CN104886061A - Paraquat oil suspension and preparation method thereof - Google Patents
Paraquat oil suspension and preparation method thereof Download PDFInfo
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- CN104886061A CN104886061A CN201510142165.7A CN201510142165A CN104886061A CN 104886061 A CN104886061 A CN 104886061A CN 201510142165 A CN201510142165 A CN 201510142165A CN 104886061 A CN104886061 A CN 104886061A
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Abstract
The invention belongs to the field of pesticide agents and relates to herbicides, especially to a paraquat oil suspension and a preparation method thereof. The paraquat oil suspension comprises the following components in parts by weight: 0.5-50 parts of paraquat; 0.1-10 parts of a dispersant; 5-25 parts of an emulsifier; 0.1-10 parts of a thickening agent; and 50-80 parts of filler vegetable oil. Compared with the prior art, the paraquat oil suspension provided by the invention has the following advantages and positive effects: the preparation method comprises the following steps: according to the invention, by taking advantage of characteristics of the filler vegetable oil, the filler vegetable oil is added into the herbicide so as to increase the affinity, stretching property and wettability of the solution on surfaces of vegetables, thus improving drug effects and effectively preventing rainfall flushing from decreasing the effect.
Description
Technical field
The invention belongs to pesticidal chemical field, relate to weed killer herbicide, particularly relate to a kind of paraquat oil-suspending agent and preparation method thereof.
Background technology
Paraquat, chemical name is 1-1-dimethyl-4-4-bipyridine cation salt, and be a kind of steriland herbicide fast, the photosynthetical system in the chloroplast of green plants absorbs luminous energy and manufactures sugar, thus provides nutrient for plant.Paraquat can accurately enter the biochemical system being referred to as photosynthetical system, this system can produce free electron to promote photosynthesis, paraquat ion and these electronics react and are formed " free radical ", these radical conversions are peroxide rapidly by oxygen, and these peroxide are easy to react with the unsaturated fatty acid in cell membrane, through this series of chemical reaction, cell membrane is destroyed, cellular content leaks and mixes, and causes larger destruction, makes it withered.Whole process is very rapid, the therefore paraquat transfer that can not can observe.And to the not effect of non-green tissue.Simultaneously paraquat is combined and passivation with soil rapidly in soil, to plant root and perennial subterranean stem and perennial root invalid.
Its structural formula:
Molecular formula: C12H14Cl2N2
Chemical name: 1-1-dimethyl-4-4-bipyridine cation salt
Physicochemical property: former medicine is white crystal, content > more than 95%, 300 DEG C decomposition, proportion 1.10, very easily water-soluble, be slightly soluble in low-molecular-weight alcohols, be insoluble to varsol.Stable in acidity and neutral solution, be hydrolyzed in alkalescence.Former medicine is corrosive to metal.
Due to paraquat site of action accurately and rapidly herbicidal effect and rain fastness energy and contacting with soil lose activity and retain weeds root system, characteristic to crop safety; make paraquat in conservation tillage system especially in no-tillage technology; play crucial and irreplaceable effect; in the use procedure of immediate and mid-term; paraquat is accepted by peasant all over the world; create huge society and economic benefit; also reduce the phenomenon of the soil erosion simultaneously, become indispensable agriculture articles for use.But paraquat preparation is mainly aqua product in the market, if but there is rainfall in the short time after aqua product dispenser, then can have a strong impact on result of use.
Summary of the invention
If there is rainfall in the short time after the present invention is directed to above-mentioned dispenser, the technical problem such as result of use reduction proposes a kind ofly to fill a prescription rationally, resistance of rainwater washing against and the good paraquat oil-suspending agent of herbicidal effect.
In order to achieve the above object, the technical solution used in the present invention is, the invention provides a kind of paraquat oil-suspending agent, and this paraquat oil-suspending agent comprises following composition by weight:
Paraquat 10 parts ~ 50 parts;
Dispersant 0.1 part ~ 10 parts;
Emulsifier 5 parts ~ 25 parts;
Thickener 0.1 part ~ 10 parts;
Filler vegetable oil 50 parts ~ 80 parts.
At above-mentioned paraquat oil-suspending agent, described dispersant is polycarboxylic acid salt, agriculture breast 602#, 33#, polycarboxylic acid salt, lignosulfonates, naphthalenesulfonate formaldehyde condensation compound, at least one material in alkylphenol polyoxyethylene, in polyether phosphate class, Pluronic PE 6800, and preferred dispersant is the combination of polycarboxylic acid salt and Pluronic PE 6800 or agriculture breast 602# and the combination of Pluronic PE 6800 or the combination of polyoxyethylene nonylphenol ether and naphthalenesulfonate formaldehyde condensation compound.
At above-mentioned paraquat oil-suspending agent, described emulsifier is alkyl benzene calcium sulfonate, agriculture breast 602#, 33#, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether, at least one material in alkylphenol polyoxyethylene formaldehyde condensation products, and preferred emulsifier is the combination of alkyl benzene calcium sulfonate and castor oil polyoxyethylene ether or agriculture breast 602# and the combination of Pluronic PE 6800 or the combination of alkyl benzene calcium sulfonate and castor oil polyoxyethylene ether.
At above-mentioned paraquat oil-suspending agent, described thickener is at least one material in organobentonite, aluminium-magnesium silicate, white carbon, urea, ammonium sulfate, and preferred thickener is the combination of organobentonite and white carbon or the combination of organobentonite and urea.
At above-mentioned paraquat oil-suspending agent, described filler vegetable oil is: at least one material in soybean oil, epoxidized soybean oil, methyl oleate, turpentine-based vegetable oil, peanut oil, palm oil, corn oil, cottonseed oil, esterification soybean oil, esterification cottonseed oil, and preferred filler vegetable oil is epoxidized soybean oil or methyl oleate or soybean oil.
Present invention also offers the preparation method of paraquat oil-suspending agent, comprise the following steps:
Get the raw materials ready: prepare in advance to produce former medicine paraquat, dispersant, emulsifier, thickener, the vegetable oil needed for this product.
Feed intake.First open the valve of measuring tank to shear and homogenize still, the vegetable oil measured is put into still.Start high speed shear and stirring, with membrane pump, the liquid adjuvants weighed up (such as emulsifier, dispersant) is pumped in still simultaneously, manually solid material (such as thickener, part dispersant) is dropped in still, stir shearing 20 ~ 30 minutes, observe, until material is even in upper and lower layer sampling respectively.
Start high speed shear and stirring, by artificial, former for load weighted paraquat medicine dropped in still, stirs shearing 30 ~ 45 minutes, evenly.
Material sand milling.Material in still is slowly pumped into by membrane pump in the 50L sand mill of 3 series connection, utilize sanding media (scandium oxide pearl) sand milling in sand mill, and pass through circulating water cooling, control temperature≤50 DEG C, discharging speed controls at 350 kilograms ~ 400 kgs/hour, detect particle diameter and reach D50≤1.5 μm, D90≤5.5 μm, particle total amount >=95% of≤6 μm.First sanding media particle diameter is 1.4 ~ 1.6 μm, and sanding media loading is 115 ~ 120 kg; Second sand mill sanding media particle diameter is 1.0 ~ 1.2 μm, and sanding media loading is 105 ~ 115 kilograms; 3rd sand mill sand mill sanding media particle diameter is 0.8 ~ 1.0 μm, and sand mill sanding media loading is 105 ~ 110 kilograms.
Filter: sand milling material out, pump into a middle batch turning tank by membrane pump, filter with 40 eye mesh screens simultaneously.
Detect: sampling detects active ingredient (paraquat) content, dispersion and emulsion (qualified), fineness (D50≤1.5 μm, D90≤5.5 μm, particle total amount >=95% of≤6 μm), the index such as suspensibility (>=90%), moisture (≤0.5%), pH (4 ~ 7), can Production and Packaging after qualified.
Compared with prior art, advantage of the present invention and good effect are, comprise following content:
The present invention utilizes the characteristic of filler vegetable oil, adds filler vegetable oil in weed killer herbicide, improves the affinity, plate-out ability, wetability etc. of liquid at plant surface, and then improves drug effect, and effectively avoids the effect reduction caused because of rain drop erosion.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme of the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing in the following describes is some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
The preparation flow figure that Fig. 1 provides for the embodiment of the present invention 1.
Embodiment
In order to more clearly understand above-mentioned purpose of the present invention, feature and advantage, below in conjunction with drawings and Examples, the present invention will be further described.It should be noted that, when not conflicting, the feature in the embodiment of the application and embodiment can combine mutually.
Set forth a lot of detail in the following description so that fully understand the present invention, but the present invention can also adopt and be different from other modes described here and implement, and therefore, the present invention is not limited to the restriction of the specific embodiment of prospectus below.
Embodiment 1: the present embodiment provides a 10% paraquat oil-suspending agent, in the present embodiment, former medicine and auxiliary agent are selected and proportioning is:
The former medicine of 95% paraquat 10.52 parts;
Dispersant is polycarboxylic acid salt 3.0 parts, Pluronic PE 6800 2.0 parts;
Emulsifier is alkyl benzene calcium sulfonate 2.5 parts, castor oil polyoxyethylene ether 5 parts;
Thickener is 2 parts of organobentonites, 1.5 parts of white carbons;
Filler vegetable oil is that methyl oleate complements to 100 parts.
Calculate each amounts of components respectively by above proportioning, in oil phase, add polycarboxylate analog assistant 3.0 parts, Pluronic PE 6800 2.0 parts, alkyl benzene calcium sulfonate 2.5 parts, castor oil polyoxyethylene ether 5 parts, mixing is uniformly dispersed; Add thickener 2 parts of organobentonites, 1.5 parts of white carbons, be uniformly mixed; 10.52 parts of paraquats are added under high shear agitation; In bead or pick pearl medium, carry out grinding 2h ~ 2.5h, circulating water cooling, ensure temperature of charge≤50 DEG C, detect particle diameter and reach D90≤6 μm; 40 mesh filter screen impurity screenings; Detect index of correlation; Packaging.Carry out Product checking according to oil-suspending agent quality control index, index comprises outward appearance, active constituent content, suspensibility, moisture, pH, fineness, dispersion and emulsion, low-temperature stability, thermodynamic stability.
Paraquat oil-suspending agent agent performance indications prepared by embodiment 1 are: appearance white oily liquids; Paraquat content 9.80%, can become cloud dispersion and emulsion; Suspensibility is 100%; Moisture 0.1%, pH5.6; Fineness D90=5.2 μm; Heat storage stability is qualified, active ingredient paraquat resolution ratio 0.5%.
Embodiment 2: the present embodiment provides a 20% paraquat oil-suspending agent, in the present embodiment, former medicine and auxiliary agent are selected and proportioning is:
The former medicine of 95% paraquat 21.05 parts;
Dispersant is agriculture breast 602#3.0 part, Pluronic PE 6800 2.0 parts;
Emulsifier is alkyl benzene calcium sulfonate 3.0 parts, fatty alcohol-polyoxyethylene ether 8 parts;
Thickener is organobentonite 1.0 parts, white carbon 0.75 part;
Filler vegetable oil is that soybean oil complements to 100 parts.
The preparation method of embodiment 2 is consistent with embodiment 1.
Paraquat oil-suspending agent agent performance indications prepared by embodiment 2 are: appearance white oily liquids; Paraquat content 20.2%; Cloud dispersion and emulsion can be become; Suspensibility is 100%; Moisture 0.1%, pH5.6; Fineness D90=5.5 μm; Heat storage stability is qualified, active ingredient paraquat resolution ratio 0.8%.
Embodiment 3: the present embodiment provides a 35% paraquat oil-suspending agent, in the present embodiment, former medicine and auxiliary agent are selected and proportioning is:
The former medicine of 95% paraquat 36.84 parts;
Dispersant is polyoxyethylene nonylphenol ether 3.5 parts, naphthalenesulfonate formaldehyde condensation compound 2.0 parts;
Emulsifier is alkyl benzene calcium sulfonate 2.5 parts, castor oil polyoxyethylene ether 8 parts;
Thickener is organobentonite 0.2 part, 0.8 part, urea;
Filler vegetable oil is that epoxidized soybean oil complements to 100 parts.
The preparation method of embodiment 3 is consistent with embodiment 1.
The concrete measurement result of each performance indications of paraquat oil-suspending agent prepared by embodiment 3 is: the paraquat oil-suspending agent agent performance indications of preparation are: appearance white oily liquids; Paraquat content 35.2%; Cloud dispersion and emulsion can be become; Suspensibility all reaches 100%; Moisture 0.3%, pH6.4; Fineness D90=5.0 μm; Heat storage stability is qualified, active ingredient paraquat resolution ratio 0.8%.
The test of pesticide effectiveness:
Compare to carry out drug effect with paraquat oil-suspending agent of the present invention, the 200g/l paraquat aqua (first just reaching Kirchhoff integral) that buying market is most widely used and domestic certain producer 200g/L paraquat aqua (green track) are for activity of weeding check experiment.
Activity of weeding is listed in following each embodiment for the weeds kind of testing postemergence herbicide activity of the present invention.These tests carry out for the weeds of land for growing field crops in all parts of the country self-sow, mainly contains lady's-grass, eleusine indica, the rhizome of nutgrass flatsedge, green foxtail, Horseweed Herb etc.
Test the test method that specifies according to GB/T17980.1-17980.50-2000 " pesticide field efficacy medicine test criterion () " and investigation method is carried out.Each process is according to recommended dose dispenser, and 4 repetitions are established in each process, and each plot area is 45m2, each community randomized arrangement; In the dispenser of weed growth animated period, water consumption calculates according to 600L/h ㎡; Respectively at after medicine 1,3,5,7,14 day, at each community Stochastic choice 3 ~ 4 points, often some 0.5m2 carried out sample investigation, the total strain number of often kind of weeds of record investigation.The average weed density in the front test region of medicine is 1105 strains/㎡, the main ruderal species class lady's-grass in this ground, eleusine indica, the rhizome of nutgrass flatsedge, green foxtail, Horseweed Herb, and accounting is classified as 40.2%, 18.5%, 15.2%, 14.3%, 11.8% routine dividing by strain number percentage.Result of the test calculates the drug effect of medicament according to the following equation: the remaining number of weeds for the treatment of region, control efficiency (%)=(the careless number of the blank district remaining work of careless number-treatment region alive) careless number × 100 alive ,/blank district.
Blank district careless number alive also does once total herbicidal effect investigation for 14 days after administration, adopts eye estimate investigation method.Classification investigation and record.
Weed control efficacy grade scale is as following table:
| Rank | Weeding situation describes |
| 1 grade | Without grass |
| 2 grades | Be equivalent to 0 ~ 2.5% of blank district weeds |
| 3 grades | Be equivalent to 2.5% ~ 5% of blank district weeds |
| 4 grades | Be equivalent to 5% ~ 10% of blank district weeds |
| 5 grades | Be equivalent to 10% ~ 15% of blank district weeds |
| 6 grades | Be equivalent to 15% ~ 25% of blank district weeds |
| 7 grades | Be equivalent to 25% ~ 35% of blank district weeds |
| 8 grades | Be equivalent to 35% ~ 67.5% of blank district weeds |
| 9 grades | Be equivalent to 67.5% ~ 100% of blank district weeds |
Raw embodiment paraquat oil-suspending agent of surveying is tested the herbicidal effect of lady's-grass
According to test requirements document, after the lady's-grass with the chemicals treatment growth animated period of embodiment and comparative example, the strain preventive effect investigating each process for 1,3,5,7,14 day after the treatment respectively, its result of the test is in table one.
Table one embodiment and comparative example are to the control efficiency (%) of lady's-grass
Can find out according to data in table, this paraquat oil-suspending agent first reaches Kirchhoff integral with contrast and compares with green track, is better than comparison example to the preventive effect of lady's-grass.
Raw embodiment paraquat oil-suspending agent of surveying is tested the herbicidal effect of eleusine indica
According to test requirements document, after the eleusine indica with the chemicals treatment growth animated period of embodiment and comparative example, the strain preventive effect investigating each process for 1,3,5,7,14 day after the treatment respectively, its result of the test is in table two.
Table two embodiment and comparative example are to the control efficiency (%) of eleusine indica
Can find out according to data in table, each embodiment of paraquat oil-suspending agent is compared with green track with comparative example's Kirchhoff integral, and quick-acting and lasting effect all show more excellent, and gap is obvious, can reach and effectively control eleusine indica and prevent and kill off.
Raw embodiment paraquat oil-suspending agent of surveying is tested the herbicidal effect of the rhizome of nutgrass flatsedge
According to test requirements document, after the rhizome of nutgrass flatsedge with the chemicals treatment growth animated period of embodiment and comparative example, the strain preventive effect investigating each process for 1,3,5,7,14 day after the treatment respectively, its result of the test is in table three.
Table three embodiment and comparative example are to the control efficiency (%) of the rhizome of nutgrass flatsedge
Can find out according to data in table, each embodiment of paraquat oil-suspending agent is compared with comparative example's Kirchhoff integral, and to the overall preventive effect of the rhizome of nutgrass flatsedge all 80% ~ 90%, drug effect difference is not remarkable; The each embodiment of paraquat oil-suspending agent is compared with the green track of comparative example, and drug effect is significantly better than the green track of comparative example.
Raw herbicidal effect test of surveying embodiment 4 pairs of green foxtail
According to test requirements document, after the green foxtail with the chemicals treatment growth animated period of embodiment and comparative example, the strain preventive effect investigating each process for 1,3,5,7,14 day after the treatment respectively, its result of the test is in table four.
Table four embodiment and comparative example are to the control efficiency (%) of green foxtail
Can find out according to data in table, each embodiment of paraquat oil-suspending agent is compared with green track with comparative example's Kirchhoff integral, to the overall preventive effect of green foxtail all more than 90%, no matter is in quick-acting and is obviously better than Kirchhoff integral and green track product the lasting period.
Raw embodiment of surveying is tested the herbicidal effect of Horseweed Herb
According to test requirements document, after the Horseweed Herb with the chemicals treatment growth animated period of 20% paraquat oil-suspending agent embodiment and comparative example, the strain preventive effect investigating each process for 1,3,5,7,14 day after the treatment respectively, its result of the test is in table five.
Table five embodiment and comparative example are to the control efficiency (%) of Horseweed Herb
Can find out according to data in table, each embodiment of paraquat oil-suspending agent is compared with comparative example's Kirchhoff integral, and to the overall preventive effect of Horseweed Herb about 85% ~ 90%, drug effect difference is not remarkable; The each embodiment of paraquat oil-suspending agent is compared with the green track of comparative example, and in quick-acting and in whole Weed control effect, drug effect is all significantly better than the green track of comparative example.
Raw survey embodiment
According to the requirement of Ministry of Agriculture's agricultural chemicals field efficacy criterion, 14 days visually technique of estimation after dispenser, investigate the general control effect of each process to more than field all weeds, investigation result is in table six.
14 days each embodiment process community Weed-control effect hierarchical table after table six medicine
| Process numbering | Embodiment 1 | Embodiment 2 | Embodiment 3 | Kirchhoff integral | Green track | Blank |
| Preventive effect rank | 1 | 1 | 1 | 1 | 2 | 9 |
By recording and can find out in table, paraquat oil-suspending agent product is compared with common paraquat aqua (Kirchhoff integral, green track) product, no matter be in quick-acting or the length in the lasting period, more excellent to the preventive effect of most weeds, be obviously better than conventional aqua product.It is a large amount of with the better vegetable oil of plant compatibility and surfactant that reason is that oil-suspending agent product with the addition of, 1, improve the affinity of liquid and plant surface, and suction speed in promoting, shows better quick-acting.2, improve weed killer herbicide in the wetting of plant leaf blade surface and expansion, plant surface is fully contacted with liquid, improves drug effect.3, improve weed killer herbicide liquid in the attachment of plant leaf blade, extend its lasting period, and resistance of rainwater washing against, especially in rainy season, show the preventive effect more outstanding than conventional aqua product.
The above; it is only preferred embodiment of the present invention; it is not restriction the present invention being made to other form; the Equivalent embodiments that any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as equivalent variations is applied to other field; but everyly do not depart from technical solution of the present invention content; according to any simple modification, equivalent variations and remodeling that technical spirit of the present invention is done above embodiment, still belong to the protection domain of technical solution of the present invention.
Claims (6)
1. a paraquat oil-suspending agent, is characterized in that, this paraquat oil-suspending agent comprises following composition by weight:
Paraquat 10 parts ~ 50 parts;
Dispersant 0.1 part ~ 10 parts;
Emulsifier 5 parts ~ 25 parts;
Thickener 0.1 part ~ 10 parts;
Filler vegetable oil 50 parts ~ 80 parts.
2. according to the paraquat oil-suspending agent described in right 1, it is characterized in that, described dispersant is at least one material in polycarboxylic acid salt, agriculture breast 602#, 33#, polycarboxylic acid salt, lignosulfonates, naphthalenesulfonate formaldehyde condensation compound, alkylphenol polyoxyethylene, in polyether phosphate class, Pluronic PE 6800.
3. according to the paraquat oil-suspending agent described in right 1, it is characterized in that, described emulsifier is at least one material in alkyl benzene calcium sulfonate, agriculture breast 602#, 33#, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene formaldehyde condensation products.
4. according to the paraquat oil-suspending agent described in right 1, it is characterized in that, described thickener is at least one material in organobentonite, aluminium-magnesium silicate, white carbon, urea, ammonium sulfate.
5. according to the paraquat oil-suspending agent described in right 1, it is characterized in that, described filler vegetable oil is: at least one material in soybean oil, epoxidized soybean oil, methyl oleate, turpentine-based vegetable oil, peanut oil, palm oil, corn oil, cottonseed oil, esterification soybean oil, esterification cottonseed oil.
6. prepare a preparation method for the paraquat oil-suspending agent described in any one of the claims 1 ~ 5, it is characterized in that, comprise the following steps:
A, mixing: dispersant, emulsifier, thickener and filler vegetable oil are mixed, obtains compound;
B, shearing: paraquat, fluoroglycofen-ethyl dropped in compound, mixes simultaneously, shear evenly;
C, sand milling: paraquat will be mixed with, fluoroglycofen-ethyl compound grinds to form particle;
D, filtration: by the compound net filtration after filtration after grinding;
E, detection: sampling detects the parameters such as active constituent content.
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| WO2018228552A1 (en) * | 2017-06-16 | 2018-12-20 | 浙江新农化工股份有限公司 | Composition comprising zinc thiazole particles and preparation method therefor |
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