CN110452072A - Fertilizer coats release membranes, film-coated and slow release fertilizer and its preparation method and application - Google Patents
Fertilizer coats release membranes, film-coated and slow release fertilizer and its preparation method and application Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01B—SOIL WORKING IN AGRICULTURE OR FORESTRY; PARTS, DETAILS, OR ACCESSORIES OF AGRICULTURAL MACHINES OR IMPLEMENTS, IN GENERAL
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Abstract
The present invention provides a kind of fertilizer cladding release membranes, film-coated and slow release fertilizer and its preparation method and application, it is related to slow-release material technical field, the fertilizer cladding release membranes include the first coating, the second coating and third coating set gradually from the inside to the outside, first coating is mainly prepared by chitosan, second coating is mainly prepared by nano silica and/or calcium hydroxide, and third coating is mainly prepared by carboxymethyl cellulose and calcium chloride.Fertilizer cladding release membranes provided by the invention can not only realize the controlled release of fertiliser granulates nutrient, and have good compatibility with soil, be easy to degrade, it not will cause environmental pollution, soil can also be improved simultaneously, improves soil pH value, ensure agricultural sustainable development.
Description
Technical field
The present invention relates to slow-release material technical field, more particularly, to a kind of fertilizer cladding release membranes, film-coated and slow release fertilizer and
Preparation method and application.
Background technique
Slow release fertilizer can control nutrient releasing speed, extend fertilizer validity period, reduces fertilizer loss, improves to greatest extent
Utilization rate of fertilizer and the economic benefit of fertilising and society, environmental benefit, meet the needs of entire growth and development stage of crop is to nutrient,
It is one of current fertilizer industry developing direction in China.Slow release fertilizer can regulate and control kernel fertilizer by adjusting coated slow-release material properties
The release of nutrient meets the nutrient demand of Different Crop.The main organic matter coated fertilizer of coated slow-release material and inorganic matter at present
Coated fertilizer, organic matter coated fertilizer mainly have wax, oil, polyolefin, polyurethane and alkyd resin, exist and soil compatibility
It is poor, not degradable and the problem of be also easy to produce environmental pollution；Inorganic matter coated fertilizer mainly has Sulfur, phosphate, silicate, gypsum
Deng, have the shortcomings that poor flexibility, fertilizer slow release performance are poor, it is difficult to realize that truly the control of nutrient is discharged.
In view of this, the present invention is specifically proposed.
Summary of the invention
One of the objects of the present invention is to provide a kind of fertilizer to coat release membranes, in control fertilizer nutrient controlled release
On the basis of, realization is well compatible with soil, is easy to degrade, reduce environmental pollution, and ensures agricultural sustainable development.
Fertilizer provided by the invention coats release membranes, including set gradually from the inside to the outside the first coating, the second coating and
Third coating, first coating are mainly prepared by chitosan, and second coating is mainly prepared by inorganic nanoparticles
It obtains, the third coating is mainly prepared by carboxymethyl cellulose and calcium chloride；The inorganic nanoparticles include nanometer
Silica and/or nanometer calcium hydroxide.
Further, the partial size of the inorganic nanoparticles is 3-30nm, preferably 3-20nm.
Preferably, the mass ratio of the carboxymethyl cellulose and the calcium chloride is 1:3-20, preferably 1:5；
Preferably, the mass ratio of the carboxymethyl cellulose and the inorganic nanoparticles is 1:50-200, preferably 1:
100。
The second object of the present invention is to provide a kind of film-coated and slow release fertilizer, including fertiliser granulates, the fertiliser granulates it is outer
Surface is coated with fertilizer cladding release membranes provided by the invention.
Further, the mass ratio of the fertiliser granulates and the chitosan is 10-300:1, preferably 200:1.
Further, the fertiliser granulates include soluble chemical fertilizer granule and/or microsolubility chemical fertilizer granule.
The third object of the present invention is to provide the preparation method of above-mentioned film-coated and slow release fertilizer, include the following steps:
(a) fertilizer is distributed in the aqueous solution of chitosan, is then granulated, it is dry, obtain the first coating coated fertilizer
First coated fertilizer particle of grain；
(b) the first coated fertilizer particle is distributed in the suspension of inorganic nanoparticles, so that inorganic nanoparticles are negative
The surface for being loaded in the first coated fertilizer particle forms the second coating, dry, obtains the second coated fertilizer particle；
(c) the second coated fertilizer particle is distributed in the mixed solution of carboxymethyl cellulose and calcium chloride, it is dry, it obtains
Third coating coats the film-coated and slow release fertilizer of the second coated fertilizer particle.
Further, in step (a), the mass concentration of the aqueous solution of chitosan is 0.1-3%, preferably 1%；
Preferably, in step (b), the solid content of nano inorganic particle suspension is 1-10wt%, preferably 5wt%；
Preferably, in step (c), the configuration method of the mixed solution of carboxymethyl cellulose and calcium chloride includes following step
Rapid: the pH value for adjusting the aqueous solution of carboxymethyl cellulose is 5.5-6.5, adds calcium chloride, obtains carboxymethyl cellulose and chlorine
Change the mixed solution of calcium；
Preferably, pH value is adjusted by the way that ammonium chloride is added in the aqueous solution of carboxymethyl cellulose；
The mass ratio of ammonium chloride and carboxymethyl cellulose is 1:2-10, preferably 1:4.
Further, step (a), step (b) and step (c) use spray dried form independent be granulated dry
It is dry；
Preferably, in step (a), when being spray-dried, spray dryer inlet temperature is 130-210 DEG C, outlet temperature
Degree is 80-130 DEG C, air velocity 35-60L/min；
Preferably, in step (a), the inlet temperature of spray dryer is 165-175 DEG C, and outlet temperature is 115-125 DEG C,
Air velocity is 52-58L/min；
Preferably, in step (b), when being spray-dried, spray dryer inlet temperature is 130-210 DEG C, outlet temperature
Degree is 90-140 DEG C, air velocity 35-60L/min；
Preferably, in step (b), spray dryer inlet temperature is 165-175 DEG C, and outlet temperature is 125-135 DEG C, empty
Gas velocity is 52-58L/min；
Preferably, in step (c), when being spray-dried, spray dryer inlet temperature is 130-210 DEG C, outlet temperature
Degree is 80-140 DEG C, air velocity 35-60L/min；
Preferably, in step (c), spray dryer inlet temperature is 175-185 DEG C, and outlet temperature is 125-135 DEG C, empty
Gas velocity is 45-55L/min.
The fourth object of the present invention is to provide above-mentioned fertilizer cladding release membranes or film-coated and slow release fertilizer in improvement acid soil
In application；
Preferably, the acid soil includes acid red soil of south China.
Fertilizer cladding release membranes provided by the invention are used for coated fertilizer particle, pass through the appearance bread in fertiliser granulates
The first coating, the second coating and third coating set gradually from the inside to the outside is covered, and the first coating is mainly prepared by chitosan
It arrives, second coating is mainly prepared by inorganic nanoparticles, and the third coating is mainly by carboxymethyl cellulose and chlorine
To change calcium to be prepared, fertilizer cladding release membranes provided by the invention can not only realize the controlled release of fertiliser granulates nutrient, and
And there is good compatibility with soil, it is easy to degrade, does not will cause environmental pollution, while soil can also be improved, improves soil
Earth pH value ensures agricultural sustainable development.
Film-coated and slow release fertilizer provided by the invention is sustained by coating cladding provided by the invention in the outer surface of fertiliser granulates
Film can not only realize the controlled release of fertiliser granulates nutrient, and have good compatibility with soil, be easy to degrade, no
It will cause environmental pollution, while soil can also be improved, ensure agricultural sustainable development.
The preparation method simple process of film-coated and slow release fertilizer provided by the invention, it is easy to operate, it is big suitable for industrialize
Production reduces production cost.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the film-coated and slow release fertilizer that the embodiment of the present invention 1 provides；
Fig. 2 is the scanning electron microscope diagram for the first coated fertilizer particle that the embodiment of the present invention 1 provides；
Fig. 3 is the scanning electron microscope diagram for the second coated fertilizer particle section that the embodiment of the present invention 1 provides；
Fig. 4 is the scanning electron microscope diagram for the film-coated and slow release fertilizer section that the embodiment of the present invention 1 provides.
Icon: 101- the first coated fertilizer particle；The second coating of 102-；103- third coating.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with embodiment, it is clear that described reality
Applying example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
According to an aspect of the present invention, the present invention provides a kind of fertilizer to coat release membranes, including from the inside to the outside successively
The first coating, the second coating and the third coating being arranged, first coating are mainly prepared by chitosan, second packet
Film is mainly prepared by inorganic nanoparticles, and the third coating is mainly prepared by carboxymethyl cellulose and calcium chloride,
Inorganic nanoparticles include nano silica and/or calcium hydroxide.
In the present invention, the inorganic nanoparticles include nano silica and/or nanometer calcium hydroxide, that is, inorganic to receive
Rice grain may include nano silica, also may include a nanometer calcium hydroxide, can also include nano silica and nanometer
The mixture of calcium hydroxide.
Nano silica is a kind of inorganic chemical industry material, can improve soil, corrects soil aciditiy, promotes organic matter
Decomposition, reduce phosphorus fixation in the soil.
Calcium hydroxide is a kind of white powdery solids, is commonly called as white lime, is a kind of diacidic base, has the general character of alkali, no
Acid soil can be only improved, is easy to crops existence, and there is anti-microbial property, crops is avoided to be corroded by insect pest.
Primary raw material by using nano silica and/or calcium hydroxide as the second coating, so that fertilizer cladding is slow
Acid soil can more effectively be improved by releasing film, improve the pH value of acid soil, promote the growth of crops.
In the present invention, the first coating is mainly prepared by chitosan, and chitosan is a kind of natural polymer, is had good
Good biocompatibility, microbic resolvability and anti-microbial property can effectively improve the antibacterial of soil after coated fertilizer particle
Performance, the second coating are mainly prepared by inorganic nanoparticles, can not only increase the nutrient of soil, and can regulate and control soil
The pH value of earth improves acid soil；Third coating is mainly prepared by carboxymethyl cellulose and calcium chloride crosslinking, close to coat
Outside the second coating, can not only Effective Regulation fertiliser granulates nutrient sustained release, and be capable of the drop of the second coating of Effective Regulation
Speed is solved, to effectively realize the Effective Regulation of the pH value of soil.
Fertilizer cladding release membranes provided by the invention are used for coated fertilizer particle, pass through the appearance bread in fertiliser granulates
The first coating, the second coating and third coating set gradually from the inside to the outside is covered, and the first coating is mainly prepared by chitosan
It arrives, second coating is mainly prepared by inorganic nanoparticles, and the third coating is mainly by carboxymethyl cellulose and chlorine
To change calcium to be prepared, fertilizer cladding release membranes provided by the invention can not only realize the controlled release of fertiliser granulates nutrient, and
And there is good compatibility with soil, it is easy to degrade, does not will cause environmental pollution, while soil can also be improved, ensures agriculture
Industry sustainable development.
In the preferred embodiment of the present invention, chitosan is low-molecular weight chitoglycan, number-average molecular weight 50-
190kDa prepares the first coating to be more conducive to the dissolution of chitosan.
It is typical but non-limiting, the number-average molecular weight of chitosan for example 50kDa, 80kDa, 100kDa, 120kDa,
150kDa, 180kDa or 190kDa.
In the preferred embodiment of the present invention, the partial size of inorganic nanoparticles is 3-30nm, preferably 3-20nm.
By control inorganic nanoparticles partial size be 3-30nm, in favor of control inorganic nanoparticles and soil it is compatible
Property, so that soil is more effectively improved, and especially when the partial size of inorganic nanoparticles is 3-20nm, more conducively soil improvement.
It is typical but non-limiting, for example 3,5,8,10,12,15,18,20,25 or 30nm of the partial size of inorganic nanoparticles.
In the preferred embodiment of the present invention, the mass ratio of carboxymethyl cellulose and calcium chloride is 1:3-20, excellent
It is selected as 1:5.
In the present invention, third coating is mainly prepared by carboxymethyl cellulose and calcium chloride crosslinking, so that the
Three coatings are more fine and close, with the rate of release of more effective conditioned fertilizer product nutrient, keep its slow release effect more excellent.
It is typical but non-limiting, the typical but non-limiting mass ratio for example 1:3 of carboxymethyl cellulose and calcium chloride, 1:
5,1:8,1:10,1:15 or 1:20, especially when the mass ratio of carboxymethyl cellulose and calcium chloride is 1:5, fertilizer cladding is slow
Release the slow controlled-release effect of film more preferably.
In the preferred embodiment of the present invention, the mass ratio of carboxymethyl cellulose and inorganic nanoparticles is 1:
50-200, preferably 1:100.
It is 1:50-200 by the mass ratio of control carboxymethyl cellulose and inorganic nanoparticles, to regulate and control inorganic nano
The release efficiency of grain, thus the improvement efficiency of Effective Regulation soil, especially when carboxymethyl cellulose and inorganic nanoparticles
Mass ratio is 1:100, and the release efficiency of inorganic nanoparticles is more preferably.
It is typical but non-limiting, the mass ratioes of carboxymethyl cellulose and inorganic nanoparticles is 1:50,1:60,1:75,
1:80,1:90,1:100,1:120,1:150 or 1:200.
According to the second aspect of the invention, the present invention provides a kind of film-coated and slow release fertilizer, including fertiliser granulates, fertilizer
The outer surface of grain is coated with fertilizer cladding release membranes provided by the invention.
Film-coated and slow release fertilizer provided by the invention is sustained by coating cladding provided by the invention in the outer surface of fertiliser granulates
Film can not only realize the controlled release of fertiliser granulates nutrient, and have good compatibility with soil, be easy to degrade, no
It will cause environmental pollution, while soil can also be improved, ensure agricultural sustainable development.
In the preferred embodiment of the present invention, the mass ratio of fertiliser granulates and chitosan is 10-300:1, preferably
For 200:1.
It is 10-300:1 by the mass ratio of control fertiliser granulates and chitosan, chitosan is enabled preferably to coat fertilizer
Expect particle, achievees the effect that antibacterial presses down worm, especially when the mass ratio of fertiliser granulates and chitosan is 200:1, chitosan pair
The covered effect of fertiliser granulates is more preferable.
It is typical but non-limiting, the mass ratio of fertiliser granulates and chitosan for example 10:1,20:1,50:1,80:1,100:
1,120:1,150:1,180:1 or 200:1.
In the preferred embodiment of the present invention, fertiliser granulates include soluble chemical fertilizer granule and/or microsolubility
Fertile particle, that is, fertiliser granulates both may include soluble chemical fertilizer granule or may include microsolubility chemical fertilizer granule, can also wrap
Include the mixture of soluble chemical fertilizer granule and microsolubility chemical fertilizer granule.
In a preferred embodiment of the present invention, fertiliser granulates include but is not limited to various fertiliser granulates, such as barnyard manure particle, chemical fertilizer
Particle and bacterial manure particle etc., details are not described herein.
In a preferred embodiment of the invention, the partial size of fertiliser granulates is not construed as limiting, and fertiliser granulates are dissolved in the water into
It can also be by way of ball milling, so that fertiliser granulates disperse in water if fertiliser granulates are slightly soluble state in water for ion
More evenly, subsequent to be dissolved in the aqueous solution of chitosan, during granulation, obtain the first coating packet of chitosan formation
Cover the first coated fertilizer particle of fertiliser granulates.
According to the third aspect of the present invention, the present invention provides the preparation method of above-mentioned film-coated and slow release fertilizer, including it is as follows
Step:
(a) fertilizer is distributed in the aqueous solution of chitosan, granulating and drying, obtains the of the first coating coated fertilizer particle
One coated fertilizer particle；
(b) the first coated fertilizer particle is distributed in the suspension of inorganic nanoparticles, so that inorganic nanoparticles are negative
The surface for being loaded in the first coated fertilizer particle forms the second coating, and granulating and drying obtains the second coated fertilizer particle；
(c) the second coated fertilizer particle is distributed in the mixed solution of carboxymethyl cellulose and calcium chloride, granulating and drying,
Obtain the film-coated and slow release fertilizer that third coating coats the second coated fertilizer particle.
In the present invention, in step (a), in the first coated fertilizer particle, chitosan is randomly wound in fertiliser granulates surface,
Even there is also chitosans inside the first coated fertilizer particle.
In the present invention, since chitosan contains hydroxyl, the first coated fertilizer particle surface has electropositive, and
Nano silica or nanometer niter gray surface have a negative electricity, in step (b), nano silica (or calcium hydroxide) and the first packet
The electrostatic self-assembled principle that fertiliser granulates are interacted by positive and negative charge is covered, by the first coated fertilizer particles coat, forms the
Two coatings.
The preparation method simple process of film-coated and slow release fertilizer provided by the invention, it is easy to operate, it is big suitable for industrialize
Production reduces production cost.
In the preferred embodiment of the present invention, the mass concentration of the aqueous solution of chitosan is 0.1-3%, preferably
1%.
Mass concentration by the aqueous solution for controlling chitosan is 0.1-3%, is gathered so that fertilizer is dissolved or dispersed in shell
It in the aqueous solution of sugar, is granulated conducive to subsequent, so that Chitosan-coated forms the first coating in the outer surface of fertiliser granulates, especially
It is the more conducively formation of the first coating when the mass concentration of the aqueous solution of chitosan is 1%.
It is typical but non-limiting, the mass concentration of the aqueous solution of chitosan for example 0.1%, 0.2%, 0.5%, 0.8%,
1%, 1.5%, 2%, 2.5% or 3%.
In the preferred embodiment of the present invention, during carrying out the aqueous solution configuration of chitosan, shell is gathered
Sugar is dissolved in the water, and suitable acetic acid can be added, to promote the dissolution of chitosan.
In the preferred embodiment of the present invention, in step (b), the solid content of nano inorganic particle suspension is 1-
10wt%, preferably 5wt%.
It in a preferred embodiment of the invention, is 1- by controlling the solid content of inorganic nanoparticles suspension
10wt% is adsorbed in the surface of the first coating of chitosan formation, forms the so that inorganic nanoparticles are under electrostatic interaction
Two coatings, especially when the solid content of nano inorganic particle suspension is 5wt%, inorganic nanoparticles are in the first envelope membrane surface
What is adsorbed is more uniform.
It is typical but non-limiting, solid content for example 1wt%, 2wt% of nano inorganic particle suspension, 2.5wt%,
3wt%, 3.5wt%, 4wt%, 4.5wt%, 5wt%, 8wt% or 10wt%.
In the preferred embodiment of the present invention, the configuration method of the mixed solution of carboxymethyl cellulose and calcium chloride
The pH value for including the following steps: to adjust the aqueous solution of carboxymethyl cellulose is 5.5-6.5, adds calcium chloride, obtains carboxymethyl
The mixed solution of cellulose and calcium chloride.
PH value by adjusting the aqueous solution of carboxymethyl cellulose is 5.5-6.5, so that calcium chloride and carboxymethyl cellulose
Crosslinking it is more abundant, the third coating of formation is more fine and close, more can Effective Regulation film-coated and slow release fertilizer rate of release.
In present invention further optimization embodiment, by the way that ammonium chloride is added in the aqueous solution of carboxymethyl cellulose
PH value is adjusted, the pH value for adjusting the aqueous solution of carboxymethyl cellulose using ammonium chloride is highly efficient, and will not quote foreign ion.
In still more preferably embodiment of the invention, the mass ratio of ammonium chloride and carboxymethyl cellulose is 1:2-
10, preferably 1:4.
It is 1:2-10 by the mass ratio of regulation ammonium chloride and carboxymethyl cellulose, effectively to realize carboxymethyl cellulose
The regulation of pH value, especially when the mass ratio of ammonium chloride and carboxymethyl cellulose is 1:4, after calcium chloride is added, carboxymethyl is fine
Dimension element carries out more abundant with calcium chloride cross-linking reaction.
It is typical but non-limiting, the mass ratio of ammonium chloride and carboxymethyl cellulose for example 1:2,1:4,1:4.5,1:5,1:
5.5,1:6,1:8 or 1:10.
In the preferred embodiment of the present invention, step (a), step (b) and step (c) are independent using spray
Mist drying mode carries out granulating and drying, slow more effectively to regulate and control the first coated fertilizer particle, the second coated fertilizer particle and coating
The partial size for releasing fertilizer, so that the partial size of film-coated and slow release fertilizer is more uniform.
In the preferred embodiment of the present invention, in step (a), when being spray-dried, spray dryer entrance
Temperature is 130-210 DEG C, and outlet temperature is 80-130 DEG C, air velocity 35-60L/min, so that the first coated fertilizer
The uniform particle sizes of grain, and drying efficiency is high.
In present invention further optimization embodiment, spray dryer inlet temperature is 165-175 DEG C, outlet temperature
It is 115-125 DEG C, air velocity 50-60L/min.
It is typical but non-limiting, in step (a), spray dryer inlet temperature for example 165,166,167,168,169,
170,171,172,173,174 or 175 DEG C；Outlet temperature for example 115,116,117,118,119,120,121,122,123,
124 or 125 DEG C, for example 50,51,52,53,54,55,56,57,58,59 or 60L/min of air velocity.
In the preferred embodiment of the present invention, in step (b), when being spray-dried, spray dryer entrance
Temperature is 130-210 DEG C, and outlet temperature is 90-140 DEG C, air velocity 35-60L/min, so that the second coated fertilizer
The partial size of grain is more uniform, and drying efficiency is higher.
In present invention further optimization embodiment, in step (b), spray dryer inlet temperature is 155-165
DEG C, outlet temperature is 115-125 DEG C, air velocity 45-55L/min.
It is typical but non-limiting, in step (b), spray dryer inlet temperature for example, 155,156,157,158,
159,160,161,162,163,164 or 165 DEG C；Outlet temperature for example 115,116,117,118,119,120,121,122,
123,124 or 125 DEG C, for example 45,46,47,48,49,50,51,52,53,54 or 55L/min of air velocity.
In the preferred embodiment of the present invention, in step (c), when being spray-dried, spray dryer entrance
Temperature is 130-210 DEG C, and outlet temperature is 80-140 DEG C, air velocity 35-60L/min, so that the grain of film-coated and slow release fertilizer
Diameter is more uniform, and drying efficiency is higher.
In present invention further optimization embodiment, in step (c), spray dryer inlet temperature is 165-
175 DEG C, outlet temperature is 125-135 DEG C, air velocity 50-60L/min.
It is typical but non-limiting, in step (c), spray dryer inlet temperature for example 165,166,167,168,169,
170,171,172,173,174 or 175 DEG C；Outlet temperature for example 125,126,127,128,129,130,131,132,133,
134 or 135 DEG C, for example 50,51,52,53,54,55,56,57,58,59 or 60L/min of air velocity.
According to the fifth aspect of the present invention, the present invention provides fertilizer cladding release membranes or the present invention provided by the invention and mentions
Application of the film-coated and slow release fertilizer of confession in improvement soil.
After fertilizer cladding release membranes provided by the invention are applied to soil, there is good compatibility with soil, be easy to drop
Solution, not will cause environmental pollution, while can also improve soil, improve soil pH value, ensure agricultural sustainable development.
Film-coated and slow release fertilizer provided by the invention coats cladding release membranes provided by the invention in the outer surface of fertiliser granulates, no
It only can be realized the controlled release of fertiliser granulates nutrient, and there is good compatibility with soil, be easy to degrade, not will cause
Environmental pollution, while soil can also be improved, the pH value of soil is improved, ensures agricultural sustainable development.
Red Soils in Southern China area cultivated area accounts for a quarter in the whole nation, and hydrothermal condition abundant makes the region become me
The important grain of state, fruit and vegetable production base.But the weather conditions of the region high temperature and rainy cause strong weathering and eluviation,
Lead to soil nutrient deficiency and constantly acidification, seriously threaten national food security, ecological safety, restricts hiding grain in the reality of ground strategy
It applies.A large amount of applications of various human activities, especially chemical fertilizer accelerate red soil acidification process simultaneously.
In the preferred embodiment of the present invention, fertilizer cladding release membranes provided by the invention or coated slow-release film are suitable
It after acid red soil of south China, can significantly improve, ensure the sustainable development of agricultural.
Technical solution provided by the invention is further described below with reference to embodiment and comparative example.
Embodiment 1
A kind of fertilizer coating slow-release fertilizer is present embodiments provided, structure is as shown in Figure 1, coating provided in this embodiment is slow
Fertilizer is released with the first coated fertilizer particle 101 as core, from the inside to the outside successively includes the second coating 102 and third coating 103,
In, the first coated fertilizer particle 101 is granulated after being mainly dispersed in the aqueous solution of chitosan by fertilizer and obtains, in the first cladding fertilizer
Expect in particle 101, chitosan, which is randomly coated on fertiliser granulates, forms the first coating, and the second coating 102 is mainly by nano-silica
SiClx is prepared, and third coating 103 is mainly prepared by carboxymethyl cellulose and calcium chloride.
Fertilizer coating slow-release fertilizer provided in this embodiment is prepared in accordance with the following steps:
It (1) is aqueous solution that 50-190kDa chitosan is configured to that mass concentration is 1% by number-average molecular weight, and water-soluble
The acetic acid that appropriate mass concentration is 1% is added in liquid, so that chitosan dissolution is completely, obtains the aqueous solution of chitosan；
(2) ammonium nitrate fertilizer is distributed in the aqueous solution of chitosan, the additional amount and shell of ammonium nitrate fertilizer particle
The mass ratio of glycan is 200:1；
(3) granulating and drying, entrance are carried out using spray dryer by the mixed liquor that spray drying obtains step (2)
Temperature is 170 DEG C, and outlet temperature is 120 DEG C, air velocity 55L/min,；Wriggling pump power output is 10%, obtains first
Coated fertilizer particle 101；
(4) the first coated fertilizer particle 101 is poured into nano silica suspension, the partial size model of nano silica
Enclose 3-30nm, the suspended fluid solid content 5wt% of nano silica；
(5) the mixed liquor stirring 30min obtained (4) carries out granulating and drying using spray dryer, and spray dryer enters
170 DEG C of temperature of mouth, 130 DEG C of outlet temperature, air velocity 55L/min, peristaltic pump output 10% obtains the second coated fertilizer
Grain；
(6) aqueous solution for the carboxymethyl cellulose that mass concentration is 1% is prepared, and ammonium chloride is added and adjusts acid, chlorination
The mass ratio of ammonium dosage and carboxymethyl cellulose is 1:4, and stirring to ammonium chloride is completely dissolved；
(7) it is added calcium chloride in the solution that (6) obtain, the mass ratio of calcium chloride and carboxymethyl cellulose is 1:5, is obtained
The mixed solution of carboxymethyl cellulose and calcium chloride；
(8) in the mixed solution for obtaining the second coated fertilizer particle addition (7), carboxymethyl cellulose and nanometer titanium dioxide
The mass ratio of silicon is 1:100, after stirring 30min, using spray dryer granulating and drying, and 180 DEG C of spray dryer inlet temperature；
130 DEG C of outlet temperature, air velocity 50L/min；Peristaltic pump output 10%, obtains film-coated and slow release fertilizer.
Embodiment 2
Present embodiments provide a kind of film-coated and slow release fertilizer, the coated slow-release film that structure is provided with embodiment 1, herein no longer
It repeats, preparation method carries out in accordance with the following steps:
It (1) is aqueous solution that 50-190kDa chitosan is configured to that mass concentration is 2% by number-average molecular weight, and water-soluble
The acetic acid that appropriate mass concentration is 1.5% is added in liquid, so that chitosan dissolution is completely, obtains the aqueous solution of chitosan；
(2) ammonium nitrate fertilizer particle is distributed in the aqueous solution of chitosan, the additional amount of ammonium nitrate fertilizer particle
Mass ratio with chitosan is 230:1；
(3) granulating and drying, entrance are carried out using spray dryer by the mixed liquor that spray drying obtains step (2)
Temperature is 150 DEG C, and outlet temperature is 110 DEG C, air velocity 35L/min,；Wriggling pump power output is 8%, obtains the first packet
Cover fertiliser granulates；
(4) the first coated fertilizer particle is poured into nano silica suspension, the particle size range of nano silica
10-30nm, the suspended fluid solid content 6wt% of nano silica；
(5) the mixed liquor stirring 30min obtained (4) carries out granulating and drying using spray dryer, and spray dryer enters
180 DEG C of temperature of mouth, 120 DEG C of outlet temperature, air velocity 50L/min, peristaltic pump output 15% obtains the second coated fertilizer
Grain；
(6) aqueous solution for the carboxymethyl cellulose that mass concentration is 2% is prepared, and ammonium chloride is added and adjusts acid, chlorination
The mass ratio of ammonium dosage and carboxymethyl cellulose is 1:3, and stirring to ammonium chloride is completely dissolved；
(7) it is added calcium chloride in the solution that (6) obtain, the mass ratio of calcium chloride and carboxymethyl cellulose is 1:8, is obtained
The mixed solution of carboxymethyl cellulose and calcium chloride；
(8) in the mixed solution for obtaining the second coated fertilizer particle addition (7), carboxymethyl cellulose and nanometer titanium dioxide
The mass ratio of silicon is 1:120, after stirring 30min, using spray dryer granulating and drying, and 160 DEG C of spray dryer inlet temperature；
115 DEG C of outlet temperature, air velocity 45L/min；Peristaltic pump output 5%, obtains film-coated and slow release fertilizer.
Embodiment 3
Present embodiments provide a kind of film-coated and slow release fertilizer, the coated slow-release film that structure is provided with embodiment 1, herein no longer
It repeats, preparation method carries out in accordance with the following steps:
It (1) is aqueous solution that 50-190kDa chitosan is configured to that mass concentration is 1.5% by number-average molecular weight, and in water
The acetic acid that appropriate mass concentration is 1% is added in solution, so that chitosan dissolution is completely, obtains the aqueous solution of chitosan；
(2) ammonium nitrate fertilizer particle is distributed in the aqueous solution of chitosan, the additional amount of ammonium nitrate fertilizer particle
Mass ratio with chitosan is 200:1；
(3) granulating and drying, entrance are carried out using spray dryer by the mixed liquor that spray drying obtains step (2)
Temperature is 160 DEG C, and outlet temperature is 120 DEG C, air velocity 45L/min,；Wriggling pump power output is 10%, obtains first
Coated fertilizer particle；
(4) the first coated fertilizer particle is poured into nanometer calcium hydroxide suspension, the particle size range 3- of nanometer calcium hydroxide
20nm, the suspended fluid solid content 5wt% of nanometer calcium hydroxide；
(5) the mixed liquor stirring 30min obtained (4) carries out granulating and drying using spray dryer, and spray dryer enters
170 DEG C of temperature of mouth, 110 DEG C of outlet temperature, air velocity 50L/min, peristaltic pump output 5% obtains the second coated fertilizer particle；
(6) aqueous solution for the carboxymethyl cellulose that mass concentration is 1% is prepared, and ammonium chloride is added and adjusts acid, chlorination
The mass ratio of ammonium dosage and carboxymethyl cellulose is 1:4, and stirring to ammonium chloride is completely dissolved；
(7) it is added calcium chloride in the solution that (6) obtain, the mass ratio of calcium chloride and carboxymethyl cellulose is 1:5, is obtained
The mixed solution of carboxymethyl cellulose and calcium chloride；
(8) in the mixed solution for obtaining the second coated fertilizer particle addition (7), carboxymethyl cellulose and nanometer titanium dioxide
The mass ratio of silicon is 1:80, after stirring 30min, using spray dryer granulating and drying, and 180 DEG C of spray dryer inlet temperature；
130 DEG C of outlet temperature, air velocity 55L/min；Peristaltic pump output 15%, obtains film-coated and slow release fertilizer.
Embodiment 4
Present embodiments provide a kind of film-coated and slow release fertilizer, the coated slow-release film that structure is provided with embodiment 1, herein no longer
It repeats, preparation method carries out in accordance with the following steps:
It (1) is aqueous solution that 50-190kDa chitosan is configured to that mass concentration is 1.5% by number-average molecular weight, and in water
The acetic acid that appropriate mass concentration is 1% is added in solution, so that chitosan dissolution is completely, obtains the aqueous solution of chitosan；
(2) ammonium nitrate fertilizer particle is distributed in the aqueous solution of chitosan, the additional amount of ammonium nitrate fertilizer particle
Mass ratio with chitosan is 200:1；
(3) granulating and drying, entrance are carried out using spray dryer by the mixed liquor that spray drying obtains step (2)
Temperature is 140 DEG C, and outlet temperature is 110 DEG C, air velocity 50L/min,；Wriggling pump power output is 5%, obtains the first packet
Cover fertiliser granulates；
(4) the first coated fertilizer particle is poured into nanometer calcium hydroxide suspension, the particle size range 3- of nanometer calcium hydroxide
20nm, the suspended fluid solid content 5wt% of nanometer calcium hydroxide；
(5) the mixed liquor stirring 30min obtained (4) carries out granulating and drying using spray dryer, and spray dryer enters
140 DEG C of temperature of mouth, 100 DEG C of outlet temperature, air velocity 50L/min, peristaltic pump output 5% obtains the second coated fertilizer particle；
(6) aqueous solution for the carboxymethyl cellulose that mass concentration is 1% is prepared, and ammonium chloride is added and adjusts acid, chlorination
The mass ratio of ammonium dosage and carboxymethyl cellulose is 1:5, and stirring to ammonium chloride is completely dissolved；
(7) it is added calcium chloride in the solution that (6) obtain, the mass ratio of calcium chloride and carboxymethyl cellulose is 1:5, is obtained
The mixed solution of carboxymethyl cellulose and calcium chloride；
(8) in the mixed solution for obtaining the second coated fertilizer particle addition (7), carboxymethyl cellulose and nanometer calcium hydroxide
Mass ratio be 1:80, after stirring 30min, using spray dryer granulating and drying, 140 DEG C of spray dryer inlet temperature；Out
110 DEG C of temperature of mouth, air velocity 55L/min；Peristaltic pump output 5%, obtains film-coated and slow release fertilizer.
Embodiment 5
Present embodiments provide a kind of film-coated and slow release fertilizer, the coated slow-release film that structure is provided with embodiment 1, preparation side
Method difference from example 1 is that, in step (2), the mass ratio of ammonium nitrate fertilizer particle and chitosan is 10:1,
Remaining step is with embodiment 1, and details are not described herein.
Embodiment 6
Present embodiments provide a kind of film-coated and slow release fertilizer, the coated slow-release film that structure is provided with embodiment 1, preparation side
Method difference from example 1 is that, in step (2), the mass ratio of ammonium nitrate fertilizer particle and chitosan is 300:1,
Remaining step is with embodiment 1, and details are not described herein.
Embodiment 7
Present embodiments provide a kind of film-coated and slow release fertilizer, the coated slow-release film that structure is provided with embodiment 1, preparation side
Method difference from example 1 is that, in step (8), the mass ratio of carboxymethyl cellulose and nano silica is 1:
50, remaining step is with embodiment 1, and details are not described herein.
Embodiment 8
Present embodiments provide a kind of film-coated and slow release fertilizer, the coated slow-release film that structure is provided with embodiment 1, preparation side
Method difference from example 1 is that, in step (8), the mass ratio of carboxymethyl cellulose and nano silica is 1:
200, remaining step is with embodiment 1, and details are not described herein.
Embodiment 9
Present embodiments provide a kind of film-coated and slow release fertilizer, the coated slow-release film that structure is provided with embodiment 1, preparation side
Method difference from example 1 is that, in step (7), the mass ratio of calcium chloride and carboxymethyl cellulose is 1:3, remaining
Step is with embodiment 1, and details are not described herein.
Embodiment 10
Present embodiments provide a kind of film-coated and slow release fertilizer, the coated slow-release film that structure is provided with embodiment 1, preparation side
Method difference from example 1 is that, in step (7), the mass ratio of calcium chloride and carboxymethyl cellulose is 1:20, remaining
Step is with embodiment 1, and details are not described herein.
Comparative example 1
This comparative example provides a kind of film-coated and slow release fertilizer, using chitosan particle as core, the outer surface of chitosan particle from
It is interior to being successively coated with the first coating being mainly prepared by nano silica outside and mainly by carboxymethyl cellulose and chlorine
Change calcium and the second coating is prepared, preparation method is with the difference of embodiment 1, step (2) is not carried out, directly by step
(1) chitosan particle is prepared by spray drying in the aqueous solution of the chitosan obtained, in the appearance bread of chitosan particle
The same embodiment step of the step of covering the first coating and the second coating (4)-(8), details are not described herein.
Comparative example 2
This comparative example provides a kind of film-coated and slow release fertilizer, and the first cladding to be formed is granulated with ammonium nitrate fertilizer and chitosan
Fertiliser granulates are core, and the outer surface of the first coated fertilizer particle is coated with the second coating, wherein the second coating is mainly by nanometer two
Silica is prepared, and preparation method is with step (1)-(5) in embodiment 1, and details are not described herein.
Comparative example 3
This comparative example provides a kind of film-coated and slow release fertilizer, and the first cladding to be formed is granulated with ammonium nitrate fertilizer and chitosan
Fertiliser granulates are core, and the outer surface of the first coated fertilizer particle is coated with the second coating, wherein the second coating is mainly by carboxymethyl
Cellulose and calcium chloride are prepared, step (1)-(3) same to embodiment step (1)-(3) in preparation method, no longer superfluous herein
It states, remaining step (4)-(6) is as follows:
(4) aqueous solution for the carboxymethyl cellulose that mass concentration is 1% is prepared, and ammonium chloride is added and adjusts acid, chlorination
The mass ratio of ammonium dosage and carboxymethyl cellulose is 1:4, and stirring to ammonium chloride is completely dissolved；
(5) it is added calcium chloride in the solution that (4) obtain, the mass ratio of calcium chloride and carboxymethyl cellulose is 1:5, is obtained
The mixed solution of carboxymethyl cellulose and calcium chloride；
(6) the first coated fertilizer particle that step (3) is prepared is added in the mixed solution that (6) obtain, carboxymethyl
Cellulose and the mass ratio of nano silica are 1:100, spraying dry using spray dryer granulating and drying after stirring 30min
180 DEG C of dry machine inlet temperature；130 DEG C of outlet temperature, air velocity 50L/min；Peristaltic pump output 10%, obtains coated slow-release
Fertilizer.
Test example 1
The first coated fertilizer, the second coated fertilizer and the coated slow-release being prepared using scanning electron microscope observation embodiment 1
The structure of fertilizer, wherein Fig. 2 is the scanning electron microscope diagram for the first coated fertilizer particle that the embodiment of the present invention 1 provides；Fig. 3
For the scanning electron microscope diagram for the second coated fertilizer particle section that the embodiment of the present invention 1 provides；Fig. 4 is the embodiment of the present invention
The scanning electron microscope diagram of the 1 film-coated and slow release fertilizer section provided.
Figure it is seen that the first coated fertilizer particle diameter distribution that the present embodiment 1 provides is more uniform, it is distributed in 1-
5um.From figure 3, it can be seen that in the second coated fertilizer that the present embodiment 1 provides, the second coating packet of nano silica formation
Cover the first coated fertilizer particle.From fig. 4, it can be seen that the outer surface for the coated slow-release film that the present embodiment 1 provides is coated with one
The film that layer carboxymethyl cellulose and calcium chloride are formed.
Test example 2
Setting test soil 1 and control soil 1, the film-coated and slow release fertilizer that embodiment 1 is provided is respectively according to every 10kg soil
The dosage for putting into 40g fertilizer cladding release membranes applies in test soil 1, while control soil 1 is arranged, and applies in control soil 1
Enter the ammonium nitrate fertilizer particle with the film-coated and slow release fertilizer moderate applied in embodiment 1, after two months, difference testing experiment soil
1 and control soil 1 pH value, the results are shown in Table 1.
In addition, setting test soil 2-13 and control soil 2-13, test soil 2-11 apply respectively embodiment 2-10 and
The film-coated and slow release fertilizer that comparative example 1-3 is provided, and applied according to the dosage of every 10kg soil investment 40g fertilizer cladding release membranes, it is right
Apply the ammonium nitrate fertilizer with the embodiment 2-10 and comparative example 1-3 film-coated and slow release fertilizer moderate provided respectively according to soil 2-13
Grain, after two months, difference testing experiment soil 2-13 and the pH value to reference examples soil 2-13, the results are shown in Table 1.
Wherein, test soil 1-13 and control soil 1-13 is with batch soil.
Table 1
Note: the meaning of above-mentioned "+" is pH value raising, and the meaning of "-" is pH value reduction.
Test example 3
According to the method and requirement of slow-release fertilizer national standard (GB/T23348-2009), the coating that embodiment 1-8 is provided
Slow-release fertilizer carries out sustained release performance test, and concrete outcome is as shown in table 2.
Table 2
| Project | Initial stage nutrient release rate (%) | 28 days accumulation nutrient release rates (%) |
| GB/T23348-2009 | ≤15 | ≤80 |
| Embodiment 1 | 10 | 65 |
| Embodiment 2 | 12 | 70 |
| Embodiment 3 | 9 | 63 |
| Embodiment 4 | 9 | 64 |
| Embodiment 5 | 14 | 75 |
| Embodiment 6 | 8 | 60 |
| Embodiment 7 | 11 | 67 |
| Embodiment 8 | 10 | 64 |
| Embodiment 9 | 10 | 63 |
| Embodiment 10 | 10 | 66 |
From table 2 it can be seen that the film-coated and slow release fertilizer that embodiment 1-10 is provided all has excellent slow release effect.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of fertilizer coats release membranes, which is characterized in that including set gradually from the inside to the outside the first coating, the second coating and
Third coating, first coating are mainly prepared by chitosan, and second coating is mainly prepared by inorganic nanoparticles
It obtains, the third coating is mainly prepared by carboxymethyl cellulose and calcium chloride；
The inorganic nanoparticles include nano silica and/or calcium hydroxide.
2. fertilizer according to claim 1 coats release membranes, which is characterized in that the partial size of the inorganic nanoparticles is 3-
30nm, preferably 3-20nm.
3. fertilizer according to claim 1 coats release membranes, which is characterized in that the carboxymethyl cellulose and the chlorination
The mass ratio of calcium is 1:3-20, preferably 1:5；
Preferably, the mass ratio of the carboxymethyl cellulose and the inorganic nanoparticles is 1:50-200, preferably 1:100.
4. a kind of film-coated and slow release fertilizer, which is characterized in that including fertiliser granulates, the outer surface cladding of the fertiliser granulates has the right to want
Seek the described in any item fertilizer cladding release membranes of 1-3.
5. film-coated and slow release fertilizer according to claim 4, which is characterized in that the quality of the fertiliser granulates and the chitosan
Than for 10-300:1, preferably 200:1.
6. film-coated and slow release fertilizer according to claim 4 or 5, which is characterized in that the fertiliser granulates include soluble chemical fertilizer
Particle and/or microsolubility chemical fertilizer granule.
7. according to the preparation method of the described in any item film-coated and slow release fertilizers of claim 4-6, which is characterized in that including walking as follows
It is rapid:
(a) fertilizer is distributed in the aqueous solution of chitosan, granulating and drying, obtains the first packet of the first coating coated fertilizer particle
Cover fertiliser granulates；
(b) the first coated fertilizer particle is distributed in the suspension of inorganic nanoparticles, so that inorganic nanoparticles are supported on
The surface of first coated fertilizer particle forms the second coating, and granulating and drying obtains the second coated fertilizer particle；
(c) the second coated fertilizer particle is distributed in the mixed solution of carboxymethyl cellulose and calcium chloride, granulating and drying obtains
Third coating coats the film-coated and slow release fertilizer of the second coated fertilizer particle.
8. preparation method according to claim 7, which is characterized in that in step (a), the quality of the aqueous solution of chitosan is dense
Spending is 0.1-3%, preferably 1%；
Preferably, in step (b), the solid content of nano inorganic particle suspension is 1-10wt%, preferably 5wt%；
Preferably, in step (c), the configuration method of the mixed solution of carboxymethyl cellulose and calcium chloride includes the following steps: to adjust
The pH value for saving the aqueous solution of carboxymethyl cellulose is 5.5-6.5, adds calcium chloride, obtains carboxymethyl cellulose and calcium chloride
Mixed solution；
Preferably, pH value is adjusted by the way that ammonium chloride is added in the aqueous solution of carboxymethyl cellulose；
Preferably, the mass ratio of ammonium chloride and carboxymethyl cellulose is 1:2-10, preferably 1:4.
9. preparation method according to claim 7, which is characterized in that step (a), step (b) and step (c) are respectively independent
Using spray dried form carry out granulating and drying；
Preferably, in step (a), when being spray-dried, spray dryer inlet temperature is 130-210 DEG C, and outlet temperature is
80-130 DEG C, air velocity 35-60L/min；
Preferably, in step (a), the inlet temperature of spray dryer is 165-175 DEG C, and outlet temperature is 115-125 DEG C, air
Flow velocity is 52-58L/min；
Preferably, in step (b), when being spray-dried, spray dryer inlet temperature is 130-210 DEG C, and outlet temperature is
90-140 DEG C, air velocity 35-60L/min；
Preferably, in step (b), spray dryer inlet temperature is 165-175 DEG C, and outlet temperature is 125-135 DEG C, air stream
Speed is 52-58L/min；
Preferably, in step (c), when being spray-dried, spray dryer inlet temperature is 130-210 DEG C, and outlet temperature is
80-140 DEG C, air velocity 35-60L/min；
Preferably, in step (c), spray dryer inlet temperature is 175-185 DEG C, and outlet temperature is 125-135 DEG C, air stream
Speed is 45-55L/min.
10. the described in any item fertilizer cladding release membranes of claim 1-3 or the described in any item coated slow-releases of claim 4-6
Application of the fertilizer in improvement acid soil；
Preferably, the acid soil includes acid red soil of south China.
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