the above-mentioned remaining emulsion that is mixed with the residue initiator solution, drip in the 2h, continue reaction 3.5h afterwards, being able to Mierocrystalline cellulose is the high molecular weight water soluble polymer coated fertilizer emulsion of main ingredient;
(2) urea or compound fertilizer granule coating and curing: (median size 3～3.5mm) is poured in the heat drying rotary drum, rolls and is preheated to 70 ℃～80 ℃ with urea or compound fertilizer; Rotary drum is with 50 rev/mins of rollings then, and the high molecular weight water soluble polymer coated fertilizer emulsion that step (1) is made is delivered to two-fluid spray nozzle or jet head sets through pump or pressure-bearing form simultaneously, and with on the fertiliser granulates that sprays to after its atomizing in the rotary drum; Fertilizer in the rotary drum is heated to 90 ℃～100 ℃ simultaneously, is heating and curing, stop to continue to be heating and curing 5 minutes after the spraying, the lactous coated fertilizer is a completely solidified;
(3) sieve and the secondary coating: the coated fertilizer particle that step (2) obtains is crossed the 5mm sieve while hot; Simultaneously that the fertiliser granulates of particle diameter＞5mm is conventional broken, merge with the fertiliser granulates of particle diameter≤5mm, the spray procedure of common repeating step (2) is carried out the secondary coating, and lactous coated fertilizer consumption is to be principle at 0.3～0.4: 9.7～9.6 with the weight ratio of urea or compound fertilizer granule and high molecular polymer;
(4) screening and packing: the fertiliser granulates behind step (3) the secondary coating is crossed the 5mm sieve, the fertiliser granulates of particle diameter≤5mm behind the collection screen, cooling back packing is stored standby; Simultaneously that the fertiliser granulates of particle diameter＞5mm is conventional broken, with the fertiliser granulates merging of the described particle diameter≤5mm of step (3), carry out coating once more.
Gained release and release control fertilizer product is under 25 ℃ of conditions, and controlled nutrient discharges and is about 90 days.
Embodiment 3:
With 75g Walocel MT 20.000PV, 75g soluble cotton, 5g Sumstar 190,20g polyvinyl alcohol, 25g polyurethane prepolymer, 30g Resins, epoxy (E44), 10g T593,5gN-n-methylolacrylamide are poured in the beaker of the 1000ml that fills 0.5g tween 80 and 250ml deionized water, the 0.5h of high speed shear emulsification at room temperature, use the 5ml deionized water with 0.005g Potassium Persulphate wiring solution-forming, as initiator simultaneously.Regulate ph value of emulsion to 7.5 with pH value conditioning agent, 1/10 and 1/5 initiator solution of getting above-mentioned emulsion adds in the four-hole bottle or in the reactor, logical nitrogen, be warming up to 75 ℃, behind the 20min, drip residue emulsion (being mixed with 4/5 initiator solution), drip in the 2h, continue to send out and answer 3h, finish reaction, obtaining with the Mierocrystalline cellulose is the water soluble polymer coated fertilizer emulsion of main ingredient.
(median size 1.6～2.8mm) adds in the rotary drums with urea or compound fertilizer granule, be preheating to 60 ℃～70 ℃, with pump or pressure-bearing form the coated fertilizer emulsion is delivered to two-fluid spray nozzle (or jet head sets) simultaneously, with the fertiliser granulates surface that sprays to after its atomizing in the rotary drum, fertilizer in the rotary drum is heated between 90 ℃～100 ℃ simultaneously, rotating speed transfers to 60 rev/mins, stop to spray about 5 minutes after, the lactous coated fertilizer is promptly curable.
Cross the 5mm sieve while hot, the fertiliser granulates that particle diameter＞5mm is inter-adhesive carries out fragmentation, the secondary coating is carried out together with the fertiliser granulates of particle diameter≤5mm in broken back, and lactous coated fertilizer consumption is to be principle at 0.3～0.4: 9.7～9.6 with the weight ratio of urea or compound fertilizer granule and high molecular polymer.
Cross 5mm sieve, the fertiliser granulates of particle diameter≤5mm behind the secondary coating is cooled off the back packing, stores.
Gained release and release control fertilizer product controlled nutrient under 25 ℃ of conditions discharges and is about 60 days.
Embodiment 4:
With 62.5g Walocel MT 20.000PV, 62.5g soluble cotton, 5g Sumstar 190,20g polyvinyl alcohol, 25g polyurethane prepolymer, 60g Resins, epoxy (E44), 10g T593,5gN-n-methylolacrylamide are poured in the beaker of the 1000ml that fills 0.5g tween 80 and 245ml deionized water, the 0.5h of high speed shear emulsification at room temperature, use the 5ml deionized water with 0.005g Potassium Persulphate wiring solution-forming, as initiator simultaneously.Regulate ph value of emulsion to 7.5 with pH value conditioning agent, 1/10 and 1/5 initiator solution of getting above-mentioned emulsion adds in the four-hole bottle or in the reactor, logical nitrogen, be warming up to 75 ℃, behind the 20min, drip residue emulsion (being mixed with 4/5 initiator solution), drip in the 2h, continue to send out and answer 3h, finish reaction, obtaining with the Mierocrystalline cellulose is the water soluble polymer coated fertilizer emulsion of main ingredient.
(median size 1.6～2.8mm) adds in the rotary drums with urea or compound fertilizer granule, be preheating to 70 ℃～80 ℃, with pump or pressure-bearing form the coated fertilizer emulsion is delivered to two-fluid spray nozzle (or jet head sets) simultaneously, on the fertiliser granulates that sprays to after its atomizing in the rotary drum, fertilizer in the rotary drum is heated between 80 ℃～90 ℃ simultaneously, rotating speed transfers to 60 rev/mins, stop to spray about 5 minutes after, the lactous coated fertilizer is promptly curable.
Cross the 5mm sieve while hot, the fertiliser granulates that particle diameter＞5mm is inter-adhesive carries out fragmentation, the secondary coating is carried out together with the fertiliser granulates of particle diameter≤5mm in broken back, and lactous coated fertilizer consumption is to be principle at 0.3～0.4: 9.7～9.6 with the weight ratio of urea or compound fertilizer granule and high molecular polymer.
Cross 5mm sieve, the fertiliser granulates of particle diameter≤5mm behind the secondary coating is cooled off the back packing, stores.
Gained release and release control fertilizer product controlled nutrient under 25 ℃ of conditions discharges and is about 90 days.
Embodiment 5:
With 40g Walocel MT 20.000PV, 40g soluble cotton, 40g carboxymethyl cellulose, 5g Sumstar 190,25g polyvinyl alcohol, 25g polyurethane prepolymer, 80g Resins, epoxy (E44), 10g T593,5gN-n-methylolacrylamide are poured in the beaker of the 1000ml that fills 0.5g tween 80 and 225ml deionized water, the 0.5h of high speed shear emulsification at room temperature, use the 5ml deionized water with 0.005g Potassium Persulphate wiring solution-forming, as initiator simultaneously.Regulate ph value of emulsion to 7.5 with pH value conditioning agent, 1/10 and 1/5 initiator solution of getting above-mentioned emulsion adds in the four-hole bottle or in the reactor, logical nitrogen, be warming up to 75 ℃, behind the 20min, drip residue emulsion (being mixed with 4/5 initiator solution), drip in the 2h, continue to send out and answer 3h, finish reaction, obtaining with the Mierocrystalline cellulose is the water soluble polymer coated fertilizer emulsion of main ingredient.
(median size 2.6～3mm) adds in the rotary drums with urea or compound fertilizer granule, be preheating to 80 ℃, with pump or pressure-bearing form the coated fertilizer emulsion is delivered to two-fluid spray nozzle (or jet head sets) simultaneously, on the fertiliser granulates that sprays to after its atomizing in the rotary drum, simultaneously the fertilizer in the rotary drum is heated between 100 ℃, rotating speed transfers to 60 rev/mins, and after about 5 minutes, the lactous coated fertilizer is promptly curable.
Cross the 5mm sieve while hot, the fertiliser granulates that particle diameter＞5mm is inter-adhesive carries out fragmentation, the secondary coating is carried out together with the fertiliser granulates of particle diameter≤5mm in broken back, and lactous coated fertilizer consumption is to be principle at 0.3～0.4: 9.7～9.6 with the weight ratio of urea or compound fertilizer granule and high molecular polymer.
Cross 5mm sieve, the fertiliser granulates of particle diameter≤5mm behind the secondary coating is cooled off the back packing, stores.
Gained release and release control fertilizer product controlled nutrient under 25 ℃ of conditions discharges and is about 120 days.
Claims (10)
1. biological biodegradable self-control slow-releasing fertilizer, controlled release layer at urea or the even spraying in compound fertilizer granule surface one deck high molecular weight water soluble polymer is made, and it is characterized in that: the weight ratio of described urea or compound fertilizer granule and high molecular polymer is 0.3～0.4: 9.7～9.6; Described high molecular weight water soluble polymer is made by the component of following weight proportion: Mierocrystalline cellulose: Sumstar 190: polyvinyl alcohol: polyurethane prepolymer: Resins, epoxy E44: epoxy curing agent T593: the linking agent N hydroxymethyl acrylamide: emulsifier tween 80: initiator potassium persulfate: deionized water is 22～35: 1～2: 4～8: 5～8: 6～18: 2～3: 1～2: 0.10～0.15: 0.001～0.002: 35～51.
2. biological biodegradable self-control slow-releasing fertilizer according to claim 1 is characterized in that: described Mierocrystalline cellulose is two kinds or three kinds in Walocel MT 20.000PV, soluble cotton, the carboxymethyl cellulose, and the mixed weight ratio between it is 1: 1 or 1: 1: 1.
3. biological biodegradable self-control slow-releasing fertilizer according to claim 1 is characterized in that: described polyvinyl alcohol mean polymerisation degree is 550～1800, and molecular weight is 27000～89000 dalton.
4. biological biodegradable self-control slow-releasing fertilizer according to claim 3 is characterized in that: described polyvinyl alcohol mean polymerisation degree is 1700～1800, and molecular weight is 84000～89000 dalton.
5. biological biodegradable self-control slow-releasing fertilizer according to claim 1, it is characterized in that: described polyurethane prepolymer is the dual-component aqueous polyurethane prepolymer, made by following method: with relative molecular weight is that 1000 210 polyethers, 98～112 weight parts are packed in the there-necked flask of 250ml, 100 ℃ of vacuum outgas 2h, loading onto fluid-tight stirs, the prolong that has drying tube, thermometer, dimethylol propionic acid 121～140 weight parts that adding was ground and the N-N-methyl-2-2-pyrrolidone N-solvent of 134～150 weight parts, after stirring, add tolylene diisocyanate 278 weight parts, 80 ℃ of reaction 3h, judge reaction end with the normal butane volumetry, in above-mentioned prepolymer, add 50 weight part triethylamines and 80 weight part acetone solvents then, 50 ℃ of reaction 40min, cooling, the deionized water that adds 1034 weight parts in above-mentioned neutralized reaction product stirs 30min with 8000～12000r/mim rotating speed simultaneously, promptly gets polyurethane prepolymer.
6. the preparation method of the described biological biodegradable self-control slow-releasing fertilizer of claim 1, realized by following steps:
(1) preparation of high molecular weight water soluble polymer coated fertilizer emulsion: each component that takes by weighing described high molecular weight water soluble polymer with the described weight proportion of claim 1 respectively, then Mierocrystalline cellulose, Sumstar 190, polyvinyl alcohol, polyurethane prepolymer, Resins, epoxy E44, epoxy curing agent T593, N hydroxymethyl acrylamide are poured in the container that fills tween 80 and deionized water, under 20 ℃～27 ℃, with 5000～12000r/mim rotating speed cutting emulsification, 0.4～0.6h, get emulsion; With the deionized water of reserving Potassium Persulphate is made into the solution that concentration is 1mg/ml simultaneously, as initiator; Transfer ph value of emulsion to 7.5; Getting the emulsion of 1/10 volume and the initiator solution of 1/5 volume adds in the four-hole bottle or in the reactor, feed nitrogen, be warming up to 75 ℃～80 ℃, behind the 20min, drip the above-mentioned remaining emulsion that is mixed with the residue initiator solution, drip in the 2h, continue reaction 3～3.5h afterwards, being able to Mierocrystalline cellulose is the high molecular weight water soluble polymer coated fertilizer emulsion of main ingredient;
(2) urea or compound fertilizer granule coating and curing: urea or compound fertilizer are poured in the heat drying rotary drum, rolled and be preheated to 60 ℃～80 ℃; Rotary drum is with 45～60 rev/mins of rollings then, and the high molecular weight water soluble polymer coated fertilizer emulsion that step (1) is made is delivered to two-fluid spray nozzle or jet head sets through pump or pressure-bearing form simultaneously, and with on the fertiliser granulates that sprays to after its atomizing in the rotary drum; Fertilizer in the rotary drum is heated to 80 ℃～100 ℃ simultaneously, is heating and curing, stop to continue to be heating and curing 5 minutes after the spraying, the lactous coated fertilizer is a completely solidified;
(3) sieve and the secondary coating: the coated fertilizer particle that step (2) obtains is crossed the 5mm sieve while hot; Simultaneously that the fertiliser granulates of particle diameter＞5mm is conventional broken, merge with the fertiliser granulates of particle diameter≤5mm, the spray procedure of common repeating step (2) is carried out the secondary coating, and lactous coated fertilizer consumption is to be principle at 0.3～0.4: 9.7～9.6 with the weight ratio of urea or compound fertilizer granule and high molecular polymer;
(4) screening and packing: the fertiliser granulates behind step (3) the secondary coating is crossed the 5mm sieve, the fertiliser granulates of collection cut size≤5mm, cooling back packing is stored standby; Simultaneously that the fertiliser granulates of particle diameter＞5mm is conventional broken, with the fertiliser granulates merging of the described particle diameter≤5mm of step (3), carry out coating once more.
7. according to the preparation method of the described biological biodegradable self-control slow-releasing fertilizer of claim 6, it is characterized in that: each component of the described high molecular weight water soluble polymer of step (1) is Mierocrystalline cellulose with the weight proportion: Sumstar 190: polyvinyl alcohol: polyurethane prepolymer: Resins, epoxy E44: epoxy curing agent T593: linking agent N hydroxymethyl acrylamide: emulsifier tween 80: initiator potassium persulfate: deionized water is 30～35: 1～2: 4～6: 5～8: 6～9: 2～3: 1～2: 0.10～0.15: 0.001～0.002: 35～51 when taking by weighing, gained release and release control fertilizer product is under 25 ℃ of conditions, and controlled nutrient time of releasing is 60 ± 1 days.
8. according to the preparation method of the described biological biodegradable self-control slow-releasing fertilizer of claim 6, it is characterized in that: each component of the described high molecular weight water soluble polymer of step (1) is Mierocrystalline cellulose with the weight proportion: Sumstar 190: polyvinyl alcohol: polyurethane prepolymer: Resins, epoxy E44: epoxy curing agent T593: linking agent N hydroxymethyl acrylamide: emulsifier tween 80: initiator potassium persulfate: deionized water is 25～29: 1～2: 4～6: 5～8: 12～15: 2～3: 1～2: 0.10～0.15: 0.001～0.002: 35～50 when taking by weighing, gained release and release control fertilizer product is under 25 ℃ of conditions, and controlled nutrient time of releasing is 90 ± 2 days.
9. according to the preparation method of the described biological biodegradable self-control slow-releasing fertilizer of claim 6, it is characterized in that: each component of the described high molecular weight water soluble polymer of step (1) is Mierocrystalline cellulose with the weight proportion: Sumstar 190: polyvinyl alcohol: polyurethane prepolymer: Resins, epoxy E44: epoxy curing agent T593: linking agent N hydroxymethyl acrylamide: emulsifier tween 80: initiator potassium persulfate: deionized water is 22～24: 1～2: 5～8: 5～8: 14～18: 2～3: 1～2: 0.10～0.15: 0.001～0.002: 35～50 when taking by weighing, gained release and release control fertilizer product is under 25 ℃ of conditions, and controlled nutrient time of releasing is 120 ± 3 days.
10. according to the preparation method of the described biological biodegradable self-control slow-releasing fertilizer of claim 6, it is characterized in that: each component of the described high molecular weight water soluble polymer of step (1) with 8000r/mim rotating speed cutting emulsification 0.5h, gets emulsion under 25 ℃; The described urea of step (2) is granular urea, and described compound fertilizer is the compound fertilizer of spray granulating type, and the median size of described urea or compound fertilizer is 1.6～2.8mm.
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