CN101693640A - Slow-release microcapsule fertilizer and manufacture method thereof - Google Patents
Slow-release microcapsule fertilizer and manufacture method thereof Download PDFInfo
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- CN101693640A CN101693640A CN200910192346A CN200910192346A CN101693640A CN 101693640 A CN101693640 A CN 101693640A CN 200910192346 A CN200910192346 A CN 200910192346A CN 200910192346 A CN200910192346 A CN 200910192346A CN 101693640 A CN101693640 A CN 101693640A
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Abstract
A slow-release microcapsule fertilizer and a manufacture method thereof belong to the field of crop fertilizer. In the invention, a special polymeric membrane is used for wrapping the fertilizer as a core material therein and the polymeric membrane comprises two components of chitosan and arabicgum, wherein the chitosan is water solution with the mass concentration of 5-15 percent, and the arabicgum is water solution with the mass concentration of 5-15 percent. The color and luster of an obtained product are pleasing, the handfeel is delicate. A soil leaching experiment proves that the fertilizer can obviously prolong the period of validity of the fertilizer, improve fertilizer efficiency, promote the growth of crops and increase production and income. Compared with quick-acting nitrogen fertilizer, the utilization rate of the fertilizer is improved by 10-30 percent.
Description
Technical field
A kind of slow-release microcapsule fertilizer and manufacture method thereof belong to farm crop fertilizer field, and outstanding being fit to prepares little capsule slow-release fertilizer with chitosan and gum arabic.
Background technology
Slow release fertilizer claims slow-release fertilizer again, is called as " fertilizer of 21 century ".Be the class new variety that development in recent years is got up, " slowly-releasing " is meant that the fertilizer nutrient rate of release is much smaller than common instantly-soluble fertilizer, this class fertilizer can be realized single fertilization, reduce the loss of nutrient in the fertilizer, the fertilizer efficiency time is long, improve fertilizer efficiency, weaken the residual pollution of fertilizer to soil, worldwide development is very fast, especially in developed country, the consumption of slow-release fertilizer increases with the speed of 4%-5%, and slow-release fertilizer is developed for many years in China, and obtained good achievement, but still relatively slowly, share of market is low for the current overall context tempo, and country and government pay much attention to this, China's chemical fertilizer Eleventh Five-Year Plan development program has been listed in the development of slow-release fertilizer and exploitation in, widelys popularize as resources conservation and environmental friendliness problem.
Microcapsulary is started in Britain in eighties of last century the thirties, and development has been widely used in the every field of people's life and production rapidly.The method of material micro encapsulation has three major types: physics, be separated and surface reaction.1, physics method: microcapsule wall material and core material particle physically combine, and the wall material flows to form microcapsule around core material particle.2, phase separation method, microcapsule form core emulsifying materials or dispersion in external phase that can not be miscible.3, interfacial reaction method: the core material is emulsification or dispersion in immiscible external phase, on the surface of core material particle interface polymerization reaction takes place then, produces microcapsule thus.Sustained-controll-release fertiliser mainly contains 3 kinds of organic synthesis slightly soluble type slow-release nitrogen fertilizer, coating (parcel) class slowly/controlled releasing fertilizer, felted organic and inorganic slow release fertilizers etc. in the world at present.Coating (parcel) class slowly/controlled releasing fertilizer can be divided into natural polymer slow-release material and synthetic macromolecule slow-release material according to the source difference of wall material.The preparation technology of slow-release microcapsule fertilizer mainly contains orifice one precipitation bath method, aqueous phase separation method, dry bath method (complex phase emulsion method) etc. at present.But the medium that is used as micro encapsulation in the dry bath method (complex phase emulsion method) is water or whiteruss, soya-bean oil an and so on oil.The emulsification system of wall material solution or core formation is distributed in the above-mentioned medium with micro-droplet status, then by heating, decompression stirring, solvent extraction, cool off or mode such as freeze is removed the solvent in the wall material solution gradually, the wall material is separated out from solution and capsule-core is coated and forms cyst wall.The manufacturing process of these slow-release microcapsule fertilizers is more numerous, operates waywardly, and the microcapsule wall film of formation causes the not high shortcoming of release performance.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology, and operational safety is easy to control, the preparation method of the microcapsule fertilizer that the microcapsule wall film densification of formation and release performance are good.
The technical solution used in the present invention is: will wrap in as the chemical fertilizer of core wherein with special polymeric membrane, and form the microcapsule slow-release fertilizer with slow-release function.
The film that the present invention selects for use is to be composited according to charge differences by chitosan and gum arabic, and it is to form in different charged species interaction neutral processes.Because to be nature unique is with cationic natural radioactivity polysaccharide for chitosan, gum arabic is a saccharan, in the aqueous solution, contain on the gum arabic molecular chain-COOH and-COO-, have negative charge.When chitosan and gum arabic in the blended aqueous solution, and regulate pH value, make chitosan form the composite film because of charged the neutralization on the contrary mutually with gum arabic, its solubleness reduces, and condenses encystation and separate out in system.Add solidifying agent again, solidifying agent and chitosan produce the condensation reaction of amine aldehyde, and chitosan molecule is cross-linked into reticulated structure, keeps the shape of micro-capsule, becomes irreversible micro-capsule.The mechanism of action of coating method is the physics controlled release, and factor of influence mainly is a temperature, so accurately realize the control of nutrient time of releasing and quantity easily, forms slow-release microcapsule.
A kind of slow-release microcapsule fertilizer that the present invention relates to comprises core and wall film, it is characterized in that the wall film comprises chitosan and gum arabic two components.
Described core is the mixture of fertilizer and auxiliary, and the mass ratio of fertilizer and auxiliary is generally 1: the described fertilizer of 0.3-0.5 is the mixture with urea and sylvite, as: urea, vitriolate of tartar; The mass ratio of the mixture of described urea and sylvite is 1: 1.1-1.3.Auxiliary is: plant-growth regulator, plant-growth regulator is: Plant hormones regulators,gibberellins, indolylacetic acid, naphthylacetic acid, ethrel, paclobutrazol, uniconazole, help strong element etc.Auxiliary can promote effect of fertilizer, and plant-growth, growth and metabolism are played the important physical regulatory function.As breaking dormancy, stratification, take root, bloom and ripe, prevent lodging, fallen flowers, shedding etc., effect is very remarkable.
Described wall putamina glycan is the soluble poly chitose of modification.Chitosan is the product of chitin behind deacetylation; chitosan has different chemical structures, has hydroxyl and ethanoyl on its molecular chain, also contains free amino etc. on the chitosan molecule chain; these groups can obtain the soluble poly chitose by various chemical modifications.Chitosan can carry out carboxymethylation, hydroxyethylation, cyanoethylation reaction with etherifying agents such as Monochloro Acetic Acid, oxyethane, vinyl cyanide, generates corresponding ionic ether and non-ionic type ether.The solvability of chitosan and deacetylation, molecular weight, viscosity are relevant, and deacetylation is high more, and molecular weight is more little, and is soluble in water more; Molecular weight is big more, and viscosity is big more.
The soluble poly chitose is a kind of fungistat of wide spectrum, can improve the soil microenvironment, promotes the probiotics increment, suppresses the pathogenic bacterium growth.
The proportioning that described wall film is formed is: the mass concentration of chitosan is that 5%～15% the aqueous solution and gum arabic mass concentration are 5%～15% the aqueous solution.
According to above-mentioned a kind of slow-release microcapsule fertilizer, its manufacturing step is as follows:
One, prepares wall film two components and core
(1) it is standby to prepare wall film two components respectively: mass concentration is that 5%～15% chitosan aqueous solution and mass concentration are 5%～15% the gum arabic aqueous solution.
(2) make the water-in-oil emulsion of core, the saturated aqueous solution of fertilizer and auxiliary is dispersed in the vegetables oil, form the water-in-oil emulsion of core, standby.The volume ratio of the saturated aqueous solution of fertilizer and auxiliary is 1: 1～2.5, and the volume ratio of the saturated aqueous solution of vegetables oil and fertilizer and auxiliary is about 1: 1, with the saturated aqueous solution interpolation stablizer of fertilizer and auxiliary, as: tween-80.Addition is approximately to add the 5ml tween-80 as stablizer in the saturated aqueous solution of the fertilizer of 100ml and auxiliary; Stablizer can increase the medicament of the stability of solution, colloid, solid, mixture.Its reaction of can slowing down keeps chemical equilibrium, reduces surface tension, prevents effects such as light, thermolysis or oxygenolysis.Here the stablizer of usefulness mainly is emulsifying agent and dispersion agent, as carboxylate salt, vitriol and sulfonate etc., prevents liquid precipitation.The emulsifying agent here is a class tensio-active agent when it is dispersed in dispersion agent surperficial, forms film or electrostatic double layer, can make disperse phase have electric charge, so just can stop the small droplets of disperse phase to condense mutually, makes the emulsion of formation more stable.
Two, the water-in-oil emulsion emulsification of chitosan solution and core obtains dual emulsion
The water-in-oil emulsion that in the chitosan solution of step 1 preparation, adds core, under temperature 25-35 ℃, stir through homogenizer (6000r/min), obtain homogeneous w/o/w[water/oil phase/water] dual emulsion (being that the water-in-oil emulsion appearance has been wrapped one deck water again), the addition of the water-in-oil emulsion of core is 10%～20% of wall film quality [Right] content.
Three, the wet microcapsule solution of preparation
In the dual emulsion that step 2 obtains, slowly add the standby gum arabic aqueous solution in the step 1, continuing low speed [50r/min] stirs, regulate the pH value, pH when making into microcapsule is 3.0, do not cohere [viscosity 10-50mPas] with capsule and be advisable, like this, chitosan and gum arabic are because of the charged formation mixture that neutralizes on the contrary mutually, its solubleness reduces, and the cohesion encystation is separated out in system.Obtain wet microcapsule solution.The complex coacervation reaction times is no less than 30min, and the time has been lacked, and the microcapsule diameter of formation increases, and the sacculus form of formation is undesirable, the form irregularity, and encapsulation rate is low.
Four, add solidifying agent
Add suitable amount of sucrose as solidifying agent in the solution that step 3 obtains, continue to stir, the interpolation quality of sucrose is 10～15% of a wall mould material content.Solidifying agent and chitosan produce the condensation reaction of amine aldehyde, and chitosan molecule is cross-linked into reticulated structure, keep the shape of micro-capsule, become irreversible micro-capsule.
Five, spraying drying
The micro-capsule solution that step 4 obtains is sprayed, and granularity is 5-15um, then, dry in spray-drier, 180 ℃ of inlet temperature, air outlet temperature is controlled at 90-100 ℃, obtain the micro-capsule powder, make the micro-capsule water ratio, collect powder and promptly obtain the microcapsule fertilizer product at 3%-8%.
Compared with the prior art, the present invention has outstanding advantage and effect:
The present invention is with low cost, uses easyly, and technology is simple; be easy to grasp and large-scale production, can significantly reduce fertilizer loss, improve fertilizer efficiency; and environmentally friendly, can be widely used in food crop, cash crop and gardening plant as wheat, oranges and tangerines, lichee, potted plant etc.
Embodiment
The present invention is further illustrated by following examples, embodiment does not also limit the present invention in any way, under the prerequisite that does not deviate from technical solution of the present invention, any change or change that those of ordinary skills that the present invention did are realized easily all will fall within the claim scope of the present invention.
Embodiment 1:
Make the slow-release microcapsule fertilizer of 250 gram weight
Prepare the 1000mL mass percent respectively and be 5% the soluble chitosan aqueous solution and 5% the gum arabic aqueous solution.Soluble chitosan adopts (1,4 glycosides)-2-amido-2-deoxidation-B-D glucose, and it is by the product behind chitin (Chitin) deacetylation.
1. the water-in-oil emulsion for preparing core
The saturated aqueous solution of 100mL fertilizer and auxiliary is dispersed in the vegetables oil of 100mL, and wherein, the fertilizer of core can adopt urea, and auxiliary can be: Plant hormones regulators,gibberellins; Vegetables oil can be: soya-bean oil; The fertilizer of core and the ratio of auxiliary are: 1: 1; Add the tween-80 of stablizer 5mL, stirrer stirs under the 6000r/min rotating speed, and homogeneous obtains the water-in-oil emulsion of core.
3, prepare dual emulsion
Add the core water-in-oil emulsion that step 2 obtains in chitosan aqueous solution, in the stirrer stirring of 6000r/min rotating speed, homogeneous gets the w/o/w dual emulsion.
4, the wet microcapsule solution of preparation
In above-mentioned dual emulsion, slowly add the gum arabic aqueous solution, continuing low speed [50r/min] stirs, regulating the pH value is 3.0, viscosity is that 10-50mPa is advisable, like this, chitosan and gum arabic are because of the charged formation mixture that neutralizes on the contrary mutually, and its solubleness reduces, and the cohesion encystation is separated out in system.Obtain wet microcapsule solution.Keep stirring 30min, obtain wet microcapsule solution.
5, add solidifying agent
Add the sucrose about 20g in the wet microcapsule solution that in step 4, obtains, stir.
6, spraying drying
The micro-capsule solution that step 5 obtains is sprayed, and granularity is 5-15um, and then, 180 ℃ of spray-drier inlet temperature, air outlet temperature is controlled at 90～100 ℃, collects powder and promptly obtains the microcapsule fertilizer product.The spray-drier working process: air is converted into the hot-air distributor of warm air access to plant at the kiln top by well heater, enter in the kiln equably then, and rotate twist, simultaneously feed liquid is delivered to the centrifugal atomizer at kiln top, feed liquid is sprayed into minimum vaporific drop, feed liquid contacts with warm air and stream, moisture content evaporates rapidly, is powdery at extremely short time (tens seconds to tens of seconds) inner drying.Finished product drying tower bottom and cyclonic separator are discharged, and waste gas is extracted emptying out by blower fan.
Embodiment 2:
Make the slow-release microcapsule fertilizer of 400 gram weight
Operation steps is substantially with embodiment 1, and difference is, changes the mass percent of the soluble chitosan and the gum arabic aqueous solution into 10%, and the core addition maintains 20%, and the sucrose addition changes 40g into.
Embodiment 3:
Make the slow-release microcapsule fertilizer of 200 gram weight
Operation steps is substantially with embodiment 1, and difference is to change the core addition into 10%.
Through check, the product color that obtains is joyful, the feel exquisiteness, and soil eluviation experiment showed, that this fertilizer can prolong the fertilizer validity period significantly, improves fertilizer efficiency, promotes plant growth, increasing both production and income.The comparable instant nitrogenousfertilizer utilization ratio of this product improves 10%-30%, and can realize disposable heavy dressing, can effectively increase productivity.The keeping validity period of base manure can reach 90-120 days in addition, and the fertilizer efficiency time is long, and general slow-release fertilizer is also with regard to about 2 months.
Claims (8)
1. a slow-release microcapsule fertilizer comprises core and wall film, and core is a fertilizer, it is characterized in that the wall film comprises chitosan and gum arabic two components.
2. a kind of slow-release microcapsule fertilizer according to claim 1 is characterized in that the proportioning of wall membrane component is: the mass concentration of chitosan is that 5%～15% the aqueous solution and gum arabic mass concentration are 5%～15% the aqueous solution.
3. a kind of slow-release microcapsule fertilizer according to claim 1 is characterized in that wall putamina glycan is the soluble poly chitose of modification.
4. according to claim 1 or 2,3 described a kind of slow-release microcapsule fertilizers, it is characterized in that described core is the mixture of fertilizer and auxiliary, its mass ratio is: fertilizer: auxiliary=1: 0.3-0.5.
5. a kind of slow-release microcapsule fertilizer according to claim 4 is characterized in that described fertilizer is the mixture of urea and sylvite.
6. a kind of slow-release microcapsule fertilizer according to claim 4 is characterized in that described auxiliary is a plant-growth regulator.
7. a kind of slow-release microcapsule fertilizer according to claim 5, the mass ratio that it is characterized in that the mixture of described urea and sylvite is 1: 1.1-1.3.
8. according to above-described a kind of slow-release microcapsule fertilizer, its manufacturing step is as follows:
One, prepares wall film two components and core
(1) it is standby to prepare wall film two components respectively: mass concentration is that 5%～15% chitosan aqueous solution and mass concentration are 5%～15% the gum arabic aqueous solution;
(2) make the water-in-oil emulsion of core, the saturated aqueous solution of fertilizer and auxiliary is dispersed in the vegetables oil, form the water-in-oil emulsion of core, the saturated aqueous solution volume ratio of fertilizer and auxiliary is 1: 1～2.5, and the saturated aqueous solution volume ratio of vegetables oil and fertilizer and auxiliary is 1: 1; The saturated aqueous solution of fertilizer and auxiliary is added stablizer;
Two, the water-in-oil emulsion emulsification of chitosan solution and core obtains dual emulsion
The water-in-oil emulsion that in the chitosan solution of step 1 preparation, adds core, under temperature 25-35 ℃, stir through homogenizer (6000r/min), obtain homogeneous w/o/w[water/oil phase/water] dual emulsion, the addition of the water-in-oil emulsion of core is 10%～20% of wall film quality [Right] content;
Three, the wet microcapsule solution of preparation
Slowly add the standby gum arabic aqueous solution in the step 1 in the dual emulsion that step 2 obtains, continue low speed [50r/min] and stir, regulating the pH value is 3.0, and viscosity is 10-50mPas, and the reaction times is no less than 30min;
Four, add solidifying agent
In the solution that step 3 obtains, add solidifying agent, continue to stir;
Five, spraying drying
The micro-capsule solution that step 4 obtains is sprayed, and granularity is 5-15um, then, dry in spray-drier, 180 ℃ of inlet temperature, air outlet temperature is controlled at 90-100 ℃, obtain the micro-capsule powder, make the micro-capsule water ratio, collect powder and promptly obtain the microcapsule fertilizer product at 3%-8%.
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| CN102731222A (en) * | 2012-06-05 | 2012-10-17 | 四川美丰化工股份有限公司 | Sustained and controlled release compound fertilizer and its preparation method |
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| CN102503663A (en) * | 2011-10-14 | 2012-06-20 | 上海市农业科学院 | Preparation method for microcapsule organic fertilizer |
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| CN103910586B (en) * | 2014-04-28 | 2015-12-02 | 成都新柯力化工科技有限公司 | Slow-release fertilizer of a kind of applicable water-fertilizer integral and preparation method thereof |
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| CN106105707A (en) * | 2016-06-28 | 2016-11-16 | 杭州儒燕科技开发有限公司 | A kind of method for culturing seedlings of bamboo |
| CN106946633A (en) * | 2017-02-23 | 2017-07-14 | 广西大学 | A kind of preparation method of cellulose fatty acid ester water-soluble chemical fertilizer micro-capsule |
| CN107950525A (en) * | 2017-10-31 | 2018-04-24 | 华南理工大学 | A kind of fertilizer microcapsules and preparation method and application |
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