CN101508616B - Water-retaining slow/controlled release fertilizer and preparation method thereof - Google Patents

Water-retaining slow/controlled release fertilizer and preparation method thereof Download PDF

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CN101508616B
CN101508616B CN2009100812893A CN200910081289A CN101508616B CN 101508616 B CN101508616 B CN 101508616B CN 2009100812893 A CN2009100812893 A CN 2009100812893A CN 200910081289 A CN200910081289 A CN 200910081289A CN 101508616 B CN101508616 B CN 101508616B
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fertilizer
water
release
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monomer
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CN101508616A (en
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胡树文
刘军
陶树明
邱小云
金可默
张远
张福锁
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China Agricultural University
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China Agricultural University
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Abstract

The invention discloses a water-retaining slow-controlled-release fertilizer and a preparation method thereof, belonging to the technical field of agricultural fertilizers and preparation thereof. The water-retaining slow-release fertilizer takes a macromolecular coated fertilizer as an inner core and a water-retaining layer as an outer layer to form the water-retaining controlled-release fertilizer with a double-layer film structure, the inner film is a macromolecular protective layer film material and has nutrient controlled-release performance, and the outer film is a water-retaining layer and has good water-retaining performance. And spraying the water-retaining agent suspension on the surface of the high-molecular coated fertilizer particles for outer-layer coating, wherein the water-retaining agent suspension is prepared by taking cyclohexane, an emulsifier, acrylic acid, acrylamide, sodium hydroxide, a cross-linking agent and an initiator as raw materials and adopting an inverse suspension polymerization method. The fertilizer has the functions of controlled release, drought resistance, water saving, water retention, soil structure improvement and the like, has the advantages of high water absorption rate, wear resistance, difficult falling and the like, can improve the utilization rate of water and fertilizer, and is widely applied to the aspects of desert control, lawn planting, soil improvement, gardening, agriculture and forestry and the like.

Description

A kind of moisture-retention sustained release and release control fertilizer and preparation method thereof
Technical field
The invention belongs to agricultural fertilizer and preparing technical field thereof, particularly a kind of moisture-retention sustained release and release control fertilizer and preparation method thereof.
Background technology
China is a large agricultural country, and the ratio of chemical fertilizer in the agriculture prodn investment accounts for 50%, but China's fertilizer utilization ratio but has only 30%, causes the huge waste on the economical energy resources thus and has caused various environmental problems.Therefore sustained-controll-release fertiliser becomes the developing direction of the future of agriculture fertilizer, and the polymer coated fertilizer then is called real sustained-controll-release fertiliser by relevant expert.It is to utilize macromolecular material to form thin film on the fertilizer surface; The dissolution rate of control fertilizer in soil; Make the growing requirements of its dissolution rate and plant consistent, thereby reach the purpose of saving fertilizer, improving utilization rate of fertilizer and increase agricultural performance.
Drought and water shortage is restriction China's agricultural development and another important factor of quickening desertification of land, improves the farmland efficiency of water application and becomes one of central task of China's agricultural.Agricultural water-loss reducer has drought-resistant water-preserving, insulation, sustained-release synergistic, improves effects such as Soil structure; Can suppress leaching loss, the raising utilization rate of fertilizer of soil water evaporation, raising saturated soil water content, minimizing leaching property nutrient, can reduce the soil weight simultaneously, improve Soil structure and hydro-thermal situation.Though water-holding agent has superpower water-absorbing-retaining effect; But do not have fertilizer nutrient, nutrient then is that farm crop produce and the necessary nutritional condition of vegetation growth, simultaneously; Water-holding agent and fertilizer are used time-consuming respectively, also are unfavorable for the performance of liquid manure interaction and liquid manure effect.
Therefore, it is combined with sustained-controll-release fertiliser, prepare can delay controlled release nutrients again can water-absorbing-retaining, the research of the function diversification fertilizer of drought resisting will become fertilizer and research and produce the new focus in the field.Moisture-retention sustained release and release control fertilizer has the effect of water-holding agent and sustained-controll-release fertiliser concurrently, has the slow controlled release dual-use function of water-absorbing-retaining and nutrient.Moisture-retention sustained release and release control fertilizer can be regulated soil moisture surplus and deficiency, improves liquid manure and interacts, and improves water, fertile utilising efficiency, reduces the fertilizer nutrient pouring and moves, fixes or volatilization loss, alleviates environmental pollution.Therefore, fertilizer and water-holding agent is compound integrated, have complementary advantages, making the moisture-retention sustained release and release control fertilizer with water retaining function and the slow control-release function of nutrient becomes fertilizer research forward position and direction, meets water saving and dry farming and produces actual needs.
It is core that the water conservation sustained-controll-release fertiliser is meant with fertilizer, for the film material carries out coating, or in fertilizer core, contains the water-absorbent material with the high water absorbency polymer, and then with non-water-absorbing material coating.HE Quan et al (Chinese invention patent, 1583684? A? 20050223) with hydrophilic ethylene propylene rubber three yuan as sulfonic acid type polymer coating material to study its effect on the release of urea was investigated high poly The synthesis conditions and the ambient temperature on the urea release rate.People such as Mazazumi (Japanese Patent, 09309785A, 1997) are core with XPA, isobutene polymer, starch derivative and fertiliser mixtures, are the film material with the urethane ester polymer, have prepared a kind of slow release fertilizer that can be used for the paddy field.People such as Liu Mingzhu (Liu M.Z., Polym.Adv.Technol., 17,430,2006) use sodium acrylate and urea reaction to make water absorbent rate in the laboratory be 680 water-absorbing-retaining slow-release nitrogen fertilizer.People such as Wang (Chinese invention patent, 1781982 A 20060607) develop organic-inorganic compoiste water-keeping slow release composite fertilizer material.He Xusheng (development of water preserving type film coated urea fertilizer and evaluation. Beijing: graduate school of the Chinese Academy of Agricultural Sciences; 2004) develop a Technology of utilizing chemical polymerization directly to become membrane prepare water-holding agent film coated urea fertilizer on the urea granules surface; This water-holding agent coating has higher water absorbent rate; Coating is wear-resistant, the advantage of difficult drop-off, and certain nutrient slowly-released effect is arranged.
At present; There is following problem in the water-maintaining slowly-releasing release and release control fertilizer of existing article and disclosed patent report: the preparation of part water-maintaining slowly-releasing/release and release control fertilizer has been adopted sustained-release and controlled release fertilizer in reactor drum; Initiated polymerization parcel one deck water-holding agent; Be confined to laboratory scale, can't realize on the technology amplify producing, thus big limitations its large-scale commercial prodn.That what adopt is the slow release fertilizers such as urea formaldehyde of expensive is more as " the fertile core " of water-maintaining slowly-releasing/release and release control fertilizer, but the release period of this series products is generally shorter, and the release performance of nutrient is unsatisfactory.Water-maintaining slowly-releasing/release and release control fertilizer is in accumulating and use, and the film material makes moist easily or in handling process, comes off, and influences its result of use.
To the problem of above-mentioned existence, the invention discloses a kind of sustained-controll-release fertiliser of agricultural water retaining function.The polymer coating sustained-controll-release fertiliser good with controlled release properties is " fertile core ", thereby it is short to have solved fertilizer releasing period, the problem that controlled release properties is not good.The water conservation coating liquid adopts the source polymerization, uses the synthetic water conservation suspension-s of method of inverse suspension polymerization, and follow-up film-forming process can successively be carried out, and makes suitability for industrialized production become possibility.Improve the water absorbent rate of water-maintaining fertilizer and repeat water-absorbent, improve the water-absorbing-retaining performance of water-maintaining fertilizer.Novel moisture-retention sustained release and release control fertilizer and preparation process thereof involved in the present invention at home and abroad do not appear in the newspapers, and do not see use at home.
Summary of the invention
The purpose of this invention is to provide a kind of moisture-retention sustained release and release control fertilizer and preparation method thereof.
A kind of moisture-retention sustained release and release control fertilizer; It is characterized in that said moisture-retention sustained release and release control fertilizer integrates the control nutrient and discharges and water retaining function, is a kind of fertilizer with nutrient slow controlled release, drought resisting, the structure of economizing on water and improve the soil; Said moisture-retention sustained release and release control fertilizer is a kernel with the polymer coat fertilizer; The water conservation layer is outer, has formed a kind of water holding controlled release fertilizer of double membrane structure, and said polymer coat fertilizer is a polymer protection tunic material coatedparticles fertilizer; The water holding controlled release fertilizer inner layer film of said double membrane structure is a polymer protection tunic material, has the nutrient controlled release properties, and outer membrane is the water conservation layer, has good water retention property.
Said polymer protection tunic material is one or more in polyolefine, urethane, polyacrylic ester, polyester, polyureas or the polycarbonate, and resist membrane material amount accounts for 2~15% of polymer coat fertilizer quality.
Said granulated fertilizer is water miscible granulated fertilizer; Particle diameter is 2~5mm; Straight fertilizer or the composite fertilizer of perhaps containing trace elements iron, manganese, boron, zinc, copper or molybdenum for straight fertilizer, composite fertilizer; Comprise urea, volatile salt, an ammonium nitrate, ammonium sulfate, one or more in vitriolate of tartar, Repone K, saltpetre, Secondary ammonium phosphate or the primary ammonium phosphate.
A kind of preparation method of moisture-retention sustained release and release control fertilizer is characterized in that, this method steps is following,
(1) take by weighing monomer, said monomer is Acrylic Acid Monomer and acrylic amide, and the Acrylic Acid Monomer quality accounts for 20~70% of monomer total mass, and the acrylic amide quality accounts for 30~80% of monomer total mass; Acrylic Acid Monomer is put into beaker; In ice-water bath,, make acrylic acid degree of neutralization reach 65~70% slowly to wherein adding sodium hydroxide solution; In above-mentioned solution, add acrylic amide, linking agent, initiator; And add water, and making the shared massfraction of aqueous phase monomer is 20~70%, fully dissolving joins mixing solutions in the tap funnel after mixing;
(2) in reaction kettle, add emulsifying agent Span-80 and external phase hexanaphthene; The ratio of the quality of emulsifying agent Span-80 and monomer total mass is 0.03~0.10; The add-on of hexanaphthene is for to make the water oil ratio hexanaphthene by mass ratio: water=(1: 2)~(9: 1); Tap funnel, whipping appts, the reflux condensing tube of step (1) are installed on the reaction kettle, stir, emulsifying agent is fully dissolved;
(3) under nitrogen protection, the drips of solution in the tap funnel is added in the reaction kettle, stir; Emulsification is warming up to 40~60 ℃, in reaction kettle, drips sodium sulfite solution; Wherein, the ratio of the quality of sodium sulfite anhy 96 and monomer total mass is 0.08~0.15%, reaction 2~5h; Obtain anti-phase suspension liquid, be water conservation coating suspension-s;
(4) in encapsulation tool, add the polymer coat fertilizer, said polymer coat fertilizer is a polymer protection tunic material coatedparticles fertilizer, 60~90 ℃ of bulging hot blasts; Make the even fluidisation of fertilizer, the ratio according to water conservation coating suspension quality and polymer coat fertilizer quality is 0.05~0.20 then, adds water conservation coating suspension-s; Nozzle with pressure 0.1~0.3MPa evenly is sprayed onto the fertiliser granulates surface with water conservation coating suspension-s; Continue the drum hot blast, drying obtains moisture-retention sustained release and release control fertilizer.
Said linking agent is a N,N methylene bis acrylamide, and the linking agent quality is 0.06~0.09% with the ratio of monomer total mass.
Said initiator is an ammonium persulphate, 0.15~0.225% of the ratio of initiator quality and monomer total mass.
Said sodium sulfite solution is that concentration is 0.1~5g/L.
Beneficial effect of the present invention is: the present invention learns a kind of high-tech product that interosculates and invent with field such as environmental ecology science with modern agriculture resisting drought saving water technology, macromolecular material, can be widely used in gardening, eagroforestry, shelterbelt construction, lawn plant build, aspect such as soil improvement.Beneficial effect is following:
1, the present invention has utilized the method for inverse suspension polymerization to prepare water conservation coating suspension-s, and this method is that the optimization of water conservation coating suspension-s synthesis technique provides great facility, and provides the foundation for the production of serialization coating.
2, adopt the source polymerization technique, the suspension-s after synthetic is sprayed to the fertilizer surface filming, the thicknesses of layers of formation is even, densification.
3, the water conservation coated fertilizer that adopts this technology to make is a kind of new-type fertilizer with double membrane structure, and inner layer material has the nutrient controlled capability, and outer field material has good water-maintaining ability.
4, under the synergy of water-keeping material and outer membrane material, prolonged the release period of the nutrient of this water-maintaining controlled release fertilizer.
5, this fertilizer is a kind of coating sustained-controll-release fertiliser, is manured into soil fertilizer nutrient is discharged according to certain rule, improves the urine fertilizer utilization ratio, reduces the loss of fertilizer leaching loss.
6, this fertilizer has water retaining function, can water-absorbing-retaining after being manured into soil, and when plant needed, its moisture that receives can be improved the efficiency of water application in the soil by the plant absorbing utilization.
7, this fertilizer can absorb water repeatedly and release water, and after the suction, has formed one by one " miniature reservoir " and " nutrient pool "; Improve fertiliser granulates water regime on every side; Be beneficial to the mutual promoter action of liquid manure, improve the absorption rate of crop water, provide powerful support for for agriculture prodn and resisting drought saving water provide.
Embodiment
Embodiment 1
A kind of moisture-retention sustained release and release control fertilizer, said moisture-retention sustained release and release control fertilizer integrate the control nutrient and discharge and water retaining function, are a kind of fertilizer with nutrient slow controlled release, drought resisting, the structure of economizing on water and improve the soil; Said moisture-retention sustained release and release control fertilizer is a kernel with the polymer coat fertilizer, and the water conservation layer is outer, has formed a kind of water holding controlled release fertilizer of double membrane structure; Said polymer coat fertilizer is that (said polymer protection tunic material is a polyolefine to polymer protection tunic material coatedparticles fertilizer; Granulated fertilizer is a urea, i.e. polyolefine coated carbamide, and the urea particle diameter is 2~5mm; Protection tunic material polyolefine quality account for polyolefine coated carbamide quality 0.08%) the water holding controlled release fertilizer inner layer film of said double membrane structure is polymer protection tunic material; Have the nutrient controlled release properties, outer membrane is the water conservation layer, has good water retention property.
A kind of preparation method of moisture-retention sustained release and release control fertilizer, this method steps is following,
(1) take by weighing monomer, said monomer is Acrylic Acid Monomer and acrylic amide, and the Acrylic Acid Monomer quality accounts for 50% of monomer total mass, and the acrylic amide quality accounts for 50% of monomer total mass, takes by weighing Acrylic Acid Monomer 21g, acrylic amide 21g; Acrylic Acid Monomer is put into beaker; In ice-water bath; Be 10% aqueous sodium hydroxide solution slowly, make acrylic acid degree of neutralization reach 65%, in above-mentioned solution, add acrylic amide, linking agent N to wherein adding massfraction; N-methylene-bisacrylamide 0.033g (the linking agent quality is 0.0785% with the ratio of monomer total mass), initiator ammonium persulfate 0.08g (the initiator quality is 0.19% with the ratio of monomer total mass); And add 19g water, and making the shared massfraction of aqueous phase monomer is 66%, fully dissolving joins mixing solutions in the tap funnel after mixing;
(2) in reaction kettle, add emulsifying agent Span-80 and external phase hexanaphthene; According to the quality of emulsifying agent Span-80 and the ratio of monomer total mass is 0.069, adds 2.9g emulsifying agent Span-80, makes the water oil ratio hexanaphthene by mass ratio: water=7.8; Add hexanaphthene 190ml; Tap funnel, whipping appts, the reflux condensing tube of step (1) are installed on the reaction kettle, stir, emulsifying agent is fully dissolved;
(3) under nitrogen protection, the drips of solution in the tap funnel is added in the reaction kettle, stir; Emulsification is warming up to 45 ℃, in reaction kettle, drips sodium sulfite solution; Wherein, the ratio of the quality of sodium sulfite anhy 96 and monomer total mass is 0.095% (the 0.04g sodium sulfite anhy 96 joins the solution that forms in the 10ml water, and sodium sulfite solution concentration is 4g/L); Reaction 2h obtains anti-phase suspension liquid, is water conservation coating suspension-s;
(4) in encapsulation tool, add polymer coat fertilizer polyolefine coated carbamide 200g (the polymer coat fertilizer is a polymer protection tunic material coatedparticles fertilizer), 80 ℃ of bulging hot blasts make the even fluidisation of fertilizer; Ratio according to water conservation coating suspension quality and polyolefine coated carbamide quality is 0.15 then; Add water conservation coating suspension-s 30g, water conservation coating suspension-s evenly is sprayed onto the fertiliser granulates surface, continue bulging hot blast with the nozzle of pressure 0.1MPa; Drying obtains moisture-retention sustained release and release control fertilizer.
Adopt water-extraction method to measure the controlled release properties of the moisture-retention sustained release and release control fertilizer of present embodiment preparation, the initial stage solubility rate is 0.4%, and the controlled release phase is 92 days.Record its multiplying power of inhaling zero(ppm) water 535 times under 25 ℃ for its water conservation layer.
Embodiment 2
A kind of moisture-retention sustained release and release control fertilizer; Said moisture-retention sustained release and release control fertilizer integrates the control nutrient and discharges and water retaining function; Be a kind of fertilizer with nutrient slow controlled release, drought resisting, the structure of economizing on water and improve the soil, said moisture-retention sustained release and release control fertilizer is a kernel with the polymer coat fertilizer, and the water conservation layer is outer; Formed a kind of water holding controlled release fertilizer of double membrane structure; Said polymer coat fertilizer is that (protection tunic material is a polyacrylic ester to polymer protection tunic material coatedparticles fertilizer, and granulated fertilizer is a 15-15-15 composite fertilizer, i.e. polyacrylic ester coating 15-15-15 composite fertilizer; 15-15-15 composite fertilizer particle diameter is 2~5mm, protection tunic material polyacrylic ester quality account for polyacrylic ester coating 15-15-15 composite fertilizer quality 4%); The water holding controlled release fertilizer inner layer film of said double membrane structure is a polymer protection tunic material, has the nutrient controlled release properties, and outer membrane is the water conservation layer, has good water retention property.
A kind of preparation method of moisture-retention sustained release and release control fertilizer, this method steps is following,
(1) take by weighing monomer, said monomer is Acrylic Acid Monomer and acrylic amide, and the Acrylic Acid Monomer quality accounts for 50% of monomer total mass, and the acrylic amide quality accounts for 50% of monomer total mass, takes by weighing Acrylic Acid Monomer 20g, acrylic amide 20g; Acrylic Acid Monomer is put into beaker; In ice-water bath; Be 10% aqueous sodium hydroxide solution slowly, make acrylic acid degree of neutralization reach 68%, in above-mentioned solution, add acrylic amide, linking agent N to wherein adding massfraction; N-methylene-bisacrylamide 0.035g (the linking agent quality is 0.0875% with the ratio of monomer total mass), initiator ammonium persulfate 0.09g (the initiator quality is 0.225% with the ratio of monomer total mass); And add 18g water, and making the shared massfraction of aqueous phase monomer is 69%, fully dissolving joins mixing solutions in the tap funnel after mixing;
(2) in reaction kettle, add emulsifying agent Span-80 and external phase hexanaphthene; According to the quality of emulsifying agent Span-80 and the ratio of monomer total mass is 0.07, adds 2.8g emulsifying agent Span-80, makes the water oil ratio hexanaphthene by mass ratio: water=7.8; Add hexanaphthene 180ml; Tap funnel, whipping appts, the reflux condensing tube of step (1) are installed on the reaction kettle, stir, emulsifying agent is fully dissolved;
(3) under nitrogen protection, the drips of solution in the tap funnel is added in the reaction kettle, stir; Emulsification is warming up to 50 ℃, in reaction kettle, drips sodium sulfite solution; Wherein, the ratio of the quality of sodium sulfite anhy 96 and monomer total mass is 0.1% (the 0.04g sodium sulfite anhy 96 joins the solution that forms in the 10ml water, and sodium sulfite solution concentration is 4g/L); Reaction 3h obtains anti-phase suspension liquid, is water conservation coating suspension-s;
(4) in encapsulation tool, add polymer coat fertilizer polyacrylic ester coating 15-15-15 composite fertilizer 200g (the polymer coat fertilizer is a polymer protection tunic material coatedparticles fertilizer); 80 ℃ of bulging hot blasts; Make the even fluidisation of fertilizer, the ratio according to water conservation coating suspension quality and polymer coat fertilizer quality is 0.16 then, adds water conservation coating suspension-s 32g; Nozzle with pressure 0.2MPa evenly is sprayed onto the fertiliser granulates surface with water conservation coating suspension-s; Continue the drum hot blast, drying obtains moisture-retention sustained release and release control fertilizer.
Adopt water-extraction method to measure the controlled release properties of the moisture-retention sustained release and release control fertilizer of present embodiment preparation, the initial stage solubility rate is 0.2%, and the controlled release phase is 78 days.Record its multiplying power of inhaling zero(ppm) water 675 times under 25 ℃ for its water conservation layer.
Embodiment 3
A kind of moisture-retention sustained release and release control fertilizer; Said moisture-retention sustained release and release control fertilizer integrates the control nutrient and discharges and water retaining function, is a kind of fertilizer with nutrient slow controlled release, drought resisting, the structure of economizing on water and improve the soil, and said moisture-retention sustained release and release control fertilizer is a kernel with the polymer coat fertilizer; The water conservation layer is outer; Formed a kind of water holding controlled release fertilizer of double membrane structure, said polymer coat fertilizer is that (protection tunic material is a polyolefine to polymer protection tunic material coatedparticles fertilizer, and granulated fertilizer is a 16-16-16 composite fertilizer; 16-16-16 composite fertilizer particle diameter is 2~5mm, protection tunic material polyolefine quality account for polyolefine coating 16-16-16 composite fertilizer quality 7%); The water holding controlled release fertilizer inner layer film of said double membrane structure is a polymer protection tunic material, has the nutrient controlled release properties, and outer membrane is the water conservation layer, has good water retention property.
A kind of preparation method of moisture-retention sustained release and release control fertilizer, this method steps is following,
(1) take by weighing monomer, said monomer is Acrylic Acid Monomer and acrylic amide, and the Acrylic Acid Monomer quality accounts for 54.5% of monomer total mass, and the acrylic amide quality accounts for 45.5% of monomer total mass, takes by weighing Acrylic Acid Monomer 24g, acrylic amide 20g; Acrylic Acid Monomer is put into beaker; In ice-water bath; Be 10% aqueous sodium hydroxide solution slowly, make acrylic acid degree of neutralization reach 69%, in above-mentioned solution, add acrylic amide, linking agent N to wherein adding massfraction; N-methylene-bisacrylamide 0.035g (the linking agent quality is 0.0795% with the ratio of monomer total mass), initiator ammonium persulfate 0.08g (the initiator quality is 0.182% with the ratio of monomer total mass); And add 20g water, and making the shared massfraction of aqueous phase monomer is 68.75%, fully dissolving joins mixing solutions in the tap funnel after mixing;
(2) in reaction kettle, add emulsifying agent Span-80 and external phase hexanaphthene; According to the quality of emulsifying agent Span-80 and the ratio of monomer total mass is 0.064, adds 2.8g emulsifying agent Span-80, makes the water oil ratio hexanaphthene by mass ratio: water=7.8; Add hexanaphthene 200ml; Tap funnel, whipping appts, the reflux condensing tube of step (1) are installed on the reaction kettle, stir, emulsifying agent is fully dissolved;
(3) under nitrogen protection, the drips of solution in the tap funnel is added in the reaction kettle, stir; Emulsification is warming up to 52 ℃, in reaction kettle, drips sodium sulfite solution; Wherein, the ratio of the quality of sodium sulfite anhy 96 and monomer total mass is 0.09% (the 0.04g sodium sulfite anhy 96 joins the solution that forms in the 10ml water, and sodium sulfite solution concentration is 4g/L); Reaction 3h obtains anti-phase suspension liquid, is water conservation coating suspension-s;
(4) in encapsulation tool, add polymer coat fertilizer polyolefine coating 16-16-16 composite fertilizer 250g (the polymer coat fertilizer is a polymer protection tunic material coatedparticles fertilizer); 75 ℃ of bulging hot blasts; Make the even fluidisation of fertilizer, the ratio according to water conservation coating suspension quality and polymer coat fertilizer quality is 0.19 then, adds water conservation coating suspension-s 47.5g; Nozzle with pressure 0.25MPa evenly is sprayed onto the fertiliser granulates surface with water conservation coating suspension-s; Continue the drum hot blast, drying obtains moisture-retention sustained release and release control fertilizer.
Adopt water-extraction method to measure the controlled release properties of the moisture-retention sustained release and release control fertilizer of present embodiment preparation, the initial stage solubility rate is 1.2%, and the controlled release phase is 56 days.Record its multiplying power of inhaling zero(ppm) water 452 times under 25 ℃ for its water conservation layer.
Embodiment 4
A kind of moisture-retention sustained release and release control fertilizer; Said moisture-retention sustained release and release control fertilizer integrates the control nutrient and discharges and water retaining function, is a kind of fertilizer with nutrient slow controlled release, drought resisting, the structure of economizing on water and improve the soil, and said moisture-retention sustained release and release control fertilizer is a kernel with the polymer coat fertilizer; The water conservation layer is outer; Formed a kind of water holding controlled release fertilizer of double membrane structure, said polymer coat fertilizer is that (protection tunic material is a polyolefine to polymer protection tunic material coatedparticles fertilizer, and granulated fertilizer is a 16-16-16 composite fertilizer; 16-16-16 composite fertilizer particle diameter is 2~5mm, protection tunic material polyolefine quality account for polyolefine coating 16-16-16 composite fertilizer quality 4%); The water holding controlled release fertilizer inner layer film of said double membrane structure is a polymer protection tunic material, has the nutrient controlled release properties, and outer membrane is the water conservation layer, has good water retention property.
A kind of preparation method of moisture-retention sustained release and release control fertilizer, this method steps is following,
(1) take by weighing monomer, said monomer is Acrylic Acid Monomer and acrylic amide, and the Acrylic Acid Monomer quality accounts for 42.9% of monomer total mass, and the acrylic amide quality accounts for 57.1% of monomer total mass, takes by weighing Acrylic Acid Monomer 18g, acrylic amide 24g; Acrylic Acid Monomer is put into beaker; In ice-water bath; Be 10% aqueous sodium hydroxide solution slowly, make acrylic acid degree of neutralization reach 65%, in above-mentioned solution, add acrylic amide, linking agent N to wherein adding massfraction; N-methylene-bisacrylamide 0.036g (the linking agent quality is 0.086% with the ratio of monomer total mass), initiator ammonium persulfate 0.078g (the initiator quality is 0.186% with the ratio of monomer total mass); And add 18g water, and making the shared massfraction of aqueous phase monomer is 70%, fully dissolving joins mixing solutions in the tap funnel after mixing;
(2) in reaction kettle, add emulsifying agent Span-80 and external phase hexanaphthene; According to the quality of emulsifying agent Span-80 and the ratio of monomer total mass is 0.076, adds 3.2g emulsifying agent Span-80, makes the water oil ratio hexanaphthene by mass ratio: water=8.23; Add hexanaphthene 190ml; Tap funnel, whipping appts, the reflux condensing tube of step (1) are installed on the reaction kettle, stir, emulsifying agent is fully dissolved;
(3) under nitrogen protection, the drips of solution in the tap funnel is added in the reaction kettle, stir; Emulsification is warming up to 55 ℃, in reaction kettle, drips sodium sulfite solution; Wherein, the ratio of the quality of sodium sulfite anhy 96 and monomer total mass is 0.095% (the 0.04g sodium sulfite anhy 96 joins the solution that forms in the 10ml water, and sodium sulfite solution concentration is 4g/L); Reaction 3.5h obtains anti-phase suspension liquid, is water conservation coating suspension-s;
(4) in encapsulation tool, add polymer coat fertilizer polyolefine coating 16-16-16 composite fertilizer 150g (the polymer coat fertilizer is a polymer protection tunic material coatedparticles fertilizer); 85 ℃ of bulging hot blasts; Make the even fluidisation of fertilizer, the ratio according to water conservation coating suspension quality and polymer coat fertilizer quality is 0.20 then, adds water conservation coating suspension-s 30g; Nozzle with pressure 0.1MPa evenly is sprayed onto the fertiliser granulates surface with water conservation coating suspension-s; Continue the drum hot blast, drying obtains moisture-retention sustained release and release control fertilizer.
Adopt water-extraction method to measure the controlled release properties of the moisture-retention sustained release and release control fertilizer of present embodiment preparation, the initial stage solubility rate is 0.8%, and the controlled release phase is 145 days.Record its multiplying power of inhaling zero(ppm) water 470 times under 25 ℃ for its water conservation layer.
Embodiment 5
A kind of moisture-retention sustained release and release control fertilizer; Said moisture-retention sustained release and release control fertilizer integrates the control nutrient and discharges and water retaining function, is a kind of fertilizer with nutrient slow controlled release, drought resisting, the structure of economizing on water and improve the soil, and said moisture-retention sustained release and release control fertilizer is a kernel with the polymer coat fertilizer; The water conservation layer is outer; Formed a kind of water holding controlled release fertilizer of double membrane structure, said polymer coat fertilizer is that (protection tunic material is a urethane to polymer protection tunic material coatedparticles fertilizer, and granulated fertilizer is a 15-15-15 composite fertilizer; Protection tunic material urethane quality accounts for 3% of polyurethane coated 15-15-15 composite fertilizer quality, and 15-15-15 composite fertilizer particle diameter is 2~5mm); The water holding controlled release fertilizer inner layer film of said double membrane structure is a polymer protection tunic material, has the nutrient controlled release properties, and outer membrane is the water conservation layer, has good water retention property.
A kind of preparation method of moisture-retention sustained release and release control fertilizer, this method steps is following,
(1) take by weighing monomer, said monomer is Acrylic Acid Monomer and acrylic amide, and the Acrylic Acid Monomer quality accounts for 58% of monomer total mass, and the acrylic amide quality accounts for 42% of monomer total mass, takes by weighing Acrylic Acid Monomer 25g, acrylic amide 18g; Acrylic Acid Monomer is put into beaker; In ice-water bath; Be 10% aqueous sodium hydroxide solution slowly, make acrylic acid degree of neutralization reach 70%, in above-mentioned solution, add acrylic amide, linking agent N to wherein adding massfraction; N-methylene-bisacrylamide 0.028g (the linking agent quality is 0.065% with the ratio of monomer total mass), initiator ammonium persulfate 0.081g (the initiator quality is 0.188% with the ratio of monomer total mass); And add 22g water, and making the shared massfraction of aqueous phase monomer is 66%, fully dissolving joins mixing solutions in the tap funnel after mixing;
(2) in reaction kettle, add emulsifying agent Span-80 and external phase hexanaphthene; According to the quality of emulsifying agent Span-80 and the ratio of monomer total mass is 0.064, adds 2.75g emulsifying agent Span-80, makes the water oil ratio hexanaphthene by mass ratio: water=6.38; Add hexanaphthene 180ml; Tap funnel, whipping appts, the reflux condensing tube of step (1) are installed on the reaction kettle, stir, emulsifying agent is fully dissolved;
(3) under nitrogen protection, the drips of solution in the tap funnel is added in the reaction kettle, stir; Emulsification is warming up to 55 ℃, in reaction kettle, drips sodium sulfite solution; Wherein, the ratio of the quality of sodium sulfite anhy 96 and monomer total mass is 0.093% (the 0.04g sodium sulfite anhy 96 joins the solution that forms in the 10ml water, and sodium sulfite solution concentration is 4g/L); Reaction 5h obtains anti-phase suspension liquid, is water conservation coating suspension-s;
(4) in encapsulation tool, add the polyurethane coated 15-15-15 composite fertilizer 225g of polymer coat fertilizer (the polymer coat fertilizer is a polymer protection tunic material coatedparticles fertilizer); 90 ℃ of bulging hot blasts; Make the even fluidisation of fertilizer, the ratio according to water conservation coating suspension quality and polymer coat fertilizer quality is 0.20 then, adds water conservation coating suspension-s 45g; Nozzle with pressure 0.3MPa evenly is sprayed onto the fertiliser granulates surface with water conservation coating suspension-s; Continue the drum hot blast, drying obtains moisture-retention sustained release and release control fertilizer.
Adopt water-extraction method to measure the controlled release properties of the moisture-retention sustained release and release control fertilizer of present embodiment preparation, the initial stage solubility rate is 1.5%, and the controlled release phase is 82 days.Record its multiplying power of inhaling zero(ppm) water 628 times under 25 ℃ for its water conservation layer.

Claims (7)

1. moisture-retention sustained release and release control fertilizer; It is characterized in that said moisture-retention sustained release and release control fertilizer integrates the control nutrient and discharges and water retaining function, is a kind of fertilizer with nutrient slow controlled release, drought resisting, the structure of economizing on water and improve the soil; Said moisture-retention sustained release and release control fertilizer is a kernel with the polymer coat fertilizer; The water conservation layer is outer, has formed a kind of water holding controlled release fertilizer of double membrane structure, and said polymer coat fertilizer is a polymer protection tunic material coatedparticles fertilizer; The water holding controlled release fertilizer inner layer film of said double membrane structure is a polymer protection tunic material, has the nutrient controlled release properties, and outer membrane is the water conservation layer, has good water retention property;
The preparation method of said moisture-retention sustained release and release control fertilizer is following:
(1) take by weighing monomer, said monomer is Acrylic Acid Monomer and acrylic amide, and the Acrylic Acid Monomer quality accounts for 20~70% of monomer total mass, and the acrylic amide quality accounts for 30~80% of monomer total mass; Acrylic Acid Monomer is put into beaker; In ice-water bath,, make acrylic acid degree of neutralization reach 65~70% slowly to wherein adding sodium hydroxide solution; In above-mentioned solution, add acrylic amide, linking agent, initiator; And add water, and making the shared massfraction of aqueous phase monomer is 20~70%, fully dissolving joins mixing solutions in the tap funnel after mixing;
(2) in reaction kettle, add emulsifying agent Span-80 and external phase hexanaphthene; The ratio of the quality of emulsifying agent Span-80 and monomer total mass is 0.03~0.10; The add-on of hexanaphthene is for to make the water oil ratio hexanaphthene by mass ratio: water=(1: 2)~(9: 1); Tap funnel, whipping appts, the reflux condensing tube of step (1) are installed on the reaction kettle, stir, emulsifying agent is fully dissolved;
(3) under nitrogen protection, the drips of solution in the tap funnel is added in the reaction kettle, stir; Emulsification is warming up to 40~60 ℃, in reaction kettle, drips sodium sulfite solution; Wherein, the ratio of the quality of sodium sulfite anhy 96 and monomer total mass is 0.08~0.15%, reaction 2~5h; Obtain anti-phase suspension liquid, be water conservation coating suspension-s;
(4) in encapsulation tool, add the polymer coat fertilizer, said polymer coat fertilizer is a polymer protection tunic material coatedparticles fertilizer, 60~90 ℃ of bulging hot blasts; Make the even fluidisation of fertilizer, the ratio according to water conservation coating suspension quality and polymer coat fertilizer quality is 0.05~0.20 then, adds water conservation coating suspension-s; Nozzle with pressure 0.1~0.3MPa evenly is sprayed onto the fertiliser granulates surface with water conservation coating suspension-s; Continue the drum hot blast, drying obtains moisture-retention sustained release and release control fertilizer.
2. moisture-retention sustained release and release control fertilizer according to claim 1; It is characterized in that; Said polymer protection tunic material is one or more in polyolefine, urethane, polyacrylic ester, polyester, polyureas or the polycarbonate, and resist membrane material amount accounts for 2~15% of polymer coat fertilizer quality.
3. moisture-retention sustained release and release control fertilizer according to claim 1; It is characterized in that; Said granulated fertilizer is water miscible granulated fertilizer, and particle diameter is 2~5mm, perhaps contains the straight fertilizer or the composite fertilizer of trace elements iron, manganese, boron, zinc, copper or molybdenum for straight fertilizer, composite fertilizer; Comprise urea, volatile salt, an ammonium nitrate, ammonium sulfate, one or more in vitriolate of tartar, Repone K, saltpetre, Secondary ammonium phosphate or the primary ammonium phosphate.
4. the preparation method of a moisture-retention sustained release and release control fertilizer is characterized in that, this method steps is following,
(1) take by weighing monomer, said monomer is Acrylic Acid Monomer and acrylic amide, and the Acrylic Acid Monomer quality accounts for 20~70% of monomer total mass, and the acrylic amide quality accounts for 30~80% of monomer total mass; Acrylic Acid Monomer is put into beaker; In ice-water bath,, make acrylic acid degree of neutralization reach 65~70% slowly to wherein adding sodium hydroxide solution; In above-mentioned solution, add acrylic amide, linking agent, initiator; And add water, and making the shared massfraction of aqueous phase monomer is 20~70%, fully dissolving joins mixing solutions in the tap funnel after mixing;
(2) in reaction kettle, add emulsifying agent Span-80 and external phase hexanaphthene; The ratio of the quality of emulsifying agent Span-80 and monomer total mass is 0.03~0.10; The add-on of hexanaphthene is for to make the water oil ratio hexanaphthene by mass ratio: water=(1: 2)~(9: 1); Tap funnel, whipping appts, the reflux condensing tube of step (1) are installed on the reaction kettle, stir, emulsifying agent is fully dissolved;
(3) under nitrogen protection, the drips of solution in the tap funnel is added in the reaction kettle, stir; Emulsification is warming up to 40~60 ℃, in reaction kettle, drips sodium sulfite solution; Wherein, the ratio of the quality of sodium sulfite anhy 96 and monomer total mass is 0.08~0.15%, reaction 2~5h; Obtain anti-phase suspension liquid, be water conservation coating suspension-s;
(4) in encapsulation tool, add the polymer coat fertilizer, said polymer coat fertilizer is a polymer protection tunic material coatedparticles fertilizer, 60~90 ℃ of bulging hot blasts; Make the even fluidisation of fertilizer, the ratio according to water conservation coating suspension quality and polymer coat fertilizer quality is 0.05~0.20 then, adds water conservation coating suspension-s; Nozzle with pressure 0.1~0.3MPa evenly is sprayed onto the fertiliser granulates surface with water conservation coating suspension-s; Continue the drum hot blast, drying obtains moisture-retention sustained release and release control fertilizer.
5. the preparation method of moisture-retention sustained release and release control fertilizer according to claim 4 is characterized in that, said linking agent is a N,N methylene bis acrylamide, and the linking agent quality is 0.06~0.09% with the ratio of monomer total mass.
6. the preparation method of moisture-retention sustained release and release control fertilizer according to claim 4 is characterized in that, said initiator is an ammonium persulphate, 0.15~0.225% of the ratio of initiator quality and monomer total mass.
7. the preparation method of moisture-retention sustained release and release control fertilizer according to claim 4 is characterized in that, said sodium sulfite solution is that concentration is 0.1~5g/L.
CN2009100812893A 2009-03-31 2009-03-31 Water-retaining slow/controlled release fertilizer and preparation method thereof Expired - Fee Related CN101508616B (en)

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