CN107897180A - A kind of broad spectrum type diquat dibromide compound synergic agent and preparation method thereof - Google Patents
A kind of broad spectrum type diquat dibromide compound synergic agent and preparation method thereof Download PDFInfo
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- CN107897180A CN107897180A CN201711212275.1A CN201711212275A CN107897180A CN 107897180 A CN107897180 A CN 107897180A CN 201711212275 A CN201711212275 A CN 201711212275A CN 107897180 A CN107897180 A CN 107897180A
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- diquat dibromide
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- broad spectrum
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/30—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
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Abstract
The present invention relates to a kind of broad spectrum type diquat dibromide compound synergic agent and preparation method thereof, is prepared and synthesized by pyrrolidones, surfactant, wetting agent, dispersant, bleeding agent, pH adjusting agent and defoamer;The convenience that the present invention can replace common market series of products and the versatility of expansion synergist and charging use significantly, the diquat dibromide aqua product stable quality of preparation, weeding drug effect significantly improves, the drug effect retention time is grown, the usage amount of herbicide can effectively be reduced, the pollution to environment is reduced, is economized on resources.
Description
Technical field
The present invention relates to pesticide field, more particularly to a kind of broad spectrum type diquat dibromide compound synergic agent and preparation method thereof.
Background technology
Diquat dibromide belongs to bipyridyl herbicides together with paraquat, and bipyridyl herbicides are by ICI companies(Now ownership is first just
Up to company)Developed in 1958, be the natural disposition cauline leaf process agent of going out of absorbability contact killing type, it is quick and upward in non-symplast
Conduction, but do not conducted downwards in bast, therefore weeds underground part cannot be killed.Such herbicide has two important grass of kind hundred
Withered (paraquat) and diquat dibromide (diquat).1,2 one one 2,2 a pair of pyridine of ethylidene of diquat dibromide chemical name, two father-in-law's salt, has
Alginates and dibromo salt, other titles Reglone, Aquacide etc., are with dibromo salt (diquatdibromide) in use
It is main.Product rat acute LD50 is 231mg/kg, moderate toxicity.Bipyridyl herbicides can be rapid, strong by soil colloid
Strong absorption, loses activity so once contacting soil, therefore extremely safe to succession crop.The product are widely used in crop field, fruit
Garden, bare place, gather in the weeding such as preceding, is also a widely used aquatic weed herbicide abroad.During for crop field, usually
It is that before seedling kills the big grass grown before crop sowing or after broadcasting, or after crop seedling is grown up, using directed spraying in the ranks.Together
When, diquat dibromide or a contact drier, can be used as urging withered/ripe and seed crop drier before and after crop harvesting.When
When urging withered for potato haulm, 420-480g/kg of dosage, when seed crop is dried, 392-784g/kg of dosage, anti-water removal
During raw weeds, 588-2950g/ha of dosage.Diquat dibromide is mainly used for broad leaved weed plot in the majority, more than grassy weed
When, to strengthen preventive effect, the mixture of it and paraquat can be used.
Diquat dibromide is identical with paraquat and similarity is very much:All belong to bipyridyliums, be similar compound;All it is 1958
Found in year, developed and promoted by ICI companies;All belong to absorbability contact killing type steriland herbicide, the mechanism of action is also identical, all
It is photosynthetic electron transport chain diversion agent;All there is weeding and urge withered double action, therefore they are all both weeding on international market
Agent, and be to urge withered dose, paraquat registration are used on the crops such as cotton, wheat urge withered, and diquat dibromide registration is for potato, big
Urged on the crops such as beans, cotton, rice, wheat withered;Status on global agrochemical market is close, at present, as the country is on hundred
After careless No. 1745 ban of low water agent are announced and implemented, i.e., from 1 day July in 2014, the registration of revocation paraquat aqua and production are permitted
, production can be stopped, retaining the outlet of Mu Yao manufacturing enterprises aqua overseas using registering, allow to specialize in outlet production, July 1 in 2016
Day stop aqua selling and use at home.And paraquat dosage is to be only second to the second largest herbicide of glyphosate, once it is domestic
Forbid selling, then diquat dibromide will become the strong substitute of paraquat aqua.So innovation is developed and matched somebody with somebody with excellent
5 property and the Additives Products of good weeding drug effect performance are the technical barriers that the current country must capture.
Domestic diquat dibromide aqua technology existing at present generally has no applicability requirement, is the non-selection natural disposition aqua that goes out, it is lacked
Point is as follows:
(1)It is poor for applicability:Existing diquat dibromide auxiliary agent general applicability is poor, cannot be general to various types of mother liquor and content, wide usage
Limit to
(2)It is poor to soak plate-out ability:For diquat dibromide aqua prepared by the prior art generally for soaking no requirement (NR), wetting time is general
In 180s or so, wetting effect needs to strengthen
(3)It is building performance not notable:For some technologies using sodium sulfate of polyethenoxy ether of fatty alcohol as synergist, drug effect is for 2 weeks,
Duration of efficacy is shorter.
(4)Extreme condition resistance is poor:Technically drug effect has a great influence diquat dibromide preparation in extreme circumstances at present, frost resistance
Have much room for improvement with high temperature resistance.
(5)The dilution stability of preparating liquid is poor, flocculation sediment phenomenon easily occurs, influences the stability of product quality.
The content of the invention
The technical problem to be solved in the present invention is design a kind of broad spectrum type diquat dibromide compound synergic agent and preparation method thereof, solution
Certainly above-mentioned existing technical problem.
The present invention provides a kind of broad spectrum type diquat dibromide compound synergic agent, by pyrrolidones, surfactant,
Wetting agent, dispersant, bleeding agent, pH adjusting agent and defoamer prepare synthesis;
Each material mass ratio of broad spectrum type diquat dibromide synergist is as follows in the present invention:
10~40 parts of pyrrolidones;
10~40 parts of surfactant;
0.1~20 part of wetting agent;
0.1~20 part of dispersant;
0.1~20 part of bleeding agent;
0.1~10 part of pH adjusting agent;
0.1~10 part of defoamer.
Further, pyrrolidone-2 compounds are polyvinylpyrrolidone, 1-methyl-2-pyrrolidinone, 3- hydroxyl -2- aryl
One or more in pyrrolidones, n-vinyl pyrrolidone, 1-Methyl-2-Pyrrolidone.
Further, surfactant is oil-based betaine, OP-10, glyceryl cocoate, lauroyl aminocarbonyl propyl beet
Alkali, AES, sodium lignin sulfonate, Tween 80, polyethylene glycol, lauric acid amide of ethanol, Potassium dodecylbenzenesulfonate, lauryl
One or more in dimethyl tertiary amine, lauryl sodium sulfate.
Further, wetting agent KY-2089(Jiangsu Kai Yuan Science and Technology Ltd.s), dodecyl benzene sulfonic acid, solubility
Azone, organosilicon, sodium sulfate of polyethenoxy ether of fatty alcohol, ethylene glycol, glycerine, dimethyl sulfoxide (DMSO), lauryl betaine, positive certain herbaceous plants with big flowers alcohol
In one or more.
Further, dispersant KY-556(Polycarboxylic acid salt/Jiangsu Kai Yuan Science and Technology Ltd.s), lignin, glycerine
One or more in oleate, fatty alcohol polyoxyethylene ether.
Further, bleeding agent is the one or more in fast T, AEO-5, JFC, JFC-1, JFC-2.
Further, pH adjusting agent is one kind in citric acid, oxalic acid, acetic acid, hydrochloric acid, sulfurous acid.
Further, defoamer AF-1501(Organic silicon)、AF-1502、AF-1503、AF-1504、AF-1505(Have
Machine silicon class)In one or more.
Present invention also offers a kind of broad spectrum type diquat dibromide compound synergic agent preparation method, include the following steps:
a)Pyrrolidones and surfactant are added into reaction vessel, 70 ° stir evenly, and obtain material A;
b)By dispersant, wetting agent, bleeding agent, it is added separately in material A, dissolves by heating, is stirred homogeneous, obtain material
B;
c)PH adjusting agent is added portionwise in material B, stirring neutralizes, and treats that cooling is eventually adding defoamer completely after the reaction was complete,
PH value is detected after stirring, is discharged, diquat dibromide finished product synergist is made.
Beneficial effect:The broad spectrum type diquat dibromide compound synergic agent of the present invention and preparation method and existing preparation process phase
It is than advantage:
1)The convenience that the present invention can expand the versatility of synergist and charging uses, the diquat dibromide aqua product quality of preparation
Stablize, efficacy time length, so as to reduce the pollution to environment, economizes on resources.
2)Lauryl sodium sulfate component is free of in synergist of the present invention, it not only ensure that synergist can have preferably
Mobility, middle charging easy to produce use, reduce the phenomenon of bubble, effectively solve the problems, such as that foaming characteristic is big.
3)Containing dispersant, wetting agent, bleeding agent component in the synergist of the present invention, the proportioning of these components, which adds, to be ensured
The diquat dibromide synergist prepared has good dispersiveness, wetting and spreading, cauline leaf permeability.
4)Contain surfactant component in the synergist of the present invention, which ensure that the diquat dibromide synergist tool of preparation
There is good emulsifiability.While keeping original good chemical effect, suitable for different manufacturers mother liquor, wide usage is greatly
By force.
Embodiment
Embodiment one:
Remove the material of row weight:1-methyl-2-pyrrolidinone 25g;Sodium sulfate of polyethenoxy ether of fatty alcohol 25g;KY-2089 18g;
KY-556 16g;JFC 12g;Citric acid 4g.25g 1-methyl-2-pyrrolidinones, 25g fat alcohol polyethenoxy ether sodium sulfate are added
Into four-hole boiling flask, 70 DEG C are heated with stirring to;Then the KY-2089 18g of metering are added;KY-556 16g;JFC 12g;Stirring
Uniformly, pH adjusting agent citric acid 4g is eventually adding, stirring neutralizes, and cooling discharging, is made broad spectrum type diquat dibromide synergist.
The pH value 4.5 of the obtained broad spectrum type diquat dibromide synergist, viscosity 120mPa.s, surface tension 50mN/m, blistering
25ml, soaks average 1m30s.
Embodiment two:
Remove the material of row weight:1-methyl-2-pyrrolidinone 12g;Sodium sulfate of polyethenoxy ether of fatty alcohol 25g;KY-2089 18g;
KY-556 16g;JFC 12g;Citric acid 4g.25g 1-methyl-2-pyrrolidinones, 25g sodium sulfate of polyethenoxy ether of fatty alcohol are added
Enter into four-hole boiling flask, be heated with stirring to 80 DEG C;Then the KY-2089 18g of metering are added;KY-556 16g;JFC 12g;Stir
Mix uniformly, be eventually adding pH adjusting agent citric acid 4g, stirring neutralizes, and cooling discharging, is made broad spectrum type diquat dibromide synergist.
The pH value 3.8 of the obtained broad spectrum type diquat dibromide synergist, viscosity 30mPa.s, surface tension 20mN/m, blistering
25ml, soaks average 1m50s.
Embodiment three:
Remove the material of row weight:1-methyl-2-pyrrolidinone 25g;Sodium sulfate of polyethenoxy ether of fatty alcohol 15g;KY-2089 18g;
KY-556 16g;JFC 12g;Citric acid 4g.15g 1-methyl-2-pyrrolidinones, 25g sodium sulfate of polyethenoxy ether of fatty alcohol are added
Enter into four-hole boiling flask, be heated with stirring to 80 DEG C;Then the KY-2089 18g of metering are added;KY-556 16g;JFC 12g;Stir
Mix uniformly, be eventually adding pH adjusting agent citric acid 4g, stirring neutralizes, and cooling discharging, is made broad spectrum type diquat dibromide synergist.
The pH value 5.2 of the obtained broad spectrum type diquat dibromide synergist, viscosity 18mPa.s, surface tension 9mN/m, blistering
28ml, soaks average 1m44s.
Example IV:
Remove the material of row weight:1-methyl-2-pyrrolidinone 25g;Sodium sulfate of polyethenoxy ether of fatty alcohol 25g;KY-2089 8g;
KY-556 16g;JFC 12g;Citric acid 4g.25g 1-methyl-2-pyrrolidinones, 25g sodium sulfate of polyethenoxy ether of fatty alcohol are added
Enter into four-hole boiling flask, be heated with stirring to 80 DEG C;Then the KY-2089 8g of metering are added;KY-556 16g;JFC 12g;Stir
Mix uniformly, be eventually adding pH adjusting agent citric acid 4g, stirring neutralizes, and cooling discharging, is made broad spectrum type diquat dibromide synergist.
The pH value 4.3 of the obtained broad spectrum type diquat dibromide synergist, viscosity 98mPa.s, surface tension 45mN/m, blistering
32ml, soaks average 2m05s.
Embodiment five:
Remove the material of row weight:1-methyl-2-pyrrolidinone 25g;Sodium sulfate of polyethenoxy ether of fatty alcohol 25g;KY-2089 18g;
KY-556 6g;JFC 12g;Citric acid 4g.25g 1-methyl-2-pyrrolidinones, 25g sodium sulfate of polyethenoxy ether of fatty alcohol are added
Enter into four-hole boiling flask, be heated with stirring to 80 DEG C;Then the KY-2089 18g of metering are added;KY-556 6g;JFC 12g;Stir
Mix uniformly, be eventually adding pH adjusting agent citric acid 4g, stirring neutralizes, and cooling discharging, is made broad spectrum type diquat dibromide synergist.
The pH value 4.2 of the obtained broad spectrum type diquat dibromide synergist, viscosity 96mPa.s, surface tension 43mN/m, blistering
28ml, soaks average 2m32s.
Embodiment six:
Remove the material of row weight:1-methyl-2-pyrrolidinone 25g;Sodium sulfate of polyethenoxy ether of fatty alcohol 25g;KY-2089 18g;
KY-556 16g;JFC 2g;Citric acid 4g.25g 1-methyl-2-pyrrolidinones, 25g sodium sulfate of polyethenoxy ether of fatty alcohol are added
Enter into four-hole boiling flask, be heated with stirring to 80 DEG C;Then the KY-2089 18g of metering are added;KY-556 16g;JFC 2g;Stir
Mix uniformly, be eventually adding pH adjusting agent citric acid 4g, stirring neutralizes, and cooling discharging, is made broad spectrum type diquat dibromide synergist.
The pH value 4.3 of the obtained broad spectrum type diquat dibromide synergist, viscosity 310mPa.s, surface tension 48mN/m, blistering
38ml, soaks average 3m05s.
Embodiment seven:
Remove the material of row weight:1-methyl-2-pyrrolidinone 25g;Sodium sulfate of polyethenoxy ether of fatty alcohol 25g;KY-2089 18g;
KY-556 16g;JFC 2g;Citric acid 1g.25g 1-methyl-2-pyrrolidinones, 25g sodium sulfate of polyethenoxy ether of fatty alcohol are added
Enter into four-hole boiling flask, be heated with stirring to 80 DEG C;Then the KY-2089 18g of metering are added;KY-556 16g;JFC 2g;Stir
Mix uniformly, be eventually adding pH adjusting agent citric acid 1g, stirring neutralizes, and cooling discharging, is made broad spectrum type diquat dibromide synergist.
The pH value 6.1 of the obtained broad spectrum type diquat dibromide synergist, viscosity 250mPa.s, surface tension 72mN/m blistering
35ml, soaks average 2m48s.
Embodiment eight:
Remove the material of row weight:1-methyl-2-pyrrolidinone 10g;Sodium sulfate of polyethenoxy ether of fatty alcohol 10g;KY-2089 18g;
KY-556 16g;JFC 2g;Citric acid 4g.210g 1-methyl-2-pyrrolidinones, 10g sodium sulfate of polyethenoxy ether of fatty alcohol are added
Enter into four-hole boiling flask, be heated with stirring to 80 DEG C;Then the KY-2089 18g of metering are added;KY-556 16g;JFC 2g;Stir
Mix uniformly, be eventually adding pH adjusting agent citric acid 4g, stirring neutralizes, and cooling discharging, is made broad spectrum type diquat dibromide synergist.
The pH value 3.5 of the obtained broad spectrum type diquat dibromide synergist, viscosity 32mPa.s, surface tension 25mN/m, blistering
38ml, soaks average 3m22s.
Table 1 carries out the broad spectrum type diquat dibromide synergist of preparation pH value, viscosity, tension force, foaming characteristic and wettability measure
Data:
Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | |
PH value | 4.5 | 3.8 | 5.2 | 4.3 | 4.2 | 4.3 | 6.1 | 3.5 |
Viscosity(mPa.s) | 120 | 30 | 18 | 98 | 96 | 310 | 250 | 32 |
Tension force(MN/m) | 50 | 20 | 9 | 45 | 43 | 48 | 72 | 25 |
Foaming characteristic(ml) | 25 | 25 | 28 | 32 | 28 | 38 | 35 | 38 |
MEBO ribbon gauze | 1m30s | 1m50s | 1m44s | 2m05s。 | 2m32s | 3m05s | 2m48s | 3m22s |
PH value measures:
Weigh 1.0g diquat dibromide builder products to be put into beaker, add deionized water to 100g, stir evenly, measured with pH meter
PH value, the pH value for measuring high glutinous type diquat dibromide synergist is 4.5.
Viscosimetric analysis:
Instrument:NDJ-1 type rotary viscosimeters(Shanghai Hengping Instrument & Meter Plant);
Test temperature:25℃;
Rotor:No. 1 rotor, rotating speed:12 revs/min;
Viscosity data is measured using rotary viscosimeter.
Surface tension test:
Instrument:ZL-2 type automatic tension instrument
Test temperature:25℃
Measuring method:Ring method
Use the surface tension of ZL-2 type automatic tensions instrument measure diquat dibromide synergist.
Foaming characteristic measures:Weigh 1.0g diquat dibromide builder products to be put into 250ml graduated cylinders, add deionized water extremely
200ml, stirs evenly, and is placed after turning upside down 30 times, and bubble was observed after 1 minute, measures its blistering rate.
Wettability determination:Weigh 1.0g diquat dibromide builder products to be put into beaker, add deionized water to 250ml, stir
Mix uniformly, insert canvas, calculate from being placed to the time required to being totally submerged sinking, totally three groups, measure its wetting time.
Many details are elaborated in the above description in order to fully understand the present invention.But above description is only
Presently preferred embodiments of the present invention, the invention can be embodied in many other ways as described herein, therefore this
Invention from specific implementation disclosed above limitation.Any those skilled in the art are not departing from the technology of the present invention at the same time
In the case of aspects, all technical solution of the present invention is made using the methods and technical content of the disclosure above many possible
Changes and modifications, or it is revised as the equivalent embodiment of equivalent variations.Every content without departing from technical solution of the present invention, according to this
The technical spirit of invention still falls within skill of the present invention to any simple modifications, equivalents, and modifications made for any of the above embodiments
In the range of the protection of art scheme.
Claims (9)
- A kind of 1. broad spectrum type diquat dibromide compound synergic agent, it is characterised in that:By pyrrolidones, surfactant, profit Humectant, dispersant, bleeding agent, pH adjusting agent and defoamer prepare synthesis;Each material mass ratio of broad spectrum type diquat dibromide synergist is as follows:10~40 parts of pyrrolidones;10~40 parts of surfactant;0.1~20 part of wetting agent;0.1~20 part of dispersant;0.1~20 part of bleeding agent;0.1~10 part of pH adjusting agent;0.1~10 part of defoamer.
- 2. broad spectrum type diquat dibromide compound synergic agent according to claim 1, it is characterised in that:The pyrrolidone-2 compounds For polyvinylpyrrolidone, 1-methyl-2-pyrrolidinone, 3- hydroxyl -2- aryl pyrrolidones, n-vinyl pyrrolidone, 1- first One or more in base -2-Pyrrolidone.
- 3. broad spectrum type diquat dibromide compound synergic agent according to claim 1, it is characterised in that:The surfactant is oil Base glycine betaine, OP-10, glyceryl cocoate, lauroyl amido propyl betaine, AES, sodium lignin sulfonate, Tween 80, poly- second One in glycol, lauric acid amide of ethanol, Potassium dodecylbenzenesulfonate, lauryl dimethyl tertiary amine, lauryl sodium sulfate Kind is several.
- 4. broad spectrum type diquat dibromide compound synergic agent according to claim 1, it is characterised in that:The wetting agent is KY- 2089th, dodecyl benzene sulfonic acid, soluble azone, organosilicon, sodium sulfate of polyethenoxy ether of fatty alcohol, ethylene glycol, glycerine, diformazan One or more in base sulfoxide, lauryl betaine, positive certain herbaceous plants with big flowers alcohol.
- 5. broad spectrum type diquat dibromide compound synergic agent according to claim 1, it is characterised in that:The dispersant is KY- 556th, the one or more in lignin, glyceryl oleate, fatty alcohol polyoxyethylene ether.
- 6. broad spectrum type diquat dibromide compound synergic agent according to claim 1, it is characterised in that:The bleeding agent for fast T, One or more in AEO-5, JFC, JFC-1, JFC-2.
- 7. broad spectrum type diquat dibromide compound synergic agent according to claim 1, it is characterised in that:The pH adjusting agent is lemon One kind in acid, oxalic acid, acetic acid, hydrochloric acid, sulfurous acid.
- 8. broad spectrum type diquat dibromide compound synergic agent according to claim 1, it is characterised in that:The defoamer is AF- 1501st, the one or more in AF-1502, AF-1503, AF-1504, AF-1505.
- 9. the broad spectrum type diquat dibromide compound synergic agent preparation method described in any of the above-described claim, it is characterised in that:Including such as Lower step:a)Pyrrolidones and surfactant are added into reaction vessel, 70 ° stir evenly, and obtain material A.b)By dispersant, wetting agent, bleeding agent, it is added separately in material A, dissolves by heating, is stirred homogeneous, obtain material B。c)PH adjusting agent is added portionwise in material B, stirring neutralizes, and treats that cooling is eventually adding defoamer completely after the reaction was complete, PH value is detected after stirring, is discharged, diquat dibromide finished product synergist is made.
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CN110547294A (en) * | 2019-08-19 | 2019-12-10 | 南京拓际生物科技有限公司 | Preparation research method of special auxiliary agent for glyphosate granules |
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CN110547294A (en) * | 2019-08-19 | 2019-12-10 | 南京拓际生物科技有限公司 | Preparation research method of special auxiliary agent for glyphosate granules |
WO2021197106A1 (en) * | 2020-04-02 | 2021-10-07 | Jiangsu Rotam Chemistry Co., Ltd | Plant protection composition having improved penetration |
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