CN102037997B - Unselective herbicide and preparation method thereof - Google Patents

Unselective herbicide and preparation method thereof Download PDF

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CN102037997B
CN102037997B CN 201110000171 CN201110000171A CN102037997B CN 102037997 B CN102037997 B CN 102037997B CN 201110000171 CN201110000171 CN 201110000171 CN 201110000171 A CN201110000171 A CN 201110000171A CN 102037997 B CN102037997 B CN 102037997B
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glyphosate
oxyfluorfen
herbicide
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surfactant
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CN102037997A (en
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王海峰
邓如自
尹文聚
喻斌
曹新瑞
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SHANDONG QILIN AGRICULTURE CHEMICALS CO Ltd
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Abstract

The invention relates to a pesticide and a preparation method thereof, in particular to an unselective herbicide and a preparation method thereof. The unselective herbicide is characterized by being an oil suspending agent prepared by mixing glyphosate, oxyfluorfen and auxiliary materials. In the invention, the glyphosate and the oxyfluorfen are combined, the oxyfluorfen has the touch killing action on the blades of a plant so as to accelerate the absorption of the glyphosate and enhance the pesticide effect of the glyphosate, and the oxyfluorfen has the certain inhibiting effect on weed seeds in the soil so as to prolong the residual life. The herbicide has the advantages of excellent performances on weeding speed, environmental friendliness and herbicide cost conservation as well as obvious effect, wide weeding spectrum, long pesticide effect, rain washing resistance, environmental friendliness and the like on the weeding effect.

Description

A kind of steriland herbicide and preparation method thereof
(1) technical field
The present invention relates to a kind of agricultural chemicals and preparation method thereof, particularly a kind of steriland herbicide and preparation method thereof.
(2) background technology
Glyphosate (Glyphosate) chemical name N-(phosphonomethyl) glycine; be the chronic wide spectrum steriland herbicide of inner sucting conduction type; the main interior enol acetonyl shikimene phosphate synthase of object that suppresses; thereby suppress shikimene to the conversion of phenyl alanine, cruel propylhomoserin and tryptophan, make synthetic being interfered of protein cause plant dead.Be transmitted to plant each position after glyphosate absorbs by cauline leaf, can prevent and kill off the plant of the sections more than 40 such as unifacial leaf and dicotyledonous, annual and perennial, herbs and shrubs.Be combined and lose activity with metal ions such as iron, aluminium very soon after glyphosate buries, seed and edaphon hiding in soil are had no adverse effects, it is before a kind of selectivity bud or post-emergence herbicide, before being used for the buds such as cotton, round onions, peanut, soybean, beet, fruit tree and vegetables, using after bud, can prevent and kill off barnyard grass, sesbania, downy brome, green foxtail, datura, quackgrass, artemisiifolia, thorn chrysanthemum sth. made by twisting, piemarker, charlock unifacial leaf and broad leaved weed etc.
At present, well-known, Monsanto company developed the broad-spectrum herbicide glyphosate (Glyphosate) that is with historically new significance at world's agriculture field in 1971, and the middle and later periods seventies is released glyphosate isopropyl amine salt, amine salt and sodium salt; ICI company released the front three sulfonium salt in 1989.At present, glyphosate has become the maximum pesticide species of most widely used, output in the world, and its annual sales amount occupies first of agricultural chemicals always.In recent years, along with the development of transgenosis glyphosate resistant crops, the glyphosate consumption increases year by year, not only affects the exploitation direction of new varieties, and the market structure of existing weed killer herbicide kind is also caused greater impact.
Glyphosate is mainly used in resistance glyphosate genetically modified crops field weeding, uncultivated area weeding, no-tillage crop-planting.Present glyphosate formulation is all 41% isopropamide AS and 10% aqua basically, the WSG that also has ammonium glyphosate, and the soluble glyphosate pulvis SP of minute quantity and wetting powder WP, for above formulation, itself has certain shortcoming in producing, as the aqua of sales volume maximum, make the in the majority of isopropyl amine salt.When isopropylamine and glyphosate react aborning, emit a large amount of heat, need quite a large amount of cooling waters in production, while isopropylamine highly volatile, inflammable, poisonous, flash-point hangs down explosive, and during operation, danger is very large.In addition, glyphosate is as the chronic wide spectrum steriland herbicide of inner sucting conduction type, for common weed, take effect about a general week after dispenser, it is larger that preventive effect is affected by temperature, but some malignant weed such as cogongrass, the rhizome of nutgrass flatsedge etc. were executed medicine 1 time in 1 month again after medication for the first time, just can reach desirable control efficiency.Drug effect takes effect slowly, how to make the drug effect performance of glyphosate rapidly, reduces impact and the lasting period of low temperature longly, and herbicide more wide spectrum is more thorough, becomes a direction of glyphosate scientific research.
Glyphosate is the blade face effect weed killer herbicide of knowing.The glyphosate of free acid form solvability in water is low, therefore, contains the water soluble salt of glyphosate in the commodity preparation, and solid soluble glyphosate formulation there is no the oil-suspending agent of glyphosate free acid form in the market.The kind that is used at present the nonirrigated farmland weedings such as orchard, tea place, economic forest land, ridge soil limit, wide row crop, be weeds inorganic agent in seedling stage as single glyphosate, gram without track etc., only limiting to has action of contace poison to the weeds that sprout, meeting soil is passivation, not yet sprout unearthed weed seed during to dispenser without control action, later still renewable harm, and mu is higher with cost when using.
(3) summary of the invention
The present invention is in order to make up the deficiencies in the prior art, and a kind of low toxicity, environmental protection, quick-acting steriland herbicide and preparation method thereof are provided.
The present invention is achieved through the following technical solutions:
A kind of steriland herbicide is characterized in that: the oil-suspending agent that forms for glyphosate (glyphosate), Oxyfluorfen (oxyfluorfen) and auxiliary material mixed preparing.
Described auxiliary material is surfactant, thickener and vegetable oil.
The active ingredient of described glyphosate is the 1-80% of gross weight, and the active ingredient of Oxyfluorfen is the 1-80% of gross weight.
As preferred Herbicidal composition, the active ingredient of glyphosate is the 10-50% of gross weight, and the active ingredient of Oxyfluorfen is the 1-10% of gross weight.
Described surfactant is the 9-11% of gross weight, and thickener is the 0.1-0.2% of gross weight, and surplus is vegetable oil.
Described glyphosate technicals solid active constituent content is 1.0-98%, and the former medicine solid of Oxyfluorfen active constituent content is 1.0-95%.
Described surfactant is the homogeneous mixture of non-ionic surface active agent polyoxyethylene nonylphenol ether (Polyoxy ethrlene nonyl phinyl ether) and anionic surfactant calcium dodecyl benzene sulfonate (emulsifier ABSCa).
Described thickener is oiliness organobentonite series, preferred organobentonite BK-88 model.
Described vegetable oil reaches the oils of being extended by vegetable oil, preferably corn oil, soybean oil in the present invention comprising vegetable oil.
In described surfactant, the percentage by weight of non-ionic surface active agent polyoxyethylene nonylphenol ether is 40-60%, and all the other are the anionic surfactant calcium dodecyl benzene sulfonate.
The preferred hydrophilic lipophilic balance of described non-ionic surface active agent polyoxyethylene nonylphenol ether (HLB value) is 6.0-12, especially surfactant TX-10; The preferred hydrophilic lipophilic balance of anionic surfactant calcium dodecyl benzene sulfonate (HLB value) is 6.0-12, especially 500# calcium salt series.
Surfactant is non-ionic surface active agent polyoxyethylene nonylphenol ether (the Polyoxy ethrlene nonyl phinyl ether) TX-10 that commonly uses and the compound emulsifying agent of anionic surfactant calcium dodecyl benzene sulfonate (emulsifier ABSCa) 500# calcium salt series, have the effects such as emulsification, dispersion, reduce surface tension, improved stability of system.Thickener oiliness organobentonite BK-88 model used, the suspension character of energy thickening, enhancing medicament as continuous phase, makes preparation environmentally friendly with corn oil on the one hand, can make more easily adhering to foliage of medicament when using on the other hand, make effect more lasting.Thickener bentonite Optimum used is 0.1-0.2%, also can require according to the viscosity of product formulation suitably to adjust.The percentage that the active ingredient of glyphosate accounts for gross weight is higher, and corresponding glyphosate technicals solid active constituent content is also higher; The percentage that the active ingredient of Oxyfluorfen accounts for gross weight is higher, and the corresponding former medicine solid of Oxyfluorfen active constituent content is also higher.
The preparation method of steriland herbicide of the present invention is characterized in that: comprise the steps:
(1) batching: glyphosate and the former medicine solid of Oxyfluorfen, surfactant, thickener are fed intake according to described ratio, supply 100% with vegetable oil at last;
(2) mixed at high speed is disperseed: turn high speed dispersion with the high speed dispersion agitator with rotating speed 5000 and stir 30-60min, until material stirring is uniformly dispersed;
(3) sand milling: by the sand mill sand milling, flow velocity remains on 150-200kg/h with the material that stirs, and sand milling is three times continuously, and the material fineness of grind is at the 700-800 order and get final product.
Using method: use this steriland herbicide, every mu of consumption is 200-250g, is watered 45 kilograms, sprays with knapsack sprayer.
The quality control index of the made steriland herbicide of the present invention:
Outward appearance: milk yellow suspension, through depositing 2 years, a little layering is arranged, shake rear resilient, without caking knot end phenomenon
Suspensibility: 〉=96%
Moisture :≤0.5%
Fineness: the particle by the 0.043mm sieve aperture 〉=98%
Low-temperature stability: qualified
Heat storage stability: qualified.
glyphosate and Oxyfluorfen composite, it is the effect that mutual synergy is arranged, the Oxyfluorfen main manifestations is contact toxicity, liquid by plant absorbing after, the protoporphyrin oxidase is suppressed, generation is to the virose tetrapyrrole of plant cell tool, gather and have an effect, thereby can promote glyphosate in plant corpus absorption and pass to, play quick-acting, the result of synergy, why adopting corn oil is the conclusion that draws on the basis that repeatedly reaches many-sided experiment, corn oil has good stabilization to whole formula, better to the suspending of glyphosate than other oils in system.The correctness of this theory by the screening of a large amount of formula and land for growing field crops give birth to test test verify.Through province, city plant protection department field experiment repeatedly, with the equal dosage condition of 41% glyphosate isopropylamine salt water solution 200-300g/ mu under, this steriland herbicide and 41% glyphosate isopropylamine salt water solution are compared (wherein having the agriculture of Meng Shandou to reach), all show the superiority of this steriland herbicide, significantly better than the preventive effect of currently marketed glyphosate isopropylamine salt water solution.
Glyphosate and Oxyfluorfen is composite by described proportioning, and both can mutually promote performances of drug effect have increased quick-acting, have improved the speed of control, also can be than common glyphosate formulation when temperature is on the low side fast three to five days; Both mutually promote, and have increased part to the not too control of responsive broad leaved weed of glyphosate, particularly broad leaved weed are prevented and treated performance excellence on quick-acting at it; In many ways evidence is developed to oil-suspending agent has further increased again drug effect; Said preparation is good to low temperature adaptability, can widen the period of using, and has changed current glyphosate conventional formulation, in bad defective of medication effect during low temperature in early stage.
The present invention is composite with glyphosate and Oxyfluorfen; the action of contace poison of Oxyfluorfen to plant leaf blade; can accelerate the absorption of glyphosate; strengthen the drug effect of glyphosate; and Oxyfluorfen has certain inhibitory action to weed seed in soil; can extend the longevity of residure, have outstanding performance on weeding speed, environmental protection, saving drug cost, show the advantages such as quick-acting, broad weed-killing spectrum, drug effect phase length, resistance of rainwater washing against, environmental protection on herbicidal effect.
(4) description of drawings
The present invention is further illustrated below in conjunction with accompanying drawing.
Fig. 1 is technological process of production block diagram of the present invention;
Fig. 2 is production technological process of the present invention.
In figure, 1 oil measurement tank, 2 batching kettles, 3 sand mill I, 4 dehvery pumps, 5 storage tanks, 6 sand mill II, 7 sand mill III, 8 finished product storage tank.
(5) embodiment
Below by specific embodiment, technical scheme of the present invention is further described in detail.
The formula table of table one embodiment 1-7 steriland herbicide
Figure BSA00000406617700051
As shown in Table 1, using embodiment 5 active ingredients is 40% steriland herbicide, and wherein containing 98% glyphosate technicals 30g, the 95% former medicine 8.0g of Oxyfluorfen, surfactant TX-104.4g, surfactant 500# calcium salt series 4.6g, organobentonite BK-8880.14g, its surplus is corn oil.Every mu of consumption is 200-250g, is watered 45 kilograms, and with the knapsack sprayer spraying, after 7 days, to the situation of preventing and treating of various grass, the situation during with use 41% glyphosate isopropylamine salt water solution, 40% soluble glyphosate powder and blank sample contrasts, and its effect is as shown in table 2.As can be seen from Table 2, this steriland herbicide is 67-100% to the preventive effect of listed various grass, can find out in addition, and this steriland herbicide is better than the preventive effect of 41% glyphosate isopropylamine salt water solution to the preventive effect of broadleaved herb.
The herbicidal effect (%) of table 2 embodiment 5 made weed killer herbicides
Figure BSA00000406617700071
Annotate: in the blank hurdle, data are the weeds strain number in 2 square metres.
In embodiment 1 to 4 in made steriland herbicide the content of each material as shown in table 1, every mu of dosage is 250g, is watered 45 kilograms, medication after 15 days herbicidal effect as shown in table 3.As can be seen from Table 3, this steriland herbicide can effectively be prevented and kill off grassy weed, broad leaved weed and nutgrass flatsedge, and control efficiency is fast, and the drug effect phase is long.
Table 3:
Figure BSA00000406617700081
the made steriland herbicide of the present invention, it is the optimum formula that draws by lot of experiments, herbicidal effect reaches with the agriculture of the best Meng Shandou of existing market to be compared, has instant effect, the advantage that herbicide is thorough and the lasting period is long, through scientific research personnel and province, city agricultural plant protection personnel's common checking, under equal formulation rate condition, the more common glyphosate drug effect of this steriland herbicide took effect the fast 2-4 of speed days, lasting period increases 1-2 doubly, and for pernicious root weeds such as cogongrass, the rhizome of nutgrass flatsedge etc., 3 days can obviously take effect, some is played obvious quick-acting to the poor broad leaved weed of glyphosate susceptibility, can reach desirable control efficiency about one week, kill the root degree of depth and reach underground 15-30 centimetre, can stop the regeneration of weeds fully, thereby extend the drug effect longevity of residure.Simultaneously, with respect to present common glyphosate, this steriland herbicide adopts fully natural edible corn oil to the person poultry harmless as synergist and solvent, has reduced the addition of harmful auxiliary agent, has reached environmentally friendly, to the effect of bio-safety.

Claims (4)

1. steriland herbicide, it is characterized in that: be the oil-suspending agent that glyphosate, Oxyfluorfen and auxiliary material mixed preparing form, the active ingredient of glyphosate is the 10-50% of gross weight, and the active ingredient of Oxyfluorfen is the 1-10% of gross weight; Described glyphosate technicals solid active constituent content is 98%, and the former medicine solid of Oxyfluorfen active constituent content is 95%; Thickener and the surplus corn oil of the 0.1-0.2% that auxiliary material is the surfactant that accounts for the 9-11% of gross weight, account for gross weight; Surfactant is the homogeneous mixture of non-ionic surface active agent polyoxyethylene nonylphenol ether and anionic surfactant calcium dodecyl benzene sulfonate, and thickener is oiliness organobentonite series.
2. steriland herbicide according to claim 1, it is characterized in that: in described surfactant, the percentage by weight of non-ionic surface active agent polyoxyethylene nonylphenol ether is 40-60%, all the other are the anionic surfactant calcium dodecyl benzene sulfonate.
3. steriland herbicide according to claim 2, it is characterized in that: described non-ionic surface active agent polyoxyethylene nonylphenol ether hydrophilic lipophilic balance is 6.0-12; Anionic surfactant calcium dodecyl benzene sulfonate hydrophilic lipophilic balance is 6.0-12.
4. the preparation method of steriland herbicide according to claim 1, is characterized in that: comprise the steps:
(1) batching: glyphosate and the former medicine solid of Oxyfluorfen, surfactant, thickener are fed intake according to described ratio, supply 100% with corn oil at last;
(2) mixed at high speed is disperseed: with the rotating speed high speed dispersion stirring 30-60min of high speed dispersion agitator with 5000 rpms, until material stirring is uniformly dispersed;
(3) sand milling: by the sand mill sand milling, flow velocity remains on 150-200kg/h with the material that stirs, and sand milling is three times continuously, and the material fineness of grind is at the 700-800 order and get final product.
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CN102845464B (en) * 2011-06-30 2014-09-03 浙江新安化工集团股份有限公司 Herbicide mixture preparation
CN102835391A (en) * 2012-08-08 2012-12-26 安徽省国家农药剂型工程技术中心 Glyphosate oil suspending agent and preparation method thereof
CN106857652A (en) * 2017-03-12 2017-06-20 安徽省益农化工有限公司 One kind is gone out natural disposition complex weedicide
CN107372502A (en) * 2017-08-09 2017-11-24 重庆市风景园林科学研究院 A kind of herbicidal composition for preventing and kill off dodders in garden platymiscium
CN109662101A (en) * 2017-10-13 2019-04-23 黄俊华 A kind of contact killing type herbicide
CN112715571A (en) * 2021-01-06 2021-04-30 合肥尚邦植保科技有限公司 Ternary weeding composition and application thereof

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CN1347645A (en) * 2000-10-10 2002-05-08 通州正大农药厂 Biocidal herbicide and its preparing process
CN101810202A (en) * 2010-04-30 2010-08-25 中国农业大学 Microbial weeding oil flowable concentrate for rice field

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RS51063B (en) * 2005-06-04 2010-10-31 Bayer Cropscience Ag. Oil suspension concentrate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1347645A (en) * 2000-10-10 2002-05-08 通州正大农药厂 Biocidal herbicide and its preparing process
CN101810202A (en) * 2010-04-30 2010-08-25 中国农业大学 Microbial weeding oil flowable concentrate for rice field

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