CN106417269A - Water-based nanoparticle aqueous dispersion preparation of liposoluble pesticide and preparation method of water-based nanoparticle aqueous dispersion preparation - Google Patents
Water-based nanoparticle aqueous dispersion preparation of liposoluble pesticide and preparation method of water-based nanoparticle aqueous dispersion preparation Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
- A01N25/10—Macromolecular compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing heterocyclic radicals
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Abstract
The invention relates to a nano aqueous dispersion preparation of a liposoluble pesticide, and a preparation method of the nano aqueous dispersion preparation. The preparation method comprises the following steps: S1, adding sodium carboxymethylcellulose into water, heating and stirring until the sodium carboxymethylcellulose is gelatinized, adding an initiator and increasing the temperature to 60-100 DEG C, dropwise adding unsaturated monomer, continuing to react for 6-12 hours after finishing dropwise adding to obtain a CMC-grafted unsaturated monomer copolymer emulsion; and S2, dropwise adding the CMC-grafted unsaturated monomer copolymer emulsion into an organic solution of the liposoluble pesticide, and uniformly mixing to obtain the nano aqueous dispersion preparation of the liposoluble pesticide, wherein the unsaturated monomer is selected from one or several of acrylate monomers, styrene monomers and acrylamide monomers. The nano aqueous dispersion preparation of the liposoluble pesticide prepared by the method is capable of achieving slow release and is also capable of increasing contact area between the pesticide preparation and crop leaves and insects and increasing the effective utilization rate of the pesticide.
Description
Technical field
The invention belongs to natural macromolecule modification and agricultural pesticide formulation art, and in particular to a kind of water of fat-soluble pesticide
Fundamental mode nanoparticle aqueous dispersion preparation and preparation method thereof.
Background technology
Regular dosage form farm chemical ingredients have that rate of release is fast, be easily lost in or leaching, utilization rate are low and easily right
Environment and be progressively restricted, efficient context close friend slow release be current pesticidal preparations development main target.Nanometer
Pesticidal preparations are a kind of novel agrochemical formulations, and with respect to traditional pesticide, nano-pesticide formulation not only can realize slow release, acceptable
Increase pesticidal preparations and crop leaf and the contact area of insect, improve the effective rate of utilization of pesticide.Domestic and international researcher is to receiving
Rice pesticidal preparations generate keen interest, at present used by existing nanometer formulation microcapsule wall material research concentrate on shitosan and
Its derivant, polylactide and its copolymer and some other carrier, and for carrier prepared by nanometer agriculture for sodium carboxymethyl cellulose
The report of medicine preparation is little.
Sodium carboxymethyl cellulose is that a class is biodegradable, abundance, renewable and cheap and easily-available product, and which has
Excellent water solublity, avirulence, salt-resistance, anti-shearing thickening property and preferable temperature resistant capability.Sodium carboxymethyl cellulose connects
Branch copolymerization is important a kind of chemical method in modified-high polymer technology, and its advantage is sodium carboxymethyl cellulose graft copolymerization
, cost not harsh to technical requirements is relatively low.Sodium carboxymethyl cellulose is also easy to same other monomers graft copolymerization formation and is available for needs
Farm chemical carrier, and easy to operate, high efficiency.In addition, being carried out using emulsifier-free emulsion polymerization method from sodium carboxymethyl cellulose
Glycerol polymerization, it is thus also avoided that the pollution for being brought using other solvents and Cost Problems.Therefore, sodium carboxymethyl cellulose is grafted
Copolymer prepares nano-pesticide formulation as carrier and has larger prospect.
Aqua type nanoparticle aqueous dispersion preparation is the preparation for replacing aromatics organic solvent in cream with water as medium, because
Its significant environmental protection advantage, becomes one of important research direction in the formulations of pesticide.Therefore, a kind of fat-soluble pesticide is studied
Aqua type nanoparticle aqueous dispersion preparation there is vast potential for future development and realistic meaning.
Content of the invention
It is an object of the invention to overcoming the deficiencies in the prior art, a kind of nanometer aqueous dispersion preparation of fat-soluble pesticide is provided
Preparation method, the nanometer aqueous dispersion preparation of the fat-soluble pesticide that the method is prepared has suitable carrying drug ratio and particle diameter,
Slow release not only can be realized, pesticidal preparations and crop leaf and the contact area of insect can also be increased, improve the effective of pesticide
Utilization rate.
Another object of the present invention is to providing the nanometer water dispersant of the fat-soluble pesticide that said method is prepared.
For achieving the above object, the present invention is adopted the following technical scheme that：
A kind of preparation method of the nanometer aqueous dispersion preparation of fat-soluble pesticide, the preparation method is：
S1：Sodium carboxymethyl cellulose is added to the water, is heated and stir to gelatinizing, add initiator and it is warming up to 60～
100 DEG C, then Deca unsaturated monomer, continue 6～12h of reaction after completion of dropwise addition, obtain final product CMC imping unsaturated monomers copolymer breast
Liquid；
S2：CMC imping unsaturated monomers copolymer emulsion is added drop-wise in the organic solution of fat-soluble pesticide, mix homogeneously
Obtain final product the nanometer aqueous dispersion preparation of fat-soluble pesticide；
Wherein, the unsaturated monomer be acrylic ester monomer, styrene monomer, in acrylamide monomers one
Plant or several.
Sodium carboxymethyl cellulose has excellent water solublity, and this makes which be very easy to carry out the glycerol polymerization of aqueous solution, protects
The uniformity of reaction is demonstrate,proved；In addition, sodium carboxymethyl cellulose be also especially susceptible to same acrylic ester monomer, styrene monomer,
These unsaturated monomer graft copolymerizations of acrylamide monomers form the fat-soluble farm chemical carrier for being available for needing.Therefore, the present invention
It is matrix from hydrophilic sodium carboxymethyl cellulose, with acrylic ester monomer, styrene monomer, acrylamide monomers
For unsaturated monomer, with radical polymerization mechanism, using emulsifier-free emulsion polymerization method, the carboxymethyl cellulose of synthesis of amphoteric
Sodium graft copolymer, and with which as carrier, using micelle compatibilization, prepared a kind of nanometer moisture of fat-soluble pesticide
Powder preparation.
In the nanometer aqueous dispersion preparation of the fat-soluble pesticide that the present invention is provided, some pesticide is covered by carrier carboxylic first
In base sodium cellulosate graft copolymer, another part pesticide is then exposed outside carrier, so by this nanometer of aqueous dispersion preparation
When being applied to crops, exposed part pesticide outside carrier is played a role after administration immediately, and is covered by carrier
Interior part pesticide then passes through slow releasing function gradually slow release, subtracts, so as to improving the utilization rate of pesticide and reaching, the mesh for applying potentiation
's.
In step S1 of the present invention, the gelatinizing method of sodium carboxymethyl cellulose can adopt any means of the prior art, preferably
Ground, the gelatinization point of sodium carboxymethyl cellulose is 60 DEG C, and gelatinization time is 1.5 hours.
Preferably, in step S1, add initiator and be warming up to 80 DEG C.
Preferably, the initiator is potassium peroxydisulfate and/or Ammonium persulfate..
Preferably, the acrylic ester monomer is Butyl Acrylate Monomer, methacrylate monomer or methacrylic acid
One or more in methylmethacrylate monomer.
The preparation method of the nanometer aqueous dispersion preparation of the fat-soluble pesticide that the present invention is provided is applied to the conventional fat of this area
Soluble pesticide, it is preferable that the fat-soluble pesticide is chlopyrifos, Acetamiprid, avilamycin, one or more in ethiprole.
Preferably, in step S1, the sodium carboxymethyl cellulose is 1 with the mass ratio of unsaturated monomer：4～16.
Preferably, in step S1, after completion of dropwise addition, continue reaction 10h.
The step of the present invention in S2, the organic solvent is ethanol, isopropanol, acetone, the one kind in ethyl acetate or
Multiple.
Preferably, the concentration of the CMC imping unsaturated monomers copolymer emulsion is 0.1～1mg/mL.
Preferably, the concentration of the fat-soluble pesticide is 1～50mg/mL；It is further preferable that the fat-soluble pesticide has
The concentration of machine solution is 2～10mg/mL.
Preferably, the mass ratio of the CMC imping unsaturated monomers copolymer emulsion and fat-soluble pesticide is 1～7：0.2
～1；It is further preferable that the mass ratio of the CMC imping unsaturated monomers copolymer emulsion and fat-soluble pesticide is 5:1～3.
The nanometer water dispersant of the fat-soluble pesticide that said method is prepared, the nanometer water dispersion of the fat-soluble pesticide
Preparation has suitable carrying drug ratio and particle diameter, not only can realize slow release, can also increase pesticidal preparations with crop leaf and evil
The contact area of worm, improves the effective rate of utilization of pesticide.
Compared with prior art, the present invention has the advantages that：
The present invention with hydrophilic sodium carboxymethyl cellulose as matrix, with radical polymerization mechanism, using soap-free emulsion
Polymerization, the sodium carboxymethyl cellulose graft copolymer of synthesis of amphoteric, and with which as carrier, using micelle compatibilization,
A kind of nanometer aqueous dispersion preparation of fat-soluble pesticide is prepared.The nanometer water dispersion system of the fat-soluble pesticide that the present invention is provided
Agent has suitable carrying drug ratio and particle diameter, with slow releasing function and preferably pesticide utilization rate, can play and subtract the purpose for applying potentiation.
In addition, the present invention provides the nanometer aqueous dispersion preparation for changing can also increase pesticidal preparations with crop leaf and the contact surface of insect
Product, improves the effective rate of utilization of pesticide.
Description of the drawings
The infared spectrum of the farm chemical carrier CMC imping unsaturated monomers copolymer that Fig. 1 is prepared for embodiment 1；
The DSC figure of the farm chemical carrier CMC imping unsaturated monomers copolymer that Fig. 2 is prepared for embodiment 1；
The DSC figure of the aqua type nanoparticle aqueous dispersion preparation of the chlopyrifos that Fig. 3 is prepared for embodiment 1；
The SEM figure of the aqua type nanoparticle aqueous dispersion preparation of the chlopyrifos that Fig. 4 is prepared for embodiment 1；
The particle size distribution figure of the aqua type nanoparticle aqueous dispersion preparation of the chlopyrifos that Fig. 5 is prepared for embodiment 1；
The Tyndall phenomenon figure of the aqua type nanoparticle aqueous dispersion preparation of the chlopyrifos that Fig. 6 is prepared for embodiment 1.
Specific embodiment
The present invention is further elaborated on reference to Figure of description and specific embodiment.Following examples of the present invention
For the present invention preferably embodiment, the replacement of the simple parameter in various embodiments of the present invention can not be gone to live in the household of one's in-laws on getting married one by one in an embodiment
State, but therefore do not limit the scope of the invention, other any spirit without departing from the present invention are lower with principle to be made
Change, modification, replacement, combination, simplify, equivalent substitute mode should be considered, be included within protection scope of the present invention.
The preparation of the aqua type nanoparticle aqueous dispersion preparation of 1 chlopyrifos of embodiment
(1) preparation of CMC imping unsaturated monomers copolymer and purification
2g CMC is added in 150g deionized water, heats and be stirred well to gelatinizing, add 1g potassium peroxydisulfate (KPS) to draw
Agent is sent out, 80 DEG C are warming up to, then the mixed solution of Deca 2g butyl acrylate (BA) and 12g methyl methacrylate (MMA), Deca
Continue reaction 8h after end, obtain white emulsion.
Graft copolymerization principle is as follows：
A certain amount of emulsion is weighed, is settled using acetone, gained precipitum is vacuum dried to constant weight, with acetone and second
Acetoacetic ester is mixed solvent, and using apparatus,Soxhlet'ses extracting 48h to remove homopolymer, gained CMC grafted acrylate is designated as CMC
Imping unsaturated monomers copolymer emulsion.
(2) preparation of the aqua type nanoparticle aqueous dispersion preparation of chlopyrifos
The CMC imping unsaturated monomers copolymer emulsion of synthesis is added to the water be configured to variable concentrations (0.1 mg/mL,
0.3mg/mL, 0.5mg/mL, 0.7mg/mL) solution.The poisoning of variable concentrations (2mg/mL, 4mg/mL, 6mg/mL) is prepared again
Tickss (CH) ethanol solution.Under continuous stirring, CMC imping unsaturated monomers copolymer emulsion is added drop-wise to chlopyrifos anhydrous
In ethanol solution, CH/CMC imping unsaturated monomers copolymer emulsion nanoparticle water dispersant, gained preparation death by poisoning is obtained
The mass concentration of Tickss is 0.1～0.7mg/mL for the mass concentration of 0.02～0.06mg/mL, CMC-g-PAE.
(3) measure of chlopyrifos load factor
The nanoparticle aqueous dispersion preparation of certain volume is centrifuged 30min with high speed centrifuge (20000r/min), with purple
External spectrum (test wavelength 229nm, standard curve y=-0.0241+16.512x, R2=0.9999) CH that dissociates is determined in supernatant
Content, and be calculated as follows the load factor of CH, the load factor of nanoparticle aqueous dispersion preparation see the table below 1.
The load factor of the nanoparticle for being formed under 1 difference CMC-g-PAE of table and chlopyrifos mass concentration
From upper table 1, the load factor of the nanometer aqueous dispersion preparation that the present embodiment is prepared works as institute all more than 65%
The mass concentration for obtaining CMC imping unsaturated monomers copolymer emulsion in preparation is 0.1mg/mL, and the mass concentration of chlopyrifos is
During 0.06mg/mL, the load factor highest of nanoparticle aqueous dispersion preparation, up to 87.1%.From upper table 1, in real work
During, can be by regulation and control carrier and the pesticide load factor of the concentration proportioning effective control nanometer water dispersant of drug solution.
The preparation of the aqua type nanoparticle aqueous dispersion preparation of 2 Acetamiprid of embodiment
Preparation method in the present embodiment is with embodiment 1, and difference is in the present embodiment to substitute in fact from Acetamiprid
Apply the chlopyrifos in example 1.
The nanoparticle for being formed under 2 difference CMC imping unsaturated monomers copolymer emulsion of table and Acetamiprid mass concentration
Load factor
From upper table 2, the load factor of the aqua type nanoparticle aqueous dispersion preparation of Acetamiprid works as institute all more than 50%
In preparation CMC imping unsaturated monomers copolymer emulsion concentration be 0.1mg/mL, the concentration of Acetamiprid in 0.02mg/mL,
The load factor highest of nanoparticle aqueous dispersion preparation, up to 72.5%.
The preparation of the aqua type nanoparticle aqueous dispersion preparation of 3 avilamycin of embodiment
Preparation method in the present embodiment is with embodiment 1, and difference is in the present embodiment from avilamycin isopropyl
Chlopyrifos ethanol solution in alcoholic solution alternate embodiment 1.
The nanoparticle for being formed under 3 difference CMC imping unsaturated monomers copolymer emulsion of table and avilamycin mass concentration
Load factor
From upper table 3, the load factor of the aqua type nanoparticle aqueous dispersion preparation of avilamycin has more than 58%
Higher load factor.When the concentration of CMC imping unsaturated monomers copolymer emulsion in gained preparation is 0.30mg/mL, Avermectin
Element concentration in 0.05mg/mL, the load factor highest of nanoparticle aqueous dispersion preparation, up to 65.7%.
The performance characterization of the aqua type nanoparticle aqueous dispersion preparation of the chlopyrifos that 4 embodiment 1 of test example is prepared
1. performance parameter and method of testing are as follows：
(1) infrared property of CMC imping unsaturated monomers copolymer
Using FTIR, the composition of each sample, sweep limitss are analyzed using KBr pressed disc method：4000～400cm-1；
(2) DSC of CMC imping unsaturated monomers copolymer and nanoparticle aqueous dispersion preparation
Using the crystallization behavior of DSC test sample, 20～250 DEG C of temperature elevating range (its Chlorpyrifos temperature elevating range is 20～
100 DEG C), heating rate is 10 DEG C/min, N2Flow 40mL/min；
(3) pattern of nanoparticle aqueous dispersion preparation
Using the pattern of the Nano microsphere of SEM observation nanoparticle aqueous dispersion preparation, voltage 15kV；
(4) particle diameter distribution of nanoparticle aqueous dispersion preparation
The particle diameter distribution of nanoparticle aqueous dispersion preparation is tested using Particle Size Analyzer；
(5) Tyndall phenomenon of nanoparticle aqueous dispersion preparation
The Tyndall phenomenon for carrying out detection sample is irradiated with laser pen.
2. the infared spectrum analysis of nanoparticle aqueous dispersion preparation
Fig. 1 is the infrared figure of CMC and CMC imping unsaturated monomers copolymer emulsion, compares CMC imping unsaturated monomers altogether
Find after the infrared figure of copolymer emulsion and CMC, the infrared curve of CMC imping unsaturated monomers copolymer emulsion is in 1729cm-1Go out
The stretching vibration of existing ester group C=O key, 1389cm-1Appearance-CH3Characteristic absorption peak, 842cm-1There is BA, MMA mix monomer
In-CH-O-CH2The stretching vibration of key, this shows that mix monomer has successfully been grafted on CMC.
3.CMC imping unsaturated monomers copolymer and the dsc analysis of nanoparticle aqueous dispersion preparation
Fig. 2 is schemed for the DSC of CMC and CMC-g-PAE, figure it is seen that CMC has an obvious peak at 135 DEG C, this
For the glass transition temperature of CMC, but after CMC and BA, MMA graft copolymerization generate CMC-g-PAE, 135 DEG C of peak disappears, 95
DEG C occur weaker transformation peaks, this be probably copolymer in PMMA segment glass transition, this explanation graft copolymerization anti-
The structure of CMC should be changed.
Fig. 3 is chlopyrifos, the DSC figure of chlopyrifos/CMC-g-PAE, from figure 3, it can be seen that chlopyrifos has at 41.5 DEG C
Obvious melting peak, this is the fusing point of chlopyrifos.But the in figure in chlopyrifos/CMC-g-PAE, the melting for chlopyrifos do not occur
Peak, illustrate chlopyrifos be in the form of amorphous in nanoparticle.
4. morphology analysis of nanoparticle aqueous dispersion preparation
Fig. 4 is schemed for the SEM of nanoparticle water dispersant dry state nanoparticle, and as seen from Figure 4, nanoparticle moisture dissipates
The smooth surface of preparation, particle diameter is 200nm or so, and size is uniform, the spheroidal particle of balling-up rounding.Make in embodiment 1
The standby fat-soluble pesticide chlopyrifos for obtaining is embedded in the hydrophobic region inside particles that the polyacrylate of grafting is formed, and CMC is grafted
The hydrophilic group of unsaturated monomer copolymer emulsion such as carboxyl and hydroxyl etc. are gathered in the surface of nanoparticle, and insert in water,
Enable that nanoparticle aqueous dispersion preparation is stable to be dispersed in water.
5. the particle diameter distribution of nanoparticle aqueous dispersion preparation
Fig. 5 is the particle size distribution figure of chlopyrifos/CMC-g-PAE nanometer water dispersant, the nanoparticle for being obtained by testing graininess
The mean diameter of son and particle diameter distribution index (PDI) are listed in table 1.
Can be seen that in scope of experiment from table 4 and Fig. 5, prepared its particle diameter of nanometer water dispersant 200～
Between 250nm, the PDI of its particle diameter is respectively less than 0.08, and minimum PDI is 0.002, it is considered that when profile exponent is 0.01, can
To think to be close to single dispersing, PDI shows that Nanoparticle Size is highly uniform, and particle diameter distribution is very narrow, and this and above-mentioned SEM figure are identical
's.
As can also be seen from Table 4, when one timing of concentration of chlopyrifos, as the concentration of CMC-g-PAE increases, chlopyrifos/
The particle diameter of CMC-g-PAE nanoparticle is substantially tapered into, and when the concentration of chlopyrifos is 0.01mg/mL, CMC-g-
The concentration of PAE is in 0.7mg/mL, and minima 204.3nm occurs in chlopyrifos/CMC-g-PAE nano particle diameter.Work as CMC-g-
One timing of concentration of PAE, with the increase of chlopyrifos concentration, the particle diameter of CH/CMC-g-PAE nanoparticle becomes in increase substantially
Gesture.There is the maximum of nanoparticle when the concentration that chlopyrifos concentration is 0.06mg/mL, CMC-g-PAE is in 0.1mg/mL
239.9nm.
The particle diameter of 4 chlopyrifos of table/CMC-g-PAE nanoparticle and particle diameter distribution
6. the Tyndall phenomenon of nanoparticle aqueous dispersion preparation
Fig. 6 is the Tyndall phenomenon figure of nanoparticle aqueous dispersion preparation, as shown in Figure 6, it can be observed that significantly fourth reaches
That phenomenon, this shows that the aqua type nanoparticle aqueous dispersion preparation of chlopyrifos defines nanoscale assembly really.
Claims (10)
1. a kind of preparation method of the nanometer aqueous dispersion preparation of fat-soluble pesticide, it is characterised in that the preparation method is：
S1：Sodium carboxymethyl cellulose is added to the water, is heated and stir to gelatinizing, add initiator and 60～100 DEG C are warming up to,
Deca unsaturated monomer, continues 6～12h of reaction, obtains final product CMC imping unsaturated monomers copolymer emulsion after completion of dropwise addition again；
S2：CMC imping unsaturated monomers copolymer emulsion is added drop-wise in the organic solution of fat-soluble pesticide, mix homogeneously is obtained final product
The nanometer aqueous dispersion preparation of fat-soluble pesticide；
Wherein, the unsaturated monomer be acrylic ester monomer, styrene monomer, the one kind in acrylamide monomers or
Several.
2. preparation method according to claim 1, it is characterised in that the acrylic ester monomer be
One or more in body, methacrylate monomer or methyl methacrylate monomer.
3. preparation method according to claim 1, it is characterised in that in step S2, the organic solvent be
One or more in alcohol, acetone, ethyl acetate.
4. preparation method according to claim 1, it is characterised in that the fat-soluble pesticide be
One or more in rhzomorph, ethiprole.
5. preparation method according to claim 1, it is characterised in that in S1, the sodium carboxymethyl cellulose and unsaturation list
The mass ratio of body is 1：4～16.
6. preparation method according to claim 1, it is characterised in that in S2, the CMC imping unsaturated monomers copolymer
The concentration of emulsion is 0.1～1mg/mL.
7. preparation method according to claim 1, it is characterised in that in step S2, the organic solution of the fat-soluble pesticide
Concentration be 1～50mg/mL.
8. preparation method according to claim 1, it is characterised in that the CMC imping unsaturated monomers copolymer emulsion and
The mass ratio of fat-soluble pesticide is 1～7：0.2～1.
9. preparation method according to claim 8, it is characterised in that the CMC imping unsaturated monomers copolymer emulsion and
The mass ratio of fat-soluble pesticide is 5:1～3.
10. the nanometer aqueous dispersion preparation of the fat-soluble pesticide that the arbitrary preparation method of claim 1～9 is prepared.
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| CN108323505A (en) * | 2018-01-18 | 2018-07-27 | 仲恺农业工程学院 | A kind of preparation method of avermectin water dispersant |
| CN112940625A (en) * | 2021-01-22 | 2021-06-11 | 仲恺农业工程学院 | Nano pesticide preparation based on biopolysaccharide grafted rosin and preparation method thereof |
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