CN104886060A - Paraquat - B fluoroglycofen effervescent granules and preparation method - Google Patents
Paraquat - B fluoroglycofen effervescent granules and preparation method Download PDFInfo
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Abstract
The invention discloses paraquat - B fluoroglycofen effervescent granules. The paraquat - B fluoroglycofen effervescent granules comprises the following components in parts by weight: 5 to 80 parts of paraquat, 0.1 to 50 parts of B fluoroglycofen, 0.1 to 15 parts of a dispersant, 0.1 to 10 parts of a wetting agent, 1 to 50 parts of a disintegration agent, 1 to 50 parts of a packing material, and 0.01 to 10 parts of a bonding agent. The present invention further discloses a preparation method of the paraquat - B fluoroglycofen effervescent granules, comprising: weighing out and mixing the components; grinding the mixture into powder by using a supermicro/airflow grinder; and performing granulation, drying, fine selection, mixing of acid and alkali granules, testing and packaging. The paraquat - B fluoroglycofen effervescent granules in the present invention have a better herbicidal effect than a same dose of solo paraquat, is not likely to be swallowed by human beings, and is stable during storage. Discarded packages do not contain residual chemical liquid, not polluting the environment.
Description
Technical field
The invention belongs to agriculture chemical compounding and formulation field, relate to a kind of effervescent and preparation method of paraquat fluoroglycofen-ethyl in particular.
Background technology
Paraquat, chemical name is 1-1-dimethyl-4-4-bipyridine cation salt, is a kind of steriland herbicide fast, has action of contace poison and certain systemic action.Can be absorbed by plant green tissues rapidly, make it withered.To the not effect of non-green tissue.Be combined and passivation with soil rapidly in soil, to plant root and perennial subterranean stem and perennial root invalid.
Paraquat structural formula:
Paraquat molecular formula: C12H14Cl2N2;
Paraquat english common name: Uniconazole;
Paraquat CAS accession number: 1910-42-5;
Paraquat chemical name: 1-1-dimethyl-4-4-bipyridine cation salt.
Paraquat 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.Fluoroglycofen-ethyl, belong to diphenyl ether herbicide, being protoporphyrin oxidase inhibitor, is a kind of selective herbicide, can prevent and kill off wheat, barley, peanut, soybean and rice field broad leaved weed and grassy weed.
Fluoroglycofen-ethyl structural formula:
Fluoroglycofen-ethyl molecular formula: C16H9ClF3NO7;
Fluoroglycofen-ethyl english common name: Benzofluorfen;
Fluoroglycofen-ethyl CAS accession number: 77501-60-1;
Fluoroglycofen-ethyl chemical name: 5-(2-chloro-trifluoromethyl phenoxy)-2-nitrobenzoic acid carboxylic methyl esters;
Fluoroglycofen-ethyl physicochemical property: amber solid, fusing point 65 DEG C; 25 DEG C of solvability <1mg/L in water, are soluble in most of organic solvent.
Because the pesticide resistance of plant in recent years increases, single paraquat component weeding raw effect of going out weakens to some extent, and this just needs to add other medicament, expands herbicide spectrum, common weeding, especially reaches high going out for some resistant weed and to come into force fruit.Existing paraquat product major product formulation is aqua simultaneously, easily takes, takes medicine once wrongly take or get excited, without special efficacy antidote, the rate of being poisoned to death can reach more than 90%, at present according to relevant policy of government, from 1 day July in 2014, cancel the registration of paraquat aqua and production permit, stop producing.This researches and develops a kind of paraquat novel form with regard to our pesticide industry of an urgent demand, avoids people to swallow as much as possible, reduces the loss of national life, property, add new medicament simultaneously, and raising plant is gone out and comes into force really.China Patent No. CN101622991; title: the microemulsion weeding group of a kind of paraquat and fluoroglycofen-ethyl; the day for announcing: 2010-01-13; be exactly that one is efficiently gone out raw herbicidal composition; according to component disclosed in this patent, can be used for nonirrigated farmland weeding, particularly; particularly orchard, forest land, Sang Di, tea place, and before the sowing of the crop field such as corn, sugarcane, soybean, cotton, broadcast rear seedling before or the spraying of its middle and late growth stage or protectiveness directed spraying carry out management of weeds.But the product of this invention is Herbicidal microemulsion, containing solvent and carrier water, has not met the problem of present water aqua type drug safety difference, and this invents the open component proportion scope of described composition very greatly, and in certain proportioning, effect is not given prominence to.
Summary of the invention
For above-mentioned existing product herbicide weak effect, the uneasy congruent problem of water aqua type, the present invention proposes a kind of with paraquat and the former medicine compound drug of fluoroglycofen-ethyl two kinds and preparation method and for effervescent, person poultry safety's property is high, preparation method is efficient, environmentally friendly, and packaging, storing and easy to use
For achieving the above object, a kind of paraquat fluoroglycofen-ethyl effervescent, described paraquat fluoroglycofen-ethyl effervescent composition weight number is than as follows:
Preferably, described paraquat fluoroglycofen-ethyl effervescent composition weight number is than as follows:
Preferably, described dispersant is selected from least one 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.
Preferably, described wetting agent is selected from least one 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.
Preferably, described disintegrant is selected from two or more in urea, potash, calcium carbonate, sodium carbonate, sodium bicarbonate, citric acid, malonic acid, succinic acid, adipic acid, tartaric acid, maleic acid, fumaric acid, benzoic acid, amino acid, potassium dihydrogen phosphate, sorbic acid etc.
Preferably, described adhesive is selected from least one in lower starch and derivative thereof, dextrin, polyvinyl alcohol, sodium carboxymethylcellulose, hydroxypropyl cellulose, polyethylene glycol, pyrrolidones, gum Arabic.
Preferably, described filler is selected from least one in stearate, precipitated calcium carbonate, talcum powder, bentonite, atlapulgite, White Carbon black, glucose, lactose, sucrose, starch, diatomite, attapulgite, potter's clay, kaolin.
Present invention also offers a kind of preparation method of paraquat fluoroglycofen-ethyl effervescent, comprise the following steps:
1. take raw material according to each composition ratio of weight and number described in claim 1, mix;
2. pulverize through ultra micro/airslide disintegrating mill, to particle diameter D90≤10 μm, obtain female powder;
3. the adhesive aqueous solution and female powder are fully mixed by mixer, shaping by granulator granulation;
4. dry, bake out temperature 82 DEG C-85 DEG C, dry 30-35 minute, it is qualified for detecting moisture≤1.0%;
5. sieve selected, the sour grain produced in 4. and alkali grain sieved, selected, Control granularity 1mm≤d≤3mm;
6. sour grain, the mixing of alkali grain;
Whether the indices 7. detecting effervescent is qualified.
Preferably, step 3. described granulation comprise disc granulation, extruder grain, fluidized granulating, fluidized bed prilling, mist projection granulating and mixed at high speed granulation; Step 7. described indices comprises that former medicine content, wetability are qualified, disintegrative, foaming characteristic, moisture, expulsion rate, pH and suspensibility.
Compared to existing technology, the present invention has following beneficial effect:
1. preparation of the present invention is faster than paraquat aqua single dose weeding speed, and broad weed-killing spectrum, has good preventive effect to some paraquat resistance weeds.
2. preparation of the present invention, people not easily swallows, and decreases because the injures and deaths that medicine causes are drunk in impulsion;
3. preparation storage-stable of the present invention is good, can preserve more than 2 years;
4., when preparation of the present invention uses, without dead space capacity in discarded packing material, the packing material of residual medicament is avoided to cause environmental pollution.
Accompanying drawing explanation
Fig. 1 paraquat fluoroglycofen-ethyl effervescent preparation technology flow chart.
Embodiment
For a better understanding of the present invention, below in conjunction with embodiment, preferred explanation is done to the present invention, experimental technique described in following embodiment, if no special instructions, be customary preparation methods; Described reagent and material, if no special instructions, be market sale.
The sour grain mentioned in preparation method of the present invention and alkali grain, sour grain refers to the particle utilizing acidic materials to cause as disintegrant; Alkali grain refers to the particle utilizing alkaline matter to cause as disintegrant, for avoiding reacting in process of production, acid grain and alkali grain are separately produce in process of production, after treating that sour grain and alkali grain are dried respectively, mix, mixed effervescent is at dilution with water again, because acid-base reaction, mutually promote in water dispersion, dissolve, independent sour grain and alkali grain in water be difficult to disperses rapidly.
Embodiment 1
Raw material is taken: a, sour grain: paraquat 5 parts by following ratio of weight and number; Fluoroglycofen-ethyl 1 part; Dispersant is dispersing agent MF 3.0 parts, calcium lignosulfonate 2.0 parts; Wetting agent lauryl sodium sulfate 2.5 parts; Disintegrant is citric acid 20 parts; Binding agent is gum Arabic 3.0 parts; Filler is attapulgite 28.5 parts, 35 parts, potter's clay.B, alkali grain: paraquat 5 parts; Fluoroglycofen-ethyl 1 part; Dispersant is dispersing agent MF 3.0 parts, calcium lignosulfonate 2.0 parts; Wetting agent lauryl sodium sulfate 2.5 parts; Disintegrant is sodium bicarbonate 20 parts; Binding agent is gum Arabic 3.0 parts; Filler is attapulgite 28.5 parts, 35 parts, potter's clay.The raw material of acid grain and alkali grain mixes respectively; Through ultra micro/air-flow crushing, granulation, oven dry, screening is selected, soda acid grain mixes, detection.Carry out Product checking according to effervescent quality control index, index includes effective component content, wetting time, disintegration rate, suspensibility, foaming characteristic, screen analysis, expulsion rate, PH and heat storage stability etc.Concrete grammar is as follows:
Liquid chromatograph (Japanese Shimadzu Corporation, L-20A) is used to detect active constituent content.
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 effervescent 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.Experimental data is as following table:
Table 1
Embodiment 2
Raw material is taken: a, sour grain: paraquat 84.2 parts by following ratio of weight and number; Fluoroglycofen-ethyl 5.2 parts; Dispersant is naphthalenesulfonate formaldehyde condensation compound 2.5 parts, sodium methylene bis-naphthalene sulfonate 2.0 parts; Wetting agent is neopelex 1 part; Disintegrant is 5.5 parts, tartaric acid; Filler is glucose 4 parts.B, alkali grain: paraquat 80 parts; Fluoroglycofen-ethyl 5 parts; Dispersant is naphthalenesulfonate formaldehyde condensation compound 2.5 parts, sodium methylene bis-naphthalene sulfonate 2.0 parts; Wetting agent is neopelex 1 part; Disintegrant is 5.5 parts, sodium carbonate; Filler is glucose 4 parts.Respectively sour grain and alkali grain raw material are mixed; Through ultra micro/air-flow crushing become powder, granulation, drying, selected, detect, be packaged to be paraquat and fluoroglycofen-ethyl effervescent.Carry out Product checking according to effervescent quality control index, index includes effective component content, wetting time, disintegration rate, suspensibility, foaming characteristic, screen analysis, expulsion rate, PH scope and heat storage stability etc.Method of testing repeats no more with embodiment 1, and experimental data is as following table:
Table 2
Embodiment 3
Raw material is taken: a, sour grain: paraquat 52 parts by following ratio of weight and number; Fluoroglycofen-ethyl 8.5 parts; Dispersant is for being dispersing agent MF 5 parts; Wetting agent is succinic acid dibutyl ester sodium sulfonate 3 parts; Disintegrant is citric acid 18 parts; Adhesive is sodium carboxymethylcellulose 3 parts; Filler is kaolin 10.5 parts.B, alkali grain: paraquat 52 parts; Fluoroglycofen-ethyl 8.5 parts; Dispersant is for being dispersing agent MF 5 parts; Wetting agent is succinic acid dibutyl ester sodium sulfonate 3 parts; Disintegrant is 10 parts, sodium carbonate, sodium bicarbonate 8 parts; Adhesive is sodium carboxymethylcellulose 3 parts; Filler is kaolin 10.5 parts.Respectively sour grain and alkali grain raw material are mixed; Become powder, granulation, drying through ultra micro/air-flow crushing, selected, soda acid grain mixes, detect, be packaged to be paraquat and fluoroglycofen-ethyl effervescent.Carry out Product checking according to effervescent quality control index, index includes effective component content, wetting time, disintegration rate, suspensibility, foaming characteristic, screen analysis, expulsion rate, PH scope and heat storage stability etc.Method of testing repeats no more with embodiment 1, and experimental data is as following table:
Table 3
Embodiment 4
Raw material is taken: a, sour grain: paraquat 5.3 parts by following ratio of weight and number; Fluoroglycofen-ethyl 1 part; Dispersant is di-2-ethylhexylphosphine oxide naphthalene sulfonate 3 parts, acrylate copolymer 2 parts; Wetting agent is Nekal BX 2 parts; Disintegrant is 25 parts, tartaric acid; Filler is kaolin 61.6 parts.B, alkali grain: paraquat 5.3 parts; Fluoroglycofen-ethyl 1 part; Dispersant is di-2-ethylhexylphosphine oxide naphthalene sulfonate 3 parts, acrylate copolymer 2 parts; Wetting agent is Nekal BX 2 parts; Disintegrant is 25 parts, calcium carbonate; Filler is kaolin 61.6 parts.Respectively acid, alkali grain raw material are mixed; Become powder, granulation, drying through ultra micro/air-flow crushing, selected, soda acid grain mixes, detect, be packaged to be paraquat and fluoroglycofen-ethyl effervescent.Carry out Product checking according to effervescent quality control index, index includes effective component content, wetting time, disintegration rate, suspensibility, foaming characteristic, screen analysis, expulsion rate, PH scope and heat storage stability etc.Method of testing repeats no more with embodiment 1, and experimental data is as following table:
Table 4
Embodiment 5
Raw material is taken: a, sour grain: paraquat 63.2 parts by following ratio of weight and number; Fluoroglycofen-ethyl 5.2 parts; Dispersant is for being Pluronic PE 6800 2 parts, naphthalenesulfonate formaldehyde condensation compound 1 part; Wetting agent is 0.5 part, ethoxylated dodecyl alcohol sodium sulphate, dibutyl naphthalenesulfonic acid 1 part; Disintegrant is sorbic acid 2 parts; Adhesive is gum Arabic 0.2 part; Filler is glucose 24.9 parts.B, alkali grain: paraquat 63.2 parts; Fluoroglycofen-ethyl 5.2 parts; Dispersant is for being Pluronic PE 6800 2 parts, naphthalenesulfonate formaldehyde condensation compound 1 part; Wetting agent is 0.5 part, ethoxylated dodecyl alcohol sodium sulphate, dibutyl naphthalenesulfonic acid 1 part; Disintegrant is 2 parts, potash; Adhesive is gum Arabic 0.2 part; Filler is glucose 24.9 parts.Respectively the raw material of sour grain, alkali grain is mixed; Become powder, granulation, drying through ultra micro/air-flow crushing, selected, soda acid grain mixes, detect, be packaged to be paraquat and fluoroglycofen-ethyl effervescent.Carry out Product checking according to effervescent quality control index, index includes effective component content, wetting time, disintegration rate, suspensibility, foaming characteristic, screen analysis, expulsion rate, PH scope and heat storage stability etc.Method of testing repeats no more with embodiment 1, and experimental data is as following table:
Table 5
Embodiment 6
Raw material is taken: a, sour grain: paraquat 31.6 parts by following ratio of weight and number; Fluoroglycofen-ethyl 5.2 parts; Dispersant is naphthalenesulfonate formaldehyde condensation compound 2 parts, lignosulfonates 2.5 parts; Wetting agent is nekal 2 parts; Disintegrant is 4 parts, tartaric acid, 1 part, benzoic acid; Binding agent is 2 parts, dextrin, and filler is atlapulgite 49.7 parts.A, alkali grain: paraquat 31.6 parts; Fluoroglycofen-ethyl 5.2 parts; Dispersant is naphthalenesulfonate formaldehyde condensation compound 2 parts, lignosulfonates 2.5 parts; Wetting agent is nekal 2 parts; Disintegrant is sodium bicarbonate 5 parts; Binding agent is 2 parts, dextrin, and filler is atlapulgite 49.7 parts.Respectively the raw material of sour grain and alkali grain is mixed; Become powder, granulation, drying through ultra micro/air-flow crushing, selected, soda acid grain mixes, detect, be packaged to be paraquat and fluoroglycofen-ethyl effervescent.Carry out Product checking according to effervescent quality control index, index includes effective component content, wetting time, disintegration rate, suspensibility, foaming characteristic, screen analysis, expulsion rate, PH scope and heat storage stability etc.Method of testing repeats no more with embodiment 1, and experimental data is as following table:
Table 6
Embodiment 7
Raw material is taken: a, sour grain: paraquat 63.2 parts by following ratio of weight and number; Fluoroglycofen-ethyl 8.3 parts; Dispersant is polycarboxylate 6 parts, di-2-ethylhexylphosphine oxide naphthalene sulfonate 2 parts; Wetting agent is succinic acid dibutyl ester sodium sulfonate 3 parts; Disintegrant is 6 parts, tartaric acid, citric acid 3 parts; Adhesive is polyethylene glycol 1 part; Filler is sucrose 2.5 parts, 5 parts, diatomite.B, alkali grain: paraquat 63.2 parts; Fluoroglycofen-ethyl 8.3 parts; Dispersant is polycarboxylate 6 parts, di-2-ethylhexylphosphine oxide naphthalene sulfonate 2 parts; Wetting agent is succinic acid dibutyl ester sodium sulfonate 3 parts; Disintegrant is sodium bicarbonate 9 parts; Adhesive is polyethylene glycol 1 part; Filler is sucrose 2.5 parts, 5 parts, diatomite.Respectively the raw material of sour grain, alkali grain is mixed; Become powder, granulation, drying through ultra micro/air-flow crushing, selected, soda acid grain mixes, detect, be packaged to be paraquat and fluoroglycofen-ethyl effervescent.Carry out Product checking according to effervescent quality control index, index includes effective component content, wetting time, disintegration rate, suspensibility, foaming characteristic, screen analysis, expulsion rate, PH scope and heat storage stability etc.Method of testing repeats no more with embodiment 1, and experimental data is as following table:
Table 7
The test of pesticide effectiveness:
Compare to carry out drug effect with paraquat of the present invention and fluoroglycofen-ethyl effervescent, 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 45m
2, 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 point, often some 0.5m
2carry 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.The drug effect that result of the test calculates medicament is according to the following equation: 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, and adopt eye estimate investigation method, classification is investigated and recorded, and weed control efficacy grade scale is as following table:
Table 8
| Rank | Weeding situation describes |
| 1 grade | Without grass |
| 2 grades | Be equivalent to the 0-2.5% of blank district weeds |
| 3 grades | Be equivalent to the 2.5%-5% of blank district weeds |
| 4 grades | Be equivalent to the 5%-10% of blank district weeds |
| 5 grades | Be equivalent to the 10%-15% of blank district weeds |
| 6 grades | Be equivalent to the 15%-25% of blank district weeds |
| 7 grades | Be equivalent to the 25%-35% of blank district weeds |
| 8 grades | Be equivalent to the 35%-67.5% of blank district weeds |
| 9 grades | Be equivalent to the 67.5%-100% of blank district weeds |
Raw test tests 1, paraquat * fluoroglycofen-ethyl effervescent liquid is tested the herbicidal effect of lady's-grass, according to test requirements document, after 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 sees the following form 9 embodiments and comparative example to the control efficiency (%) of lady's-grass, can find out according to data in table, described paraquat first reaches Kirchhoff integral with second carboxylic effervescent with contrast and compares with green track, comparison example is better than to the preventive effect of lady's-grass
Table 9
Raw test tests 2, test paraquat and fluoroglycofen-ethyl effervescent are tested the herbicidal effect of eleusine indica: according to test requirements document, after eleusine indica with the chemicals treatment growth animated period of embodiment and comparative example, distinguish 1 after the treatment, 3, 5, 7, within 14 days, investigate the strain preventive effect of each process, its result of the test sees the following form 10 embodiments and comparative example to the control efficiency (%) of eleusine indica, can find out according to data in table, paraquat described in 5 is compared with green track with comparative example's Kirchhoff integral with each embodiment of second carboxylic effervescent, quick-acting and lasting effect all show more excellent, gap is obvious, can reach and eleusine indica effectively be controlled and prevents and kill off,
Table 10
Raw test tests 3, test grass is withered to be tested the herbicidal effect of the rhizome of nutgrass flatsedge with fluoroglycofen-ethyl effervescent, according to test requirements document, after the rhizome of nutgrass flatsedge with the chemicals treatment growth animated period of embodiment and comparative example, distinguish 1 after the treatment, 3, 5, 7, within 14 days, investigate the strain preventive effect of each process, its result of the test sees the following form 11 embodiments and comparative example to the control efficiency (%) of the rhizome of nutgrass flatsedge, can find out according to data, described paraquat and each embodiment of second carboxylic effervescent are compared with comparative example's Kirchhoff integral, to the overall preventive effect of the rhizome of nutgrass flatsedge all at 80%-90%, drug effect difference is not remarkable, described paraquat and each embodiment of second carboxylic effervescent compared with the green track of comparative example, drug effect significantly better than the green track of comparative example,
Table 11
Raw test tests 4, test paraquat and fluoroglycofen-ethyl effervescent are tested the herbicidal effect of green foxtail: according to test requirements document, after green foxtail with the chemicals treatment growth animated period of embodiment and comparative example, distinguish 1 after the treatment, 3, 5, 7, within 14 days, investigate the strain preventive effect of each process, its result of the test sees the following form 12 embodiments and comparative example to the control efficiency (%) of green foxtail, can find out according to data in table, described paraquat is compared with green track with comparative example's Kirchhoff integral with each embodiment of second carboxylic effervescent, to the overall preventive effect of green foxtail all more than 90%, no matter be in quick-acting and be obviously better than Kirchhoff integral and green track product the lasting period, table 12
Raw test tests 5, test paraquat and fluoroglycofen-ethyl effervescent are tested the herbicidal effect of Horseweed Herb, according to test requirements document, after growing the Horseweed Herb of animated period by the chemicals treatment of paraquat and second carboxylic effervescent embodiment and comparative example, distinguish 1 after the treatment, 3, 5, 7, within 14 days, investigate the strain preventive effect of each process, its result of the test sees the following form 13 embodiments and comparative example to the control efficiency (%) of Horseweed Herb, can find out according to data in table, described paraquat and each embodiment of second carboxylic effervescent are compared with comparative example's Kirchhoff integral, to the overall preventive effect of Horseweed Herb at about 85%-90%, drug effect difference is not remarkable, described paraquat and each embodiment of second carboxylic effervescent compared with the green track of comparative example, in quick-acting and in whole Weed control effect, drug effect all significantly better than the green track of comparative example,
Table 13
Raw test tests 6
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 sees the following form 14 days each embodiment process community Weed-control effect hierarchical table after 14 medicines, by recording and can find out in table, described paraquat and second carboxylic effervescent product and common paraquat aqua (Kirchhoff integral, green track) product compares, 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, obviously be better than conventional aqua product,
Table 14
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 (9)
1. paraquat fluoroglycofen-ethyl effervescent, is characterized in that, described composition weight number is than as follows:
2. paraquat fluoroglycofen-ethyl effervescent according to claim 1, is characterized in that, described paraquat fluoroglycofen-ethyl effervescent composition weight number is than as follows:
3. paraquat fluoroglycofen-ethyl effervescent according to claim 2, it is characterized in that, described dispersant is selected from least one 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 effervescent according to claim 2, it is characterized in that, described wetting agent is selected from least one 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 effervescent according to claim 2, it is characterized in that, described disintegrant be selected from urea, potash, calcium carbonate, sodium carbonate, sodium bicarbonate, citric acid, malonic acid, succinic acid, adipic acid, tartaric acid, maleic acid, fumaric acid, benzoic acid, amino acid, potassium dihydrogen phosphate, sorbic acid etc. two or more.
6. paraquat fluoroglycofen-ethyl effervescent according to claim 2, it is characterized in that, described adhesive is selected from least one in following material: starch and derivative, dextrin, polyvinyl alcohol, sodium carboxymethylcellulose, hydroxypropyl cellulose, polyethylene glycol, pyrrolidones, gum Arabic etc.
7. paraquat fluoroglycofen-ethyl effervescent according to claim 2, it is characterized in that, described filler is selected from least one in stearate, precipitated calcium carbonate, talcum powder, bentonite, atlapulgite, White Carbon black, glucose, lactose, sucrose, starch, diatomite, attapulgite, potter's clay, kaolin.
8. prepare a preparation method for the paraquat fluoroglycofen-ethyl effervescent described in any one of the claims 1 ~ 7, it is characterized in that, comprise the following steps:
1. take raw material according to each composition ratio of weight and number described in claim 1, mix;
2. pulverize through ultra micro/airslide disintegrating mill, to particle diameter D90≤10 μm, obtain female powder;
3. the adhesive aqueous solution and female powder are fully mixed, by Granulation Equipments granulating and forming by mixing;
4. dry, bake out temperature 82 DEG C-85 DEG C, dry 30-35 minute, it is qualified for detecting moisture≤1.0%;
5. sieve selected, the sour grain produced in 4. and alkali grain sieved, selected, control particle size 1mm≤d≤3mm;
6. sour grain, the mixing of alkali grain; Acid grain is the granule produced with acid disintegrant, and alkali grain is the granule that alkaline disintegrant is produced.Acid grain, alkali grain mixed proportion are: 1:25 ~ 25:1.
Whether the indices 7. detecting effervescent is qualified.
9. the preparation method of paraquat fluoroglycofen-ethyl effervescent according to claim 8, it is characterized in that, step 3. described granulation comprises disc granulation, extruder grain, fluidized granulating, fluidized bed prilling, mist projection granulating and mixed at high speed granulation; Step 7. described indices comprises that former medicine content, wetability are qualified, disintegrative, foaming characteristic, moisture, expulsion rate, pH and suspensibility.
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| CN106472511A (en) * | 2016-08-30 | 2017-03-08 | 枣阳市先飞高科农药有限公司 | A kind of synthesis technique of fluoroglycofen-ethyl active compound |
| WO2019227166A1 (en) * | 2018-05-31 | 2019-12-05 | Sumitomo Chemical Australia Pty Ltd | "herbicidal composition" |
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