CN101953336B - Metribuzin water dispersible granules and preparation method thereof - Google Patents
Metribuzin water dispersible granules and preparation method thereof Download PDFInfo
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- CN101953336B CN101953336B CN2010105190235A CN201010519023A CN101953336B CN 101953336 B CN101953336 B CN 101953336B CN 2010105190235 A CN2010105190235 A CN 2010105190235A CN 201010519023 A CN201010519023 A CN 201010519023A CN 101953336 B CN101953336 B CN 101953336B
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- piperazine humulone
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Abstract
The invention relates to metribuzin water dispersible granules and a preparation method thereof. The metribuzin water dispersible granules are regular or irregular granules, of which the formula comprises the following raw materials in percentage by weight: 50 to 80 percent of crude metribuzin, 2 to 10 percent of humectant, 2 to 10 percent of dispersing agent, 1 to 5 percent of stabilizing agent and 10 to 40 percent of stuffing. The preparation method for the metribuzin water dispersible granules comprises the following steps of: soaking raw medicinal materials in acid, washing, filtering and drying the raw medicinal materials, weighing the raw medicinal materials according to proportion, blending and roughly crushing the raw medicinal materials, blending and roughly crushing the raw medicinal materials again, sieving the raw medicinal materials to obtain fine powder, adding water into the fine powder, pelleting the fine powder and drying the granules to obtain the metribuzin water dispersible granules. The metribuzin water dispersible granules overcome the defects of the traditional metribuzin formulations, reduce the using cost of farmers and environmental pollution, have the advantages of high active material content, high suspension rate, low pollution, convenient storage and transportation, high stability, easy use, high disintegrating speed and good dispersibility and fluidity, and is applicable to prevention and control of amaranthus retroflexus, goosefoots and siberian cocklebur in alfalfa field.
Description
Technical field
The invention belongs to pesticide field, particularly a kind of piperazine humulone water dispersible granules and preparation method thereof.
Background technology
Pesticide water dispersible granules be the water-insoluble solid pesticide original medicine with wetting agent, dispersant, other function additive and filler after fully mixing; Be ground into trickle powdery solid, then through operations such as kneading, granulation, drying, sieve part formed in water rapidly disintegration be the primary granule size and the formulations of pesticide that are dispersed into stable suspension.The not only solvent-free and dust of water dispersible granules to operator's safety, and has reduced the pollution to environment.
Piperazine humulone (4-amino-6-tertiary butyl-4,5-dihydro-3-methyl mercapto-1,2; 4-triazine-5 (4H)-ketone MTB) is selective herbicide, and its effective ingredient is absorbed by the weeds root system and conducts to top with transpiration current; Also can be done limited conduction in vivo by the blade absorption, main through suppressing the photosynthesis performance removing activity of sensitive plant, each susceptible weeds sprouting is emerged unaffected after the dispenser; The rear blade chlorisis of emerging, last nutrition is exhausted and dead.The piperazine humulone is widely used as preventing and kill off before soybean, potato, tomato and other crop seedlings and the weed killer herbicide of weeds behind the seedling, can effectively prevent and treat potato fields Siberian cocklebur, lamb's-quarters, weeds such as green foxtail.
Siberian cocklebur is a composite family annual herb plant.Plant height 90cm.The leaf triangular shape is avette or heart-shaped, long 4～9cm, and wide 5～10cm, base go out three arteries and veins, and there is coarse volt hair on the two sides; Long 3～the 11cm of petiole.Male capitulum is spherical, and female capitulum is oval, internal layer phyllary structure cryptomere.The phyllary of ripe tool achene becomes hard, green, faint yellow or bronzing, and the involucre thorn of giving birth to the tool hook is dredged in the outside, the long 1～1.5mm of bud thorn, the long 1.5～2.5mm of beak.
Lamb's-quarters is a Chenopodiaceae annual herb plant.60～120 milliliters of plant heights.Stem is upright, branch.The leaf alternate, the avette or near triangle of water chestnut shape, tip point, the wide wedge shape of base portion, the irregular sawtooth of leaf margin tool; Leaf tool long handle.The flower both sexes, flowers gather into close or thin panicle, and give birth on the top or armpit is given birth to.Utricle is wrapped in the perianth or reveal slightly at the top.Seed grows wild, the biconvex shape, and black tool gloss, there is the shallow ridges line on the surface.Seminal propagation.
Green foxtail is also claimed " green bristlegrass ", " paddy green bristlegrass ".Grass family.Annual herb.Blade is wealthy linear, narrow lanceolar or wire lanceolar.The cylindric bristle of panicle is coarse, and is green or isabelline usually.Likeness in form dog tail, bloom summer; On the branch that small ear two to several pieces of clusters shorten.It is one of harm potato fields main weeds; It is close by the field to take place can to form dominant population when serious, and contention rich water power is strong, causes crop failure; Herba setariae viridis grass also is the host of many insects such as leafhopper, thrips, aphid, black cutworm, has a strong impact on the productive rate of crop.
At present, the formulation of piperazine humulone is mainly wetting powder on the market, does not see the patent report of piperazine humulone water dispersible granules as yet.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that overcomes prior art, and a kind of piperazine humulone water dispersible granules is provided.
The present invention also will provide a kind of preparation method of piperazine humulone piperazine humulone water dispersible granules simultaneously, and its cost is lower, and gained piperazine humulone water dispersible granules good drug efficacy.
For solving above technical problem, a kind of technical scheme that the present invention adopted is: a kind of piperazine humulone water dispersible granules, be rule or irregular graininess body, and its composition of raw materials is following:
The former medicine 50%～80% of piperazine humulone;
Wetting agent 2%～10%;
Dispersant 2%～10%;
Stabilizing agent 1%～5%;
Filler 10%～40%.
According to the present invention, said wetting agent, dispersant, stabilizing agent, filler all are conventional substances that use this area.Preferably, wetting agent is to be selected from lauryl sodium sulfate, lignin, naphthalene sulfonate, APES and the alkyl sulfonates one or more.Dispersant is a polycarboxylate.Stabilizing agent is to be selected from ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate and the tetrasodium ethylenediamine tetraacetate one or more.Filler is to be selected from kaolin, diatomite, bentonite, corn starch, precipitated calcium carbonate and the ammonium sulfate one or more.
Said piperazine humulone piperazine humulone water dispersible granules can adopt the water dispersible granules technology of preparing of the routine of this area to carry out.
Another technical scheme provided by the invention is: a kind of preparation method of piperazine humulone water dispersible granules, it comprises the steps:
(1), the watery hydrochloric acid washing by soaking of the former medicinal 1wt%-10wt% of piperazine humulone is stirred, treat piperazine humulone come-up after, filter oven dry;
(2), by prescription, with the former medicine of piperazine humulone after step (1) processing, wetting agent; Dispersant, stabilizing agent and filler fully mix, and pulverize through coarse crushing, mixing again, airslide disintegrating mill; Enter into cone-type mixer and mix, get fine powder through 325 mesh standard sieves, afterwards; In fine powder, add water and mediate, extruder grain promptly gets piperazine humulone water dispersible granules in 40 ℃～60 ℃ oven dry.
Preparation in accordance with the present invention, the concentration of the used watery hydrochloric acid of step (1) is preferably 4wt%-6wt%, most preferably 5wt%.
The inventor is surprised to find that; Use the particle water dispersible granule of the former medicine preparation of the piperazine humulone of handling through watery hydrochloric acid; Compare with the particle water dispersible granule of the former medicine preparation of piperazine humulone of using process watery hydrochloric acid processing; Its suspensibility and stability all increase significantly, and this possibly be because some metal ions and the alkaline impurities that remain in wherein that contain in the former medicine of piperazine humulone can cause adverse effect to water dispersible granules, and can effectively eliminate this influence through simple acid treatment.
Because adopt above technical scheme, the present invention compared with prior art has following advantage:
The invention provides a kind of piperazine humulone novel form, it is prone to, and packing is used, storing is convenient, do not have injury and environmentally safe to the people is healthy, and cost is lower, pollutes little.
The initial suspensibility of piperazine humulone water dispersible granules>=92% according to preparation method's gained of the present invention; 54 ± 2 heat storages suspensibility>=85% after 30 days; Disintegration time≤60s; Wetting time 60s; Lasting foaming characteristic (behind the 1min)≤20ml.
Embodiment
Embodiment 1
A kind of piperazine humulone water dispersible granules, in weight portion, its composition of raw materials consists of: 70 parts of the former medicines of piperazine humulone, 5 parts of wetting agent naphthalene sulfonates, 3 parts of dispersant polycarboxylate, 2 parts of stabilizing agent ethylenediamine tetra-acetic acids, 20 parts of filler corn starchs.The all commercially available acquisition of each raw material components.
Piperazine humulone water dispersible granules prepares through following method:
(1), get the commercially available former medicine of piperazine humulone, the watery hydrochloric acid washing by soaking with 5% stirs, and treats piperazine humulone come-up back filtering drying, and is for use.
(2), 70 parts of the former medicine of piperazine humulone of weighing watery hydrochloric acid after handling, 5 parts of wetting agent naphthalene sulfonates, 3 parts of dispersant polycarboxylate, 2 parts of stabilizing agent ethylenediamine tetra-acetic acids; 20 parts of filler corn starchs fully mix, and mixed material is pulverized through coarse crushing, mixing again, airslide disintegrating mill successively; Enter into cone-type mixer then and mix, cross 325 mesh standard sieves and get fine powder, afterwards; In fine powder, add water and mediate, extruder grain, 40 ℃～60 ℃ dry piperazine humulone water dispersible granules.
This piperazine humulone water dispersible granules technical indicator is following:
Suspensibility 95.2%; Disintegration time≤60s; Wetting time≤60s; Moisture≤2.5%; PH value 6.0～8.0; Wet screening test (through 75 μ m testing sieves)>=98%; Lasting foaming characteristic (behind the 1min)≤20ml; 54 ± 2 ℃ of heat are store suspensibility>=85% after 30 days.
Embodiment 2
A kind of piperazine humulone water dispersible granules, in weight portion, its composition of raw materials consists of: 75 parts of the former medicines of piperazine humulone, 5 parts of wetting agent naphthalene sulfonates, 3 parts of dispersant polycarboxylate, 2 parts of stabilizing agent disodium ethylene diamine tetraacetates, 15 parts of filler precipitated calcium carbonates.The all commercially available acquisition of each raw material components.
The preparation method is with embodiment 1.
This piperazine humulone water dispersible granules technical indicator is following:
Suspensibility 94.1%; Disintegration time≤60s; Wetting time≤60s; Moisture≤2.5%; PH value 6.0～8.0; Wet screening test (through 75 μ m testing sieves)>=98%; Lasting foaming characteristic (behind the 1min)≤20ml; 54 ± 2 ℃ of heat are store suspensibility>=85% after 30 days.
Embodiment 3
A kind of piperazine humulone water dispersible granules, in weight portion, its composition of raw materials consists of: 80 parts of the former medicines of piperazine humulone, 3 parts of wetting agent naphthalene sulfonates, 3 parts of dispersant polycarboxylate, 2 parts of stabilizing agent ethylenediamine tetra-acetic acids, 12 parts of filler corn starchs.
The preparation method is with embodiment 1.
This piperazine humulone water dispersible granules technical indicator is following:
Suspensibility 93.6%; Disintegration time≤60s; Wetting time≤60s; Moisture≤2.5%; PH value 6.0～8.0; Wet screening test (through 75 μ m testing sieves)>=98%; Lasting foaming characteristic (behind the 1min)≤20ml; 54 ± 2 ℃ of heat are store suspensibility>=85% after 30 days.
Embodiment 4
A kind of piperazine humulone water dispersible granules, its composition of raw materials are with embodiment 3, and different is that its used former medicine of piperazine humulone is directly commercially available product, the processing of process watery hydrochloric acid.
This piperazine humulone water dispersible granules technical indicator is following:
Suspensibility 85.3%; Disintegration time≤60s; Wetting time≤60s; Moisture≤2.5%; PH value 6.0～8.0; Wet screening test (through 75 μ m testing sieves)>=98%; Lasting foaming characteristic (behind the 1min)≤20ml; 54 ± 2 ℃ of heat are store suspensibility≤75% after 30 days.
Visible through comparing embodiment 1-4; Use the particle water dispersible granule of the former medicine preparation of the piperazine humulone of handling through watery hydrochloric acid; Compare with the particle water dispersible granule of the former medicine preparation of piperazine humulone of using process watery hydrochloric acid processing, its suspensibility and stability all increase significantly.
Use the piperazine humulone water dispersible granules of embodiment 1-4, to alfalfa ground annual broadleaf weed Amaranthus retroflexus, lamb's-quarters, Siberian cocklebur carries out field control effectiveness test.The result sees table 1.
The result of the test of table 1 field efficacy (after the dispenser 30 days)
Visible from table 1, piperazine humulone water dispersible granules provided by the invention has all shown the control efficiency more excellent than piperazine humulone wettable powder.
To sum up, piperazine humulone water dispersible granules provided by the invention has good dispersiveness, suspensibility is high, disintegration time is short, redispersibility can be superior, and heat storage stability is good, is convenient to advantages such as storage, transportation and environmental pollution are little.The present invention's weeding usefulness in production application is high, and to alfalfa ground Amaranthus retroflexus, lamb's-quarters, the Siberian cocklebur control efficiency all reaches more than 90%, and crops are not had poisoning.
The foregoing description only is explanation technical conceive of the present invention and characteristics; Its purpose is to let the personage who is familiar with this technology can understand content of the present invention and enforcement according to this; Can not limit protection scope of the present invention with this; All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (7)
1. the preparation method of a piperazine humulone water dispersible granules is characterized in that: said piperazine humulone water dispersible granules is rule or irregular graininess body, and its composition of raw materials is following:
The former medicine 50%～80% of piperazine humulone;
Wetting agent 2%～10%;
Dispersant 2%～10%;
Stabilizing agent 1%～5%;
Filler 10%～40%,
Said preparation method comprises the steps:
(1), the watery hydrochloric acid washing by soaking of the former medicinal 1wt%-10wt% of piperazine humulone is stirred, treat piperazine humulone come-up after, filter oven dry;
(2), by prescription, with the former medicine of piperazine humulone after step (1) processing, wetting agent; Dispersant, stabilizing agent and filler fully mix, and pulverize through coarse crushing, mixing again, airslide disintegrating mill; Enter into cone-type mixer and mix, get fine powder through 325 mesh standard sieves, afterwards; In fine powder, add water and mediate, extruder grain promptly gets piperazine humulone water dispersible granules in 40 ℃～60 ℃ oven dry.
2. preparation method according to claim 1 is characterized in that: the concentration of the used watery hydrochloric acid of step (1) is 4 wt%-6wt%.
3. preparation method according to claim 2 is characterized in that: the concentration of watery hydrochloric acid is 5wt%.
4. preparation method according to claim 1 is characterized in that: said wetting agent is to be selected from lauryl sodium sulfate, lignin, naphthalene sulfonate, APES and the alkyl sulfonates one or more.
5. preparation method according to claim 1 is characterized in that: said dispersant is a polycarboxylate.
6. preparation method according to claim 1 is characterized in that: said stabilizing agent is to be selected from ethylenediamine tetra-acetic acid, disodium ethylene diamine tetraacetate and the tetrasodium ethylenediamine tetraacetate one or more.
7. preparation method according to claim 1 is characterized in that: said filler is to be selected from kaolin, diatomite, bentonite, corn starch, precipitated calcium carbonate and the ammonium sulfate one or more.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102696584A (en) * | 2012-05-09 | 2012-10-03 | 安徽华星化工股份有限公司 | Method for preparing pesticide granules |
| EP3087836B1 (en) * | 2015-04-28 | 2019-02-13 | Rotam Agrochem International Company Limited | Herbicidal composition and method for controlling plant growth |
| CN105010412A (en) * | 2015-07-09 | 2015-11-04 | 潍坊友容实业有限公司 | Herba patriniae extract containing herbicide and application thereof in saline-alkaline-land potato planting |
| CN106376553A (en) * | 2016-08-26 | 2017-02-08 | 安徽久易农业股份有限公司 | Pinoxaden-compounded water dispersible granule |
| CN106376552A (en) * | 2016-08-26 | 2017-02-08 | 安徽久易农业股份有限公司 | Pyrazosulfuron water dispersible granule |
| CN106332880A (en) * | 2016-08-26 | 2017-01-18 | 安徽久易农业股份有限公司 | Metribuzin water dispersible granules |
| CN106359432A (en) * | 2016-08-26 | 2017-02-01 | 安徽久易农业股份有限公司 | Methiopyrisulfuron compound water dispersible granule |
| CN109090120A (en) * | 2018-08-14 | 2018-12-28 | 江苏七洲绿色化工股份有限公司 | A kind of dry suspending agent and preparation method thereof containing metribuzin |
| CN109362720A (en) * | 2018-11-08 | 2019-02-22 | 镇江先锋植保科技有限公司 | Chlorimuronethyl water dispersible granules preparation method |
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| CN101167456A (en) * | 2007-12-05 | 2008-04-30 | 张少武 | Fenpyroximate water dispersible granule and preparation method thereof |
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| CN101167456A (en) * | 2007-12-05 | 2008-04-30 | 张少武 | Fenpyroximate water dispersible granule and preparation method thereof |
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