CN110885270B - Plant enzyme responsive controlled release fertilizer, nano carrier and preparation method thereof - Google Patents
Plant enzyme responsive controlled release fertilizer, nano carrier and preparation method thereof Download PDFInfo
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- CN110885270B CN110885270B CN201911290997.8A CN201911290997A CN110885270B CN 110885270 B CN110885270 B CN 110885270B CN 201911290997 A CN201911290997 A CN 201911290997A CN 110885270 B CN110885270 B CN 110885270B
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
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Abstract
The invention relates to the technical field of plant nutrition, in particular to a plant enzyme responsive controlled release fertilizer, a nano carrier and a preparation method thereof. Plant nutrients (chemical fertilizer, trace elements and plant growth regulator) are loaded in the tube cavity of the nanotube in a negative pressure adsorption mode, and then a layer of degradable modified carboxymethyl polysaccharide with good biocompatibility is coated on the outer layer of the nanotube through chemical grafting, so that the stability of the fertilizer is improved. The invention can directly enter the crop body through the plant leaf surface, and the outer wall material of the nano carrier is cracked by the plant active enzyme in the crop body, so that the mesoporous or lumen port on the surface of the nano carrier is opened, and the nutrient substance in the lumen is released.
Description
Technical Field
The invention relates to the field of agriculture and chemistry, in particular to a plant enzyme responsive controlled release fertilizer, a nano carrier and a preparation method thereof.
Background
Modern agricultural production relies on chemical fertilizers and pesticides to a great extent to provide sufficient nutrients for crop growth, control various plant diseases and insect pests and remove weeds to ensure healthy growth of crops. However, the soil structure is changed by applying agricultural and chemical products in large quantities for a long time, resulting in a significant reduction in the organic matter content in the soil, resulting in loss of the amount of nutrients in the farmland and a decrease in the soil fertility. The excessive application of chemical fertilizers brings about a plurality of problems, and the main reason is that the absorption and utilization rate of crops to traditional agricultural chemical products is low.
In recent years, the rapid development of nanotechnology provides a new idea for solving the main problem in agricultural production. Nano agriculture applies nano technology to the agricultural field, and is an application for researching nano-scale special materials in agriculture. A brand new nano fertilizer formed by applying nano material technology to construct, modifying and chemically polymerizing by utilizing medical microcapsule technology and chemical microemulsion technology is emerging. The adsorption, wrapping and loading of the traditional fertilizer by using the nano material is an effective way for manufacturing the novel controlled-release nano fertilizer, the fertilizer can be effectively protected from degradation caused by illumination, high temperature and microorganism infection, and the loaded fertilizer can be slowly released due to the adsorption of the nano material, so that the effect of prolonging the fertilizer efficiency is achieved, but the fertilizer loading rate is difficult to guarantee by simple adsorption, and the fertilizer is easy to wash away by water especially in the prior treatment process. In addition, the processing technology of the nano fertilizer, particularly the nano slow/controlled release fertilizer, is not mature and stable, and the action mode and mechanism of the nano slow/controlled release fertilizer in the crop body are not clear, so that the further development and the wide use of the nano slow/controlled release fertilizer are seriously restricted.
In order to solve the problem of the capability of a nano material for efficiently loading a fertilizer, the invention provides a plant enzyme responsive controlled release fertilizer, a nano carrier and a preparation method thereof, which can effectively improve the stability and the loading rate of the fertilizer, and realize the sustained controlled release of the fertilizer and the prolongation of the fertilizer efficiency.
Disclosure of Invention
The invention provides a plant enzyme responsive nano-carrier, and the preparation raw materials of the carrier comprise modified carboxymethyl polysaccharide and a halloysite nanotube with a modified surface amino group.
As an embodiment of the invention, the carrier is prepared from modified carboxymethyl polysaccharide and halloysite nanotubes with surface amino modified through esterification reaction.
As an embodiment of the present invention, the modified carboxymethyl polysaccharide is a modified carboxymethyl polysaccharide;
the carboxymethyl polysaccharide is at least one selected from carboxymethyl cellulose, carboxymethyl starch, sodium alginate, carboxymethyl chitosan and carboxymethyl dextran.
As one embodiment of the invention, the raw materials for preparing the halloysite nanotubes with the surface modified by amino comprise a silane coupling agent and the halloysite nanotubes.
In one embodiment of the present invention, the silane coupling agent is at least one selected from the group consisting of 3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, gamma-aminopropyltrimethoxysilane and gamma-aminopropyltriethoxysilane.
The invention provides a plant enzyme-responsive controlled-release fertilizer, which comprises the plant enzyme-responsive nano-carrier.
The third aspect of the invention provides a preparation method of the plant enzyme-responsive controlled-release fertilizer, which comprises the following steps:
s1, preparation of halloysite nanotubes with surface amino modification
Putting the halloysite nanotube, an organic solvent and a silane coupling agent into a reaction kettle, heating and reacting under the inert gas environment, and centrifugally washing reacted substances to obtain an aminated halloysite nanotube;
s2. functionalized halloysite nanotube loaded fertilizer
Dispersing the aminated halloysite nanotubes obtained in S1 in a plant nutrient solution, and vacuumizing under ultrasonic to obtain aminated halloysite nanotubes loaded with plant nutrient substances;
s3, preparation of modified carboxymethyl polysaccharide
Dissolving carboxymethyl polysaccharide in deionized water to form carboxymethyl polysaccharide solution, adding a modifier and acid, stirring, heating for reaction for 24 hours, washing with absolute ethyl alcohol, and drying to obtain modified carboxymethyl polysaccharide powder;
s4, combination of composite nano controlled release carrier
Dissolving the modified carboxymethyl polysaccharide in deionized water to obtain a modified carboxymethyl polysaccharide solution, adding a certain amount of aminated halloysite nanotubes carrying plant nutrients and sodium bicarbonate, stirring and heating at 50 ℃ for reaction for 24 hours, centrifuging, washing and drying to obtain the plant enzyme-responsive controlled-release fertilizer.
In an embodiment of the present invention, in S1, the organic solvent is at least one selected from the group consisting of toluene, ethanol, and methanol.
In an embodiment of the present invention, the modifier in S3 is at least one selected from epichlorohydrin, epibromohydrin, chloropropene, and bromopropene.
The fourth aspect of the invention provides a use method of the plant enzyme-responsive controlled-release fertilizer, wherein the controlled-release fertilizer is suspended in water and is sprayed on leaf surfaces, so that the controlled-release fertilizer is absorbed by crops and enters plant bodies.
Has the advantages that:
1) the plant enzyme responsive controlled release fertilizer provided by the invention belongs to a nano-scale fertilizer, and can effectively improve the absorption and utilization rate of crops on the fertilizer.
2) After the fertilizer-loaded nano carrier is subjected to functional modification, the fertilizer-loaded nano carrier has plant enzyme stimulation responsiveness, is influenced by crops to release the fertilizer in the nano carrier, and is not stimulated or released.
3) The nano fertilizer can be acted by cellulase or amylase and the like in crops, degrade wall materials on the outer layer of the nano tube, open the mesopores and the lumen ports on the surface of the nano tube and release the fertilizer in the lumen. The controlled release fertilizer with plant enzyme responsiveness can promote the technical development of novel fertilizers and provide a new idea for the research of the novel fertilizers.
Drawings
FIG. 1 is TEM image of polysaccharide and halloysite nanotube composite nanocarrier
FIG. 2 is an SEM image of a composite nanocarrier
FIG. 3 shows the cumulative release rate of salicylic acid at different concentrations of cellulase
FIG. 4 shows the absorption of wheat root subcellular cells to nano-carriers (black dots in the figure are nano-carriers)
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The term "prepared from …" as used herein is synonymous with "including". As used herein, the terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase will render the claim closed except for the materials described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
Approximating language, as used herein in the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received by modifying or otherwise modifying such quantity without substantially changing the basic function to which it is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
The invention provides a plant enzyme responsive nano-carrier, and the preparation raw materials of the carrier comprise modified carboxymethyl polysaccharide and a halloysite nanotube with a modified surface amino group.
Modified carboxymethyl polysaccharide
The modified carboxymethyl polysaccharide is carboxymethyl polysaccharide modified by a modifier.
In one embodiment of the present invention, the carboxymethyl polysaccharide is at least one selected from the group consisting of carboxymethyl cellulose, carboxymethyl starch, sodium alginate, carboxymethyl chitosan, and carboxymethyl dextran.
As an embodiment of the present invention, the modifier is at least one selected from epichlorohydrin, epibromohydrin, chloropropene, and bromopropene.
The preparation method of the modified carboxymethyl polysaccharide comprises the following steps:
s3, dissolving 4-6 g of carboxymethyl polysaccharide in deionized water to obtain a carboxymethyl polysaccharide solution; adding a modifier and an acid in a certain mass ratio, stirring and heating for reaction for 24 hours, then washing with absolute ethyl alcohol for three times, and obtaining a precipitated substance which is modified carboxymethyl polysaccharide, then drying and grinding into powder, and storing in a dryer for later use.
Wherein the mass concentration of the carboxymethyl polysaccharide solution is 1-1.5 wt%; the concentration of the acid is 5-10 mol/L; and the dosage of the acid is 0.2-1 mL. The volume ratio of the acid to the modifier is 1: (5-10); the acid is hydrochloric acid or sulfuric acid.
The preferable technical scheme of the invention is that the mass ratio of the modifier to the carboxymethyl polysaccharide is (1-10): 1, more preferably in a mass ratio of 2: 1.
halloysite nanotube with surface modified by amino
The halloysite nanotube modified by the amino group on the surface is a halloysite nanotube modified by a silane coupling agent with the amino group.
The silane coupling agent with amino is selected from at least one of 3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, gamma-aminopropyltrimethoxysilane and gamma-aminopropyltriethoxysilane.
The preparation method of the halloysite nanotube with the surface modified by amino comprises the following steps:
s1, dispersing the purified halloysite nanotube in a reaction kettle containing an organic solvent, adding a silane coupling agent with amino, heating and reacting under the protection of inert gas, and centrifugally washing the reacted substance to obtain the halloysite nanotube modified by the amino.
In S1, the organic solvent is at least one of toluene, 95 wt% ethanol, 50 wt% ethanol and methanol; the inert gas is at least one of helium, nitrogen and argon; the heating temperature is controlled to be 75-85 ℃, and more preferably 80 ℃.
The invention provides a plant enzyme-responsive controlled-release fertilizer, which comprises the plant enzyme-responsive nano-carrier.
The third aspect of the invention provides a preparation method of the plant enzyme-responsive controlled-release fertilizer, which comprises the following steps:
s1, preparation of halloysite nanotubes with surface amino modification
Putting the halloysite nanotube, an organic solvent and a silane coupling agent into a reaction kettle, heating and reacting under the inert gas environment, and centrifugally washing reacted substances to obtain an aminated halloysite nanotube;
s2. functionalized halloysite nanotube loaded fertilizer
Dispersing the aminated halloysite nanotubes obtained in S1 in a plant nutrient solution, and vacuumizing under ultrasonic to obtain aminated halloysite nanotubes loaded with plant nutrient substances;
s3, preparation of modified carboxymethyl polysaccharide
Dissolving carboxymethyl polysaccharide in deionized water to form carboxymethyl polysaccharide solution, adding a modifier and acid, stirring, heating for reaction for 24 hours, washing with absolute ethyl alcohol, and drying to obtain modified carboxymethyl polysaccharide powder;
s4, combination of composite nano controlled release carrier
Dissolving the modified carboxymethyl polysaccharide in deionized water to obtain a modified carboxymethyl polysaccharide solution, adding a certain amount of aminated halloysite nanotubes carrying plant nutrients and sodium bicarbonate, stirring and heating at 50 ℃ for reaction for 24 hours, centrifuging, washing and drying to obtain the plant enzyme-responsive controlled-release fertilizer.
In a preferred embodiment of the present invention, the organic solvent in S1 is at least one of toluene, 95% ethanol, 50% ethanol, and methanol;
the inert gas is at least one of helium, nitrogen and argon; the heating temperature is controlled to be 75-85 ℃, and more preferably 80 ℃;
in S1, the mass ratio of the halloysite nanotube to the silane coupling agent is (1-5): 1, more preferably in a mass ratio of 2.5: 1.
as a preferred technical solution of the present invention, in S1, the mass-to-volume ratio of the halloysite nanotubes to the organic solvent is 1: (75-85) g/mL.
In a preferred embodiment of the present invention, in S2, the mass ratio of the aminated halloysite nanotube to the plant nutrient is 1: (0.5-5). More preferably, the mass ratio is 1: 1.
in a preferred embodiment of the present invention, the modified carboxymethyl polysaccharide in S4 has a mass concentration of 0.8% to 3%, and more preferably a mass concentration of 0.9% to 1.5%.
As a preferred technical scheme of the invention, the mass ratio of the aminated halloysite nanotube to the modified carboxymethyl polysaccharide is 1: (1-10), and the more preferable mass ratio is 1: 2.5.
in a preferred embodiment of the present invention, the amount of sodium bicarbonate added is 0.5 to 2g, and more preferably 1.0 g.
The fourth aspect of the invention provides a method for using the plant enzyme responsive controlled release fertilizer, the controlled release fertilizer powder is suspended in water, sprayed on leaf surfaces and absorbed into the plant body by crops, the outer cellulose polysaccharide wall material is cracked into small segments under the action of plant active plant enzymes such as cellulase in the body, and the outer layer of the integral nano carrier is degraded, so that the fertilizer substances in the nano tube are released for the crops to absorb.
The following is a detailed description of specific embodiments.
Example 1
S1, amination modification of halloysite nanotube surface
Dispersing 2.5g of halloysite nanotubes in a reaction kettle containing 200mL of toluene, then adding 1.0g of 3-aminopropyltrimethoxysilane, heating to 80 ℃ under the protection of nitrogen gas for reflux reaction for 24 hours, centrifugally separating the reacted substances, washing the solid substances with deionized water for multiple times, and obtaining the halloysite nanotubes modified by amino.
S2, loading fertilizer for functionalized halloysite nanotubes
Adding 2.0g of salicylic acid into 100mL of ethyl acetate solution, then adding 2.0g of amino-functionalized halloysite nanotubes, carrying out ultrasonic treatment for 30 minutes, then vacuumizing, reacting for 24 hours under the vacuum condition at room temperature, carrying out centrifugal separation after the reaction is finished, then washing with deionized water, and drying at 60 ℃.
S3, graft modification of carboxymethyl polysaccharide
Dissolving 5g of carboxymethyl cellulose in 400mL of deionized water to obtain a carboxymethyl cellulose solution, then adding 10g of epichlorohydrin and 1mL of 6mol/L hydrochloric acid, stirring and heating to 50 ℃ for reaction for 24 hours, subsequently washing with absolute ethyl alcohol for three times, and obtaining a precipitated substance, namely modified carboxymethyl cellulose, then drying, grinding into powder, and storing in a dryer for later use.
S4, combination of composite nano controlled release carrier
Dissolving 5g of modified carboxymethyl cellulose in 500mL of deionized water to obtain a modified carboxymethyl cellulose solution, then simultaneously adding 5g of amino functionalized halloysite nanotubes loaded with salicylic acid and 1.0g of sodium bicarbonate, stirring and heating at 50 ℃, reacting for 24 hours, finally, centrifugally separating reactants at 10000rpm, washing solids with deionized water for multiple times, and drying at 60 ℃ to obtain the plant enzyme-responsive controlled release fertilizer.
S5, analyzing the controlled release performance of the plant enzyme responsive controlled release fertilizer
In the enzyme responsiveness experiment, 2g of controlled release fertilizer was weighed and dispersed in 100mL of 40% (v/v) methanol aqueous solution, no enzyme was added, supernatants were collected at different time intervals to determine the concentration of salicylic acid, and the cumulative release rate was calculated.
Example 2
The invention provides a plant enzyme responsive controlled release fertilizer, which is characterized in that the specific implementation mode is the same as that of example 1, and the difference is that toluene described in S1 is replaced by absolute ethyl alcohol. 3-aminopropyltrimethoxysilane was replaced by 3-aminopropyltriethoxysilane. In the enzyme responsiveness experiments, 6.0ml of 0.2% (wt%) aqueous cellulase solution was added.
Example 3
The invention provides a plant enzyme responsive controlled release fertilizer, which has the same specific implementation mode as that of example 1, and is characterized in that salicylic acid described in S2 is replaced by gibberellin. In the enzyme responsiveness experiments, 6.0ml of 0.4% (wt%) aqueous cellulase solution was added.
Example 4
The invention provides a plant enzyme responsive controlled release fertilizer, which is the same as the specific implementation mode of example 1, and is characterized in that epichlorohydrin described in S3 is replaced by chloropropane. In the enzyme responsiveness experiments, 6.0ml of 0.5% (wt%) aqueous cellulase solution was added.
Example 5
The invention provides a plant enzyme responsive controlled release fertilizer, which has the same specific implementation mode as that of example 1, and is characterized in that sodium alginate is replaced by carboxymethyl cellulose described in S3, and 1.5mL of 6mol/L sulfuric acid is used. In the enzyme responsiveness experiments, 6.0ml of 0.5% (wt%) aqueous cellulase solution was added.
Example 6
The invention provides a plant enzyme responsive controlled release fertilizer, which has the same specific implementation mode as that of example 1, and is characterized in that: dissolving 5g of modified carboxymethyl cellulose described in S4 in 500mL of deionized water to obtain a modified carboxymethyl cellulose solution, then simultaneously adding 1g of salicylic acid-loaded amino-functionalized halloysite nanotubes and 1.0g of sodium bicarbonate, stirring and heating at 50 ℃ for reaction for 24 hours, finally, centrifugally separating reactants at 10000rpm, washing solids with deionized water for multiple times, and drying at 60 ℃. In the enzyme responsiveness experiments, 6.0ml of 0.75% (wt%) aqueous cellulase solution was added.
Example 7
The invention provides a plant enzyme responsive controlled release fertilizer, which is implemented in the same way as example 1, except that 6ml of 1.0% (wt%) cellulase aqueous solution is added in an enzyme responsive experiment.
Performance testing
| Examples | Cumulative Release Rate (%) | Enzyme responsiveness test |
| Example 1 | 22.37 | Does not respond to |
| Example 2 | 54.35 | Response to |
| Example 3 | 66.29 | Response + |
| Example 4 | 73.72 | Response + |
| Example 5 | 74.94 | Response + |
| Example 6 | 86.67 | Response + + + |
| Example 7 | 93.96 | Response + + + |
Note: the intensity of the enzymatic response is indicated by "+", with a greater number of "+" indicating greater responsiveness.
The above description is only exemplary of the present invention, and not intended to limit the present invention, and any modifications, equivalents and alternatives falling within the spirit and principles of the present invention are included within the scope of the present invention.
Claims (4)
1. A plant enzyme-responsive controlled-release fertilizer is characterized by comprising a plant enzyme-responsive nano-carrier;
the plant enzyme responsive nano-carrier is prepared from modified carboxymethyl polysaccharide through esterification and a halloysite nanotube with a surface amino group modified;
the modified carboxymethyl polysaccharide is carboxymethyl polysaccharide modified by a modifier; the carboxymethyl polysaccharide is selected from at least one of carboxymethyl cellulose, carboxymethyl starch, sodium alginate, carboxymethyl chitosan and carboxymethyl glucan;
the preparation method of the biological enzyme responsive controlled release fertilizer comprises the following steps:
s1, preparing a halloysite nanotube with a surface amino-modified surface;
putting the halloysite nanotube, an organic solvent and a silane coupling agent into a reaction kettle, heating and reacting under the inert gas environment, and centrifugally washing reacted substances to obtain an aminated halloysite nanotube;
s2. functionalized halloysite nanotube loaded fertilizer
Dispersing the aminated halloysite nanotubes obtained in S1 in a plant nutrient solution, and vacuumizing under ultrasonic to obtain aminated halloysite nanotubes loaded with plant nutrient substances;
s3, preparation of modified carboxymethyl polysaccharide
Dissolving carboxymethyl polysaccharide in deionized water to form carboxymethyl polysaccharide solution, adding a modifier and acid, stirring, heating for reaction for 24 hours, washing with absolute ethyl alcohol, and drying to obtain modified carboxymethyl polysaccharide powder;
s4, combination of composite nano controlled release carrier
Dissolving modified carboxymethyl polysaccharide in deionized water to obtain a modified carboxymethyl polysaccharide solution, adding a certain amount of aminated halloysite nanotubes carrying plant nutrient substances and sodium bicarbonate, stirring and heating at 50 ℃ for reaction for 24 hours, centrifuging, washing and drying to obtain the plant enzyme responsive controlled release fertilizer;
and the modifier in the S3 is at least one selected from epichlorohydrin, epoxy bromopropane, chloropropene and bromopropylene.
2. The plant enzyme-responsive controlled-release fertilizer according to claim 1, wherein the silane coupling agent in S1 is at least one selected from the group consisting of 3-aminopropyltriethoxysilane, 3-aminopropyltrimethoxysilane, gamma-aminopropyltrimethoxysilane, and gamma-aminopropyltriethoxysilane.
3. The plant enzyme-responsive controlled-release fertilizer according to claim 1, wherein in S1, the organic solvent is at least one selected from the group consisting of toluene, ethanol and methanol.
4. The method of using a plant enzyme-responsive controlled release fertilizer of claim 1, wherein the controlled release fertilizer is suspended in water and absorbed into the plant by the crop through foliar spray.
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