CN107136079A - A kind of aqueous cyhalofop-butyl emulsion and preparation method thereof - Google Patents

Abstract

A kind of aqueous cyhalofop-butyl emulsion and preparation method thereof, belongs to herbicide preparing technical field, is made up of the raw material of following mass ratio：Cyhalofop-butyl 6%~12%, solvent 8%~15%, emulsifying agent 6%~15%, antifreezing agent 2%~6%, surplus is water.Instant component is reasonable, preparation principle is clear, by low-energy emulsification method be prepared for efficiently, environment-protective water emulsion, simplify work flow, reduce production cost, improve product stability, and to the effect of weed control.Meanwhile, present invention improves decoction in the deposition of target surface, diffusion and permeance property, further increase drug effect.

Description

A kind of cyhalofop-ethyl aqueous emulsion and preparation method thereof

technical field

The invention belongs to the technical field of herbicide preparation, and relates to a cyhalofop-ethyl aqueous emulsion and a preparation method thereof.

Background technique

Cyhalofop-ethyl is an aryloxyphenoxypropionic acid herbicide, which belongs to the selective herbicide for paddy fields. Undergraduate weeds. Cyhalofop-ethyl is a systemic conductive herbicide, which is absorbed by plant leaves and leaf sheaths, conducted by phloem, and accumulated in the meristem area of plants, inhibiting acetyl-CoA carboxylase (ACCase), stopping fatty acid synthesis, cell The growth and division of the plant cannot proceed normally, and finally leads to the death of the plant. Therefore, the effective deposition, diffusion and penetration of the liquid on the weed leaves is of great significance for the herbicidal effect of cyhalofop-ethyl.

The traditional processing formulations of cyhalofop-ethyl are emulsifiable concentrate, microemulsion and water-emulsion. Although the emulsifiable concentrate has certain advantages in the control effect, it uses aromatic solvents such as xylene, which is flammable and explosive, and the production cost is high. It is not only harmful to humans and animals. , pollute the environment, and are prone to phytotoxicity. The amount of emulsifier used in microemulsion is large, usually 1.5 to 2 times that of emulsifiable oil or water emulsion, and sometimes polar solvents such as DMF and methanol are used. From the perspective of production cost, control effect and environmental protection, the promotion and application of microemulsion exists. Certain difficulty. At present, the main processing formulation of cyhalofop-ethyl is a dispersible oil suspension concentrate, but this formulation uses an organic solvent (such as methyl oleate) as a dispersion medium, and there are few available dispersants, difficult processing, poor formulation stability and relatively low cost. higher disadvantages.

Water emulsion replaces all or most of the organic solvents with water, and its appearance is white milk. Compared with emulsifiable concentrate, it has the following advantages: (1) no or less toxic and flammable organic solvents are used, which reduces environmental pollution and greatly improves the safety of production, storage, transportation and use; (2) uses water as the medium to produce The cost is significantly reduced; (3) the toxicity to warm-blooded animals is significantly reduced, it is not easy to cause phytotoxicity to crops, and it has good miscibility with other pesticides and fertilizers, and there is no phenomenon such as fruit powder falling off after application; It has excellent deposition, diffusion and penetration properties on the surface of plant leaves or insects.

At present, the Chinese patent with the publication number of 101627758 discloses a cyhalofop-ester aqueous emulsion and its preparation method, which not only uses up to 20%-35% of aromatic hydrocarbon solvents such as toluene and xylene, but also alkylphenol polyoxygen The consumption of emulsifiers such as vinyl ether (APEO) is relatively large, and there is serious pollution problem; Publication No. is 101627758A Chinese patent discloses a kind of cyhalofop-ester aqueous emulsion and preparation method thereof, although this method has reduced product cost, Improve the efficacy, but use aromatic hydrocarbon solvents such as toluene and xylene, which have certain negative effects on the human body and the environment; the Chinese patent with the publication number 105454228A discloses a biodegradable cyhalofop-in-water emulsion and its The preparation method, however, uses a large amount of emulsifier, has a lot of ingredients, and is too complicated.

Contents of the invention

The purpose of the invention is to address the deficiencies in the preparation of existing herbicides, to propose a cyhalofop-ethyl aqueous emulsion and a preparation method thereof, and to prepare the cyhalofop-ethyl aqueous emulsion by using a low-energy emulsification method, which has simple processing and low production cost, and can Improving the use stability and weed control effect can improve the deposition, diffusion and penetration performance of the liquid medicine on the target surface, and further improve the efficacy of the medicine.

The technical solution of the present invention is: a cyhalofop-ethyl aqueous emulsion, which is characterized in that the cyhalofop-ethyl aqueous emulsion is composed of the following raw materials in mass proportions: cyhalofop-ethyl 6% to 12%, solvent 8% to 15%, emulsifier 6% to 15%, antifreeze 2% to 6%, and the balance is water.

Described solvent is mineral oil.

The antifreeze is a mixture of ethylene glycol and glycerol.

The emulsifier is styrylphenyl polyoxyethylene ether, tristyrylphenol polyoxyethylene polyoxypropylene ether, alkylaryl polyoxypropylene polyoxyethylene ether, castor oil polyoxyethylene ether, alkyl glycoside , alcohol ether glycoside, polyoxyethylene sorbitan fatty acid ester, fatty alcohol polyoxyethylene ether carboxylate, and a mixture of any two or more of calcium dodecylbenzenesulfonate.

A preparation method of cyhalofop-ethyl aqueous emulsion, is characterized in that, comprises the steps:

(1) Dissolve 6% to 12% of cyhalofop-ethyl technical material in 8% to 15% solvent, and stir until transparent by magnetic force;

(2) Add 6% to 15% emulsifier in the above steps, and continue to stir to form a uniform oil phase;

(3) Add 2% to 6% antifreeze to deionized water to form a water phase;

(4) Under the action of magnetic stirring, add the water phase to the oil phase drop by drop, and stir at a speed of 500-1500r/min for 10-30min to obtain the cyhalofop-in-water emulsion.

The beneficial effects of the present invention are: a kind of cyhalofop-ethyl water-emulsion and its preparation method provided by the present invention have reasonable components and clear preparation principle, and high-efficiency and environment-friendly water-emulsion is prepared by low-energy emulsification method, which simplifies the processing flow and reduces the Reduce production costs, improve product stability, and the effect of weed control. At the same time, the invention improves the deposition, diffusion and penetration properties of the medicinal liquid on the surface of the target (plant leaf or insect body surface), and further improves the medicinal effect.

Description of drawings

Fig. 1 is the emulsion stability diagram of the cyhalofop-ethyl aqueous emulsion prepared in the present invention.

Fig. 2 is a schematic diagram of the dynamic contact angle of the aqueous emulsion of cyhalofop-methyl prepared by the present invention on barnyard grass blades.

Fig. 3 is a measurement chart of the average particle diameter (0.5 μm) of the cyhalofop-ethyl aqueous emulsion sample prepared by the present invention.

Fig. 4 is a graph showing the control effect of different dosages of the cyhalofop-ester aqueous emulsion of the present invention on barnyard grass.

detailed description

The present invention will be further described below in conjunction with accompanying drawing:

A cyhalofop-ethyl aqueous emulsion, which is composed of the following raw materials in mass proportion: cyhalofop-ethyl 6%-12%, solvent 8%-15%, emulsifier 6%-15%, antifreeze 2% ~ 6%, the balance is water.

A cyhalofop-ester aqueous emulsion, the solvent is mineral oil; the antifreeze is a mixture of ethylene glycol and glycerol; the emulsifier is styrylphenyl polyoxyethylene ether, tristyrylphenol polyoxyethylene poly Oxypropylene ether, alkyl aryl polyoxypropylene polyoxyethylene ether, castor oil polyoxyethylene ether, alkyl glycoside, alcohol ether glycoside, polyoxyethylene sorbitan fatty acid ester, fatty alcohol polyoxyethylene ether carboxylic acid A mixture of any two or more of salt and calcium dodecylbenzenesulfonate.

A preparation method of cyhalofop-ethyl aqueous emulsion, comprising the steps of:

(1) Dissolve 6% to 12% of cyhalofop-ethyl technical material in 8% to 15% solvent, and stir until transparent by magnetic force;

(2) Add 6% to 15% emulsifier and continue to stir to form a uniform oil phase;

(3) Add 2% to 6% antifreeze to deionized water to form a water phase;

(4) Under the action of magnetic stirring, add the water phase to the oil phase drop by drop, and stir at a speed of 500-1500r/min for 10-30min to obtain the cyhalofop-in-water emulsion.

Example 1:

(1) Add 4g of cyhalofop-ethyl technical material into a beaker, add 4g of solvent to it, add 4g of emulsifier after fully dissolving, and fully stir to form a homogeneous oil phase;

(2) Under magnetic stirring, 25 g of water in which 3 g of glycerin was dissolved was added dropwise to the oil phase;

(3) After the dropwise addition of water was completed, magnetic stirring was maintained at 1200r/min for 20min to obtain 40g of cyhalofop-ester aqueous emulsion.

Example 2:

(1) Add 4g of cyhalofop-ethyl technical material into a beaker, add 3.2g of solvent to it, add 4g of emulsifier after fully dissolving, and fully stir to form a homogeneous oil phase;

(2) In the case of magnetic stirring, 25.8 g of water in which 3 g of glycerol was dissolved was added dropwise to the oil phase;

(3) After the dropwise addition of water was completed, magnetic stirring was maintained at 1200r/min for 20min to obtain 40g of cyhalofop-ester aqueous emulsion.

Example 3:

(1) Add 4g of cyhalofop-ethyl technical material into the beaker, add 6g of solvent to it, add 4g of emulsifier after fully dissolved, and fully stir to form a homogeneous oil phase;

(2) In the case of magnetic stirring, 21 g of water in which 3 g of glycerol was dissolved was added dropwise to the oil phase;

(3) After the dropwise addition of water was completed, magnetic stirring was maintained at 1200r/min for 15 minutes to obtain 40g of cyhalofop-ester aqueous emulsion.

Example 4:

(1) Add 4g of cyhalofop-ethyl technical material into a beaker, add 4g of solvent to it, add 2.4g of emulsifier after fully dissolved, and fully stir to form a homogeneous oil phase;

(2) In the case of magnetic stirring, 26.6 g of water in which 3 g of glycerol was dissolved was added dropwise to the oil phase;

(3) After the dropwise addition of water was completed, magnetic stirring was maintained at 1200r/min for 20min to obtain 40g of cyhalofop-ester aqueous emulsion.

Example 5:

(1) Add 4g of cyhalofop-ethyl technical material into a beaker, add 4g of solvent to it, add 3.2g of emulsifier after fully dissolving, and fully stir to form a homogeneous oil phase;

(2) In the case of magnetic stirring, 25.8 g of water in which 3 g of glycerol was dissolved was added dropwise to the oil phase;

(3) After the dropwise addition of water was completed, magnetic stirring was maintained at 1200r/min for 20min to obtain 40g of cyhalofop-ester aqueous emulsion.

Embodiment 6:

(1) Add 4g of cyhalofop-ethyl technical material into a beaker, add 4g of solvent to it, add 4.8g of emulsifier after fully dissolving, and fully stir to form a homogeneous oil phase;

(2) In the case of magnetic stirring, 24.2 g of water dissolved with 3 g of glycerin was added dropwise to the oil phase;

(3) After the dropwise addition of water was completed, magnetic stirring was maintained at 1200r/min for 20min to obtain 40g of cyhalofop-ester aqueous emulsion.

Embodiment 7:

(1) Add 2.4g of cyhalofop-ethyl technical material into a beaker, add 4g of solvent to it, add 4g of emulsifier after fully dissolving, and fully stir to form a homogeneous oil phase;

(2) In the case of magnetic stirring, 26.6 g of water in which 3 g of glycerol was dissolved was added dropwise to the oil phase;

(3) After the dropwise addition of water was completed, magnetic stirring was maintained at 1200r/min for 20min to obtain 40g of cyhalofop-ester aqueous emulsion.

Embodiment 8:

(1) Add 4.8g of cyhalofop-ethyl technical material into a beaker, add 4g of solvent to it, add 4g of emulsifier after fully dissolving, and fully stir to form a homogeneous oil phase;

(2) In the case of magnetic stirring, 24.2 g of water dissolved with 3 g of glycerin was added dropwise to the oil phase;

(3) After the dropwise addition of water was completed, magnetic stirring was maintained at 1200r/min for 20min to obtain 40g of cyhalofop-ester aqueous emulsion.

The products that above-mentioned 6 embodiments obtain carry out mean particle diameter and stability test, and the results are shown in Table 1:

Table 1 Average particle size and stability test results of cyhalofop-ethyl emulsion in water

Note:

(1) Emulsion stability CIPAC MT 36 (342 ppm standard hard water diluted 20 times qualified) GB/T 1603-2001 Determination of emulsion stability performance (342 ppm standard hard water diluted 200 times qualified).

(2) Heat storage stability: GB/T 19136-2003.

(3) Cold storage stability: GB/T 19137-2003.

(4) Determination method of persistent foaming property CIPAC Volume F MT 31.

The aqueous emulsion prepared by the present invention is used for the prevention and control of barnyardgrass in paddy fields, and the use effect is as shown in Figure 4 (wherein: CK is a contrast; a sample 60g/mu; b sample 80g/mu; c sample 100g/mu; d contrast Medicine 60g/mu; e contrast medicine 80g/mu; f contrast medicine 100g/mu), test result is as shown in table 2 below:

Table 2 Effects of different dosages of cyhalofop-ester water emulsion on control of barnyardgrass in paddy fields

As can be drawn from Table 2, the control effect of cyhalofop-ethyl water-emulsion of the present invention on barnyard grass is better than that of the contrast agent, showing that the cyhalofop-ethyl water-emulsion of the present invention can significantly improve the control effect; The standard error of the ester-in-water emulsion is less than that of the control agent, indicating that the cyhalofop-in-water emulsion of the present invention can significantly improve the stability of the product.

Claims (5)

1. a kind of aqueous cyhalofop-butyl emulsion, it is characterised in that the aqueous cyhalofop-butyl emulsion by following mass ratio raw material group Into：Cyhalofop-butyl 6%~12%, solvent 8%~15%, emulsifying agent 6%~15%, antifreezing agent 2%~6%, surplus is water.

2. a kind of aqueous cyhalofop-butyl emulsion according to claim 1, it is characterised in that：Described solvent is mineral oil.

3. a kind of aqueous cyhalofop-butyl emulsion according to claim 1, it is characterised in that：Described antifreezing agent be ethylene glycol, The mixture of glycerine composition.

4. a kind of aqueous cyhalofop-butyl emulsion according to claim 1, it is characterised in that：Described emulsifying agent is styryl Phenyl APEO, triphenyl vinyl phenol polyoxyethylene poly-oxygen propylene aether, alkylaryl polyoxyethylene polyoxypropylene ether again, castor Sesame oil APEO, APG, alcohol ether glucoside, polyoxyethylene sorbitan fatty acid ester, AEO The mixture of two or more any compositions in carboxylate, calcium dodecyl benzene sulfonate.

5. a kind of preparation method of aqueous cyhalofop-butyl emulsion as claimed in claim 1, it is characterised in that comprise the following steps：

(1) 6%~12% cyhalofop-butyl active compound is dissolved in 8%~15% solvent, through magnetic agitation to transparent；

(2) 6%~15% emulsifying agent is added in step (1), continues to stir composition homogeneous oil phase；

(3) 2%~6% antifreezing agent is added in deionized water, constitutes aqueous phase；

(4) under magnetic agitation effect, oil phase is added dropwise in aqueous phase, 10~30min is stirred with 500~1500r/min rotating speeds, Produce aqueous cyhalofop-butyl emulsion.