CN105851000A - Nano titanium dioxide compound abamectin pesticide and preparation method thereof - Google Patents
Nano titanium dioxide compound abamectin pesticide and preparation method thereof Download PDFInfo
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- CN105851000A CN105851000A CN201610265943.6A CN201610265943A CN105851000A CN 105851000 A CN105851000 A CN 105851000A CN 201610265943 A CN201610265943 A CN 201610265943A CN 105851000 A CN105851000 A CN 105851000A
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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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- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
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- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
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- Environmental Sciences (AREA)
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- Agricultural Chemicals And Associated Chemicals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses nano titanium dioxide compound abamectin pesticide and a preparation method thereof and belongs to the technical field of compound pesticide. The technical scheme disclosed by the invention has essentials that the nano titanium dioxide compound abamectin pesticide is prepared by adding nano titanium dioxide suspension liquid into an ethanol solution of stearic acid, mixing the solution and decompressing and filtering to obtain stearic acid modified nano titanium dioxide powder, adding the stearic acid modified nano titanium dioxide powder and cyclohexanone into abamectin missible oil, adding a de-ionized water solution of sodium dodecyl sulfate, and uniformly stirring and mixing. The process method disclosed by the invention is simple and can easily realize industrial production; and the prepared nano titanium dioxide compound abamectin pesticide has the advantages of environmental friendliness, short chemical remaining time and the like.
Description
Technical field
The invention belongs to composite pesticide technical field, be specifically related to a kind of nano titanium oxide be combined avilamycin pesticide and
Its preparation method.
Background technology
At present, for solving Pesticide Residue, the degraded to avilamycin pesticide does not has good solution, although have
Utilizing nano material to avilamycin of degrading, but its degradation efficiency is low.Therefore, one to be developed is had can to improve degraded Avermectin
The pesticide of element efficiency, can either play the effect of parasite killing, can shorten again the residence time in crop.
Summary of the invention
Present invention solves the technical problem that there is provided a kind of nano titanium oxide is combined avilamycin pesticide and preparation thereof
Method.
The present invention solves that above-mentioned technical problem adopts the following technical scheme that, a kind of nano titanium oxide is combined avilamycin
The preparation method of pesticide, it is characterised in that concretely comprise the following steps:
Step (1), is dissolved in Butyl Phthalate in the dehydrated alcohol that mass ratio is 2-7 times of Butyl Phthalate quality and obtains solution A；
Step (2), is 1-5 times of phthalandione fourth by dehydrated alcohol and the mass ratio that mass ratio is 2-6.5 times of Butyl Phthalate quality
The pure water mix homogeneously of ester quality, adds and the glacial acetic acid of Butyl Phthalate equimolar amounts be uniformly mixed and obtain solution B；
Step (3), the temperature controlling solution A is 25-45 DEG C, continuously stirred under nitrogen protection, solution B is added drop-wise in solution A
And the pH value by hydrochloric acid control reaction system is 2-4.5, wherein the drop rate of solution B is that 90-170 drips/min；
Step (4), the pH value continuing to control reaction system after solution B dropping is complete is 2-4.5, solution after reaction 1.5-3.5h
Become transparent or light yellow gel, gel slice is put in surface plate, place in vacuum drying oven in 35-52 DEG C of dry 6-
18h obtains yellow crystalline presoma, is put into by presoma in ball mill, is simultaneously introduced the 12 of presoma quality 0.12%-1.5%
Sodium alkyl benzene sulfonate, ball milling 20-50min is to the TiO 2 precursor forming 200-500 mesh；
Step (5), is placed in Muffle furnace calcining by TiO 2 precursor, uses temperature programming, is warming up to 240-280 DEG C of calcining
1-8h, is warming up to 340-380 DEG C of calcining 1-8h, is warming up to 440-480 DEG C of calcining 1-8h, is warming up to 540-580 DEG C of calcining 3-8h,
Successively with water and ethanol purge after cooling, place in drying baker and obtain nano titanium oxide in 100-140 DEG C of dry 3-7h；
Step (6), joins the deionization that mass ratio is 100-1200 times of nano titanium oxide quality by nano titanium oxide
In water, obtain nano titanium oxide suspension in 10-50 DEG C of stirring 15min；
Step (7), adds nano titanium oxide suspension and the tristearin that mass fraction is 13% that its mass ratio is 1.5-3:1
In acid ethanol solution, stir 20-70min, then the sucking filtration that reduced pressure by above-mentioned mixed solution in 50-76 DEG C of constant temperature, and use deionized water
Clean 2-4 time, then in 40-85 DEG C of dry 1-4h, grind 10-30min after being cooled to room temperature and obtain stearic acid modified nanometer two
Titanium oxide powder；
Step (8), adding mass ratio in the abamectin emulsifiable concentrate that mass fraction is 5% is 0.016-0.058 times of avilamycin
The stearic acid modified nano-titanium dioxide powder of cream and mass ratio are the hexamethylene of 0.001-0.034 times of abamectin emulsifiable concentrate
Ketone, add with above-mentioned solution total mass ratio be 1.5-3:1 containing the sodium lauryl sulphate that mass fraction is 11% go from
Sub-aqueous solution, then obtains nano titanium oxide in 25-59 DEG C of stirring mixing 38-72min and is combined avilamycin pesticide.
Nano titanium oxide of the present invention is combined avilamycin pesticide, prepares according to the method described above.
The process of the present invention is simple, it is easy to industrialized production, and obtained nano titanium oxide is combined avilamycin
Pesticide has environmental friendliness and the advantage such as the chemical residual time is short.
Detailed description of the invention
By the following examples the foregoing of the present invention is described in further details, but this should be interpreted as this
The scope inventing above-mentioned theme is only limitted to below example, and all technology realized based on foregoing of the present invention belong to this
Bright scope.
Embodiment 1
1, Butyl Phthalate is dissolved in the dehydrated alcohol that mass ratio is 2 times of Butyl Phthalate quality and obtains solution A；
2, by the dehydrated alcohol that mass ratio is 2 times of Butyl Phthalate quality and the pure water that mass ratio is 1 times of Butyl Phthalate quality
Mix homogeneously, adds and the glacial acetic acid of Butyl Phthalate equimolar amounts be uniformly mixed and obtain solution B；
3, the temperature controlling solution A is 25 DEG C, continuously stirred under nitrogen protection, solution B is added drop-wise in solution A and uses hydrochloric acid control
The pH value of reaction system processed is 2, and wherein the drop rate of solution B is 90/min；
4, the pH value continuing to control reaction system after solution B dropping is complete is 2, and after reaction 1.5h, solution becomes light yellow solidifying
Glue, puts into gel slice in surface plate, places in vacuum drying oven and obtains yellow crystalline presoma in 35 DEG C of dry 6h, by front
Driving body and put in ball mill, be simultaneously introduced the dodecylbenzene sodium sulfonate of presoma quality 0.12%, ball milling 20min is to forming two
Titania precursor body；
5, TiO 2 precursor is placed in Muffle furnace calcining, uses temperature programming, be warming up to 240 DEG C of calcining 1h, be warming up to
340 DEG C of calcining 1h, are warming up to 440 DEG C of calcining 1h, are warming up to 540 DEG C of calcining 3h, use water and ethanol purge successively, then put after cooling
Enter in drying baker and obtain nano titanium oxide in 100 DEG C of dry 3h；
6, nano titanium oxide is joined in the deionized water that mass ratio is 100 times of nano titanium oxide quality, in 10 DEG C
Stirring 15min obtains nano titanium oxide suspension；
7, nano titanium oxide suspension is added molten with the stearic acid ethanol that the mass fraction that its mass ratio is 1.5:1 is 13%
In liquid, stir 20min, then the sucking filtration that reduced pressure by above-mentioned mixed solution in 50 DEG C of constant temperature, and clean 2 times with deionized water, then in
40 DEG C of dry 1h, grind 10min and obtain stearic acid modified nano-titanium dioxide powder after being cooled to room temperature；
8, in the abamectin emulsifiable concentrate that mass fraction is 5%, the stearic acid that mass ratio is 0.016 times of abamectin emulsifiable concentrate is added
Modified nano-titanium dioxide powder body and the Ketohexamethylene that mass ratio is 0.001 times of abamectin emulsifiable concentrate, add and above-mentioned solution
Total mass ratio is the deionized water solution containing the sodium lauryl sulphate that mass fraction is 11% of 1.5:1, then stirs in 25 DEG C
Mix mixing 38min to obtain nano titanium oxide and be combined avilamycin pesticide.
Embodiment 2
1, Butyl Phthalate is dissolved in the dehydrated alcohol that mass ratio is 5 times of Butyl Phthalate quality and obtains solution A；
2, by the dehydrated alcohol that mass ratio is 4 times of Butyl Phthalate quality and the pure water that mass ratio is 3 times of Butyl Phthalate quality
Mix homogeneously, adds and the glacial acetic acid of Butyl Phthalate equimolar amounts be uniformly mixed and obtain solution B；
3, the temperature controlling solution A is 35 DEG C, continuously stirred under nitrogen protection, solution B is added drop-wise in solution A and uses hydrochloric acid control
The pH value of reaction system processed is 3.2, and wherein the drop rate of solution B is 120/min；
4, the pH value continuing to control reaction system after solution B dropping is complete is 3.2, and after reaction 2h, solution becomes light yellow solidifying
Glue, puts into gel slice in surface plate, places in vacuum drying oven and obtains yellow crystalline presoma in 45 DEG C of dry 12h, will
Presoma is put in ball mill, is simultaneously introduced the dodecylbenzene sodium sulfonate of presoma quality 0.85%%, and ball milling 30min is to being formed
TiO 2 precursor；
5, TiO 2 precursor is placed in Muffle furnace calcining, uses temperature programming, be warming up to 260 DEG C of calcining 4h, be warming up to
360 DEG C of calcining 4h, are warming up to 460 DEG C of calcining 4h, are warming up to 560 DEG C of calcining 6h, use water and ethanol purge successively, then put after cooling
Enter in drying baker and obtain nano titanium oxide in 120 DEG C of dry 5h；
6, nano titanium oxide is joined in the deionized water that mass ratio is 600 times of nano titanium oxide quality, in 30 DEG C
Stirring 15min obtains nano titanium oxide suspension；
7, nano titanium oxide suspension is added and the stearic acid ethanol solution that mass fraction is 13% that its mass ratio is 2:1
In, stir 50min, then the sucking filtration that reduced pressure by above-mentioned mixed solution in 60 DEG C of constant temperature, and clean 3 times with deionized water, then in 65
DEG C dry 3h, grinds 20min and obtains stearic acid modified nano-titanium dioxide powder after being cooled to room temperature；
8, in the abamectin emulsifiable concentrate that mass fraction is 5%, the stearic acid that mass ratio is 0.038 times of abamectin emulsifiable concentrate is added
Modified nano-titanium dioxide powder body and the Ketohexamethylene that mass ratio is 0.018 times of abamectin emulsifiable concentrate, add and above-mentioned solution
Total mass ratio is the deionized water solution containing the sodium lauryl sulphate that mass fraction is 11% of 2:1, then in 45 DEG C of stirrings
Mixing 48min obtains nano titanium oxide and is combined avilamycin pesticide.
Embodiment 3
1, Butyl Phthalate is dissolved in the dehydrated alcohol that mass ratio is 7 times of Butyl Phthalate quality and obtains solution A；
2, it is the pure of 5 times of Butyl Phthalate quality by dehydrated alcohol that mass ratio is 6.5 times of Butyl Phthalate quality with mass ratio
Water mix homogeneously, adds and the glacial acetic acid of Butyl Phthalate equimolar amounts be uniformly mixed and obtain solution B；
3, the temperature controlling solution A is 45 DEG C, continuously stirred under nitrogen protection, solution B is added drop-wise in solution A and uses hydrochloric acid control
The pH value of reaction system processed is 4.5, and wherein the drop rate of solution B is 170/min；
4, the pH value continuing to control reaction system after solution B dropping is complete is 4.5, and after reaction 3.5h, solution becomes transparent solidifying
Glue, puts into gel slice in surface plate, places in vacuum drying oven and obtains yellow crystalline presoma in 52 DEG C of dry 18h, will
Presoma is put in ball mill, is simultaneously introduced the dodecylbenzene sodium sulfonate of presoma quality 1.5%, and ball milling 50min is to forming two
Titania precursor body；
5, TiO 2 precursor is placed in Muffle furnace calcining, uses temperature programming, be warming up to 280 DEG C of calcining 8h, be warming up to
380 DEG C of calcining 8h, are warming up to 480 DEG C of calcining 8h, are warming up to 580 DEG C of calcining 8h, use water and ethanol purge successively, then put after cooling
Enter in drying baker and obtain nano titanium oxide in 140 DEG C of dry 7h；
6, nano titanium oxide is joined in the deionized water that mass ratio is 1200 times of nano titanium oxide quality, in 50 DEG C
Stirring 15min obtains nano titanium oxide suspension；
7, nano titanium oxide suspension is added and the stearic acid ethanol solution that mass fraction is 13% that its mass ratio is 3:1
In, stir 70min, then the sucking filtration that reduced pressure by above-mentioned mixed solution in 76 DEG C of constant temperature, and clean 4 times with deionized water, then in 85
DEG C dry 4h, grinds 30min and obtains stearic acid modified nano-titanium dioxide powder after being cooled to room temperature；
8, in the abamectin emulsifiable concentrate that mass fraction is 5%, the stearic acid that mass ratio is 0.058 times of abamectin emulsifiable concentrate is added
Modified nano-titanium dioxide powder body and the Ketohexamethylene that mass ratio is 0.034 times of abamectin emulsifiable concentrate, add and above-mentioned solution
Total mass ratio is the deionized water solution containing the sodium lauryl sulphate that mass fraction is 11% of 3:1, then in 59 DEG C of stirrings
Mixing 72min obtains nano titanium oxide and is combined avilamycin pesticide.
Comparative example 1
Step 1-3 is same as in Example 2, except removing the step adding stearic acid modified nano-titanium dioxide powder in step 4
Outward, 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 0.378(50 minute, do not stop to stir lower illumination) | Within 31 minutes, do not settle or be layered |
| Embodiment 2 | Within 0.376(50 minute, do not stop to stir lower illumination) | Within 45 minutes, do not settle or be layered |
| Embodiment 3 | Within 0.374(50 minute, do not stop to stir lower illumination) | Within 26 minutes, do not settle or be layered |
| Comparative example 1 | Within 0.545(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, by inhaling
The contrast of luminosity finds that the dulling luminosity ratio embodiment of comparative example is many greatly, illustrates to be not added with its photocatalytic degradation of nano titanium oxide
Very slowly, change hardly, and embodiment 1-3 is relatively good.Illustrate that the product prepared according to the present invention is at stability, photocatalytic degradation
Aspect all shows excellence.
Embodiment above describes the ultimate principle of the present invention, principal character and advantage, the technical staff of the industry should
Understanding, the present invention is not restricted to the described embodiments, and the simply explanation present invention's described in above-described embodiment and description is former
Reason, 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
In the scope of protection of the invention.
Claims (2)
1. a nano titanium oxide is combined the preparation method of avilamycin pesticide, it is characterised in that concretely comprise the following steps:
Step (1), is dissolved in Butyl Phthalate in the dehydrated alcohol that mass ratio is 2-7 times of Butyl Phthalate quality and obtains solution A；
Step (2), is 1-5 times of phthalandione fourth by dehydrated alcohol and the mass ratio that mass ratio is 2-6.5 times of Butyl Phthalate quality
The pure water mix homogeneously of ester quality, adds and the glacial acetic acid of Butyl Phthalate equimolar amounts be uniformly mixed and obtain solution B；
Step (3), the temperature controlling solution A is 25-45 DEG C, continuously stirred under nitrogen protection, solution B is added drop-wise in solution A
And the pH value by hydrochloric acid control reaction system is 2-4.5, wherein the drop rate of solution B is that 90-170 drips/min；
Step (4), the pH value continuing to control reaction system after solution B dropping is complete is 2-4.5, solution after reaction 1.5-3.5h
Become transparent or light yellow gel, gel slice is put in surface plate, place in vacuum drying oven in 35-52 DEG C of dry 6-
18h obtains yellow crystalline presoma, is put into by presoma in ball mill, is simultaneously introduced the 12 of presoma quality 0.12%-1.5%
Sodium alkyl benzene sulfonate, ball milling 20-50min is to the TiO 2 precursor forming 200-500 mesh；
Step (5), is placed in Muffle furnace calcining by TiO 2 precursor, uses temperature programming, is warming up to 240-280 DEG C of calcining
1-8h, is warming up to 340-380 DEG C of calcining 1-8h, is warming up to 440-480 DEG C of calcining 1-8h, is warming up to 540-580 DEG C of calcining 3-8h,
Successively with water and ethanol purge after cooling, place in drying baker and obtain nano titanium oxide in 100-140 DEG C of dry 3-7h；
Step (6), joins the deionization that mass ratio is 100-1200 times of nano titanium oxide quality by nano titanium oxide
In water, obtain nano titanium oxide suspension in 10-50 DEG C of stirring 15min；
Step (7), adds nano titanium oxide suspension and the tristearin that mass fraction is 13% that its mass ratio is 1.5-3:1
In acid ethanol solution, stir 20-70min, then the sucking filtration that reduced pressure by above-mentioned mixed solution in 50-76 DEG C of constant temperature, and use deionized water
Clean 2-4 time, then in 40-85 DEG C of dry 1-4h, grind 10-30min after being cooled to room temperature and obtain stearic acid modified nanometer two
Titanium oxide powder；
Step (8), adding mass ratio in the abamectin emulsifiable concentrate that mass fraction is 5% is 0.016-0.058 times of avilamycin
The stearic acid modified nano-titanium dioxide powder of cream and mass ratio are the hexamethylene of 0.001-0.034 times of abamectin emulsifiable concentrate
Ketone, add with above-mentioned solution total mass ratio be 1.5-3:1 containing the sodium lauryl sulphate that mass fraction is 11% go from
Sub-aqueous solution, then obtains nano titanium oxide in 25-59 DEG C of stirring mixing 38-72min and is combined avilamycin pesticide.
2. a nano titanium oxide is combined avilamycin pesticide, it is characterised in that be to be prepared by the method described in claim 1
Obtain.
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| CN201610265943.6A CN105851000A (en) | 2016-04-27 | 2016-04-27 | Nano titanium dioxide compound abamectin pesticide and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610265943.6A CN105851000A (en) | 2016-04-27 | 2016-04-27 | Nano titanium dioxide compound abamectin pesticide and preparation method thereof |
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Citations (5)
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| CN1468937A (en) * | 2002-07-18 | 2004-01-21 | 青岛海洋大学 | Residual pesticide degrading agent |
| CN1843113A (en) * | 2006-03-15 | 2006-10-11 | 厦门大学 | Method for organochlorine pesticide photocatalytic degradation on nano titania |
| CN101288397A (en) * | 2007-06-06 | 2008-10-22 | 贵州大学 | Nano composite pesticides new formulation and preparation method thereof |
| CN104920449A (en) * | 2015-05-05 | 2015-09-23 | 贺州学院 | Nano-zinc oxide composite triazophos pesticide and preparation method therefor |
-
2016
- 2016-04-27 CN CN201610265943.6A patent/CN105851000A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1338211A (en) * | 2000-08-16 | 2002-03-06 | 秦泽荣 | Photocytalytic agricultural chemical and its application |
| CN1468937A (en) * | 2002-07-18 | 2004-01-21 | 青岛海洋大学 | Residual pesticide degrading agent |
| CN1843113A (en) * | 2006-03-15 | 2006-10-11 | 厦门大学 | Method for organochlorine pesticide photocatalytic degradation on nano titania |
| CN101288397A (en) * | 2007-06-06 | 2008-10-22 | 贵州大学 | Nano composite pesticides new formulation and preparation method thereof |
| CN104920449A (en) * | 2015-05-05 | 2015-09-23 | 贺州学院 | Nano-zinc oxide composite triazophos pesticide and preparation method therefor |
Non-Patent Citations (2)
| Title |
|---|
| 周光红等: "《可降解的复合农药—纳米TiO2制剂的研究》", 《全国纳米材料和技术应用会议论文集》 * |
| 李梅金等: "《纳米TiO2光催化转化下有机氯农药与AgN03的光谱特性研究》", 《光谱学与光谱分析》 * |
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