CN105875603A - Nano-selenium composite avermectin selenium-rich pesticide and preparation method thereof - Google Patents
Nano-selenium composite avermectin selenium-rich pesticide and preparation method thereof Download PDFInfo
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- CN105875603A CN105875603A CN201610265258.3A CN201610265258A CN105875603A CN 105875603 A CN105875603 A CN 105875603A CN 201610265258 A CN201610265258 A CN 201610265258A CN 105875603 A CN105875603 A CN 105875603A
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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
- A01N25/32—Ingredients for reducing the noxious effect of the active substances to organisms other than pests, e.g. toxicity reducing compositions, self-destructing compositions
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/02—Elemental selenium or tellurium
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Abstract
The invention discloses nano-selenium composite avermectin selenium-rich pesticide and a preparation method thereof and belongs to the technical field of composite pesticides. The technical scheme of the invention is characterized in that the nano-selenium composite avermectin selenium-rich pesticide is obtained by: dissolving nano-selenium in deionized water, stirring and mixing at 10-50 DEG C for 15 min to obtain nano-selenium suspension, adding the nano-selenium suspension into ethanol solution of stearic acid to obtain stearic acid-modified nano-selenium powder, adding the stearic acid-modified nano-selenium powder and petroleum ether into avermectin emulsifiable concentrate 5% in mass fraction, adding deionized water solution containing sodium dodecyl sulfate 10% in mass fraction, and stirring and mixing at 25-65 DEG C for 35-60 min. The method of the invention is simple and is easy to use in industrial production, and the nano-selenium composite avermectin selenium-rich pesticide has the advantages such as environment-friendliness and short chemical residue time.
Description
Technical field
The invention belongs to composite pesticide technical field, be specifically related to a kind of nanometer selenium and be combined avilamycin selenium-rich pesticide and preparation method thereof.
Background technology
At present, for solving Pesticide Residue, the degraded to avilamycin pesticide does not has good solution, although utilizing nano material to avilamycin of degrading, but its degradation efficiency is low.Therefore, there is a kind of pesticide that can improve degraded avilamycin efficiency to be developed, the effect of parasite killing can either be played, the residence time in crop can be shortened again.
Summary of the invention
Present invention solves the technical problem that there is provided a kind of nanometer selenium is combined avilamycin selenium-rich pesticide and preparation method thereof.
The present invention solves that above-mentioned technical problem adopts the following technical scheme that, a kind of nanometer selenium is combined the preparation method of avilamycin selenium-rich pesticide, it is characterised in that concretely comprise the following steps:
Step (1); nanometer selenium is dissolved in the deionized water that mass ratio is 100-1000 times of nanometer selenium quality; nanometer selenium suspension is obtained in 10-50 DEG C of stirring mixing 15min; by nanometer selenium suspension add with its mass ratio be 1.5-3:1 containing the stearic ethanol solution that mass fraction is 10%; reduce pressure after 26-59 DEG C of stirring mixing 30-70min sucking filtration; with deionized water rinsing 2-4 time; then it is vacuum dried 1-4h in 20-55 DEG C; being cooled to room temperature, nitrogen protection lower grinding 10-30min obtains stearic acid modified nanometer selenium powder body；
Step (2), in the abamectin emulsifiable concentrate that mass fraction is 5%, add mass ratio be the stearic acid modified nanometer selenium powder body of 0.04-0.12 times of abamectin emulsifiable concentrate and mass ratio is the petroleum ether of 0.0015-0.04 times of abamectin emulsifiable concentrate, add and the deionized water solution containing the sodium lauryl sulphate that mass fraction is 10% that above-mentioned solution total mass ratio is 1.2-3:1, then obtain nanometer selenium in 25-65 DEG C of stirring mixing 35-60min and be combined avilamycin selenium-rich pesticide.
Further preferably, the concrete building-up process of described nanometer selenium is: is dissolved in distilled water by Monohydrated selenium dioxide and forms the Monohydrated selenium dioxide solution that molar concentration is 0.1-3.1mol/L, the sodium lauryl sulphate of 0.01-0.1 times of Monohydrated selenium dioxide mole is added in Monohydrated selenium dioxide solution, in 10-50 DEG C of stirring mixing 10-20min, add the ascorbic acid solution that molar concentration is 0.1-5.2mol/L of 2-4 times of Monohydrated selenium dioxide mole, stirring mixing 1-20min, the sodium sulfite solution that molar concentration is 0.1-3.0mol/L being subsequently adding above-mentioned liquor capacity 1% pH regulating solution are 3-6, in the water-bath of 12-38 DEG C, react 0.1-0.5h be precipitated thing；Clean 1-5 time with deionized water after precipitate is centrifuged, then obtain elemental selenium 1-5 time with washes of absolute alcohol, elemental selenium is placed on ball milling 2-4h in the ball mill of nitrogen protection in 10-100 DEG C of vacuum drying 1-8h and obtains nanometer selenium.
Nanometer selenium of the present invention is combined avilamycin selenium-rich pesticide, prepares according to the method described above.
The process of the present invention is simple, it is easy to industrialized production, and obtained nanometer selenium is combined avilamycin selenium-rich pesticide and has environmental friendliness and the advantage such as the chemical residual time is short.
Detailed description of the invention
Being described in further details the foregoing of the present invention by the following examples, but this should not being interpreted as, the scope of the above-mentioned theme of the present invention is only limitted to below example, all technology realized based on foregoing of the present invention belong to the scope of the present invention.
Embodiment 1
1, Monohydrated selenium dioxide is dissolved in distilled water the Monohydrated selenium dioxide solution that formation molar concentration is 0.1mol/L, the sodium lauryl sulphate of 0.01 times of Monohydrated selenium dioxide mole is added in Monohydrated selenium dioxide solution, 10min is shaken with shaking table in 10 DEG C, add the ascorbic acid solution that molar concentration is 0.1mol/L of 2 times of Monohydrated selenium dioxide moles, shaking table shakes 1min, it is subsequently adding the sodium sulfite solution that molar concentration is 0.1mol/L of above liquor capacity 1% and to regulate pH be 3, control bath temperature and obtain precipitate at 12 DEG C of reaction 0.1h；
2, being centrifuged by precipitate, taking precipitate also cleans 1 time with deionized water, then obtains elemental selenium 1 time with washes of absolute alcohol, gained elemental selenium is vacuum dried at 10 DEG C 1h, is subsequently placed in ball milling 2h in the ball mill of nitrogen protection and obtains nanometer selenium；
3, nanometer selenium is dissolved in the deionized water that mass ratio is 100 times of nanometer selenium quality; nanometer selenium suspension is obtained in 10 DEG C of stirring 15min; by nanometer selenium suspension add with its mass ratio be 1.5:1 containing the stearic ethanol solution that mass fraction is 10%; reduce pressure after 26 DEG C of magnetic agitation mix 30min sucking filtration; with deionized water rinsing 2 times; then being vacuum dried 1h in 20 DEG C, be cooled to room temperature, nitrogen protection lower grinding 10min obtains stearic acid modified nanometer selenium powder body；
4, in the abamectin emulsifiable concentrate that mass fraction is 5%, add the stearic acid modified nanometer selenium powder body that mass ratio is 0.04 times of abamectin emulsifiable concentrate and the petroleum ether that mass ratio is 0.0015 times of abamectin emulsifiable concentrate, add and the deionized water solution containing the sodium lauryl sulphate that mass fraction is 10% that above-mentioned solution total mass ratio is 1.2:1, then obtain nanometer selenium in 25 DEG C of stirring mixing 35min and be combined avilamycin selenium-rich pesticide.
Embodiment 2
1, Monohydrated selenium dioxide is dissolved in distilled water the Monohydrated selenium dioxide solution that formation molar concentration is 2.0mol/L, the sodium lauryl sulphate of 0.06 times of Monohydrated selenium dioxide mole is added in Monohydrated selenium dioxide solution, 15min is shaken with shaking table in 30 DEG C, add the ascorbic acid solution that molar concentration is 3.2mol/L of 3 times of Monohydrated selenium dioxide moles, shaking table shakes 10min, it is subsequently adding the sodium sulfite solution that molar concentration is 2.0mol/L of above liquor capacity 1% and to regulate pH be 5, control bath temperature and obtain precipitate at 25 DEG C of reaction 0.3h；
2, being centrifuged by precipitate, taking precipitate also cleans 3 times with deionized water, then obtains elemental selenium 3 times with washes of absolute alcohol, gained elemental selenium is vacuum dried at 60 DEG C 4h, is subsequently placed in ball milling 3h in the ball mill of nitrogen protection and obtains nanometer selenium；
3, nanometer selenium is dissolved in the deionized water that mass ratio is 600 times of nanometer selenium quality; nanometer selenium suspension is obtained in 30 DEG C of stirring 15min; by nanometer selenium suspension add with its mass ratio be 2.2:1 containing the stearic ethanol solution that mass fraction is 10%; reduce pressure after 45 DEG C of stirring mixing 50min sucking filtration; with deionized water rinsing 3 times; then being vacuum dried 3h in 40 DEG C, be cooled to room temperature, nitrogen protection lower grinding 20min obtains stearic acid modified nanometer selenium powder body；
4, in the abamectin emulsifiable concentrate that mass fraction is 5%, add the stearic acid modified nanometer selenium powder body that mass ratio is 0.08 times of abamectin emulsifiable concentrate and the petroleum ether that mass ratio is 0.02 times of abamectin emulsifiable concentrate, add and the deionized water solution containing the sodium lauryl sulphate that mass fraction is 10% that above-mentioned solution total mass ratio is 2:1, then obtain nanometer selenium in 45 DEG C of stirring mixing 50min and be combined avilamycin selenium-rich pesticide.
Embodiment 3
1, Monohydrated selenium dioxide is dissolved in distilled water the Monohydrated selenium dioxide solution that formation molar concentration is 3.1mol/L, the sodium lauryl sulphate of 0.1 times of Monohydrated selenium dioxide mole is added in Monohydrated selenium dioxide solution, 20min is shaken with shaking table in 50 DEG C, add the ascorbic acid solution that molar concentration is 5.2mol/L of 4 times of Monohydrated selenium dioxide moles, shaking table shakes 20min, it is subsequently adding the sodium sulfite solution that molar concentration is 3.0mol/L of above liquor capacity 1% and to regulate pH be 6, control bath temperature and obtain precipitate at 38 DEG C of reaction 0.5h；
2, being centrifuged by precipitate, taking precipitate also cleans 5 times with deionized water, then obtains elemental selenium 5 times with washes of absolute alcohol, gained elemental selenium is vacuum dried at 100 DEG C 8h, is subsequently placed in ball milling 4h in the ball mill of nitrogen protection and obtains nanometer selenium；
3, nanometer selenium is dissolved in the deionized water that mass ratio is 1000 times of nanometer selenium quality; nanometer selenium suspension is obtained in 50 DEG C of stirring 15min; by nanometer selenium suspension add with its mass ratio be 3:1 containing the stearic ethanol solution that mass fraction is 10%; reduce pressure after 59 DEG C of stirring mixing 70min sucking filtration; with deionized water rinsing 4 times; then being vacuum dried 4h in 55 DEG C, be cooled to room temperature, nitrogen protection lower grinding 30min obtains stearic acid modified nanometer selenium powder body；
4, in the abamectin emulsifiable concentrate that mass fraction is 5%, add the stearic acid modified nanometer selenium powder body that mass ratio is 0.12 times of abamectin emulsifiable concentrate and the petroleum ether that mass ratio is 0.04 times of abamectin emulsifiable concentrate, add and the deionized water solution containing the sodium lauryl sulphate that mass fraction is 10% that above-mentioned solution total mass ratio is 3:1, then obtain nanometer selenium in 65 DEG C of stirring mixing 60min and be combined avilamycin selenium-rich pesticide.
Comparative example 1
Step 1-3 is same as in Example 2, and in step 4 in addition to removing the step adding stearic acid modified nanometer selenium powder body, other is consistent with the step 4 in embodiment 2.
The absorbance of the different pesticide of table 1 and the rate of settling
| Absorbance | The rate of settling (stability) | |
| Embodiment 1 | Within 0.273(50 minute, do not stop to stir lower illumination) | Within 30 minutes, do not settle or be layered |
| Embodiment 2 | Within 0.271(50 minute, do not stop to stir lower illumination) | Within 35 minutes, do not settle or be layered |
| Embodiment 3 | Within 0.275(50 minute, do not stop to stir lower illumination) | Within 28 minutes, do not settle or be layered |
| Comparative example 1 | Within 0.345(50 minute, do not stop to stir lower illumination) | Sedimentation layering in 3 minutes |
Find that comparative example does not have good stability by table 1, within 3 minutes, i.e. start significantly to settle layering, found that by the contrast of absorbance the dulling luminosity ratio embodiment of comparative example is many greatly, illustrate that being not added with its photocatalytic degradation of nanometer selenium changes very slowly hardly, and embodiment 1-3 is relatively good.Illustrate that the product prepared according to the present invention all shows excellence in terms of stability, photocatalytic degradation.
Embodiment above describes the ultimate principle of the present invention, principal character and advantage; skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle that the present invention is simply described described in above-described embodiment and description; under the scope without departing from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements each fall within the scope of protection of the invention.
Claims (3)
1. a nanometer selenium is combined the preparation method of avilamycin selenium-rich pesticide, it is characterised in that concretely comprise the following steps:
Step (1); nanometer selenium is dissolved in the deionized water that mass ratio is 100-1000 times of nanometer selenium quality; nanometer selenium suspension is obtained in 10-50 DEG C of stirring mixing 15min; by nanometer selenium suspension add with its mass ratio be 1.5-3:1 containing the stearic ethanol solution that mass fraction is 10%; reduce pressure after 26-59 DEG C of stirring mixing 30-70min sucking filtration; with deionized water rinsing 2-4 time; then it is vacuum dried 1-4h in 20-55 DEG C; being cooled to room temperature, nitrogen protection lower grinding 10-30min obtains stearic acid modified nanometer selenium powder body；
Step (2), in the abamectin emulsifiable concentrate that mass fraction is 5%, add mass ratio be the stearic acid modified nanometer selenium powder body of 0.04-0.12 times of abamectin emulsifiable concentrate and mass ratio is the petroleum ether of 0.0015-0.04 times of abamectin emulsifiable concentrate, add and the deionized water solution containing the sodium lauryl sulphate that mass fraction is 10% that above-mentioned solution total mass ratio is 1.2-3:1, then obtain nanometer selenium in 25-65 DEG C of stirring mixing 35-60min and be combined avilamycin selenium-rich pesticide.
nullNanometer selenium the most according to claim 1 is combined the preparation method of avilamycin selenium-rich pesticide，The concrete building-up process that it is characterized in that described nanometer selenium is: is dissolved in distilled water by Monohydrated selenium dioxide and forms the Monohydrated selenium dioxide solution that molar concentration is 0.1-3.1mol/L，The sodium lauryl sulphate of 0.01-0.1 times of Monohydrated selenium dioxide mole is added in Monohydrated selenium dioxide solution，In 10-50 DEG C of stirring mixing 10-20min，Add the ascorbic acid solution that molar concentration is 0.1-5.2mol/L of 2-4 times of Monohydrated selenium dioxide mole，Stirring mixing 1-20min，The sodium sulfite solution that molar concentration is 0.1-3.0mol/L being subsequently adding above-mentioned liquor capacity 1% pH regulating solution are 3-6，In the water-bath of 12-38 DEG C, react 0.1-0.5h be precipitated thing；Clean 1-5 time with deionized water after precipitate is centrifuged, then obtain elemental selenium 1-5 time with washes of absolute alcohol, elemental selenium is placed on ball milling 2-4h in the ball mill of nitrogen protection in 10-100 DEG C of vacuum drying 1-8h and obtains nanometer selenium.
3. a nanometer selenium is combined avilamycin selenium-rich pesticide, it is characterised in that be to be prepared by the method described in claim 1 or 2.
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| CN201610265258.3A CN105875603A (en) | 2016-04-26 | 2016-04-26 | Nano-selenium composite avermectin selenium-rich pesticide and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109042130A (en) * | 2018-07-11 | 2018-12-21 | 界首市红旭农业发展有限公司 | A kind of pepper planting method improving Quality of Capsicum |
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| CN104920449A (en) * | 2015-05-05 | 2015-09-23 | 贺州学院 | Nano-zinc oxide composite triazophos pesticide and preparation method therefor |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104920449A (en) * | 2015-05-05 | 2015-09-23 | 贺州学院 | Nano-zinc oxide composite triazophos pesticide and preparation method therefor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109042130A (en) * | 2018-07-11 | 2018-12-21 | 界首市红旭农业发展有限公司 | A kind of pepper planting method improving Quality of Capsicum |
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