CN115843809A - Climate response type nano herbicide and preparation method thereof - Google Patents
Climate response type nano herbicide and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a climate response type nano herbicide and a preparation method thereof. The weather-responsive nano herbicide is mainly formed by ZIF-8 loaded bispyribac-sodium, can respond to stimulation of ultraviolet light of the sun and different pH conditions to release the coated bispyribac-sodium, and can improve the adhesion capability of leaves under the scouring action of rainwater and play a role in stronger drug property. The prepared weather response type herbicide is a novel green herbicide, has no toxicity to non-target microorganisms, plants and animals, and has a good weeding effect; the preparation method of the weather-responsive nano herbicide is characterized in that bispyribac-sodium (BIS) is directly added in the synthesis process of ZIF-8 by a one-pot method and stirred, and the synthesis process is simple. The application of the climate response type nano herbicide is that the water solution of the nano herbicide is sprayed on the surface of a plant, and the weeding effect is better than that of a bispyribac-sodium agent after the water solution is irradiated by sunlight or washed by rainwater.
Description
Technical Field
The invention relates to a preparation method and application of a weather-responsive nano herbicide for responding to solar ultraviolet light and environmental pH value and improving the rain erosion resistance, belonging to the technical field of nano pesticides.
Background
The novel nano material has wide application in the field of pesticides. Combines the development of novel nano materials and pesticides, and forms a new nano pesticide research field. The nanometer material is used as the carrier of the original pesticide for improving the properties of the active ingredients of the pesticide, such as solubility, dispersibility, uniformity, stability and the like, improving the bioavailability of the pesticide, and simultaneously reducing pesticide residue and environmental pollution. The nanometer medicine carrying particle has also pesticide releasing function, and can protect environment sensitive pesticide, control the release speed of the pesticide, prolong the lasting period, reduce leaching, decomposition and other pesticide effect loss. Zeolite imidazolate framework material (ZIF-8) is a typical zinc-based material of class Zeolite Imidazole Framework (ZIFs) series in MOFs material, ZIF-8 is a porous metal organic framework prepared by self-assembly of Zn (II) and 2-methylimidazole, has the advantages of good biocompatibility, high porosity, large load capacity, easy modification and the like, is widely applied to material carriers, and at present, ZIF-8 is mainly and widely applied to the fields of gas storage, catalysis, medical drug carriers, slow release, adsorption of environmental pollutants and the like, but the research of combining ZIF-8 with traditional pesticides to improve the utilization rate of pesticides is rarely reported.
Bispyribac-sodium (BIS) belongs to pyrimidine carboxylic acid herbicides, can be quickly absorbed by plants after being used, has quick drug effect exertion, small drug consumption and broad spectrum, can effectively prevent and control various weeds in a rice-tobacco rotation system, is widely used in recent years due to excellent drug effect, but is frequently subjected to phytotoxicity due to the property of the Bispyribac-sodium, weather reasons or improper use, so that the economic income is reduced. Therefore, how to reduce the consumption of bispyribac-sodium in use and improve the utilization rate of pesticides have important significance for agricultural production and ecological safety. Therefore, there is a great need to develop environmentally friendly green herbicides.
Disclosure of Invention
In view of the problems existing at present, the invention aims to prepare a functional nano composite as a pesticide delivery carrier by using ZIF-8 as a matrix material. The mode pesticide is bispyribac-sodium which is easy to generate phytotoxicity and has serious loss, the nanometer ZIF-8 (BIS @ ZIF-8) wrapped with bispyribac-sodium is synthesized by a one-pot method, and the solar ultraviolet light responsiveness, the environmental pH value, the rain-wash resistance, the stability, the biological activity and the like of the BIS @ ZIF-8 are researched. Through a simple preparation method, the ZIF-8 is applied to the preparation of the traditional herbicide bispyribac-sodium, so that the environmental climate responsiveness of the herbicide bispyribac-sodium can be improved, and the rainwater erosion resistance of the herbicide can be improved.
In order to achieve the above object, the technical solution of the present invention is:
a weather-responsive nano herbicide is composed of herbicide bispyribac-sodium and a carrier nano ZIF-8, wherein the herbicide bispyribac-sodium is loaded on the carrier nano ZIF-8; wherein the weight concentration of the herbicide bispyribac-sodium in the climate response type nano herbicide is 14.86 wt%.
The preparation method of the weather response type nano herbicide comprises the following steps:
(1) Respectively dissolving Zn (II), 2-methylimidazole and herbicide bispyribac-sodium in water;
(2) Firstly, adding a herbicide bispyribac-sodium solution into a 2-methylimidazole solution, stirring and mixing uniformly, then dropwise adding the mixed solution into a Zn (II) solution, and realizing the loading of the herbicide bispyribac-sodium in the process of self-assembling to form the nano ZIF-8.
Further, the molar ratio of Zn (II) to 2-methylimidazole is 1: 36.91.
Further, the Zn (II) is zinc nitrate hexahydrate.
Further, the stirring time is more than or equal to 2 hours.
The chemical formula of the nano ZIF-8 is as follows:
a preparation method of nano ZIF-8 with climate responsiveness comprises the following operation steps:
first, 8 g of 2-methylimidazole was dissolved in 32 mL of distilled water, and 0.8 g of Zn (NO) was weighed 3 ） 2 •6H 2 O was dissolved in 3.2 mL of distilled water, and the solution was stirred at room temperature for 5 min to completely dissolve. Subsequently adding Zn (NO) under stirring 3 ） 2 •6H 2 Dropwise adding the O aqueous solution into the 2-methylimidazole aqueous solution, continuously stirring at room temperature of 1200 r/min for 2 hours, then enabling the solution to be milky, indicating that ZIF-8 nanoparticles are spontaneously formed, centrifuging to obtain a white precipitate sample, washing the obtained sample with distilled water for 3 times to remove unreacted reagents, and drying at 65 ℃ overnight to obtain a product, namely ZIF-8.
Further, the preparation of the climate response type nano herbicide by using the ZIF-8 obtained by the method comprises the following steps:
an aqueous bispyribac-sodium solution (40 mg/mL) is prepared. Then 8 g of 2-methylimidazole are dissolved in 32 g of H 2 In O, 0.8 g of Zn (NO) was weighed 3 ） 2 •6H 2 O dissolved in 3.2 g H 2 In O, the mixture was stirred at room temperature for 5 min to dissolve completely. Adding 8 mL of bispyribac-sodium aqueous solution into the 2-methylimidazole solution, stirring and mixing for 5 min, and then dropwise adding the mixed solution to Zn (NO) 3 ） 2 •6H 2 Stirring at room temperature of 1200 r/min for 2 h in O water solution, spontaneously forming ZIF-8 nanometer herbicide nanoparticles (BIS @ ZIF-8) to obtain white suspension, centrifuging to obtain white precipitate, washing with water for 3 times to remove excessive reactant, and drying at 65 deg.C overnight to obtain BIS @ ZIF-8 product.
The technical principle of the invention is as follows: the herbicide bispyribac-sodium and the ZIF-8 are mainly combined through electrostatic attraction, and the Zeta potential of the BIS @ ZIF-8 is changed under the stimulation of ultraviolet rays, so that the electrostatic attraction between the bispyribac-sodium and the ZIF-8 is changed, and the bispyribac-sodium is easier to release. The surface wax layer of the weed leaf is usually composed of higher fatty acid, alcohol and aldehyde and is negatively charged, the BIS @ ZIF-8 is positively charged, and the polar group on the surface of the leaf and the ZIF-8 nano particles form stronger static electricity or hydrogen bond action, so that the BIS @ ZIF-8 solution has better affinity with the weed leaf surface, the contact angle of bispyribac-sodium and the weed leaf surface can be reduced, and the wettability is improved. In addition, BIS @ ZIF-8 nanoparticles can be evenly distributed on the leaves, a layer of film consisting of nanoparticles is formed on the surfaces of the leaves of the weeds, and part of the nanoparticles can be embedded into cracks of a waxy layer structure, so that the rainwater erosion resistance of the herbicide is improved.
The invention has the following advantages:
1) The preparation method does not need complicated and severe conditions, has low preparation threshold, is easy to operate, can be finished at room temperature, and has low preparation cost.
2) BIS @ ZIF-8 can respond to natural ultraviolet rays to release the medicament, can reduce the contact angle between the medicament and the leaf surface of weeds, improve the wettability and reduce the medicament loss caused by rain wash.
3) ZIF-8 has good safety to non-target organisms, can be degraded in the environment and cannot cause secondary pollution.
Drawings
FIG. 1 a) thermogravimetric analysis of BIS @ ZIF-8; b) The Zeta potential diagram of BIS @ ZIF-8; c) ZIF-8 transmission electron microscopy; d) BIS @ ZIF-8 transmission electron microscopy;
FIG. 2 a) BIS @ ZIF-8 cumulative release in PBS at pH 5.0 and 7.4; b) BIS @ ZIF-8 accumulates the release under ultraviolet irradiation and dark conditions; c) Performing ultraviolet-visible spectrum analysis on BIS @ ZIF-8 under different conditions; d) And e) BIS @ ZIF-8 under different conditions (d-1) darkness, (d-2) ultraviolet irradiation, (e-1) SEM images and particle size distribution at pH7.4 and (e-2) pH 5.0;
in FIG. 3 a) the residual rate of barnyard grass leaves for different treatments after the rain wash was simulated; b) Contact angles between different treatments and barnyard grass blades; c) Simulating the influence of different treatments on the growth of barnyard grass after rainfall washing, d) fresh weight, e) plant height and f) chlorophyll content. Note that different lower case letters represent significant differences (P<0.05)。
FIG. 4 is ZIF-8 biosafety: (a-d) the number, plant height, weight and chlorophyll content of rice treated with distilled water, ZIF-8, BIS @ ZIF-8 and bispyribac-sodium for 10 days; (e, f) pictures and body lengths of silkworms treated by ZIF-8 with different concentrations; (g, h) treating goldfish pictures and survival rates by using ZIF-8 with different concentrations.
Detailed Description
The specific implementation mode of the invention is as follows:
a preparation method and application of a climate response type nano herbicide,
(1) Taking a certain amount of bispyribac-sodium technical material and adding distilled water to prepare bispyribac-sodium mother liquor (40 mg/mL);
(2) Weighing 8 g of 2-methylimidazole and 0.8 g of Zn (NO) in 32 mL of distilled water 3 ） 2 •6H 2 Dissolving O in 3.2 mL of distilled water, and stirring at room temperature for 5 min respectively to dissolve the O fully;
(3) Adding 8 mL of bispyribac-sodium mother solution into the 2-methylimidazole solution, stirring and mixing for 5 minutes, and then dropwise adding the mixed solution to Zn (NO) 3 ） 2 •6H 2 Stirring at room temperature of 1200 r/min for 2 h in O water solution, spontaneously forming ZIF-8 nanometer herbicide nanoparticles (BIS @ ZIF-8) to obtain white suspension, centrifuging to obtain white precipitate, washing with water for 3 times to remove excessive reactant, and drying at 65 deg.C overnight to obtain BIS @ ZIF-8 product;
(4) Respectively taking a proper amount of bispyribac-sodium, ZIF-8 and BIS @ ZIF-8 powder samples in a thermogravimetric analyzer, and analyzing the weight change of the samples at different temperatures. The test temperature range is 28-800 ℃, and the reaction gas medium is N 2 The heating rate is 10 ℃/min −1 . Respectively preparing appropriate amount of bispyribac-sodium, ZIF-8 and BIS @ ZIF-8 aqueous solutions, wherein the concentrations are 1 mg/mL, and testing the Zeta potential values of different samples by a Zeta potentiometer; taking appropriate amount of ZIF-8 and BIS @ ZIF-8 powders, respectively, and observing the nanoparticle form with transmission electron microscope. The experimental results are shown in FIG. 1;
(5) The cumulative release amount of BIS @ ZIF-8 under different pH conditions was determined by the room temperature static release method. An accurately weighed sample of 10.0 mg BIS @ ZIF-8 was added to 10 mL of PBS buffer at various pH values, and 0.2 mL of the suspension was removed from the system at regular intervals, followed by 0.2 mL of PBS buffer at the same pH. After filtration through a 0.22 μm filter, the absorbance of the filtrate at 247 nm was measured using UV-Vis, and the concentration of BIS in the filtrate was calculated according to the formula:
the Release Ratio (RR) for BIS @ ZIF-8 was calculated. m is a unit of 0 : initial mass of BIS in BIS @ ZIF-8;V total : the total volume of the solution;C t : BIS concentration at each sampling time point;V t : volume of solution withdrawn at each sampling time point. 5 mL of BIS @ ZIF-8 aqueous solution at a concentration of 1 mg/mL was prepared and placed in the dark and under ultraviolet irradiation conditions, respectively (ultraviolet light from a UVA lamp having a wavelength of 352 nm and a UVB lamp having a wavelength of 306 nm, both at an intensity of 15W). Preheating the solution for 15 minutes before ultraviolet irradiation, continuously irradiating for 12 hours on a rotary platform 20 cm away from an ultraviolet lamp in a small 25 mL glass beaker, measuring an absorbance value by using UV-vis, and calculating the release amount of the BIS agent; and (3) preparing a BIS @ ZIF-8 aqueous solution with the concentration of 1 mg/mL, respectively placing the aqueous solution in the dark and under ultraviolet irradiation, continuously treating for 12 h, and then determining the release condition of the bispyribac-sodium medicament. The method comprises the steps of utilizing UV-vis to carry out ultraviolet absorption spectroscopy on BIS @ ZIF-8 under different conditions, utilizing a scanning electron microscope to observe the morphology of the BIS @ ZIF-8 under different conditions, and utilizing Nano Measurer 1.2 software to carry out statistics on particle size. The experimental results are shown in FIG. 2;
(6) Leaf surface retention rate: 5 mL of aqueous solutions of BIS and BIS @ ZIF-8 with appropriate concentrations were uniformly sprayed on barnyard grass blades, respectively, and the weeds were placed on a glass petri dish with an inclination of 30 °. The control was then made by uniformly spraying 5 mL PBS (pH 5.0) to simulate rain erosion with the same size leaf that was not washed with PBS. After the leaf surface liquid drops are naturally dried, the leaves are immersed into 5 mL PBS and shaken at 150 r/min for 10 min, and the rest BIS is extracted from the leaf surface into the solution. Finally, the concentration of BIS in the solution was determined at 247 nm using UV-Vis. Before assay washing (C 0 ) And after washing: (C 1 ) Concentration of BIS on leavesTo do so byC 1 /C 0 As the retention rate of the pesticide on the leaves. Contact angle measurement: selecting fresh barnyard grass leaves with the same size, carefully cleaning the leaves with distilled water for several times, and removing dust on the surfaces of the leaves to ensure that the surfaces of the leaves are not damaged. After the leaf surface was air-dried at room temperature for moisture, the leaf was cut into 5 cm × 2 cm, and laid flat on a contact angle measuring platform. Using a sampler, 100. Mu.L of BIS @ ZIF-8 suspension (1 mg/mL), aqueous BIS solution (0.05 mg/mL), aqueous ZIF-8 solution (1 mg/mL) and distilled water were dropped on barnyard grass blades, and the contact angles of the different samples with the barnyard grass blades were measured. 5 mL of bispyribac-sodium (0.05 mg/mL) and BIS @ ZIF-8 (1 mg/mL) aqueous solutions of appropriate concentrations were uniformly sprayed over the weed leaves, respectively. Then 5 mL of phosphate buffer (pH 5.7) was uniformly sprayed to simulate rain erosion, and the herbicidal effect was observed and the plant height, fresh weight and chlorophyll content of barnyard grass were determined after 10D cultivation in a climatic incubator (T =26 ± 1 ℃, RH =60 ± 5%, L: D = 16) with the same size of leaves not washed with phosphate buffer as a control, and the experimental results are shown in fig. 3;
(7) 5 mL of BIS @ ZIF-8 aqueous solution (1 mg/mL), bispyribac-sodium aqueous solution (0.05 mg/mL), ZIF-8 aqueous solution (1 mg/mL) and clear water were sprayed on rice leaves at room temperature, respectively. Culturing the treated rice in an artificial climate incubator for 10 days, and measuring the plant height, fresh weight and chlorophyll content of the rice; ZIF-8 aqueous solutions (2 mL) of different concentrations (0.01, 0.06 and 0.11 mg/mL) were uniformly sprayed on the same size of mulberry leaves, treated with clear water as a control. After natural drying, second-instar silkworms (n = 10/dish) were continuously fed with the treated mulberry leaves. Finally, after 15D of rearing in a climatic incubator (T =26 ± 1 ℃, RH =60 ± 5%, L: D = 16), the body length of silkworms was measured with a digital caliper; healthy goldfish (n = 6) with stable growth were selected, placed in 5L pots, respectively, and ZIF-8 aqueous solutions (0.01, 0.06, and 0.11 mg/mL) at different concentrations were added, and treated with clear water as a control. During the experiment, the whole aqueous solution was refreshed every 24 h to maintain the ZIF-8 concentration and water quality. 120 After h, the number of dead fish in each pot was recorded and the mortality was calculated. The results of the experiment are shown in FIG. 4.
As can be seen from FIG. 1, ZIF-8 has better thermal stability and poor stability of bispyribac-sodium, ZIF-8 has a certain mass loss (20.30%) at a temperature of 27 ℃ to 200 ℃, which is mainly the evaporation loss of water in the sample and the decomposition of impurities remaining in the pore size. When the temperature rises to about 400 ℃, the organic ligand of ZIF-8 starts to be rapidly thermally decomposed, and the quality of the sample is also rapidly reduced. When the temperature approaches 700 ℃, the mass does not change any more, and a stable equilibrium state is gradually reached, at which time the ZIF-8 has been completely decomposed, and the rest is mainly carbon and a small amount of high temperature resistant impurities. As can be seen from the thermogravimetric curve of BIS, the mass of BIS decreases significantly when the temperature is around 200 ℃, indicating that thermal decomposition of BIS starts at 200 ℃. Because BIS @ ZIF-8 contains BIS and the thermogravimetric change curve of BIS @ ZIF-8 is basically consistent with that of ZIF-8, ZIF-8 and BIS @ ZIF-8 can be controlled at 200-400 DEG C
The thermal weight loss difference is regarded as the drug loading rate, and the drug loading rate in BIS @ ZIF-8 is analyzed and calculated to be about 14.86%; the surface potential of the ZIF-8 is positive, the bispyribac-sodium is negative, the BIS @ ZIF-8 is positive, but the potential value is reduced, which indicates that the bispyribac-sodium and the ZIF-8 can be combined together through electrostatic attraction; agglomeration of the ZIF-8 nano particles loaded with bispyribac-sodium is increased;
as can be seen from FIG. 2, 2 h before release, BIS @ ZIF-8 released faster in both pH7.4 and pH 5.0 PBS due to hydrolysis of BIS @ ZIF-8 in aqueous solution, and BIS release rates were 60.00 + -2.29% and 68.53 + -5.37%, respectively. After 6 h of treatment, the cumulative release rate of BIS @ ZIF-8 nanoparticles reached 65.22. + -. 1.28% at pH7.4, and gradually reached equilibrium. However, at pH 5.0, the cumulative release rate of BIS @ ZIF-8 was still faster due to the dissociation of ZIF-8 under acidic conditions, reaching equilibrium of release gradually after 10 h. The release rate of BIS @ ZIF-8 under ultraviolet irradiation is 15.84 + -0.23%, while the release rate of BIS @ ZIF-8 under dark irradiation is only 8.74 + -0.24% ((R))P<0.05). The average particle size of the nanoparticles in the dark (96.78 + -16.68 nm) is significantly larger than the average particle size after UV irradiation (79.54 + -14.33 nm). Compared with pH7.4, the BIS @ ZIF-8 nanoparticles treated at pH 5.0 have severe morphological disruption and agglomeration, and the average particle size is reduced from 100.41 + -15.25 nm to 63.37 + -9.62 nm. Thus, it is possible to provideThe results show that the BIS @ ZIF-8 can respond to the stimulation of pH and ultraviolet rays, and the shape and the particle size of the product are changed to release more medicaments. Note: ultraviolet rays are generated by UVA lamp tubes (with the wavelength of 352 nm) and UVB lamp tubes (with the wavelength of 306 nm), the intensity is 15W, and the distance is 12.5 cm;
as can be seen from figure 3, after the simulated rain wash, the retention rate of BIS on barnyard grass leaves is 53.88%, the retention rate of BIS treated by BIS @ ZIF-8 is 76.26%, and the BIS @ ZIF-8 has higher leaf surface retention rate than that of individual bispyribac-sodium, which indicates that the retention amount of bispyribac-sodium on the leaf surfaces of weeds can be increased. The CA of the BIS solution, the clear water and the leaf surface are respectively larger and are respectively 130.58 +/-5.35 degrees and 105.40 +/-2.71 degrees, while the CA of the ZIF-8 solution and the leaf between 91.84 +/-1.66 degrees is smaller, which indicates that the affinity of the ZIF-8 and the leaf surface is better, and the CA of the leaf surface is also smaller and is 92.36 +/-1.65 degrees compared with BIS @ ZIF-8, and the CA is reduced by about 38.22 degrees, which indicates that the introduction of the ZIF-8 can reduce the CA of pesticide and the leaf surface. After the simulation of rain wash, compared with the plant height, fresh weight and chlorophyll content of the barnyard grass after different treatments, the single bispyribac has a certain weeding effect on the weeding of the barnyard grass, but the BIS @ ZIF-8 has a better weeding effect on the barnyard grass, and has obvious inhibiting effects on the plant height, fresh weight and chlorophyll content of the barnyard grass.
As can be seen from FIG. 4, after 15 days of ZIF-8 nanoparticle treatment, the fresh weight, plant height and chlorophyll content of rice are not significantly affected (P> 0.05). In addition, after the mulberry leaves treated by ZIF-8 with different concentrations are continuously fed for 15 days, the growth and development of the silkworms are not affected (P> 0.05). For goldfish, there was no significant difference in survival rate after continuous feeding for 120 h with ZIF-8 at different concentrations: (P> 0.05). Therefore, ZIF-8 has good biological safety to non-target organisms (rice, goldfish and silkworm).
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the overall concept of the present invention, and these should also be construed as the protection scope of the present invention.
Claims (5)
1. The climate response type nano herbicide is characterized by consisting of herbicide bispyribac-sodium and carrier nano ZIF-8, wherein the herbicide bispyribac-sodium is loaded on the carrier nano ZIF-8; wherein the weight concentration of the herbicide bispyribac-sodium in the climate response type nano herbicide is 14.86 wt%.
2. A process for preparing a weather-responsive nano-herbicide as claimed in claim 1, comprising the steps of:
(1) Respectively dissolving Zn (II), 2-methylimidazole and herbicide bispyribac-sodium in water;
(2) Firstly, adding a herbicide bispyribac-sodium solution into a 2-methylimidazole solution, stirring and mixing uniformly, then dropwise adding the mixed solution into a Zn (II) solution, and realizing the loading of the herbicide bispyribac-sodium in the process of self-assembling to form the nano ZIF-8.
3. The method according to claim 2, wherein the molar ratio of Zn (II) to 2-methylimidazole is 1: 36.91.
4. Preparation method according to claim 2, characterized in that the Zn (II) is in particular zinc nitrate hexahydrate.
5. The method of claim 2, wherein the stirring is carried out for a period of time not less than 2 hours.
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