CN104872133A - Paraquat-fluoroglycofen ethyl water-soluble granule and preparation method thereof - Google Patents

Paraquat-fluoroglycofen ethyl water-soluble granule and preparation method thereof Download PDF

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Publication number
CN104872133A
CN104872133A CN201510142172.7A CN201510142172A CN104872133A CN 104872133 A CN104872133 A CN 104872133A CN 201510142172 A CN201510142172 A CN 201510142172A CN 104872133 A CN104872133 A CN 104872133A
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China
Prior art keywords
paraquat
fluoroglycofen
parts
ethyl
soluble granula
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CN201510142172.7A
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Chinese (zh)
Inventor
丁绍武
张鹏
邢超峰
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Jinan Tian Bang Chemical Co Ltd
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Jinan Tian Bang Chemical Co Ltd
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Priority to CN201510142172.7A priority Critical patent/CN104872133A/en
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Abstract

The present invention belongs to the field of pesticide formulations and relates to a herbicide, especially a paraquat-fluoroglycofen ethyl water-soluble granule and a preparation method thereof. The paraquat-fluoroglycofen ethyl water-soluble granule comprises the following components in weight part: 5-80 parts of paraquat, 0.1-20 parts of fluoroglycofen ethyl, 0.5-15 parts of dispersant, 0.1-10 parts of wetting agent, 0.1-20 parts of disintegrating agent and 1-60 parts of fillings. Compared with the prior art, based on the characteristics of paraquat and fluoroglycofen ethyl, the paraquat and the fluoroglycofen ethyl are perfectly combined together. In this way, the paraquat-fluoroglycofen ethyl water-soluble granule is faster in weeding speed and wider in herbicide controlling spectrum compared with the paraquat aqueous solution. Meanwhile, the paraquat-fluoroglycofen ethyl water-soluble granule is in the form of a granule, so that people cannot easily swallow the paraquat-fluoroglycofen ethyl water-soluble granule. Therefore, the casualties caused by the swallowing of the paraquat-fluoroglycofen ethyl water-soluble granule in a sudden impulse can be reduced.

Description

Paraquat * fluoroglycofen-ethyl soluble granula and preparation method thereof
Technical field
The invention belongs to pesticidal chemical field, relate to weed killer herbicide, particularly relate to a kind of paraquat * fluoroglycofen-ethyl soluble granula 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 97%, 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.
Paraquat preparation is mainly aqua product in the market, because paraquat aqua is after people wrongly takes, without special efficacy antidote, lethality rate reaches 90%, country, for this situation, from 1 day July in 2014, cancels the registration of paraquat aqua and production permit, stop producing, stop aqua selling at home and use on July 1st, 2016.But; 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.Therefore this researches and develops a kind of paraquat novel form with regard to an urgent demand pesticide industry.
In order to reduce the intoxication accident caused because of paraquat toxicity, paraquat is made to continue to serve agricultural production, countries in the world conduct in-depth research paraquat, be wrongly take the toxicity problem caused to propose solution for people, proposing by changing paraquat aqua general at present in patent application CN00813298.4 and CN99119405.5 and US5635445 is that the mode of paraquat solid or semisolid dosage form improves paraquat safety, but, although this solid of present production or semisolid dosage form can solve the problem of accidental poisoning, but it endangers surrounding environment and water source with rear packing material dead space capacity, and interior herbicide limited efficiency, the herbicide effect of traditional paraquat aqua cannot be reached.
Summary of the invention
The present invention is directed to the technical problems such as the insecticidal effect of the solid of above-mentioned paraquat or semisolid dosage form is limited, propose a kind of formula rationally, low toxicity, environmentally friendly, and packaging, storing and paraquat * fluoroglycofen-ethyl soluble granula easy to use.
In order to achieve the above object, the technical solution used in the present invention is, the invention provides a kind of paraquat * fluoroglycofen-ethyl soluble granula, this paraquat * fluoroglycofen-ethyl soluble granula comprises following composition by weight:
Paraquat 5 parts ~ 80 parts;
Fluoroglycofen-ethyl 0.1 part ~ 20 parts;
Dispersant 0.5 part ~ 15 parts;
Wetting agent 0.1 part ~ 10 parts;
Disintegrant 0.1 part ~ 20 parts;
Filler 1 part ~ 60 parts.
At above-mentioned paraquat * fluoroglycofen-ethyl soluble granula, also comprise synergist, adhesive, described synergist is 0.1 part ~ 30 parts at this paraquat * fluoroglycofen-ethyl soluble granula parts by weight; Described adhesive is 0.1 ~ 20 part at this paraquat * fluoroglycofen-ethyl soluble granula parts by weight.
At above-mentioned paraquat * fluoroglycofen-ethyl soluble granula, described dispersant is at least one material in polycarboxylate, di-2-ethylhexylphosphine oxide methyl naphthalene sulfonic acid salt, acrylate copolymer, di-2-ethylhexylphosphine oxide naphthalene sulfonate, lignosulfonates, naphthalenesulfonate formaldehyde condensation compound, Pluronic PE 6800, and preferred dispersant is the combination of dispersing agent MF and Pluronic PE 6800 or the combination of naphthalenesulfonate formaldehyde condensation compound and sodium lignin sulfonate or this kind of material of dispersing agent MF.
At above-mentioned paraquat * fluoroglycofen-ethyl soluble granula, described wetting agent is at least one material in Nekal BX, ethoxylated dodecyl alcohol sodium sulphate, polyoxyethylene nonylphenol ether, lauryl sodium sulfate, neopelex, nekal, succinic acid dibutyl ester sodium sulfonate, fatty alcohol-polyoxyethylene ether, and preferred wetting agent is neopelex or lauryl sodium sulfate.
At above-mentioned paraquat * fluoroglycofen-ethyl soluble granula, described disintegrant is at least two kinds of materials in urea, white sugar, gluconic acid sodium salt, sodium carboxymethylcellulose, ammonium sulfate, ammonium chloride, anhydrous sodium sulfate, layer silicon, bentonite, polyethyl acrylate, and preferred disintegrant is white sugar or glucose or gluconic acid sodium salt.
At above-mentioned paraquat * fluoroglycofen-ethyl soluble granula, described synergist is at least one material in alkyl glycoside, fatty alcohol-polyoxyethylene ether (sulphate), organic silicone, Tea Saponin, polyoxyethylene nonylphenol ether, quaternary ammonium salt, humate, and preferred synergist is alkyl glycoside or Tea Saponin.
At above-mentioned paraquat * fluoroglycofen-ethyl soluble granula, described adhesive is at least one material in starch and derivative thereof, dextrin, polyvinyl alcohol, sodium carboxymethylcellulose, hydroxypropyl cellulose, polyethylene glycol, pyrrolidones, gum Arabic, and preferred adhesive is cyclodextrin or sodium carboxymethylcellulose.
At above-mentioned paraquat * fluoroglycofen-ethyl soluble granula, described filler is at least one material in glucose, lactose, sucrose, sodium sulphate, ammonium sulfate, ammonium chloride, urea, fine particle calcium carbonate, talcum powder, white carbon, and preferred filler is ammonium sulfate or sodium sulphate.
Present invention also offers the preparation method of above-mentioned paraquat * fluoroglycofen-ethyl soluble granula, comprise the following steps:
A, mixing: by paraquat, fluoroglycofen-ethyl, dispersant, wetting agent, disintegrant,
Fillers etc. mix and obtain mixture;
B, pulverizing: by mixture through air-flow or ultramicro grinding, obtain female powder;
C, granulation: adhesive and female powder are fully mixed by mixer, passes through granulation
Machine granulating and forming;
D, oven dry: the particle obtained is dried.
E, screening: the particle of oven dry is screened according to grain graininess size.
As preferably, described granulation step comprises disc granulation, extruder grain, fluidized granulating, fluidized bed prilling, mist projection granulating or mixed at high speed granulation.
Compared with prior art, advantage of the present invention and good effect are,
1, the present invention is according to the characteristic of paraquat and fluoroglycofen-ethyl, paraquat and fluoroglycofen-ethyl are perfectly combined, make preparation of the present invention faster than paraquat aqua single dose weeding speed, broad weed-killing spectrum, this preparation is granule simultaneously, people not easily swallows, and decreases because the injures and deaths that medicine causes are drunk in impulsion.
2, preparation storage-stable of the present invention is good, can preserve more than 2 years.When preparation of the present invention uses simultaneously, without dead space capacity in packing material, the packing material of residual medicament is avoided to cause environmental pollution.
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 flow process chart 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.
Experimental technique described in following embodiment, if no special instructions, is conventional method; Described reagent and material, if no special instructions, all can obtain from commercial channels; " part " representative " parts by weight " in following embodiment.
Embodiment 1: the formula present embodiments providing one group of concrete paraquat * fluoroglycofen-ethyl soluble granula, in the present embodiment, former medicine and auxiliary agent are selected and proportioning is:
The former medicine of 95% paraquat 5.26 parts;
The former medicine of 96% fluoroglycofen-ethyl 1.04 parts;
Dispersant is dispersing agent MF 3.0 parts, Pluronic PE 6800 2.0 parts;
Wetting agent neopelex 2.5 parts;
Synergist is alkyl glycoside 5 parts;
Disintegrant is white sugar 20 parts;
Adhesive is cyclodextrin 3.0 parts;
Filler is that ammonium sulfate complements to 100 parts.
Calculate each amounts of components respectively by above proportioning, weigh, mix, paraquat, fluoroglycofen-ethyl, dispersant, wetting agent, disintegrant, filler etc. are mixed and obtains mixture.
By the mixture of above-mentioned steps through air-flow/ultramicro grinding, to particle diameter D90≤10 μm, obtain female powder.
The aqueous solution of adhesive and synergist and female powder are fully mixed by mixer; shaping by granulator granulation; the mode of granulating and forming has a variety of; in the present embodiment, disc granulation, extruder grain, fluidized granulating, fluidized bed prilling, mist projection granulating and mixed at high speed granulation is mainly comprised.
Dry, bake out temperature 82 DEG C ~ 85 DEG C, dries 30 ~ 35 minutes, and it is qualified for detecting moisture≤1.0 part.
Sieve selected.To dry after produce particle size sieve, selected, Control granularity 0.2mm≤d≤0.3mm.
Detected by the particle mixed, whether the main indices detecting effervescent is qualified, comprises the indexs such as former medicine content, wetability are qualified, disintegrative, foaming characteristic, moisture, expulsion rate, pH, suspensibility.Concrete grammar is as follows:
Liquid chromatograph (Japanese Shimadzu Corporation, L-20A) is used to detect the content of active ingredient paraquat and fluoroglycofen-ethyl.
Take 1.0 grams of samples and pour the band plug graduated cylinder that 250 milliliters of standard hard water are housed into, the time that record product all departs from liquid level is wetability; Repeatedly put upside down graduated cylinder back and forth, the number of times (or time) of the whole disintegration dispersion of record sample is disintegrative; After putting upside down graduated cylinder 30 times back and forth, leave standstill 30 seconds recording foam volume is afterwards the foaming characteristic of product; Leave standstill after 30 minutes, the dried and clean culture dish of graduated cylinder upper strata 90% bulk solution to the W1 that weighs is removed with vavuum pump, and move to culture dish 3 times with a small amount of standard hard water flushing graduated cylinder, dry to constant weight W2 for 80 DEG C, calculate suspensibility %=(1-(W2-W1)) × 10/9 × 100%.
Take 1.0 grams of samples and pour the band plug graduated cylinder that 100 milliliters of standard hard water are housed into, put upside down 30 times back and forth, measure pH scope with pH meter;
Take the soluble granula sample of certain mass M1, put into the standard screen (420 μm, aperture) filling 2 steel balls (Φ 30 ± 2) or porcelain ball, sieve is placed on chassis and adds a cover, to move in vibrating machine fixing after to vibrate 15min, accurately take and meet sample mass M2 (being accurate to 0.1g) in dish, expulsion rate %=M2/M1 × 100 of sample.
The sample taking certain mass packs, and places 14 days, carries out active ingredient index evaluation for 54 DEG C, calculates active ingredient heat storage resolution ratio.
Paraquat * fluoroglycofen-ethyl soluble granula performance indications prepared by embodiment 1 are: paraquat content 5.02%, fluoroglycofen-ethyl 1.0%, wetability qualified (10s), disintegration (30s), foaming characteristic qualified (15 milliliters), moisture 1.0%, expulsion rate 0.6%, pH value 5.4, suspensibility 97%, screen analysis 99%, heat storage stability is qualified, active ingredient resolution ratio 0.3%.
Embodiment 2: the formula present embodiments providing one group of 86% paraquat * fluoroglycofen-ethyl soluble granula (80 parts+6 parts), in the present embodiment, former medicine and auxiliary agent are selected and proportioning is:
The former medicine of 95% paraquat 84.2 parts
96 parts of former medicines of fluoroglycofen-ethyl 6.25 parts
Dispersant is naphthalenesulfonate formaldehyde condensation compound 2.5 parts, sodium lignin sulfonate 2.0 parts,
Wetting agent lauryl sodium sulfate 1.0 parts,
Disintegrant is glucose 2.5 parts,
Filler sodium sulphate complements to 100 parts.
Calculate each amounts of components respectively by above proportioning, weigh, mix; Formulation material is through ultra micro/air-flow crushing, granulation, oven dry, selected.Product checking is carried out according to soluble granula quality control index, index includes effective component content, disintegration time limited, suspensibility, foaming characteristic, screen analysis, powder and fragment rate, pH scope and heat storage stability etc. (in the present embodiment, utilize water to be cohered by mixture, therefore save adhesive in the present embodiment).Its detection method concrete grammar is as follows:
Liquid chromatograph (Japanese Shimadzu Corporation, L ~ 20A) is used to detect active ingredient paraquat and fluoroglycofen ether content.
Take 1.0 grams of samples and pour the band plug graduated cylinder that 250 milliliters of standard hard water are housed into; After putting upside down graduated cylinder 30 times back and forth, leave standstill 30 seconds recording foam volume is afterwards the foaming characteristic of product; Leave standstill after 30 minutes, the dried and clean culture dish of graduated cylinder upper strata 90% bulk solution to the W1 that weighs is removed with vavuum pump, and move to culture dish 3 times with a small amount of standard hard water flushing graduated cylinder, dry to constant weight W2 for 80 DEG C, calculate suspensibility %=(1 ~ (W2 ~ W1)) × 10/9 × 100%.
Take 1.0 grams of samples and pour the band plug graduated cylinder that 100 milliliters of standard hard water are housed into, put upside down 30 times back and forth, measure pH scope with pH meter;
Get a slice sample and put into the culture dish (Φ 100mm) filling water, start stopwatch, measure disintegration time limited;
Take the soluble granula sample of certain mass Q1, collect whole powder and fragment (be no more than granule quality, be considered as powder) and accurately claim to obtain quality Q 2 (being accurate to 0.01 gram), chip index %=Q2/Q1 × 100% of sample
The sample taking certain mass packs, and places 14 days, carries out active ingredient index evaluation for 54 DEG C, calculates active ingredient heat storage resolution ratio.
The each performance indications of paraquat infusion prepared by embodiment 2: paraquat content 80.2%, fluoroglycofen ether content 5.8%, wetability qualified (21s), disintegration time limited qualified (35s), foaming characteristic qualified (25 milliliters), expulsion rate 0.6%, moisture 1.2%, pH value 6.0, suspensibility paraquat is 100%, fluoroglycofen-ethyl 96 parts, screen analysis 99%, heat storage stability is qualified, active ingredient resolution ratio 0.6%.
Embodiment 3: the formula present embodiments providing one group of 52% paraquat second carboxylic soluble granula (50%+2%), in the present embodiment, former medicine and auxiliary agent are selected and proportioning is:
The former medicine of 95% paraquat 52.63 parts;
96 parts of former medicines of fluoroglycofen-ethyl 2.10 parts;
Dispersant is dispersing agent MF 5.0 parts;
Wetting agent is neopelex 3.0 parts;
Disintegrant is gluconic acid sodium salt 20 parts;
Synergist is Tea Saponin 5 parts;
Adhesive is sodium carboxymethylcellulose 3.0 parts;
Filler is that ammonium sulfate supplies 100 parts.
Concrete preparation process and experiment testing process consistent with embodiment 1, embodiment 2.
The assay method of each performance indications of paraquat * fluoroglycofen-ethyl soluble granula prepared by embodiment 3 is with embodiment 1.Concrete measurement result is: paraquat content 49.80%, fluoroglycofen-ethyl 2.0%, wetability qualified (30 seconds), disintegration qualified (48 seconds), foaming characteristic qualified (24 milliliters), moisture 1.0%, expulsion rate 0.2%, pH value 6.5, suspensibility paraquat 100%, second carboxylic 96%, screen analysis 99%, heat storage stability is qualified, active ingredient resolution ratio 0.6%.
Three embodiment experimental result contrasts
Embodiment 1 Embodiment 2 Embodiment 3
Paraquat content 5.02% 80.2% 49.8%
Fluoroglycofen-ethyl 1.0% 5.8% 2.0%
Wetability Qualified (10s) Qualified (21s) Qualified (30s)
Disintegration 30s 35s 48s
Foaming characteristic Qualified (15ml) Qualified (25ml) Qualified (24ml)
Moisture 1.0% 1.2% 1.0%
Expulsion rate 0.6% 0.6% 0.2%
PH value 5.4 6.0 6.5
Suspensibility 97% 100% 100%
Screen analysis 99% 99% 99%
Heat storage stability Qualified Qualified Qualified
Active ingredient resolution ratio 0.3% 0.6% 0.6%
The test of pesticide effectiveness:
Compare to carry out drug effect with paraquat second carboxylic soluble granula 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, especially paraquat produced to the weeds of obvious resistance, mainly contained 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 of blank district careless number ~ treatment region alive, 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 second carboxylic soluble granula 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 second carboxylic soluble granula 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 second carboxylic soluble granula 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 second carboxylic soluble granula 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 second carboxylic soluble granula 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 second carboxylic soluble granula 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 second carboxylic soluble granula 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 second carboxylic soluble granula 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 paraquat second carboxylic soluble granula 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 second carboxylic soluble granula 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 second carboxylic soluble granula 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 second carboxylic soluble granula 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, the preventive effect of antagonism weeds, is obviously better 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 (10)

1. a paraquat * fluoroglycofen-ethyl soluble granula, is characterized in that, this paraquat * fluoroglycofen-ethyl soluble granula comprises following composition by weight:
Paraquat 5 parts ~ 80 parts;
Fluoroglycofen-ethyl 0.1 part ~ 20 parts;
Dispersant 0.5 part ~ 15 parts;
Wetting agent 0.1 part ~ 10 parts;
Disintegrant 0.1 part ~ 20 parts;
Filler 1 part ~ 60 parts.
2. paraquat * fluoroglycofen-ethyl soluble granula according to claim 1, is characterized in that, also comprise synergist, adhesive, and described synergist is 0.1 part ~ 30 parts at this paraquat * fluoroglycofen-ethyl soluble granula parts by weight; Described adhesive is 0.1 ~ 20 part at this paraquat * fluoroglycofen-ethyl soluble granula parts by weight.
3. paraquat * fluoroglycofen-ethyl soluble granula according to claim 1, is characterized in that: described dispersant is at least one material in polycarboxylate, di-2-ethylhexylphosphine oxide methyl naphthalene sulfonic acid salt, acrylate copolymer, di-2-ethylhexylphosphine oxide naphthalene sulfonate, lignosulfonates, naphthalenesulfonate formaldehyde condensation compound, Pluronic PE 6800.
4. paraquat * fluoroglycofen-ethyl soluble granula according to claim 1, is characterized in that: described wetting agent is at least one material in Nekal BX, ethoxylated dodecyl alcohol sodium sulphate, polyoxyethylene nonylphenol ether, lauryl sodium sulfate, neopelex, nekal, succinic acid dibutyl ester sodium sulfonate, fatty alcohol-polyoxyethylene ether.
5. paraquat * fluoroglycofen-ethyl soluble granula according to claim 1, is characterized in that: described disintegrant is at least two kinds of materials in urea, white sugar, gluconic acid sodium salt, sodium carboxymethylcellulose, ammonium sulfate, ammonium chloride, anhydrous sodium sulfate, layer silicon, bentonite, polyethyl acrylate.
6. paraquat * fluoroglycofen-ethyl soluble granula according to claim 2, is characterized in that: described synergist is at least one material in alkyl glycoside, fatty alcohol-polyoxyethylene ether (sulphate), organic silicone, Tea Saponin, polyoxyethylene nonylphenol ether, quaternary ammonium salt, humate.
7. paraquat * fluoroglycofen-ethyl soluble granula according to claim 2, is characterized in that: described adhesive is at least one material in starch and derivative thereof, dextrin, polyvinyl alcohol, sodium carboxymethylcellulose, hydroxypropyl cellulose, polyethylene glycol, pyrrolidones, gum Arabic.
8. paraquat * fluoroglycofen-ethyl soluble granula according to claim 1, is characterized in that: described filler is at least one material in glucose, lactose, sucrose, sodium sulphate, ammonium sulfate, ammonium chloride, urea, fine particle calcium carbonate, talcum powder, white carbon.
9. prepare a preparation method for the paraquat * fluoroglycofen-ethyl soluble granula described in any one of the claims 1 ~ 8, it is characterized in that, comprise the following steps:
A, mixing: paraquat, fluoroglycofen-ethyl, dispersant, wetting agent, disintegrant, filler etc. are mixed and obtains mixture;
B, pulverizing: by mixture through air-flow or ultramicro grinding, obtain female powder;
C, granulation: adhesive and female powder are fully mixed by mixer, shaping by granulator granulation;
D, oven dry: the particle obtained is dried;
E, screening: the particle of oven dry is screened according to granule size.
10. the preparation method of paraquat * fluoroglycofen-ethyl soluble granula according to claim 9; it is characterized in that; it is characterized in that, described granulation step comprises disc granulation, extruder grain, fluidized granulating, fluidized bed prilling, mist projection granulating or mixed at high speed granulation.
CN201510142172.7A 2015-03-28 2015-03-28 Paraquat-fluoroglycofen ethyl water-soluble granule and preparation method thereof Pending CN104872133A (en)

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