A stable and efficient oil suspension additive and a preparation method thereof

By combining ionic surface energy regulators, aliphatic ether compounds and block polymers, the emulsification, dispersibility and stability problems of oil suspensions are solved, and the stability and application range of pesticide formulations are improved.

CN116076496BActive Publication Date: 2025-10-17SHANDONG TIANDAO NEW MATERIALS CO LTD
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Patent Information

Application Number
CN202211010062.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-08-22
Publication Date
2025-10-17
Estimated Expiration
2042-08-22

AI Technical Summary

Technical Problem

The comprehensive performance of existing dispersible oil suspensions fails to meet the growing demands of consumers. There are problems such as poor emulsification and dispersibility and easy precipitation, which affect the actual effect of pesticides.

Method used

A combination of ionic surface energy regulators, aliphatic ether compounds and block polymers is used to improve the surface energy and interaction between particles in pesticide formulations through synergistic effects, thereby enhancing emulsification, dispersibility and stability.

Benefits of technology

The prepared oil suspension additive has excellent emulsification and dispersibility, avoids oil separation, stratification and precipitation, improves the stability of the pesticide formulation and the adhesion of the active ingredients, and expands the scope of application.

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Abstract

The present application relates to A01N pesticide adjuvant technical field, more specifically, the present application provides a kind of stable and efficient oil suspension additive and preparation method thereof.The present application uses sodium dodecyl benzene sulfonate, aliphatic ether compound with saponification value of 90-100mgKOH / g, block polymer with average molecular weight of 8350 and HLB value of 29 as raw materials, and the prepared additive has excellent emulsification stability, which is applied to oil suspension to effectively avoid the phenomenon that oil suspension is prone to stratification and sedimentation.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of A01N pesticide adjuvant, more particularly, the present application provides a kind of stable and efficient oil suspension additive and preparation method thereof. BACKGROUND

[0002] Oil suspension is an important adjuvant in pesticide preparation, which can improve the efficacy of pesticides to some extent and is widely used in the field of pesticides. In recent years, with the continuous updating of oil suspension, consumers have provided higher requirements for the comprehensive performance of oil suspension. The emergence of dispersible oil suspension has expanded the application range of oil suspension to some extent. However, the comprehensive performance of the dispersible oil suspension in the prior art still cannot meet the growing requirements of consumers.

[0003] Chinese patent CN102239899A discloses a composite adjuvant for oil suspension and a preparation method thereof. In the present patent, castor oil polyoxyethylene ether, nonylphenol polyoxyethylene ether, sodium bicarbonate and ammonium sulfate are used as active ingredients to solve the problem of easy precipitation of the pesticide suspension dispersion system in the prior art. However, the emulsifying and dispersing properties of the product are not reflected, which may affect the actual effect of the pesticide and significantly limit the practical use of the composite adjuvant.

[0004] Therefore, it is urgent to develop an oil suspension additive with less oil separation, no bottoming and excellent emulsifying and dispersing stability, which has potential application value in the field of pesticide adjuvant. SUMMARY

[0005] To solve the above technical problems, the present application provides a stable and efficient oil suspension additive. The preparation raw materials include the following components in terms of mass percentage: 20-40% of ionic surface energy modifier, 35-45% of aliphatic ether compound, 5-10% of block polymer, and the balance of oil solvent to 100%.

[0006] As a preferred technical solution of the present application, the ionic surface energy modifier includes a combination of one or more of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, triethanolamine lauryl sulfate, sodium secondary alkyl sulfonate, sodium cocoyl methyl taurate, sodium lauryl polyoxyethylene ether carboxylate and potassium dodecyl phosphate.

[0007] As a more preferred technical solution of the present application, the ionic surface modifier is sodium dodecyl benzene sulfonate.

[0008] As a preferred technical solution of the present application, the aliphatic ether compound includes a combination of one or more of hydroxyl, ester and double bond.

[0009] As a preferred technical solution of the present application, the saponification value of the aliphatic ether compound is 80-120 mgKOH / g.

[0010] As a more preferred technical solution of the present application, the saponification value of the aliphatic ether compound is 90-100 mgKOH / g.

[0011] As a preferred technical solution of the present application, the block polymer is a block polymer formed by random copolymerization of polyoxyethylene and polyoxypropylene.

[0012] As a preferred technical solution of the present application, the average molecular weight of the block polymer is 6000-10000.

[0013] As a more preferred technical solution of the present application, the average molecular weight of the block polymer is 8350.

[0014] As a preferred technical solution of the present application, the HLB value of the block polymer is 20-40.

[0015] As a more preferred technical solution of the present application, the HLB value of the block polymer is 29.

[0016] As a preferred technical solution of the present application, the mass ratio of the ionic surface energy modifier, the aliphatic ether compound, and the block polymer is (2.5-3.5):(3.5-4.5):(5-1.5).

[0017] As a more preferred technical solution of the present application, the mass ratio of the ionic surface energy modifier, the aliphatic ether compound, and the block polymer is 3:4:1.

[0018] As a preferred technical solution of the present application, the oily solvent includes one or more combinations of soybean oil, castor bean oil, corn oil, paraffin solvent oil, naphthene solvent oil, and aromatic solvent oil.

[0019] As a more preferred technical solution of the present application, the oily solvent is aromatic solvent oil.

[0020] As a preferred technical solution of the present application, the aromatic solvent oil includes one or more combinations of 100# aromatic solvent oil and 150# aromatic solvent oil.

[0021] As a more preferred technical solution of the present application, the aromatic solvent oil is 150# aromatic solvent oil.

[0022] The second aspect of the present application provides a preparation method of a stable and efficient oil suspension additive, comprising the following steps:

[0023] (1) Stir the aliphatic ether compound and the block polymer at 30-40℃ for 20-40 min to obtain a heated mixture;

[0024] (2) After adding the ion-type surface modifier of step to the heated mixture of step (1), add the oily solvent and stir until uniform, then heat, incubate, filter and discharge to obtain the oil suspension additive.

[0025] The temperature of the heating of step (2) is 40-45℃;

[0026] The incubation time of step (2) is 20-40 min.

[0027] Compared with the prior art, the present application has the following beneficial effects:

[0028] 1. The oil suspension additive prepared by the present application can improve the surface energy between solid particles in the pesticide preparation by adding the aliphatic compound containing hydroxyl, ester and double bond to the system and controlling the saponification value of the aliphatic ether compound to be 90-100 mgKOH / g, and can effectively avoid the phenomenon of particle aggregation in the long-term storage of the pesticide preparation, especially for the pesticide containing C-S bond and S-S bond active ingredient, and can be widely applied to the oil-soluble herbicide, and can significantly improve the long-term storage stability of the oil-soluble herbicide containing C-S bond and S-S bond active ingredient.

[0029] 2. The oil suspension additive prepared by the present application can improve the mutual interaction between the particles in the oil suspension by adding the block polymer formed by random copolymerization of polyoxyethylene and polyoxypropylene to the system, especially when the average molecular weight of the block polymer is 8350 and the HLB value is 29, and can have more excellent adsorption effect on the surface of the particles in the oil suspension by the synergistic effect between the aliphatic ether compound with a saponification value of 90-100 mgKOH / g and sodium dodecylbenzenesulfonate in the system, and can effectively solve the problem of poor emulsion stability caused by the flocculation of the dispersible oil suspension, and can also avoid the phenomena of oil separation, stratification and precipitation.

[0030] 3、The oil suspension additive prepared by the method has the advantages that when the sodium dodecyl benzene sulfonate, the aliphatic ether compound with a saponification value of 90-100 mgKOH / g, and the block polymer with an average molecular weight of 8350 and an HLB value of 29 are added into the system at a mass ratio of 3:4:1, the distribution of lipophilic groups and hydrophilic groups in the oil suspension can be improved, the difference in interfacial tension between different particles in the pesticide preparation, especially the pesticide containing active ingredients with C-S bonds and S-S bonds, can be reduced, the uniform dispersion stability of the active ingredients in the system can be improved, the viscosity and stability of the oil suspension can be improved, the stability of the pesticide preparation can be improved, the adhesion of the active ingredients on the surface of the organism can be improved, and the application range of the oil suspension in the field of pesticide preparation is expanded.

[0031] 4、The oil suspension additive prepared by the method has the advantages that when the sodium dodecyl benzene sulfonate, the aliphatic ether compound with a saponification value of 90-100 mgKOH / g, and the block polymer with an average molecular weight of 8350 and an HLB value of 29 are added into the system at a mass ratio of 3:4:1, the distribution of lipophilic groups and hydrophilic groups in the oil suspension can be improved, the difference in interfacial tension between different particles in the pesticide preparation, especially the pesticide containing active ingredients with C-S bonds and S-S bonds, can be reduced, the uniform dispersion stability of the active ingredients in the system can be improved, the viscosity and stability of the oil suspension can be improved, the stability of the pesticide preparation can be improved, the adhesion of the active ingredients on the surface of the organism can be improved, and the application range of the oil suspension in the field of pesticide preparation is expanded. Embodiment

[0032] Example 1

[0033] Embodiment 1 provides a stable and efficient oil suspension additive, and the preparation raw materials include the following components in percentage by mass: 30% of an ionic surface energy regulator, 40% of an aliphatic ether compound, 10% of a block polymer, and the balance of an oily solvent to 100%.

[0034] The ionic surface energy regulator is sodium dodecyl benzene sulfonate, and the CAS number of the sodium dodecyl benzene sulfonate is 25155-30-0.

[0035] The aliphatic ether compound is purchased from Tianjin Daixu Chemical Trade Co., Ltd., and the model number is EL-20, which contains hydroxyl groups, ester groups and double bonds, and has a saponification value of 90-100 mgKOH / g.

[0036] The block polymer is a block polymer formed by random copolymerization of polyoxyethylene and polyoxypropylene, and is purchased from Jinan Huijinchuan Business and Trade Co., Ltd., has an average molecular weight of 8350 and an HLB value of 29.

[0037] The oily solvent is 150# aromatic hydrocarbon solvent oil, which is purchased from Jinan Weite Chemical Technology Co., Ltd.

[0038] The preparation method of the stable and efficient oil suspension additive comprises the following steps:

[0039] (1) Stir the aliphatic ether compound and the block polymer at 35℃ for 30 min to obtain a heated mixture;

[0040] (2) After the ionic surface modifier of step is added to the stirred tank, the heated mixture of step (1) is added, and then the oily solvent is stirred uniformly, and after temperature rising, temperature keeping, and filtration, the oil suspension additive is obtained.

[0041] In step (2), the temperature of the temperature rising is 45℃;

[0042] The temperature keeping time of step (2) is 30 min.

[0043] Example 2

[0044] Example 2 provides a stable and efficient oil suspension additive, and the preparation raw materials include the following components in percentage by mass: ionic surface energy modifier 20%, aliphatic ether compound 35%, block polymer 5%, and the rest is supplemented with oily solvent to 100%.

[0045] The ionic surface energy modifier is sodium dodecyl benzene sulfonate, and the CAS number of sodium dodecyl benzene sulfonate is 25155-30-0;

[0046] The aliphatic ether compound is purchased from Tianjin Daixu Chemical Trade Co., Ltd., and the model is EL-20, which contains hydroxyl, ester, double bond, and saponification value is 90-100 mgKOH / g;

[0047] The block polymer is a block polymer formed by random copolymerization of polyoxyethylene and polyoxypropylene, which is purchased from Jinan Huijinchuan Business and Trade Co., Ltd., and the average molecular weight is 8350 and the HLB value is 29;

[0048] The oily solvent is 150# aromatic hydrocarbon solvent oil, which is purchased from Jinan Weite Chemical Technology Co., Ltd.

[0049] The preparation method of the stable and efficient oil suspension additive is the same as that of example 1.

[0050] Example 3

[0051] The embodiment 3 provides a stable and efficient oil suspension additive, and raw materials for preparation in percentage by mass include the following components: ionic surface energy modifier 20%, aliphatic ether compound 40%, block polymer 10%, and the rest is supplemented by oil solvent to 100%.

[0052] The ionic surface energy modifier is sodium dodecyl benzene sulfonate, and the CAS number of the sodium dodecyl benzene sulfonate is 25155-30-0.

[0053] The aliphatic ether compound is purchased from Tianjin Daixu Chemical Trade Co., Ltd., and the model is EL-20, wherein the aliphatic ether compound contains hydroxyl, ester, double bond, and a saponification value of 90-100 mgKOH / g.

[0054] The block polymer is a block polymer formed by random copolymerization of polyoxyethylene and polyoxypropylene, and is purchased from Jinan Huijinchuan Business and Trade Co., Ltd., and has an average molecular weight of 8350 and an HLB value of 29.

[0055] The oil solvent is 150# aromatic hydrocarbon solvent oil, and is purchased from Jinan Weite Chemical Technology Co., Ltd.

[0056] The preparation method of the stable and efficient oil suspension additive

[0057] Comparative Example 1

[0058] The embodiment of the comparative example 1 is the same as that of the embodiment 1, except that the block polymer is replaced by polyisobutylene sorbitol succinate.

[0059] Comparative Example 2

[0060] The embodiment of the comparative example 2 is the same as that of the embodiment 1, except that the aliphatic ether compound is not added.

[0061] Comparative Example 3

[0062] The embodiment of the comparative example 3 is the same as that of the embodiment 1, except that the saponification value of the aliphatic ether compound is 70-80 mgKOH / g, and the aliphatic ether compound is purchased from Tianjin Daixu Chemical Trade Co., Ltd., and the model is EL-30.

[0063] Performance evaluation

[0064] (1) Emulsion stability test

[0065] The additives prepared in the embodiment 1-3 and the comparative examples 1-3 are subjected to emulsion stability test according to GB / T3776.3-1983 "Pesticide emulsifier emulsion performance determination method", and the measured data are shown in Table 1.

[0066] (2) Moisture content and pH value detection

[0067] The additive prepared in Example 1 was respectively detected for moisture content and pH value according to Karl Fischer method in GB / T11275-2007 "Determination of Moisture Content of Surfactants" and GB / T6368-2008 "Determination of pH Value of Surfactant Aqueous Solution", and the data measured are shown in Table 2.

[0068] Table 1 Test results of emulsification stability of the additive

[0069] Emulsion stability Example 1 Pass Example 2 Pass Example 3 Pass Comparative Example 1 Fail Comparative Example 2 Fail Comparative Example 3 Fail

[0070] Table 2 Test results of physicochemical properties of the additive

[0071] Moisture content (%) pH value Example 1 ≤0.5 5-8

Claims

1. A stable and efficient oil suspension additive, characterized in that: The raw materials for the preparation are the following components by weight percentage: 20-40% of ionic surface energy regulator, 35-45% of aliphatic ether compound, 5-10% of block polymer, and the oily solvent is added to make up the balance to 100%; The ionic surface energy regulator is one or a combination of sodium dodecylbenzenesulfonate, sodium dodecyl sulfate, triethanolamine lauryl sulfate, sodium secondary alkylsulfonate, sodium cocoylmethyl taurate, sodium lauryl polyoxyethylene ether carboxylate, and potassium dodecyl phosphate; The saponification value of the aliphatic ether compound is 80-120 mgKOH / g; The aliphatic ether compound is one or a combination of hydroxyl group, ester group, and double bond; The block polymer is a block polymer formed by random copolymerization of polyoxyethylene and polyoxypropylene; The block polymer has an average molecular weight of 6000-10000 and an HLB value of 20-40; The oily solvent is aromatic solvent oil.

2. The oil suspension additive according to claim 1, characterized in that The mass ratio of the ionic surface energy regulator, the aliphatic ether compound and the block polymer is (2.5-3.5): (3.5-4.5): (5-1.5).

3. A method for preparing the oil suspension additive according to any one of claims 1 to 2, characterized in that: The following steps are involved: (1) stirring the aliphatic ether compound and the block polymer at 30-40° C. for 20-40 minutes to obtain a heated mixture; (2) Add the ionic surface conditioner in the stirring tank, add the heated mixture in step (1), add the oily solvent and stir evenly, and then heat, keep warm, filter and discharge to obtain the oil suspension additive.

Citation Information

Patent Citations

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