A special adjuvant for pesticide aqueous suspension and a preparation method thereof

By using a combination of phosphate surfactants and triethanolamine, a special additive for pesticide aqueous suspension with high fluidity, high dispersibility and high stability is prepared. This solves the problems of precipitation, stratification and paste formation of pesticide aqueous suspension during storage, achieves efficient dispersion and stability of pesticide aqueous suspension, and is suitable for large-scale industrial production.

CN116076490BActive Publication Date: 2025-10-10SHANDONG TIANDAO NEW MATERIALS CO LTD
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Patent Information

Application Number
CN202211049986.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-08-30
Publication Date
2025-10-10
Estimated Expiration
2042-08-30

AI Technical Summary

Technical Problem

Existing pesticide aqueous suspensions suffer from unstable dispersants, leading to problems such as precipitation, stratification, paste formation, and even solidification during storage. Furthermore, the preparation process is complex, making it unsuitable for large-scale industrial production.

Method used

A special adjuvant for pesticide aqueous suspension with high fluidity, high dispersibility and high stability is prepared by combining phosphate surfactant, triethanolamine and ethylene glycol with a controlled mass ratio of (8-12): (55-65), thereby enhancing the wetting ability and adhesion.

Benefits of technology

The dispersion and stability of the pesticide aqueous suspension are significantly improved, the storage time is prolonged, and it is easy to produce on a large scale industrially at a low cost.

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Abstract

The application relates to the field of A01N25 / 30, in particular to a pesticide water suspending agent special additive and a preparation method thereof, which adopts 50-70 parts of a phosphate ester salt type surfactant, 5-15 parts of an alcohol amine compound, and 25-35 parts of an alcohol solvent, provides a pesticide water suspending agent special additive with high flowability, high dispersibility and high stability, can be directly added into a pesticide water suspending agent, has good compatibility, is practically applied to the pesticide water suspending agent, significantly improves the dispersibility and stability of the pesticide water suspending agent system, helps to enhance the pesticide wetting capacity and adhesion, makes pesticide droplets easy to spread and adhere on a leaf surface, and improves pesticide durability; solves the problems that the existing pesticide water suspending agent system is unstable in dispersing agents, causes precipitation, stratification, creaming and even solidification in the storage process, the method is simple, the cost is low, large-scale industrial production can be easily carried out, and the application has high practical application value.
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Description

Technical Field

[0001] The present invention relates to the field of A01N25 / 30, and in particular to a special adjuvant for pesticide aqueous suspension and a preparation method thereof. Background Art

[0002] Pesticides are the guarantee of agricultural production and harvest, and can prevent plants from or reduce the damage caused by pests such as diseases, insects, and weeds. Pesticide research and development is changing rapidly, but many high-performance pesticide technicals on the market are difficult to dissolve in water, which greatly limits the efficiency of pesticide use.

[0003] Pesticide aqueous suspensions use water as a solvent, and the active ingredient (TP) accounts for a large proportion, which helps improve the utilization efficiency of the active ingredient. Chinese patent CN110506737B discloses a method for preparing a pesticide suspension concentrate and the resulting pesticide suspension concentrate. The method primarily uses crushed kaolin as the main raw material, which is irradiated and then mixed with sodium metabisulfite and sodium acrylate to prepare the pesticide suspension concentrate. The suspension concentrate has a high suspension rate and pesticide adhesion, but high-particle-size kaolin is prone to agglomeration, affecting suspension dispersibility. Chinese patent CN111567517B discloses a novel aqueous pesticide suspension concentrate and a method for preparing the same. The method primarily utilizes a click chemistry reaction with a water-soluble compound containing a thiol group and a carbon-carbon double bond, using photocatalysis to graft water-soluble functional groups onto the surface of the active ingredient (TP) molecules via coating. While this method improves the dispersibility of the active ingredient in an aqueous medium to a certain extent, the preparation process is complex and the method has certain limitations, making it unsuitable for large-scale industrial production.

[0004] Therefore, a special adjuvant for pesticide aqueous suspension with high fluidity, high dispersibility and high stability is provided, which can be directly added to the pesticide aqueous suspension, has good compatibility, helps to enhance the wetting ability and adhesion of the pesticide, and solves the problem of precipitation, stratification, paste formation and even solidification during storage of the existing pesticide aqueous suspension system due to the instability of the dispersant. The method is simple, low in cost and easy to carry out large-scale industrial production, which has high practical application value. Summary of the Invention

[0005] In order to solve the above problems, the present invention provides a special adjuvant for pesticide aqueous suspension, which comprises, by weight, at least 50-70 parts of phosphate surfactant, 5-15 parts of alcoholamine compound, and 25-35 parts of alcohol solvent;

[0006] The phosphate ester surfactant has excellent performance and wide application. As an optimal technical scheme, the phosphate ester surfactant is at least one of alkyl phosphate, aryl phosphate, fatty alcohol polyoxyethylene ether phosphate, alkyl phenol polyoxyethylene ether phosphate, alkyl phenol polyoxyethylene ether phosphate, alkyl alcohol amide phosphate and imidazoline phosphate. Preferably, the phosphate ester surfactant is alkyl phenol polyoxyethylene ether phosphate. Preferably, the alkyl phenol polyoxyethylene ether phosphate is triphenyl styrene phenol resin polyoxyethylene ether phosphate. The triphenyl styrene phenol resin polyoxyethylene ether phosphate has excellent wetting property and thermal stability, and can provide the pesticide suspension concentrate special additive with excellent compatibility and thermal stability. Preferably, the triphenyl styrene phenol resin polyoxyethylene ether phosphate is one or a combination of 600#, 601#, 602#, 603#, 604#, 605# and 606#. Preferably, the triphenyl styrene phenol resin polyoxyethylene ether phosphate has a cloud point of 90-95°C and an HLB value of 17-20. In the application, the triphenyl styrene phenol resin polyoxyethylene ether phosphate with a cloud point of 90-95°C and an HLB value of 17-20 is used in the presence of an alcohol amine compound, so that the pesticide suspension concentrate special additive has high flowability and high stability, is actually applied to the pesticide suspension concentrate, significantly improves the dispersibility and stability of the pesticide suspension concentrate system, and helps to enhance the wetting capacity and adhesion of the pesticide, solves the problems of precipitation, stratification, creaming and even solidification of the existing pesticide suspension concentrate system due to the instability of the dispersant during storage, has a simple method, low cost, and is easy to be mass-produced, and has high practical value.

[0007] The triphenyl styrene phenol resin polyoxyethylene ether phosphate is 603# purchased from Xingtai Blue Sky Fine Chemical Co., Ltd.

[0008] As an optimal technical scheme, the alcohol solvent is one or a combination of ethanol, isopropyl alcohol, ethylene glycol, butanediol and propylene glycol. Preferably, the alcohol solvent is ethylene glycol, and the mass ratio of the ethylene glycol to the triphenyl styrene phenol resin polyoxyethylene ether phosphate is (28-32):(55-65). In the application, the ethylene glycol is used as the solvent, and the mass ratio of the ethylene glycol to the triphenyl styrene phenol resin polyoxyethylene ether phosphate is controlled to be (28-32):(55-65), so that the triphenyl styrene phenol resin polyoxyethylene ether phosphate in the system is effectively dissolved, the flowability and stability of the pesticide suspension concentrate special additive are ensured, the pesticide suspension concentrate special additive is well compatible with the pesticide raw material and other components in actual application, and the storage time of the pesticide suspension concentrate is prolonged.

[0009] As a preferred technical solution, the alcoholamine compound is selected from one or more of triethanolamine, monoethanolamine, methyldiethanolamine, and ethanolamine; preferably, the alcoholamine compound is triethanolamine; the mass ratio of triethanolamine to tristyrylphenol resin polyoxyethylene ether phosphate is (8-12): (55-65); the present applicant has found through a large number of experimental explorations that when the alcoholamine compound added to the system is triethanolamine, the tristyrylphenol resin polyoxyethylene ether phosphate in the system is promoted to be well dissolved in ethylene glycol, thereby ensuring the high dispersibility of the special auxiliary agent for pesticide aqueous suspension; in addition, the present applicant unexpectedly found that, especially by controlling the reaction of triethanolamine and tristyrylphenol resin polyoxyethylene ether phosphate, When the mass ratio of triethanolamine and tristyrylphenol resin polyoxyethylene ether phosphate is (8-12): (55-65), the synergistic compounding effect of the two is maximized, so that the provided special adjuvant for pesticide aqueous suspension has excellent wettability, dispersion stability and high temperature resistance. This may be because the triethanolamine and tristyrylphenol resin polyoxyethylene ether phosphate in the system are effectively combined to form triethanolamine and tristyrylphenol resin polyoxyethylene ether phosphate triethanolammonium salt. The tristyrylphenol resin polyoxyethylene ether phosphate triethanolammonium salt cooperates with the tristyrylphenol resin polyoxyethylene ether phosphate to effectively improve the special adjuvant for pesticide aqueous suspension with excellent wettability, dispersion stability and high temperature resistance, so that the pesticide droplets are easy to spread and adhere to the leaf surface, thereby improving the persistence of the pesticide.

[0010] On the other hand, the present application provides a method for preparing a special adjuvant for pesticide aqueous suspension, which comprises adding an alcohol solvent, a phosphate-type surfactant, and an alcoholamine compound in parts by weight into a stirring container and stirring for 15-20 minutes.

[0011] Beneficial effects

[0012] 1. The present invention provides a special adjuvant for pesticide aqueous suspension with high fluidity, high dispersibility and high stability, which can be directly added to the pesticide aqueous suspension, has good compatibility, and helps to enhance the wetting ability and adhesion of the pesticide.

[0013] 2. In this application, tristyrylphenol resin polyoxyethylene ether phosphate with a cloud point of 90-95°C and an HLB value of 17-20 is used to give the special additive for pesticide aqueous suspension excellent compatibility and heat stability; in the presence of an alcoholamine compound, the provided special additive for pesticide aqueous suspension has outstanding high fluidity and high stability. When actually applied to pesticide aqueous suspension, it significantly improves the dispersibility and stability of the pesticide aqueous suspension system, helps to enhance the wetting ability and adhesion of the pesticide, and solves the problem of precipitation, stratification, paste formation and even solidification in the existing pesticide aqueous suspension system due to the instability of the dispersant during storage. The method is simple, low cost, easy to carry out large-scale industrial production, and has high practical application value.

[0014] 3. By using ethylene glycol as a solvent and controlling the mass ratio of ethylene glycol to tristyrylphenol resin polyoxyethylene ether phosphate to be (28-32): (55-65), the tristyrylphenol resin polyoxyethylene ether phosphate in the system is effectively dissolved, thereby ensuring the fluidity and stability of the special additive for the pesticide aqueous suspension, and helping the special additive for the aqueous suspension to be well compatible with the pesticide technical and other ingredients in actual application, thereby extending the storage time of the pesticide aqueous suspension.

[0015] 4. In the system of this application, triethanolamine, an alcoholamine compound, is added to promote the good dissolution of tristyrylphenol resin polyoxyethylene ether phosphate in ethylene glycol, thereby ensuring the high dispersibility of the special auxiliary agent for pesticide aqueous suspension.

[0016] 5. By controlling the mass ratio of triethanolamine and tristyrylphenol resin polyoxyethylene ether phosphate to (8-12): (55-65), the synergistic combination of the two is maximized, so that the provided special adjuvant for pesticide aqueous suspension has excellent wettability, dispersion stability and high temperature resistance, making it easy for pesticide droplets to spread and adhere to the leaf surface, thereby improving the persistence of the pesticide. DETAILED DESCRIPTION

[0017] Example

[0018] Example 1

[0019] Example 1 of the present invention provides a special adjuvant for pesticide aqueous suspension, wherein the raw materials for its preparation include, by weight, 60 parts of phosphate surfactant, 10 parts of alcoholamine compound, and 30 parts of alcohol solvent.

[0020] The phosphate ester surfactant is alkylphenol polyoxyethylene ether phosphate; the alkylphenol polyoxyethylene ether phosphate is tristyrylphenol resin polyoxyethylene ether phosphate; the tristyrylphenol resin polyoxyethylene ether phosphate has a cloud point of 90-95° C. and an HLB value of 20.

[0021] The tristyrylphenol resin polyoxyethylene ether phosphate was of model 603# and was purchased from Xingtai Lantian Fine Chemical Co., Ltd.

[0022] The alcohol solvent is ethylene glycol, and the mass ratio of the ethylene glycol to tristyrylphenol resin polyoxyethylene ether phosphate is 30:60.

[0023] The alcoholamine compound is triethanolamine; the mass ratio of triethanolamine to tristyrylphenol resin polyoxyethylene ether phosphate is 10:60.

[0024] Another embodiment 1 of the present application provides a method for preparing a special adjuvant for pesticide aqueous suspension, which comprises adding an alcohol solvent, a phosphate-type surfactant, and an alcoholamine compound into a stirring container and stirring for 20 minutes.

[0025] Example 2

[0026] Example 2 of the present invention provides a special adjuvant for pesticide aqueous suspension, wherein the raw materials for its preparation include, by weight, 62 parts of phosphate surfactant, 12 parts of alcoholamine compound, and 32 parts of alcohol solvent.

[0027] The phosphate ester surfactant is alkylphenol polyoxyethylene ether phosphate; the alkylphenol polyoxyethylene ether phosphate is tristyrylphenol resin polyoxyethylene ether phosphate; the tristyrylphenol resin polyoxyethylene ether phosphate has a cloud point of 90-95° C. and an HLB value of 20.

[0028] The tristyrylphenol resin polyoxyethylene ether phosphate was of model 603# and was purchased from Xingtai Lantian Fine Chemical Co., Ltd.

[0029] The alcohol solvent is ethylene glycol, and the mass ratio of ethylene glycol to tristyrylphenol resin polyoxyethylene ether phosphate is 32:62.

[0030] The alcoholamine compound is triethanolamine; the mass ratio of triethanolamine to tristyrylphenol resin polyoxyethylene ether phosphate is 12:62.

[0031] Another embodiment 2 of the present application provides a method for preparing a special adjuvant for pesticide aqueous suspension, which comprises adding an alcohol solvent, a phosphate-type surfactant, and an alcoholamine compound into a stirring container and stirring for 20 minutes.

[0032] Example 3

[0033] Example 3 of the present invention provides a special adjuvant for pesticide aqueous suspension, and its preparation raw materials include, by weight, 58 parts of phosphate surfactant, 8 parts of alcoholamine compound, and 28 parts of alcohol solvent.

[0034] The phosphate ester surfactant is alkylphenol polyoxyethylene ether phosphate; the alkylphenol polyoxyethylene ether phosphate is tristyrylphenol resin polyoxyethylene ether phosphate; the tristyrylphenol resin polyoxyethylene ether phosphate has a cloud point of 90-95° C. and an HLB value of 20.

[0035] The tristyrylphenol resin polyoxyethylene ether phosphate was of model 603# and was purchased from Xingtai Lantian Fine Chemical Co., Ltd.

[0036] The alcohol solvent is ethylene glycol, and the mass ratio of ethylene glycol to tristyrylphenol resin polyoxyethylene ether phosphate is 28:58.

[0037] The alcoholamine compound is triethanolamine; the mass ratio of triethanolamine to tristyrylphenol resin polyoxyethylene ether phosphate is 8:58.

[0038] Another embodiment 1 of the present application provides a method for preparing a special adjuvant for pesticide aqueous suspension, which comprises adding an alcohol solvent, a phosphate-type surfactant, and an alcoholamine compound into a stirring container and stirring for 20 minutes.

[0039] Comparative Example 1

[0040] Comparative Example 1 of the present invention provides a special adjuvant for pesticide aqueous suspension and a preparation method thereof. The specific implementation manner is the same as that of Example 1, except that the mass ratio of triethanolamine to tristyrylphenol resin polyoxyethylene ether phosphate is 3:60.

[0041] Comparative Example 2

[0042] Comparative Example 2 of the present invention provides a special adjuvant for pesticide aqueous suspension and a preparation method thereof. Its specific implementation manner is the same as that of Example 1, except that the mass ratio of ethylene glycol to tristyrylphenol resin polyoxyethylene ether phosphate is 20:60.

[0043] Comparative Example 3

[0044] Comparative Example 3 of the present invention provides a special adjuvant for pesticide aqueous suspension and a preparation method thereof. Its specific implementation method is the same as Example 1, except that the model of the tristyrylphenol resin polyoxyethylene ether phosphate is 606#, which is purchased from Xingtai Lantian Fine Chemical Co., Ltd.

[0045] Performance testing methods

[0046] (1) pH value: Referring to the national standard GB / T6368, the pH values ​​of the special adjuvants for the pesticide aqueous suspension prepared in the examples and comparative examples were measured. The test results are shown in Table 1.

[0047] (2) Determination of water content: Referring to the national standard GB / T11275, the water content (mass fraction) of the special adjuvant for the pesticide aqueous suspension prepared in the examples and comparative examples was determined. The test results are shown in Table 1.

[0048] (3) Thermal storage stability: Referring to GB / T 19136-2003, the special adjuvants for pesticide aqueous suspensions prepared in the examples and comparative examples were placed at 54±2°C. After storage for 14 days, the special adjuvants for pesticide aqueous suspensions were observed to see whether precipitation, stratification, creaming, or solidification occurred. If precipitation, stratification, creaming, or solidification did not occur, the thermal storage stability of the special adjuvant for pesticide aqueous suspensions was recorded as "qualified"; if precipitation, stratification, creaming, or solidification occurred, the thermal storage stability of the special adjuvant for pesticide aqueous suspensions was recorded as "unqualified".

[0049] Performance test data

[0050] The performance of the special adjuvants for the pesticide aqueous suspension prepared in Examples 1-3 and Comparative Examples 1-3 was evaluated. See Table 1, which shows the performance test data of the special adjuvants for the pesticide aqueous suspension prepared in Examples 1-3 and Comparative Examples 1-3.

[0051] Table 1

[0052] Test items pH Water content (%) Hot storage stability Example 1 7.1 0.2 qualified Example 2 7 0.3 qualified Example 3 6.9 0.3 qualified Comparative Example 1 5.5 0.5 Unqualified Comparative Example 2 6.8 0.5 Unqualified Comparative Example 3 6.6 0.5 Unqualified

Claims

1. A special adjuvant for pesticide aqueous suspension, characterized in that: The preparation raw materials include at least 50-70 parts by weight of a phosphate ester surfactant, 5-15 parts of an alcohol amine compound, and 25-35 parts of an alcohol solvent; the phosphate ester surfactant is alkylphenol polyoxyethylene ether phosphate; the alkylphenol polyoxyethylene ether phosphate is tristyrylphenol resin polyoxyethylene ether phosphate, the tristyrylphenol resin polyoxyethylene ether phosphate has a cloud point of 90-95°C and an HLB value of 17-20; the alcohol solvent is ethylene glycol, and the mass ratio of the ethylene glycol to the tristyrylphenol resin polyoxyethylene ether phosphate is (28-32):(55-65); the alcohol amine compound is triethanolamine, and the mass ratio of the triethanolamine to the tristyrylphenol resin polyoxyethylene ether phosphate is (8-12):(55-65).

2. A method for preparing a special adjuvant for pesticide aqueous suspension according to claim 1, characterized in that: The alcohol solvent, phosphate surfactant and alcoholamine compound are added into a stirring container and stirred for 15-20 minutes to obtain the product.

Citation Information

Patent Citations

  • A method for preparing a pesticide suspension and the resulting pesticide suspension.

    CN110506737B

  • A novel water-based pesticide suspension and its preparation method

    CN111567517B

  • Phosphate wetting dispersant, and preparation method and application thereof

    CN106359375A