CN108378048A - A kind of white tricyclazole suspending agent and preparation method thereof - Google Patents
A kind of white tricyclazole suspending agent and preparation method thereof Download PDFInfo
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- CN108378048A CN108378048A CN201810367209.XA CN201810367209A CN108378048A CN 108378048 A CN108378048 A CN 108378048A CN 201810367209 A CN201810367209 A CN 201810367209A CN 108378048 A CN108378048 A CN 108378048A
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- tricyclazole
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- agricultural chemicals
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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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- 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
- A01N25/02—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 containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- 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
- A01N25/22—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 containing ingredients stabilising the active ingredients
-
- 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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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
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- Environmental Sciences (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of agricultural chemicals suspension agent and preparation method thereof of white tricyclazole, the agricultural chemicals suspension agent of the white tricyclazole is made of following materials by weight percentage：Tricyclazole 5 60%；Surfactant 2 9%；Ethylene glycol 3 7%；Aluminium-magnesium silicate 0.01 2%；Stabilizer：0.1 10%, titanium dioxide：1 10%；20 methacrylate copolymer 0.1 2% of alcohol ether；Methylol acid 0.2 0.4%；Surplus is water.The white tricyclazole agricultural chemicals suspension agent for reducing grain diameter up to the present invention is crushed by colloid mill, ultramicro grinding, high-pressure homogeneous three steps.The tricyclazole agricultural chemicals suspension agent white in appearance or off-white color of the present invention, appearance stablity is non-discolouring, and suspensibility is high, and properties of product are stablized.
Description
Technical field
The invention belongs to Pesticide formulation technical fields, and in particular to a kind of white tricyclazole suspending agent and its preparation side
Method.
Background technology
Tricyclazole is also known as Tricyclazole, gram pest spirit, than gorgeous, rice blast azoles, is a kind of selectivity developed by Lilly Co., Eli.
Interior suction protects fungicide, patent No. BP1419121.
Tricyclazole sterling is white crystals, and vapour pressure is 266.6448 × 10-7 pas when 187~188 DEG C, 25 DEG C of fusing point.25
DEG C when solubility be：1.6 grams per liter of water, dichloromethane 33%, ethyl alcohol 25%, methanol 25%, acetone 10.4%, acetonitrile 10.4%,
Cyclohexanone 10.0%, benzene 4.2%, dimethylbenzene 2.1%, chloroform>500 grams per liters.Property is stablized, and is not easy by water and photodegradation, to heat
Stablize.Its structural formula is as follows：
Tricyclazole is one kind, and there is the stronger protectiveness thiazole series bactericidal agent of interior suction performance, prevention rice blast to have spy
Effect, can be absorbed by the root, stem, leaf of rice after dispenser, and can the transporting in plant, sprayed 1~2 time during entire paddy growth
Medicine can effectively prevent the generation of rice blast.Tricyclazole anti-impact brushing force is strong, and spray meets rain and is not required to the medicine that fills spray after 1 hour.Mainly
It is that spore germination and attachment spore is inhibited to be formed, to effectively prevent germ from invading and reduce the generation of magnaporthe grisea spore.Three
Ring azoles has very strong interior suction and behavior in service, and slow, 7~10 weeks longevities of residure are decomposed in plant body and in soil.It can mix
Kind, dip the seedling root in or foliage spray, preventive effect are good.
Tricyclazole pesticidal preparations are in the majority with wettable powder, with the development of suspending agent technology, gradually have in recent years outstanding
Floating agent product emerges.Industrial goods Mensurating Tricyclazole Technical is generally in orange, yellow even red crystals, so conventional tricyclic in the market
Azoles product colour is also based on orange.The tricyclazole formulation products of this kind of color color in storage process can also constantly occur
Variation, color can constantly deepen, and the impression of unstable product quality is caused to user, influence product sale.So current city
There is the unstable technical problems of color for tricyclazole on field, and the product colour difference of different manufacturers is big, same producer's difference batch
Secondary product also can be with larger difference.
Invention content
To solve the deficiencies in the prior art, a kind of white tricyclazole suspending agent of present invention offer and its preparation side
Method.It is achieved especially by following technical proposals：
It is a kind of white tricyclazole agricultural chemicals suspension agent be made of following materials by weight percentage：Tricyclazole：5-60%；Surface
Activating agent 2-9%；Ethylene glycol 3-7%；Aluminium-magnesium silicate 0.01-2%；Stabilizer：0.1-10%, titanium dioxide：1-10%；Alcohol ether
20- methacrylate copolymers 0.1-2%；Hydroxymethylglycinate 0.01-0.03%；Surplus is water.
Preferably, a kind of agricultural chemicals suspension agent of white tricyclazole is made of following materials by weight percentage：Tricyclazole：20-
55%；Surfactant 3-7%；Ethylene glycol 3-5%；Aluminium-magnesium silicate 0.01-2%；Stabilizer：0.1-10%, titanium dioxide：1-
10%；Alcohol ether 20- methacrylate copolymers 0.1-2%；Hydroxymethylglycinate 0.01-0.03%；Surplus is water.
The surfactant is：Dodecyl polyoxyethylene (3) ether sulfuric acid triethanolamine and/or different tridecanol ether (6)
Phosphate kalium salt anion surfactant.
The surfactant, dodecyl polyoxyethylene (3) ether sulfuric acid triethanolamine and different tridecanol ether (6) phosphate
The mass ratio of sylvite is 1:1-1:5.
The stabilizer is：Citric acid, acetic acid, any one of phosphoric acid, potassium dihydrogen phosphate or several combinations.
A method of the agricultural chemicals suspension agent preparing above-mentioned white tricyclazole mainly includes the following steps：
(1) according to formula tricyclazole, surfactant, aluminium-magnesium silicate, stabilizer, titanium dioxide, alcohol ether 20- methyl-props
Olefin(e) acid ester copolymer, hydroxymethylglycinate, water are stirred pulp object, and coarse crushing is carried out by colloid mill.
(2) material after coarse crushing in step (1) is placed in grinding machine and carries out ultramicro grinding, control material grain size D (90)
2 μm of ＜；
(3) material for obtaining ultramicro grinding in step (2) will be placed in homogeneous in homogenizer again, and will make material uniform particle
Change, that is, is prepared into the agricultural chemicals suspension agent of white tricyclazole.
Sand mill zirconium bead diameter is 0.5mm in the step (2), crushes temperature control at 20-30 DEG C.
Homogenizer described in the step (3) is high pressure homogenizer, the high pressure homogenizer operating pressure 70MPa.
Compared with prior art, the present invention haing the following advantages：
(1) present invention adds acidic materials as stabilizer, to keep impurity in tricyclazole to be under stabilizer function
Existing white, while color change not occurring during storage；(2) titanium dioxide is added as brightening agent, improves preparation
Whiteness exists by milled titanium dioxide in micro/nano level state, and can aid in reduces the residual of tricyclazole in the environment；
(3) invention introduces dodecyl polyoxyethylene (3) ether sulfuric acid triethanolamine, different tridecanol ether (6) phosphate kalium salt conducts
Wetting dispersing agent, surface tension is lower, while can be effectively increased the permeability of preparation, and drug effect is turned up；(4) using present invention system
The white tricyclazole agricultural chemicals suspension agent for the present invention that Preparation Method obtains, suspensibility is high, and plate-out ability and good penetrability, properties of product are steady
It is fixed, and there is strong uptake and translocation effect as Pesticide use, it can be by each site absorption of rice, and accumulate and arrive leaf portion tissue, lead to
It can take effect within 2-3 days after normal dispenser, show as that rice leaf is obviously turned green, scab reduces, the lasting period, protecting effect of leaves was shown up to 15 days or so
It writes, while controlling disease, stimulates root growth, transplanting rice is accelerated to turn green；Ear period use can promote photosynthesis, delay leaf
Piece aging enhances plant resistance, can especially adjust spike of rice kernel grouting, improves setting percentage and mass of 1000 kernel, increases yield, and
Rice quality can be improved.
Specific implementation mode
Below the technical scheme of the invention is illustrated by a specific example, but protection scope of the present invention be not limited to it is following
Embodiment, the accommodation in any form and/or change made to the present invention fall within the scope of the present invention.
Embodiment 1
20% tricyclazole suspending agent
(1) according to formula tricyclazole, surfactant, aluminium-magnesium silicate, stabilizer, titanium dioxide, alcohol ether 20- methyl-props
Olefin(e) acid ester copolymer, hydroxymethylglycinate, water are stirred pulp object, and coarse crushing is carried out by colloid mill.
(2) material after coarse crushing in step (1) is placed in grinding machine and carries out ultramicro grinding, control material grain size D (90)
2 μm of ＜；Grinding temperature control is at 20-30 DEG C, sand mill zirconium bead diameter 0.5mm.
(3) material for obtaining ultramicro grinding in step (2) is placed in homogeneous in homogenizer, makes material particle homogenization, i.e.,
It is prepared into the agricultural chemicals suspension agent of white tricyclazole.High pressure homogenizer operating pressure 70MPa.
Suspending agent obtained, the sticky homogeneous liquid of appearance, through Malvern laser fineness gage measure, grain size
(D90) it is 1.6 μm.
Table 1：20% tricyclazole suspending agent formula table
Embodiment 2
40% tricyclazole suspending agent
Raw material is weighed by 2 corresponding embodiment of table, 2 data, is prepared as described in Example 1, suspending agent obtained, grain
Diameter (D90) is 1.6 μm.
Table 2：40% tricyclazole suspending agent formula table
Embodiment 3
55% tricyclazole suspending agent
Raw material is weighed by 3 corresponding embodiment of table, 3 data, is prepared as described in Example 1, suspending agent obtained, grain
Diameter (D90) is 1.6 μm.
Table 3：55% tricyclazole suspending agent formula table
Comparative example 1
(1) tricyclazole, various auxiliary agents are added according to formula in table 4 by cutting kettle, shearing is uniform.
(2) material obtained in step (1) being ground to material particular diameter D (90) with sand mill and is less than 5 μm, grinding terminates,
Stir evenly the suspending agent of obtained tricyclazole, appearance is orange, sticky uniform liquid.
Table 4：40% tricyclazole suspending agent formula table
1 surface tension of test case detects
By the tricyclazole suspending agent prepared in embodiment 1,2,3 and comparative example 1 and certain 75% tricyclic of company in the market
Azoles wettable powder dilution agent dilutes 1000,2000 times of measurement surface tension respectively, and measurement result is shown in Table 5.
The experimental results showed that tricyclazole suspending agent surface tension of the invention is significantly lower than the tricyclazole using conven-tional adjuvants
Suspending agent, product of the invention field using when liquid can more effectively be sprawled on rice leaf, improve pesticide utilize
Rate.
2 color of test case, suspensibility Detection of Stability
The tricyclazole suspending agent of gained will be prepared in embodiment 1,2,3 and comparative example 1 respectively in room temperature storage 14 days, 54
High temperature storage 14 days under the conditions of DEG C ± 2 DEG C, uses《GB/T14825-2006 agricultural-chemical suspension rate assay methods》Suspensibility is surveyed, specifically
Data see the table below 4.Work as suspensibility>When 85%, then it is assumed that the product is certified products.
Table 6：Tricyclazole color, suspensibility determination data table
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | |
| Color before heat storage | White | White | White | It is orange |
| Color after heat storage | White | White | White | Reddish orange |
| After room temperature 14 days | 99.5% | 99.6% | 99.1% | 95.3% |
| After heat storage 14 days | 99.3% | 99.4% | 99.0% | 93.2% |
Suspension refers to that the active compound particle of dispersion keeps the ability of suspension time length in suspension, usually uses suspensibility
To indicate.One good suspending agent should have good storage stability, i.e., higher suspensibility.It can be with from the data in table 4
Find out, is all up to 99% or more using the suspensibility of tricyclazole suspending agent obtained by preparation method of the present invention, hence it is evident that more outstanding than comparative example
Floating rate higher, present invention gained tricyclazole suspending agent colour stable, unchanged before and after heat-storage, color adds after comparative example heat-storage
It is deep, it illustrates that the tricyclazole suspending agent product that the present invention obtains all is certified products, there is very high suspensibility and storage stability.
Claims (8)
1. a kind of agricultural chemicals suspension agent of white tricyclazole, which is characterized in that be made of following materials by weight percentage：Tricyclazole 5-
60%, surfactant 2-9%, ethylene glycol 3-7%, aluminium-magnesium silicate 0.01-2%, stabilizer 0.1-10%, titanium dioxide 1-
10%, alcohol ether 20- methacrylate copolymers 0.1-2%, hydroxymethylglycinate 0.01-0.03%, surplus are water.
2. the agricultural chemicals suspension agent of white tricyclazole according to claim 1, which is characterized in that former by following weight percentage
Material composition：Tricyclazole 20-55%, surfactant 3-7%, ethylene glycol 3-5%, aluminium-magnesium silicate 0.01-2%, stabilizer 0.1-
10%, titanium dioxide 1-10%, alcohol ether 20- methacrylate copolymers 0.1-2%, hydroxymethylglycinate 0.01-0.03%,
Surplus is water.
3. the agricultural chemicals suspension agent of white tricyclazole according to claim 1 or 2, which is characterized in that the surfactant
For dodecyl polyoxyethylene (3) ether sulfuric acid triethanolamine and/or different tridecanol ether (6) phosphate kalium salt anion surface active
Agent.
4. white tricyclazole agricultural chemicals suspension agent according to claim 3, which is characterized in that the surfactant, 12
Alkyl polyoxyethylene (3) ether sulfuric acid triethanolamine and different tridecanol ether (6) phosphate kalium salt mass ratio are 1:1-1:5.
5. tricyclazole agricultural chemicals suspension agent according to claim 1 or 2, which is characterized in that the stabilizer is citric acid,
Acetic acid, any one of phosphoric acid, potassium dihydrogen phosphate or several.
6. a kind of method preparing the agricultural chemicals suspension agent of white tricyclazole described in claims 1 or 2, which is characterized in that main packet
Include following steps：
(1) according to formula tricyclazole, surfactant, ethylene glycol, aluminium-magnesium silicate, stabilizer, titanium dioxide, alcohol ether 20- first
Base acrylate copolymer, hydroxymethylglycinate, water are stirred pulp object, and coarse crushing is carried out by colloid mill；
(2) material after coarse crushing in step (1) is placed in grinding machine and carries out ultramicro grinding, 2 μ of control material grain size D (90) ＜
m；
(3) material for obtaining ultramicro grinding in step (2) is placed in homogeneous in homogenizer, makes material particle homogenization, that is, prepares
At the agricultural chemicals suspension agent of white tricyclazole.
7. a kind of preparation method of the agricultural chemicals suspension agent of white tricyclazole according to claim 6, which is characterized in that described
Sand mill zirconium bead diameter is 0.5mm in step (2), and sand mill crushed work temperature is controlled at 20-30 DEG C.
8. a kind of preparation method of the agricultural chemicals suspension agent of white tricyclazole according to claim 6, which is characterized in that described
Homogenizer described in step (3) is high pressure homogenizer, the high pressure homogenizer operating pressure 70MPa.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111869661A (en) * | 2020-08-20 | 2020-11-03 | 蚌埠格润生物科技有限公司 | High-concentration tricyclazole suspending agent and preparation method thereof |
| CN113045745A (en) * | 2021-03-26 | 2021-06-29 | 南京拓际生物科技有限公司 | Preparation method and application of tristyrylphenol polyoxyethylene ether phosphate ester agricultural surfactant |
| CN115886015A (en) * | 2022-11-28 | 2023-04-04 | 江苏艾津作物科技集团有限公司 | Rain-wash-resistant tricyclazole suspending agent and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111869661A (en) * | 2020-08-20 | 2020-11-03 | 蚌埠格润生物科技有限公司 | High-concentration tricyclazole suspending agent and preparation method thereof |
| CN111869661B (en) * | 2020-08-20 | 2023-01-24 | 蚌埠格润生物科技有限公司 | High-concentration tricyclazole suspending agent and preparation method thereof |
| CN113045745A (en) * | 2021-03-26 | 2021-06-29 | 南京拓际生物科技有限公司 | Preparation method and application of tristyrylphenol polyoxyethylene ether phosphate ester agricultural surfactant |
| CN115886015A (en) * | 2022-11-28 | 2023-04-04 | 江苏艾津作物科技集团有限公司 | Rain-wash-resistant tricyclazole suspending agent and preparation method thereof |
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