Chlorpyrifos emulsion and its preparation method and application

Abstract

The present application provides chlorpyrifos emulsifiable concentrate, characterized in that the preparation raw materials comprise: chlorpyrifos, emulsifier, solvent; wherein the mass percentage of chlorpyrifos is 40-60%. The present application adjusts the solvent formula as a whole, and the application of chlorpyrifos emulsifiable concentrate on rice replaces the traditional aromatic hydrocarbon solvent; the appropriate emulsifier is selected to play a synergistic effect with the plant solvent, thereby improving the use effect of chlorpyrifos emulsifiable concentrate. The formula provided by the present application is safe and environmentally friendly, simple in process, and low in cost.

Description

Technical Field

[0001] This invention relates to the field of pesticide technology, and in particular to chlorpyrifos emulsifiable concentrate, its preparation method, and its application. Background Technology

[0002] Chlorpyrifos is a highly effective, broad-spectrum organophosphate insecticide, primarily used to control rice planthoppers on rice, fruit trees, and wheat. Chlorpyrifos is a highly effective, low-residue, moderately toxic insecticide with contact, stomach poison, and other triple-action mechanisms. It also possesses penetrability and a short residual time on leaves. Its main metabolite, 3,5,6-trichloro-2-pyridinephenol (TCP), has strong penetrability, rapidly seeping into groundwater and surface water, causing widespread and serious pollution to aquatic environments and soil. Studies have shown that TCP accumulation inhibits microorganisms in the environment, suppressing not only their own growth and reproduction but also their degradation of TCP.

[0003] The United States, European countries and other regions have introduced regulations prohibiting the use of organic solvents such as toluene and xylene in pesticide formulations. Subsequently, Taiwan has implemented limits on the use of various organic solvents in pesticide products, such as xylene, aniline and benzene. For example, the content of xylene and cyclohexanone in finished pesticide products cannot exceed 10%, dimethylformamide and methanol should be less than 30%, and the content of ethylbenzene cannot exceed 2%.

[0004] Therefore, for systems that require the use of organic solvents, adopting green solvents to partially eliminate toxic and harmful organic solvents is a future societal development requirement. Summary of the Invention

[0005] The purpose of this invention is to provide chlorpyrifos emulsifiable concentrate, the raw materials for which include chlorpyrifos, emulsifier, and solvent; wherein the mass percentage of chlorpyrifos is 40-60%.

[0006] In a preferred embodiment, the chlorpyrifos contains 40-50% by weight.

[0007] More preferably, the emulsifier is a nonionic surfactant and / or an ionic surfactant.

[0008] More preferably, the emulsifier comprises a block polyether ionic surfactant containing alkylphenols and an ionic surfactant containing phenols.

[0009] More preferably, the emulsifier comprises emulsifiers from the Solvay Geronol series of products.

[0010] More preferably, the solvent comprises a vegetable oil solvent.

[0011] More preferably, the vegetable oil solvent is selected from one or more of castor oil, palm oil, and rosin-based vegetable oil.

[0012] More preferably, the solvent comprises xylene.

[0013] Secondly, a method for preparing the chlorpyrifos emulsifiable concentrate comprises the following steps: weighing each component according to the ratio, mixing them evenly, and then homogenizing them in a high-speed shearing machine to obtain the chlorpyrifos emulsifiable concentrate.

[0014] Thirdly, the application of the chlorpyrifos emulsifiable concentrate in the control of rice planthoppers.

[0015] By adopting the above technical solution, the present invention has the following beneficial effects:

[0016] 1) The overall solvent formulation was adjusted, and the application of chlorpyrifos emulsifiable concentrate on rice replaced traditional aromatic solvents;

[0017] 2) Selecting appropriate emulsifiers and plant solvents to complement each other can enhance the effectiveness of chlorpyrifos emulsifiable concentrate.

[0018] 3) The formula provided by this invention is safe and environmentally friendly, with a simple process and low cost. Detailed Implementation

[0019] The technical solution of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0020] This invention provides chlorpyrifos emulsifiable concentrate, the raw materials for which are prepared include: chlorpyrifos, emulsifier, and solvent; wherein the mass percentage of chlorpyrifos is 40-60%.

[0021] Chlorpyrifos

[0022] Chlorpyrifos, also known as chlorpyrifos or chlorpyrifos thiophosphate, has the chemical name O,O-diethyl-O-(3,5,6-trichloro-2-pyridyl)thiophosphate; its molecular formula is C9H. 11 C l3 NO3PS is a white crystalline substance with a slight thiol odor. It is a non-systemic broad-spectrum insecticide and acaricide with high volatility in the soil.

[0023] In a preferred embodiment of the present invention, the mass percentage of chlorpyrifos is 40-50%; more preferably 44%.

[0024] emulsifier

[0025] Emulsifiers are substances that enable the formation of stable emulsions from mixtures of two or more immiscible components. Their working principle is that during emulsification, the dispersed phase is dispersed in the continuous phase in the form of microdroplets (micrometer-scale). The emulsifier reduces the interfacial tension of the components in the mixture and forms a relatively robust film on the surface of the microdroplets, or an electric double layer on the surface of the microdroplets due to the charge provided by the emulsifier, preventing the microdroplets from agglomerating and maintaining a homogeneous emulsion.

[0026] Preferably, the emulsifier is a nonionic surfactant and / or an ionic surfactant.

[0027] More preferably, the emulsifier comprises a block polyether ionic surfactant containing alkylphenols and an ionic surfactant containing phenols.

[0028] More preferably, the emulsifier comprises emulsifiers from the Solvay Geronol series of products.

[0029] In this invention, the emulsifier is a mixture of Solvay surfactant Geronol Ff / 4-E, Solvay surfactant Soprophor S-40 / 70, calcium dodecylbenzenesulfonate, and alkylphenol formaldehyde resin polyoxyethylene ether (agricultural emulsion 700), with a specific mass ratio of 1:0.2:0.5:1.

[0030] solvent

[0031] The solvents described in this invention include vegetable oil solvents and xylene.

[0032] More preferably, the vegetable oil solvent is selected from one or more of castor oil, palm oil, and rosin-based vegetable oil.

[0033] The solvent used in this invention is a mixture of castor oil, rosin-based vegetable oil and xylene, and the ratio of castor oil, rosin-based vegetable oil DN60 and xylene is 0.1:8:0.9.

[0034] Secondly, a method for preparing the chlorpyrifos emulsifiable concentrate comprises the following steps: weighing each component according to the ratio, mixing them evenly, and then homogenizing them in a high-speed shearing machine to obtain the chlorpyrifos emulsifiable concentrate.

[0035] Thirdly, the application of the chlorpyrifos emulsifiable concentrate in the control of rice planthoppers.

[0036] The present invention will be further explained below with reference to specific embodiments.

[0037] Example 1

[0038] This embodiment provides chlorpyrifos emulsifiable concentrate, the raw materials for which, by weight, are: chlorpyrifos 44%, emulsifier 10%, solvent balance;

[0039] The emulsifier is a mixture of Solvay surfactant Geronol Ff / 4-E, Solvay surfactant Soprophor S-40 / 70, calcium dodecylbenzene sulfonate, and alkylphenol formaldehyde resin polyoxyethylene ether (agricultural emulsion 700), with a specific mass ratio of 1:0.2:0.5:1.

[0040] The solvent is a mixture of castor oil, rosin-based vegetable oil and xylene, and the ratio of castor oil, rosin-based vegetable oil DN60 and xylene is 0.1:8:0.9.

[0041] A method for preparing the chlorpyrifos emulsifiable concentrate comprises the following steps: weighing each component according to the formula, mixing them evenly, and then homogenizing them in a high-speed shear mixer to obtain the chlorpyrifos emulsifiable concentrate.

[0042] Example 2

[0043] This embodiment provides chlorpyrifos emulsifiable concentrate, the raw materials for which, by weight, are: chlorpyrifos 44%, emulsifier 10%, solvent balance;

[0044] The emulsifier is a mixture of Solvay surfactant Geronol Ff / 4-E, calcium dodecylbenzene sulfonate, and alkylphenol formaldehyde resin polyoxyethylene ether (agricultural emulsion 700), with a specific mass ratio of 1:0.5:1.

[0045] The solvent is a mixture of castor oil, rosin-based vegetable oil and xylene, and the ratio of castor oil, rosin-based vegetable oil DN60 and xylene is 0.1:8:0.9.

[0046] A method for preparing the chlorpyrifos emulsifiable concentrate comprises the following steps: weighing each component according to the formula, mixing them evenly, and then homogenizing them in a high-speed shear mixer to obtain the chlorpyrifos emulsifiable concentrate.

[0047] Example 3

[0048] This embodiment provides chlorpyrifos emulsifiable concentrate, the raw materials for which, by weight, are: chlorpyrifos 44%, emulsifier 10%, solvent balance;

[0049] The emulsifier is a mixture of Solvay surfactant Soprophor S-40 / 70, calcium dodecylbenzene sulfonate, and alkylphenol formaldehyde resin polyoxyethylene ether (agricultural emulsion 700), with a specific mass ratio of 0.2:0.5:1.

[0050] The solvent is a mixture of castor oil, rosin-based vegetable oil and xylene, and the ratio of castor oil, rosin-based vegetable oil DN60 and xylene is 0.1:8:0.9.

[0051] A method for preparing the chlorpyrifos emulsifiable concentrate comprises the following steps: weighing each component according to the formula, mixing them evenly, and then homogenizing them in a high-speed shear mixer to obtain the chlorpyrifos emulsifiable concentrate.

[0052] Example 4

[0053] This embodiment provides chlorpyrifos emulsifiable concentrate, the raw materials for which, by weight, are: chlorpyrifos 44%, emulsifier 10%, solvent balance;

[0054] The emulsifier is a mixture of Solvay surfactant Geronol Ff / 4-E, Solvay surfactant Soprophor S-40 / 70, calcium dodecylbenzene sulfonate, and alkylphenol formaldehyde resin polyoxyethylene ether (agricultural emulsion 700), with a specific mass ratio of 1:0.2:0.5:1.

[0055] The solvent is a mixture of rosin-based vegetable oil and xylene, and the ratio of rosin-based vegetable oil DN60 to xylene is 8:0.9.

[0056] A method for preparing the chlorpyrifos emulsifiable concentrate comprises the following steps: weighing each component according to the formula, mixing them evenly, and then homogenizing them in a high-speed shear mixer to obtain the chlorpyrifos emulsifiable concentrate.

[0057] Example 5

[0058] This embodiment provides chlorpyrifos emulsifiable concentrate, the raw materials for which, by weight, are: chlorpyrifos 44%, emulsifier 10%, solvent balance;

[0059] The emulsifier is a mixture of Solvay surfactant Geronol Ff / 4-E, Solvay surfactant Soprophor S-40 / 70, calcium dodecylbenzene sulfonate, and alkylphenol formaldehyde resin polyoxyethylene ether (agricultural emulsion 700), with a specific mass ratio of 1:0.2:0.5:1.

[0060] The solvent is a mixture of castor oil and xylene, and the ratio of castor oil to xylene is 0.1:8.9.

[0061] A method for preparing the chlorpyrifos emulsifiable concentrate comprises the following steps: weighing each component according to the formula, mixing them evenly, and then homogenizing them in a high-speed shear mixer to obtain the chlorpyrifos emulsifiable concentrate.

[0062] Example 6

[0063] This embodiment provides chlorpyrifos emulsifiable concentrate, the raw materials for which, by weight, are: chlorpyrifos 44%, emulsifier 10%, solvent balance;

[0064] The emulsifier is a mixture of Solvay surfactant Geronol Ff / 4-E, Solvay surfactant Soprophor S-40 / 70, calcium dodecylbenzene sulfonate, and alkylphenol formaldehyde resin polyoxyethylene ether (agricultural emulsion 700), with a specific mass ratio of 1:0.2:0.5:1.

[0065] The solvent is a mixture of palm oil, rosin-based vegetable oil and xylene, and the ratio of palm oil, rosin-based vegetable oil DN60 and xylene is 0.1:8:0.9.

[0066] A method for preparing the chlorpyrifos emulsifiable concentrate comprises the following steps: weighing each component according to the formula, mixing them evenly, and then homogenizing them in a high-speed shear mixer to obtain the chlorpyrifos emulsifiable concentrate.

[0067] Example 7

[0068] This embodiment provides chlorpyrifos emulsifiable concentrate, the raw materials for which, by weight, are: chlorpyrifos 44%, emulsifier 10%, solvent balance;

[0069] The emulsifier is a mixture of Solvay surfactant Geronol Ff / 4-E, calcium dodecylbenzene sulfonate, and alkylphenol formaldehyde resin polyoxyethylene ether (agricultural emulsion 700), with a specific mass ratio of 1:0.5:1.

[0070] The solvent is a mixture of rosin-based vegetable oil and xylene, and the ratio of rosin-based vegetable oil DN60 to xylene is 8:0.9.

[0071] A method for preparing the chlorpyrifos emulsifiable concentrate comprises the following steps: weighing each component according to the formula, mixing them evenly, and then homogenizing them in a high-speed shear mixer to obtain the chlorpyrifos emulsifiable concentrate.

[0072] Performance testing

[0073] Test 1: Emulsion stability test: Dilute with standard hard water 200 times and conduct the test according to the method specified in GB / T 1603-2001 to check the stability;

[0074] Test 2: Low temperature stability test: Conducted according to GB / T19137-2003, stored at 0±2℃ for 7 days, centrifuged for 15 min, and the volume of the precipitate at the bottom of the tube was recorded (accurate to 0.05 ml). The volume of the precipitate not exceeding 0.3 ml is considered qualified.

[0075] Test 3: Conducted according to section 2.1 of GB / T 19136-2003, stored at 54±2℃ for 14 days, and then judged as qualified.

[0076] Test 4: Conducted according to the Karl Fischer method in GB / T 1600-2001.

[0077] Test 5: Content in Soil

[0078] The sample was dissolved in acetone, and n-octadecane was used as an internal standard. Gas chromatography was employed to separate and test the chlorpyrifos in the sample using a stainless steel column packed with 5% OV-1 / Chromosorb W-HP and a flame ionization detector. (The specific soil samples were randomly collected 14 days after the field efficacy test.) The maximum value obtained in Examples 1-7 was used as the relative value 1, and the remaining values ​​were divided by the maximum value multiplied by 100% to obtain the relative percentage.

[0079] Test TCP using the same method.

[0080]

[0081] Test 5: Field efficacy test

[0082] Demonstration Site: No. 8 Brigade, Chahe Town, Rudong County, Jiangsu Province

[0083] Soil data: The soil type of the experimental site is brown clay, with an organic matter content of 1.8% and a pH value of 7.2. The soil fertility is moderate, the irrigation and drainage conditions are good, and the previous crop was wheat.

[0084] Weather conditions at the time of application: July 29, sunny, southeast wind level 2, average temperature 28.0℃, highest temperature 35.6℃, lowest temperature 25.0℃. It did not rain for 7 days after application, rained on the 8th day, and did not rain for the next 14 days.

[0085] Application method: Apply a single, even spray to the entire rice plant. Apply both during and after application.

[0086] Maintain a 3-5cm water layer in the field and irrigate slowly after the water has dried naturally.

[0087] Insect population reduction rate = (Number of insects before application - Number of insects after application) / Number of insects before application * 100%

[0088] Prevention and control effect = (PT - CK) / (100 - CK) * 100%

[0089] Where: CK - insect population reduction rate in the blank control area, PT - insect population reduction rate in the pesticide-treated area

[0090] The treatment dose was 65 ml / mu, the area was 2 hectares, and the CK area was sprayed with clean water.

[0091] Based on performance tests 1-4, field efficacy tests were conducted, and some data are as follows.

[0092]

[0093] Therefore, it can be seen that the present invention uses a specific solvent and emulsifier, which can not only improve the stability and emulsification of the product, but also reduce its permeability to soil. At the same time, the inventors found that although the Solvay surfactant Geronol Ff / 4-E has a good effect, its emulsification performance is poor. Adding a solvent that is easier to emulsify and an emulsifier of a different system to the system can improve the overall stability of the system.

[0094] Example 1: Conventional

[0095] Example 2: The emulsifier does not contain Solvay surfactant Soprophor S-40 / 70

[0096] Example 3: The emulsifier does not contain Solvay surfactant Geronol Ff / 4-E

[0097] Example 4: The solvent does not contain castor oil.

[0098] Example 5: Solvent does not contain rosin-based vegetable oil DN60 (replacing it with xylene yields similar results)

[0099] Example 6: Castor oil replaced with palm oil

[0100] Example 7: The emulsifier does not contain Solvay surfactant Soprophor S-40 / 70 and castor oil.

[0101] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. Chlorpyrifos emulsifiable concentrate, characterized in that, Its raw materials include: 44% chlorpyrifos, 10% emulsifier, and the remainder solvent; The emulsifier is a mixture of Solvay surfactant Geronol Ff / 4-E, Solvay surfactant Soprophor S-40 / 70, calcium dodecylbenzene sulfonate, and alkylphenol formaldehyde resin polyoxyethylene ether, with a specific mass ratio of 1:0.2:0.5:

1. The solvent is a mixture of castor oil, rosin-based vegetable oil and xylene, and the ratio of castor oil, rosin-based vegetable oil DN60 and xylene is 0.1:8:0.

9.

2. A method for preparing the chlorpyrifos emulsifiable concentrate according to claim 1, characterized in that, The steps are as follows: Weigh each component according to the ratio, mix them evenly, and then homogenize them in a high-speed shearing machine to obtain the chlorpyrifos emulsifiable concentrate.

3. The application of the chlorpyrifos emulsifiable concentrate according to claim 1 in the control of rice planthoppers.

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