CN103819292B - A kind of solvent-free film-coated controlled release fertilizer and preparation method thereof - Google Patents
A kind of solvent-free film-coated controlled release fertilizer and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of solvent-free film-coated controlled release fertilizer and preparation method thereof.Described film-coated controlled release fertilizer is made up of fertiliser granulates and the coating layer be coated on outside described fertiliser granulates; The mass percentage of described fertiliser granulates is 93% ~ 97%, and the mass percentage of described coating layer is 3% ~ 7%; Described coating layer is obtained by the polymerization of polyisocyanates, polyester polyol and microcrystalline wax.2 kinds of polymkeric substance are successively sprayed application to particle surface by preparation method provided by the invention respectively, solve a shared pipeline, problem that nozzle and the blocking caused make coating interrupt, make the probability that particle adhesion occurs in equipment significantly reduce simultaneously, the stability of coating process is obviously strengthened.Solve the problem that coating speed and coating homogeneity can not be taken into account, complete being uniformly distributed of rete in fast filming process.
Description
Technical field
The present invention relates to a kind of solvent-free film-coated controlled release fertilizer and preparation method thereof.
Background technology
Day by day to reduce in arable land and under the ever-increasing pressure of urban population, from now on quite over a long time in, use chemical fertilizer and be still the agriculture important measures of stablizing sustainable development of China.But along with the increase of Term Fertilization, occurred that fertilizer amount significantly increases and situation that crop yield fluctuates, the nitrogen phosphorus of a large amount of loss simultaneously causes the problems such as serious environmental pollution.These have become one of fundamental issue of restriction China's grain security and environmental safety.For this reason, central authorities' No. 1 file advances the important force of sustained-controll-release fertiliser as agricultural science and technology in continuous 3 years, since including slow-release or control-release fertilizer in Preferential Developmental Industry first from 2011, within 2012, require to put forth effort to break through agrotechnique bottleneck, great practical technique achievement is obtained in novel fertile medicine etc., especially within 2013, define the grant programme for slow-release or control-release fertilizer first, make the promotion and application of slow-release or control-release fertilizer obtain unprecedented opportunity to develop and strong policy support.
Over nearly 10 years, there is negative growth in the common fertilizer amount in the world, but the consumption of slow, release and release control fertilizer every year with about 4 ~ 5% speed increment, the ratio accounting for world Fertilizer total quantity consumed by nineteen ninety-five 0.12% rise to 2006 0.45%.Since 2005, the application of sustained-controll-release fertiliser on field crop develops rapidly, and China, slow-release or control-release fertilizer production capacity that the is Canadian and U.S. also increase rapidly.China's sustained-controll-release fertiliser industry has developed rapidly since the nineties, and the research of sulphur coated urea, resin coated controlled release fertilizer has developed into a higher height, and Technology reaches its maturity, and nutrient controlled release properties is good.Domestic existing more than 30 families of scientific research institution being engaged in slow-release or control-release fertilizer research at present, existing more than 70 families of unit being engaged in industrialization development and applying, yearly capacity is more than 1,000,000 tons, and sustained-controll-release fertiliser has become the important directions of China's fertilizer industry development.
China obtains some progress in the research and extension of slow, release and release control fertilizer, also there are problems simultaneously.First domestic slow, release and release control fertilizer price compared with conventional fertilizers is higher; Next be delay, release and release control fertilizer application is slow, lack slowly/controlled releasing fertilizer application technique support system, fertilizer application evaluation test lacks, with sustained-controll-release fertiliser research and develop coordinate Special experimental room, test base and the relative incomplete problem of Applied D emonstration popularization system construction.The slow-release or control-release fertilizer of research and development high-efficiency environment friendly, no matter economizing on resources, realize agriculture production and Ecological harmony develops, cost-saving synergistic and energy-saving and emission-reduction, equal tool is of great significance.China's nitrogenous fertilizer excessive is used with consequent environmental problem very urgent, and the slow controlled release of nitrogenous fertilizer will become the Main Means addressed this problem future.Domestic and international Controlled Release Fertilizer development is just towards the future development of low cost, high-environmental.Polymer coated fertilizer is field with fastest developing speed in sustained-controll-release fertiliser in recent years, and typical technology and product mainly contain following several in the world:
1) Japanese Chisso company developing comparatively early take polyolefin resin as the Controlled Release Fertilizer of coated fertilizer, adopts organic solvent to be dissolved by the material at high temperature such as polyethylene, polypropylene, is coated on the fertiliser granulates in coating tower by spraying plant, simultaneously recycling design.Main products has with the coated carbamide of meister name with the coated compound fertilizer of nutricote trade(brand)name.
2) Dutch Xi Le company (Sierra Europe B.V) is with cyclopentadiene and glycerol resin copolymer for coated fertilizer, in intermittent type coating cylinder, carry out multilayer coating to dissolved fertilizer core.During spray solution in succession, dry desolvation and solvent recuperation can be carried out simultaneously.Coating quantity is between 10%-20%, and its typical products is Osmocote series coated compound fertilizer.
3) film-coating technique of Haifa, Israel company (Haifa Chemical Ltd.) can be grouped into this class of reaction film forming, but non-polymer coating.Heated on rotating disk by granulated fertilizer, use lipid acid and metal hydroxides (as hard fatty acids and calcium hydroxide) process, both react and generate fatty acid metal salt (as calcium stearate) coating layer simultaneously.Multilayer soap at particle surface generation reaction in－situ, last additional paraffin coating.Main products has coated compound fertilizer, coated carbamide and coating saltpetre, and its trade(brand)name is Multicote.
4) Canadian AGRIUM company adopts responding layer coating (Reactive Layer Coating) novel process to produce release and release control fertilizer.The main points of this Technology carry out coating by a series of home position polymerization reaction in succession on fertilizer core granule.First fertiliser granulates core uses diphenylmethanediisocyanate coating, and at coated polyhydric alcohol polymer more above, these two kinds of coating generation reaction in－situs generate polyurethane.The advantage of this technique can carry out coating in coating cylinder or mixing drum, and do not need solvent and relevant recovery system, and therefore its production cost is lower than other polymer capsule techniques existing.
Along with Agriculture Production Modes development, society is very strong to the demand of Controlled Release Fertilizer, and the high-yield and high-efficiency of field crop is produced in the urgent need to application Controlled Release Fertilizer.Although film-coating technique is progress constantly, but still be subject to certain limitation on cost and product type, the application on field crop can't obtain spread.Osmocote product coating rate as being mainly used on garden crop is high, solvent recuperation cost is needed to decline limited, the technical sophistication of Multicote, multilayer, intermittent type coating are also unfavorable for that production cost reduces, and Meister Controlled Release Fertilizer is also because solvent recuperation is affected in environmental protection and cost.The reaction film-forming products of AGRIUM company is most competitive power on cost, and not only dressing rate is low but also can continuous prodution, but also has technology specialty strong, and the deficiencies such as product release period is short, rete is easily torn, are further improved.
For the key issue in China's sustained-controll-release fertiliser industry development, aim at the Disciplinary Frontiers of fertilizer technology in the world, development of new coated fertilizer is current important developing direction.Reaction for forming films adapts to the new development trend of low cost, high-environmental, and it adopts particle surface in-situ polymerization principle, forms slim, tough and tensile rete, belongs to international research frontier.This technology no longer with an organic solvent, belongs to environmentally friendly film-coated controlled release fertilizer, has good promoter action to the international competitiveness improving China's release and release control fertilizer industry.Domestic Duo Jia unit is all stepping up to develop this technology, and the development for Controlled Release Fertilizer new generation product provides support by the maturation of this technology.
U.S. Serial No (US4711659, US4804403 and US4969947) film-coating technique reporting solvent-free reaction film forming comparatively early, isocyanic ester and urea granules surface reaction is utilized to form the first tunic, then the coated second layer forms polyurethane film, and spraying increases thicknesses of layers to control nutrients release repeatedly.In order to improve the release performance of polyurethane film, patent (US7682656 afterwards, US20070137274) scope of further clear and definite coating material, as adopted diphenylmethanediisocyanate (MDI), tolylene diisocyanate (TDI), with polyether glycol, polyester polyol reacting generating copolymer rete.The simultaneously relevant improvement of fertilizer production device is also constantly being carried out, and US Patent No. 7682656 reports the radius, rotating speed, the relation between particle speed that utilize coating rotary drum, reaches the object of adjustment Controlled Release Fertilizer release rate.
The principle of foregoing invention is all the reaction film-forming based on isocyanic ester and polyvalent alcohol, but because polymkeric substance and fertilizer surface also exist surface tension, while reduction polymer loading, the coating effect of particle will significantly decline, so some polymer film coating ratios can reach 8 ~ 12%, coating number of times reaches 16 ~ 20 times more than, and its cost also will increase greatly.Once coating quantity is reduced to 3 ~ 5%, the controlled-release effect of nutrient obviously weakens, and discharges and will not reach the standard of release and release control fertilizer.How by the improvement of equipment and the optimization of spraying, make a small amount of coating material can at short notice, or minority coating several times just can be evenly distributed in all particle surfaces, is the problem to be solved in the present invention.
Summary of the invention
The object of this invention is to provide a kind of solvent-free film-coated controlled release fertilizer and preparation method thereof, coating solution to spray mainly through a kind of pair of shower nozzle technology and equipment and obtain release and release control fertilizer of the present invention on the particle of motion by the present invention in proportion respectively, the invention solves coating liquid problem pockety on particle in solvent-free coating process.
The solvent-free film-coated controlled release fertilizer of one provided by the invention, it is made up of fertiliser granulates and the coating layer be coated on outside described fertiliser granulates;
The mass percentage of described fertiliser granulates is 93% ~ 97%, and the mass percentage of described coating layer is 3% ~ 7%;
Described coating layer is obtained by the polymerization of polyisocyanates, polyester polyol and microcrystalline wax.
Above-mentioned solvent-free film-coated controlled release fertilizer, the mass percentage of described fertiliser granulates specifically can be 93.5% ~ 94.0%, 93.5%, 93.7% or 94.0%, and the mass percentage of described coating layer specifically can be 6.0% ~ 6.5%, 6.0%, 6.3% or 6.5%.
Above-mentioned solvent-free film-coated controlled release fertilizer, the particle diameter of described fertiliser granulates can be 2mm ~ 4mm, can be granular urea or composite fertilizer;
Described isocyanic ester is ditan polyisocyanates (PAPI);
Described polyester polyol is phthalic anhydride polyester glycol, as auspicious company of polyester type SKR-T4(Cisco);
The fusing point of described microcrystalline wax can be 60 DEG C ~ 75 DEG C.
Above-mentioned solvent-free film-coated controlled release fertilizer, in described coating layer, the mass percentage of described isocyanic ester can be 37.9 ~ 45.3%;
The mass percentage of described polyester polyol can be 47.7 ~ 57.6%;
The mass percentage of described microcrystalline wax can be 4.42 ~ 8.54%.
Above-mentioned solvent-free film-coated controlled release fertilizer, also adds catalyzer and tensio-active agent in described polymerization process;
Described catalyzer can be stannous octoate or isocaprylic acid zinc;
Described tensio-active agent can be polysiloxane or polyester based modified polyorganosiloxane (D5500, De Qian company).
Above-mentioned solvent-free film-coated controlled release fertilizer, in described coating layer, the mass percentage of described isocyanic ester specifically can be 38.7% ~ 43.1%, 38.7%, 42.8% or 43.1%;
The mass percentage of described polyester polyol specifically can be 48.2% ~ 55.2%, 48.2%, 50.4% or 55.2%;
The mass percentage of described microcrystalline wax specifically can be 5.2% ~ 7.12%, 5.2%, 6.0% or 7.12%;
The mass percentage of described catalyzer specifically can be 0.42% ~ 0.99%, 0.66% ~ 0.86%, 0.66%, 0.72% or 0.86%;
The mass percentage of described tensio-active agent specifically can be 0.11% ~ 0.25%, 0.13% ~ 0.18%, 0.13%, 0.16% or 0.18%.
Above-mentioned solvent-free film-coated controlled release fertilizer, described coating layer is polymerized by described isocyanic ester, described polyester polyol and described microcrystalline wax and obtains under described catalyzer and described tensio-active agent existent condition, and described in described coating layer, the mass ratio of isocyanic ester, described polyester polyol, described microcrystalline wax, described catalyzer and described tensio-active agent is specific as follows states 1)-3) in any one:
1）43.1：48.2：7.12：0.76：0.16；
2）42.8：50.4：6.0：0.66：0.13；
3）38.7：55.2：5.2：0.72：0.18。
Invention further provides the preparation method of described film-coated controlled release fertilizer, comprise the steps:
(1) described fertiliser granulates is heated to 75 ~ 80 DEG C, and makes it move back and forth under drum wind action;
(2) be heated to 75 ~ 85 DEG C by described polyisocyanates or by the described polyisocyanates of described quality proportioning and the mixture of described tensio-active agent, and be coated on reciprocating described fertiliser granulates; Then by the mixture of described polyester polyol and described microcrystalline wax or the mixture of described polyester polyol, described microcrystalline wax and described catalyzer is heated to 85 ~ 95 DEG C, and be coated on reciprocating described fertiliser granulates, the described polyisocyanates then successively applied, described polyester polyol and described microcrystalline wax or described polyisocyanates, described polyester polyol, described microcrystalline wax, described tensio-active agent and described catalyzer carry out polyreaction on the surface of described fertiliser granulates, namely obtain described film-coated controlled release fertilizer.
Above-mentioned preparation method can carry out in two shower nozzle coating machine, and described pair of shower nozzle coating machine comprises a spouted bed, and the sidewall of described spouted bed is provided with opening for feed, and the bottom of described spouted bed connects a discharging pipeline; Be provided with high-pressure airless nozzle I and high-pressure airless nozzle II in described discharging pipeline, described high-pressure airless nozzle I and high-pressure airless nozzle II are connected with high-pressure pump II with the high-pressure pump I be located at outside described spouted bed respectively; The outlet of described high-pressure airless nozzle I and high-pressure airless nozzle II is all arranged towards the bottom of described spouted bed; Concrete steps are as follows:
Described fertiliser granulates, in described spouted bed, moves back and forth under drum wind action;
Described polyisocyanates or the described polyisocyanates of described quality proportioning and the mixture of described tensio-active agent are coated on reciprocating described fertiliser granulates by described high-pressure pump I and described high-pressure airless nozzle I;
The mixture of described polyester polyol and described microcrystalline wax or the mixture of described polyester polyol, described microcrystalline wax and described catalyzer is coated on reciprocating described fertiliser granulates by described high-pressure pump II and described high-pressure airless nozzle II.
In above-mentioned preparation method, coating solution is divided into 2 different paths by high-pressure airless nozzle I and high-pressure airless nozzle II to enter in spouted bed, avoids that two kinds of polymkeric substance react in same pipeline and the viscosity that causes increases, the dispersed problem being deteriorated and finally causing rete ununiformity to increase.The problems such as the pipeline that causes of the residual solidification of pipeline interpolymer is not smooth after shower nozzle blocking and coating complete can be reduced simultaneously.
In above-mentioned preparation method, described reciprocating shape can be ellipse, and the long axis vertical direction of described ellipse is arranged.
In above-mentioned preparation method, the spacing of described high-pressure airless nozzle I and described high-pressure airless nozzle II and described reciprocating lower-most point can be 10 ~ 15cm;
The pressure controlling described high-pressure pump I and described high-pressure pump II can be 3 ~ 5MPa.
In above-mentioned preparation method, step (2) repeats 3 times, and each interval time can be 2 ~ 3 minutes, thus according to building rete waterproof construction from inside to outside.
Tool of the present invention has the following advantages:
(1) 2 kinds of polymkeric substance are successively sprayed application to particle surface respectively, solve a shared pipeline, problem that nozzle and the blocking caused make coating interrupt, make the probability that particle adhesion occurs in equipment significantly reduce simultaneously, the stability of coating process is obviously strengthened.Solve the problem that coating speed and coating homogeneity can not be taken into account, complete being uniformly distributed of rete in fast filming process.
(2) by high-pressure airless hydrojet Controlling System, the dispersiveness of coating solution is significantly strengthened, significantly improve the uniform distribution of liquid on particle, the basis ensureing controlled release properties reduces coating consumption.
(3) build coating formula and the polymerization time of each spraying according to rete waterproof construction from inside to outside, complete production quality control by 3 coatings.
(4) the solvent-free recovery link of coating process, safety and environmental protection, rapid reaction film forming shortens the coating time, output in the unit time is obviously promoted, is beneficial to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the structural representation of the two shower nozzle coating machines used in the preparation method of film-coated controlled release fertilizer of the present invention.
In Fig. 1, each mark is as follows:
1 opening for feed, 2 spouted beds, 3 heating reservoir II, 4 high-pressure pump II, 5 high-pressure airless nozzle II, 6 high-pressure airless nozzle I, 7 high-pressure pump I, 8 heat reservoir I, 9 fly-ash separator, 10 discharging pipelines.
Heating the material placed in reservoir I in Fig. 1 is isocyanic ester (B) and tensio-active agent (E); The material placed in heating reservoir II is polyester polyol (A), microcrystalline wax (C) and catalyzer (D).
Embodiment
The experimental technique used in following embodiment if no special instructions, is ordinary method.
Material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
As shown in Figure 1, this pair of shower nozzle coating machine comprises a spouted bed 2 to the structural representation of the two shower nozzle coating machines used in following embodiment, and the sidewall of this spouted bed 2 is provided with opening for feed 1, and the bottom of this spouted bed 2 connects a discharging pipeline 10.The top of spouted bed 2 connects a fly-ash separator 9.High-pressure airless nozzle I 6 and high-pressure airless nozzle II 5 is provided with in this discharging pipeline 10, wherein, high-pressure airless nozzle I 6 is connected with the high-pressure pump I 7 be located at outside spouted bed 2, and high-pressure airless nozzle II 5 is connected with the high-pressure pump II 4 be located at outside spouted bed 2, for spraying coating solution provides power.The outlet of high-pressure airless nozzle I 6 and high-pressure airless nozzle II 5 is all arranged towards the bottom of spouted bed 2.
Modified polyorganosiloxane used in following embodiment for the model that De Qian company provides be the polysiloxane of D5500.
Embodiment 1, prepare film-coated controlled release fertilizer
The formula table of the present embodiment is as shown in table 1.
Table 1 coating polymer formulators table
(1) 2 ~ 3mm large grain urea 3kg is weighed for subsequent use.Weigh ditan polyisocyanates (PAPI, Beyer Co., Ltd) 31.2 grams, be placed in heating reservoir I 8 and be warming up to 75 DEG C, instillation tensio-active agent 0.11g, stirs and is incubated 75 DEG C; Weigh polyester polyol 33.8g simultaneously, be placed in another heating reservoir II 3, weigh Microcrystal paraffin (fusing point 70 DEG C, commercially available) 3.15g, put into heating reservoir II 3 and be warming up to 85 DEG C, be incubated and stir, making Microcrystal paraffin be dispersed in polyhydric alcohol solutions, finally instilling catalyzer 0.6g and continue to stir.
While (2) two kinds of solution warms, according to above-mentioned steps, continue the coating solution being equipped with second time spraying, weigh PAPI30.1g and tensio-active agent 0.12g respectively, heated and stirred and be incubated 75 DEG C stand-by, take polyvalent alcohol 33.6g and microcrystalline wax 5.94g and catalyzer 0.6g respectively, heated and stirred and be incubated 85 DEG C stand-by; Third time spray solution be respectively PAPI30.4g and tensio-active agent 0.12g, heated and stirred and be incubated 75 DEG C stand-by, take polyvalent alcohol 33.9g and Microcrystalline Wax 5.88g and catalyzer 0.6g respectively, heated and stirred and be incubated 85 DEG C stand-by.
(3), while coating solution heating and thermal insulation, urea granules is added in the spouted bed 2 of two shower nozzle coating machine shown in Fig. 1, open hot air blower, make particle start to circulate and be warmed up to 75 DEG C.The path of particles circulating is the ellipse that major axis is vertically arranged.Open high-pressure pump I 7 and boost to 3MPa, start spraying, high-pressure pump I 7 the isocyanic ester coating mixed solution got ready is sucked the pump housing and even application just on reciprocating urea granules, the distance controlling the lower-most point that high-pressure airless nozzle I 6 is moved with urea granules is 15cm, after reservoir I 8 inner investment liquid to be heated is finished, close high-pressure pump I 7, material continues reciprocal 1 minute in spouted bed 2.Open high-pressure pump II 4, the polyvalent alcohol mixing coating liquid be contained in heating reservoir II 3 is sprayed on reciprocating urea granules, the distance controlling the lower-most point that high-pressure airless nozzle II 5 is moved with urea granules is 15cm, after solution has sprayed, urea granules continues soak cycles, makes 2 kinds of coating liquids at particle surface film-forming.Start second time coating after 2 minutes, the coating liquid above-mentioned second time prepared is according to the method coating film forming of first time spraying.Carry out third time spraying after 3 minutes, after spraying terminates, be incubated 3 minutes, turn off thermal source, continue air blast, for material is lowered the temperature 2 minutes, turn off the blast, draw off material, be coating controlled-release fertilizer finished product.
Measure the Nitrogen releasing effect of film-coated controlled release fertilizer prepared by the present embodiment, adopt thermostat(t)ed water infusion method to test the nitrogen leaching amount of the different time of this film-coated controlled release fertilizer, concrete steps are as follows:
Take above-mentioned control release urea 10.00g, load in nylon net bag, bag is placed in Plastic Bottle, then adds 250ml distilled water, build bottle cap, put into the thermostat container of 25 DEG C.If 3 repetitions.Early stage, sampling was carried out according to the 1st, 3,7,14,21 and 28 day interval, during every sub-sampling, nylon net bag is taken out and puts into the new Plastic Bottle continuation immersion adding distilled water in advance, vat liquor in the Plastic Bottle of the control release urea soaked is shaken up rear sampling and measuring urea content, calculates N element stripping ratio.Release period longer later stage sampling determine sample time according to rate of release.The mensuration of urea adopts dimethyl amino formaldehyde-spectrophotometry, and composite fertilizer's nitrogen adopts Micro-kjoldahl method.
Coating rate measures, if 3 repetitions, precise coated fertilizer 5.00g, puts into mortar and smash to pieces, grind, and be dissolved in water filtration, and gained rete is air-dry, weighs, and the per-cent that calculating rete accounts for coated fertilizer is coating rate.
After measured, the coating rate of the present embodiment is that the 5.3%, 51st day stripping nitrogen accounts for 82% of total nitrogen quality.
Embodiment 2, prepare film-coated controlled release fertilizer
The formula table of the present embodiment is as shown in table 2.
Table 2 coating polymer formulators table
(1) 3 ~ 4mm large grain urea 3kg is weighed for subsequent use.Weigh polyisocyanates (PAPI, Beyer Co., Ltd) 30.9 grams, be placed in heating reservoir I 8 and be warming up to 80 DEG C, instillation tensio-active agent 0.12g, stirs and is incubated 80 DEG C; Weigh polyester polyol 34.8g simultaneously, be placed in heating reservoir II 3, weigh Microcrystal paraffin (fusing point 75 DEG C, commercially available) 3.81g, put into heating reservoir II 3 and be warming up to 95 DEG C, be incubated and stir, making Microcrystal paraffin be dispersed in polyhydric alcohol solutions, finally instilling catalyzer 0.45g and continue to stir.
While (2) two kinds of solution warms, according to above-mentioned steps, continue the coating solution being equipped with second time spraying, weigh PAPI32.0g and tensio-active agent 0.09g respectively, heated and stirred and be incubated 80 DEG C stand-by, take polyvalent alcohol 33.8g and microcrystalline wax 4.84g and catalyzer 0.3g respectively, heated and stirred and be incubated 95 DEG C stand-by; Third time spray solution be respectively PAPI24.1g and tensio-active agent 0.06g, heated and stirred and be incubated 80 DEG C stand-by, take polyvalent alcohol 33.7g and Microcrystalline Wax 3.48g and catalyzer 0.6g respectively, heated and stirred and be incubated 95 DEG C stand-by.
(3), while coating solution heating and thermal insulation, urea granules is added in the spouted bed 2 of two shower nozzle coating machine shown in Fig. 1, open hot air blower, make particle start to circulate and be warmed up to 80 DEG C.Open high-pressure pump I 7 and boost to 4MPa, start spraying, high-pressure pump I 7 the isocyanic ester coating mixed solution got ready is sucked the pump housing and even application just on reciprocating urea granules, the distance controlling the lower-most point that high-pressure airless nozzle I 6 is moved with urea granules is 10cm, after reservoir I 8 inner investment liquid to be heated is finished, close high-pressure pump I 7, material continues circulation 1 minute in spouted bed.Open high-pressure pump II 4, the polyvalent alcohol mixing coating liquid be contained in heating reservoir II 3 is sprayed on reciprocating urea granules, the distance controlling the lower-most point that high-pressure airless nozzle II 5 is moved with urea granules is 10cm, after solution has sprayed, urea granules continues soak cycles, makes 2 kinds of coating liquids at particle surface film-forming.Start second time coating after 2 minutes, the coating liquid above-mentioned second time prepared is according to the method coating film forming of first time spraying.Carry out third time spraying after 3 minutes, after spraying terminates, be incubated 3 minutes, turn off thermal source, continue air blast, for material is lowered the temperature 3 minutes, turn off the blast, draw off material, be coating controlled-release fertilizer finished product.
Measure the Nitrogen releasing effect of film-coated controlled release fertilizer prepared by the present embodiment, adopt the thermostat(t)ed water infusion method in embodiment 1 to measure nitrogen leaching.
After measured, the coating rate of film-coated controlled release fertilizer prepared by the present embodiment is that the 5.03%, 45th day stripping nitrogen accounts for 80% of total nitrogen quality.
Embodiment 3, prepare film-coated controlled release fertilizer
The formula table of the present embodiment is as shown in table 3.
Table 3 coating polymer formulators table
(1) 2 ~ 3mm composite fertilizer (N:P is weighed
2o
5: K
2o=15:15:15, mass ratio) 5kg is for subsequent use.Spray solution is PAPI40.0g for the first time, tensio-active agent 0.2g adds in heating reservoir I 8 and stirs and be heated to 85 DEG C, polyvalent alcohol 60.8g, microcrystalline wax 70#(fusing point 70 DEG C) 4.67g and catalyzer 0.67 gram, add in heating reservoir II 3 stir and be heated to 90 DEG C for subsequent use.2 kinds of materials needed for being sprayed by secondary according to filling a prescription shown in table 3 add in heating reservoir I 8 and stir and be heated to 80 DEG C, 3 kinds of materials corresponding in table 3 are added in heating reservoir II 3 and stir and be heated to 90 DEG C, according to the method described above by table 3 third time material requested weigh respectively in the heating container adding correspondence and to stir and to be warming up to described temperature for subsequent use.
(2), while coating solution heating and thermal insulation, compound fertilizer granules is added in the spouted bed 2 of two shower nozzle coating machine shown in Fig. 1, open hot air blower, make particle start to circulate and be warmed up to 80 DEG C.Open high-pressure pump I 7 and boost to 5MPa, start spraying, high-pressure pump I 7 the isocyanic ester coating mixed solution got ready is sucked the pump housing and even application just on reciprocating fertiliser granulates, the distance controlling the lower-most point that high-pressure airless nozzle I 6 is moved with fertiliser granulates is 12cm, after container inner investment liquid is finished, close high-pressure pump I 7, material continues to-and-fro movement 1 minute in spouted bed.Open high-pressure pump II 4, the polyvalent alcohol mixing coating liquid be contained in heating reservoir II 3 is sprayed on the fertiliser granulates of circulation, the distance controlling the lower-most point that high-pressure airless nozzle II 5 is moved with fertiliser granulates is 12cm, after solution has sprayed, particle continues soak cycles, makes 2 kinds of coating liquids at particle surface film-forming.Start second time coating after 2 minutes, the coating liquid above-mentioned second time prepared is according to the method coating film forming of first time spraying.Carry out third time spraying after 3 minutes, after spraying terminates, be incubated 3 minutes, turn off thermal source, continue air blast, for material is lowered the temperature 3 minutes, turn off the blast, draw off material, be coating controlled-release fertilizer finished product.
Measure the Nitrogen releasing effect of film-coated controlled release fertilizer prepared by the present embodiment, adopt the thermostat(t)ed water infusion method in embodiment 1 to measure nitrogen leaching.
After measured, the coating rate of film-coated controlled release fertilizer prepared by the present embodiment is that the 4.7%, 43rd day stripping nitrogen accounts for 83% of total nitrogen quality.
Claims (3)
1. a solvent-free film-coated controlled release fertilizer, it is made up of fertiliser granulates and the coating layer be coated on outside described fertiliser granulates;
The mass percentage of described fertiliser granulates is 93% ~ 97%, and the mass percentage of described coating layer is 3% ~ 7%;
Described coating layer is obtained by the polymerization of polyisocyanates, polyester polyol and microcrystalline wax;
The particle diameter of described fertiliser granulates is 2mm ~ 4mm;
Described polyisocyanates is ditan polyisocyanates;
Described polyester polyol is phthalic anhydride polyester glycol;
The fusing point of described microcrystalline wax is 60 DEG C ~ 75 DEG C;
In described coating layer, the mass percentage of described polyisocyanates is 37.9 ~ 45.3%;
The mass percentage of described polyester polyol is 47.7 ~ 57.6%;
The mass percentage of described microcrystalline wax is 4.42 ~ 8.54%;
Catalyzer and tensio-active agent is also added in described polymerization process;
Described catalyzer is stannous octoate or isocaprylic acid zinc;
Described tensio-active agent is polysiloxane or polyester based modified polyorganosiloxane;
In described coating layer, the mass percentage of described catalyzer is 0.42% ~ 0.99%;
The mass percentage of described tensio-active agent is 0.11% ~ 0.25%;
The preparation method of described film-coated controlled release fertilizer, comprises the steps:
(1) described fertiliser granulates is heated to 75 ~ 80 DEG C, and makes it move back and forth under drum wind action;
(2) mixture of described polyisocyanates and described tensio-active agent is heated to 75 ~ 85 DEG C, and is coated on reciprocating described fertiliser granulates; Then the mixture of described polyester polyol, described microcrystalline wax and described catalyzer is heated to 85 ~ 95 DEG C, and be coated on reciprocating described fertiliser granulates, the described polyisocyanates then successively applied, described polyester polyol, described microcrystalline wax, described tensio-active agent and described catalyzer carry out polyreaction on the surface of described fertiliser granulates, namely obtain described film-coated controlled release fertilizer;
Described preparation method carries out in two shower nozzle coating machine, and described pair of shower nozzle coating machine comprises a spouted bed, and the sidewall of described spouted bed is provided with opening for feed, and the bottom of described spouted bed connects a discharging pipeline; Be provided with high-pressure airless nozzle I and high-pressure airless nozzle II in described discharging pipeline, described high-pressure airless nozzle I and high-pressure airless nozzle II are connected with high-pressure pump II with the high-pressure pump I be located at outside described spouted bed respectively; The outlet of described high-pressure airless nozzle I and high-pressure airless nozzle II is all arranged towards the bottom of described spouted bed; Concrete steps are as follows:
Described fertiliser granulates, in described spouted bed, moves back and forth under drum wind action;
The mixture of described polyisocyanates and described tensio-active agent is coated on reciprocating described fertiliser granulates by described high-pressure pump I and described high-pressure airless nozzle I;
The mixture of described polyester polyol, described microcrystalline wax and described catalyzer is coated on reciprocating described fertiliser granulates by described high-pressure pump II and described high-pressure airless nozzle II;
The spacing of described high-pressure airless nozzle I and described high-pressure airless nozzle II and described reciprocating lower-most point is 10 ~ 15cm;
The pressure controlling described high-pressure pump I and described high-pressure pump II is 3 ~ 5MPa;
Step (2) repeats 3 times, and each interval time is 2 ~ 3 minutes.
2. the preparation method of film-coated controlled release fertilizer according to claim 1, comprises the steps:
(1) described fertiliser granulates is heated to 75 ~ 80 DEG C, and makes it move back and forth under drum wind action;
(2) mixture of described polyisocyanates and described tensio-active agent is heated to 75 ~ 85 DEG C, and is coated on reciprocating described fertiliser granulates; Then the mixture of described polyester polyol, described microcrystalline wax and described catalyzer is heated to 85 ~ 95 DEG C, and be coated on reciprocating described fertiliser granulates, the described polyisocyanates then successively applied, described polyester polyol, described microcrystalline wax, described tensio-active agent and described catalyzer carry out polyreaction on the surface of described fertiliser granulates, namely obtain described film-coated controlled release fertilizer;
Described preparation method carries out in two shower nozzle coating machine, and described pair of shower nozzle coating machine comprises a spouted bed, and the sidewall of described spouted bed is provided with opening for feed, and the bottom of described spouted bed connects a discharging pipeline; Be provided with high-pressure airless nozzle I and high-pressure airless nozzle II in described discharging pipeline, described high-pressure airless nozzle I and high-pressure airless nozzle II are connected with high-pressure pump II with the high-pressure pump I be located at outside described spouted bed respectively; The outlet of described high-pressure airless nozzle I and high-pressure airless nozzle II is all arranged towards the bottom of described spouted bed; Concrete steps are as follows:
Described fertiliser granulates, in described spouted bed, moves back and forth under drum wind action;
The mixture of described polyisocyanates and described tensio-active agent is coated on reciprocating described fertiliser granulates by described high-pressure pump I and described high-pressure airless nozzle I;
The mixture of described polyester polyol, described microcrystalline wax and described catalyzer is coated on reciprocating described fertiliser granulates by described high-pressure pump II and described high-pressure airless nozzle II;
The spacing of described high-pressure airless nozzle I and described high-pressure airless nozzle II and described reciprocating lower-most point is 10 ~ 15cm;
The pressure controlling described high-pressure pump I and described high-pressure pump II is 3 ~ 5MPa;
Step (2) repeats 3 times, and each interval time is 2 ~ 3 minutes.
3. preparation method according to claim 2, is characterized in that: described reciprocating shape is for oval, and the long axis vertical direction of described ellipse is arranged.
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| CN104447026B (en) * | 2014-12-12 | 2017-06-23 | 华南农业大学 | A kind of vegetable oil film-coated controlled release fertilizer of controllable nutrient release rate and preparation method thereof |
| CN104447027B (en) * | 2014-12-12 | 2017-04-12 | 华南农业大学 | Preparation method of in-situ reaction film-forming and hole-forming type controlled-release fertilizers |
| CN106045669A (en) * | 2016-05-30 | 2016-10-26 | 山西华鑫肥业股份有限公司 | Compound fertilizer and preparation method thereof |
| CN106380315B (en) * | 2016-08-31 | 2020-01-10 | 山东农大肥业科技有限公司 | Modified biological wax coated controlled release fertilizer and preparation method thereof |
| CN111423281A (en) * | 2019-01-09 | 2020-07-17 | 北京市农林科学院 | Polyurethane coated controlled release fertilizer and preparation method thereof |
| CN110698304A (en) * | 2019-11-19 | 2020-01-17 | 南华大学 | Coated controlled release fertilizer and preparation method thereof |
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