CN102428917A - Acetochlor nanoemulsion and preparation method thereof - Google Patents

Abstract

The invention discloses an acetochlor nanoemulsion and a preparation method thereof. Under the condition of constant temperature, the amount of water in the mixture of emulsifier and acetochlor is increased to promote the emulsion to invert the phase, so that the nano-scale pesticide emulsion provided by the invention is obtained, and the components of the acetochlor nanoemulsion and the weight percentage content of each component are as follows: 5.0 to 40 percent of acetochlor, 3.0 to 30 percent of emulsifier, 0.5 to 10 percent of antifreeze, 0 to 5 percent of pH regulator and the balance of water. The invention eliminates environmental pollution caused by a large amount of solvent in conventional emulsion preparations, moreover, compared with microemulsion, the emulsion is more stable and has higher permeating capability because of the nano-scale grain size, meanwhile, the dosage of the emulsifier and the polar solvent is greatly reduced, consequently, the cost is saved, and the acetochlor nanoemulsion is more compatible with the environment.

Description

Acetochlor nanoemulsion and preparation method thereof

Technical field

The present invention relates to pesticide field, particularly relate to a kind of non-water-soluble liquid pesticidal preparations, specifically is a kind of Acetochlor nanoemulsion and preparation method thereof.

Background technology

Acetochlor chemistry 2-ethyl-6 methyl--N-ethoxyl methyl-alpha-chloro acetanil by name.Chemical structural formula is as follows:

Acetochlor is a kind of weed killer herbicide of extensive use.Being succeeded in developing in 1971 by U.S. Monsanto Company, is one of most important in the world weed killer herbicide kind at present, also is the maximum a kind of weed killer herbicide of present China usage amount.Main hypocotyl through monocotyledonous coleoptile or dicotyledon absorbs, and absorbs upwards conduction of back, and cell growth inhibiting stops weeds young shoot, young root growth through impede protein matter is synthetic, and then dead.Acetochlor as bud before processing soil treatment agent grassy weed is had the better prevention effect.Present stage, main formulation was 50%, 90% cream preparation, also relevant for the relevant report of microemulsion, aqueous emulsion.

Cream preparation preparation is simple, drug effect is high, in the preparation market of China still in occupation of suitable share.Organic solvent not only causes the waste of petroleum resources; Increase production cost; And environment had pollution, and operator there is harm, the missible oil that contains aromatic hydrocarbon solvent in some countries is limited the use of or is forbidden; Thereby impelled the continual renovation and the development of the formulations of pesticide, wherein Water-borne modification is exactly one of dominant direction of formulations of pesticide development.

Nanoemulsion (Nanoemulsion) is a kind of emerging formulation, and particle diameter is between the 20-500 nm, and is suitable with microemulsion.Though nanoemulsion belongs to a kind of thermodynamic unstable system, because its nano level particle diameter makes the emulsion ageing stability increase greatly.Nanoemulsion has not only been avoided the use of a large amount of organic solvents in the cream preparation, and has reduced the use of microemulsion Semi-polarity cosolvent.In the concrete preparation, nanoemulsion mainly utilizes low-energy emulsification method (Low-energy emulsification methods), through changing temperature or changing recipe ingredient the spontaneous curvature of surfactant is changed, and then impels the phase inversion of emulsion to make.Not only processing technology is simple, good stability, and be a kind of novel form of environmental protection.Up to the present, do not see the correlative study report of Acetochlor nanoemulsion and preparation method thereof as yet.

Summary of the invention

The purpose of this invention is to provide a kind of Acetochlor nanoemulsion and preparation method thereof; Its technology path is to adopt low-energy emulsification to prepare the method for nano level pesticide emulsion; Under constant temperature; Through the increase gradually of the water yield in Acetochlor, the agent mixture, impel emulsion generation phase inversion, thereby obtain Acetochlor nano level pesticide emulsion.

Acetochlor nanoemulsion of the present invention, the quality percentage composition of its component and each component is following:

Acetochlor 5.0%～40%

Emulsifier 3.0%～30%

Antifreezing agent 0.5～10%

PH regulator agent 0～5%

Water surplus

Described emulsifier is alkylbenzenesulfonate, aliphatic alcohol sulfate, APES, phenethyl phenyl polyoxyethyl propyl ether, alkyl phenyl phenol polyethenoxy ether, alkylphenol-polyethenoxy polyethenoxy ether, alkyl phenyl phenol polyethenoxy polyethenoxy ether, castor oil polyoxyethylene ether, alkylphenol-formaldehyde resin polyoxy ethyl ether, bitter edible plant sulfonic acid and formaldehyde, 1,2-di-n-butyl naphthalene-6-sodium sulfonate, to the mixture of a kind of or any several kinds of arbitrary proportions in methoxyl group fatty acyl amido benzene sulfonic acid sodium salt, lignosulfonates, carboxymethyl cellulose salt class, alkylsulfonate (calcium dodecyl benzene sulfonate), aliphatic alcohol sulfate, alkyl sulfate (lauryl sodium sulfate), oleate, dioctyl sulfosuccinate, dibutyl naphthalene sulfonate or the peregal;

Described antifreezing agent is the mixture of a kind of or any several kinds of arbitrary proportions in ethylene glycol, propane diols, glycerine, urea, diethylene glycol (DEG), triethylene glycol or the polyethylene glycol;

Described pH regulator agent is the mixture of a kind of or any several kinds of arbitrary proportions in sodium dihydrogen phosphate, sodium hydrogen phosphate, sodium citrate, phosphoric acid or the citric acid.

The preparation method of Acetochlor nanoemulsion of the present invention, realize through following steps successively:

(1) by said quality percentage composition emulsifier and Acetochlor are mixed, obtain oil phase;

(2) by said quality percentage composition antifreezing agent and pH regulator agent are added in the entry, dissolving obtains water fully:

(3) water is added drop-wise in the oil phase, at the uniform velocity stirs 2～10 min, obtain transparent or semitransparent Acetochlor nanoemulsion.

Advantage of the present invention is:

The Acetochlor nanoemulsion particle diameter that the present invention makes is at 20～500 nm; Not only eliminated in traditional cream preparation high amounts of solvents to the pollution of environment; Simultaneously, make that with the similar nanoscale particle diameter of microemulsion emulsion is stable more, infiltration capacity is stronger, avoided the use of organic solvent and polar latent solvent simultaneously; Not only provide cost savings, and further increased the compatibility with environment.

Embodiment

Below in conjunction with concrete embodiment Acetochlor nanoemulsion provided by the present invention and preparation method thereof is described; Described embodiment is in order to explain the present invention better; Rather than to the restriction of claim protection domain of the present invention; All all belong to the present invention and ask for protection scope based on the modification and the change of basic thought of the present invention.

Embodiment 1

1) 0.6 g phenethyl phenyl polyoxyethyl propyl ether (1600#) and 1 g acetochlor tc are mixed, obtain oil phase;

2) 0.1 g ethylene glycol is joined in the 18.3 g water, dissolving obtains water fully;

3) water is added drop-wise in the oil phase, at the uniform velocity stirs 2 min, obtain transparent Acetochlor nanoemulsion.

The Acetochlor nanoemulsion that said method makes is separated out through 0～4 ℃ of cold storage two no crystallization of week, and 54 ± 2 ℃ of heat storages still presented pellucidity at two weeks, and resolution ratio is 0.8%; After the emulsion dilution, present light blue fluorescence, stability of emulsion is better.

Embodiment 2

1) 20 g alkylphenol-formaldehyde resin polyoxy ethyl ethers (700#) and the acetochlor tc of 10 g calcium dodecyl benzene sulfonates (500#) with 40 g are mixed, obtain oil phase;

2) 5 g glycerine, 1 g sodium hydrogen phosphate, 0.8 g sodium dihydrogen phosphate are joined in the 123 g water, dissolving obtains water fully;

3) water is added drop-wise in the oil phase, at the uniform velocity stirs 3 min, obtain the nanoemulsion of transparent Acetochlor.

The Acetochlor nanometer formulation of method for preparing is separated out through 0～4 ℃ of cold storage two no crystallization of week, and 54 ± 2 ℃ of heat still present pellucidity after two weeks of storage, and resolution ratio is 0.3%; After the emulsion dilution, present light blue fluorescence, stability of emulsion is better.

Embodiment 3

1) 200 g castor oil polyoxyethylene ethers (EL-40), 150 g lauryl sodium sulfate are mixed with 500 g acetochlor tcs, obtain oil phase;

2) 80 g urea, 25 g sodium hydrogen phosphates, 10g citric acid are joined in the 1040 g water, dissolving obtains water fully;

3) water is added drop-wise in the oil phase, at the uniform velocity stirs 5 min, obtain the nanoemulsion of transparent or semitransparent Acetochlor.

The Acetochlor nanometer formulation of method for preparing is separated out through 0～4 ℃ of cold storage two no crystallization of week, and 54 ± 2 ℃ of heat storages still presented transparent or semitransparent state at two weeks, and resolution ratio is 0.4%; After the emulsion dilution, present light blue fluorescence, stability of emulsion is better.

Embodiment 4

1) 0.4 g alkylphenol-polyethenoxy polyethenoxy ether is mixed with 0.6 g acetochlor tc, obtain oil phase;

2) 0.02 g diethylene glycol (DEG), 0.02 g polyethylene glycol, 0.04 g sodium hydrogen phosphate, 0.01 g phosphoric acid are joined in the 0.91 g water, dissolving obtains water fully;

3) water is added drop-wise in the oil phase, at the uniform velocity stirs 7 min, obtain transparent or semitransparent nanoemulsion.

The Acetochlor nanometer formulation of method for preparing is separated out through 0～4 ℃ of cold storage two no crystallization of week, and 54 ± 2 ℃ of heat storages still presented pellucidity at two weeks, and resolution ratio is 0.5%; After the emulsion dilution, present light blue fluorescence, stability of emulsion is better.

Embodiment 5

1) 0.5 g alkyl phenyl phenol polyethenoxy polyethenoxy ether is mixed with 0.7 g acetochlor tc, obtain oil phase;

2) 0.05 g polyethylene glycol, 0.05 g ethylene glycol, 0.05 g sodium citrate, 0.02 g phosphoric acid are joined in the 0.63 g water, dissolving obtains water fully;

3) water is added drop-wise in the oil phase, at the uniform velocity stirs 9 min, obtain transparent or semitransparent nanoemulsion.

The Acetochlor nanometer formulation of method for preparing is separated out through 0～4 ℃ of cold storage two no crystallization of week, and 54 ± 2 ℃ of heat storages still presented pellucidity at two weeks, and resolution ratio is 0.2%; After the emulsion dilution, present light blue fluorescence, stability of emulsion is better.

Embodiment 6

1) with 0.40 g alkylphenol-polyethenoxy polyethenoxy ether, 0.2 g 1,2-di-n-butyl naphthalene-6-sodium sulfonate and 0.8 g acetochlor tc mix, and obtain oil phase;

2) 0.10 g triethylene glycol, 0.05g urea, 0.07 g sodium citrate, 0.03 g citric acid are joined in the 0.35 g water, dissolving obtains water fully;

3) water is added drop-wise in the oil phase, at the uniform velocity stirs 10 min, obtain transparent or semitransparent nanoemulsion.

The Acetochlor nanometer formulation of method for preparing is separated out through 0～4 ℃ of cold storage two no crystallization of week, and 54 ± 2 ℃ of heat storages still presented pellucidity at two weeks, and resolution ratio is 0.6%; After the emulsion dilution, present light blue fluorescence, stability of emulsion is better.

Claims (3)

1. an Acetochlor nanoemulsion is characterized in that, the quality percentage composition of its component and each component is following:

Acetochlor 5.0%～40%

Emulsifier 3.0%～30%

Antifreezing agent 0.5～10%

PH regulator agent 0～5%

Water surplus.

2. Acetochlor nanoemulsion according to claim 1; It is characterized in that; Described emulsifier is alkylbenzenesulfonate, aliphatic alcohol sulfate, APES, phenethyl phenyl polyoxyethyl propyl ether, alkyl phenyl phenol polyethenoxy ether, alkylphenol-polyethenoxy polyethenoxy ether, alkyl phenyl phenol polyethenoxy polyethenoxy ether, castor oil polyoxyethylene ether, alkylphenol-formaldehyde resin polyoxy ethyl ether, bitter edible plant sulfonic acid and formaldehyde, 1,2-di-n-butyl naphthalene-6-sodium sulfonate, to the mixture of a kind of or any several kinds of arbitrary proportions in methoxyl group fatty acyl amido benzene sulfonic acid sodium salt, lignosulfonates, carboxymethyl cellulose salt class, alkylsulfonate (calcium dodecyl benzene sulfonate), aliphatic alcohol sulfate, alkyl sulfate (lauryl sodium sulfate), oleate, dioctyl sulfosuccinate, dibutyl naphthalene sulfonate or the peregal;

Described antifreezing agent is the mixture of a kind of or any several kinds of arbitrary proportions in ethylene glycol, propane diols, glycerine, urea, diethylene glycol (DEG), triethylene glycol or the polyethylene glycol;

Described pH regulator agent is the mixture of a kind of or any several kinds of arbitrary proportions in sodium dihydrogen phosphate, sodium hydrogen phosphate, sodium citrate, phosphoric acid or the citric acid.

3. the preparation method of the described Acetochlor nanoemulsion of claim 1 is characterized in that, realizes through following steps successively:

(1) by said quality percentage composition emulsifier and Acetochlor are mixed, obtain oil phase;

(2) by said quality percentage composition antifreezing agent and pH regulator agent are added in the entry, dissolving obtains water fully:

(3) water is added drop-wise in the oil phase, at the uniform velocity stirs 2～10 min, obtain transparent or semitransparent Acetochlor nanoemulsion.