Multifunctional additive for glyphosate dispersible oil suspending agent as well as preparation method and application of multifunctional additive

Abstract

The invention relates to a multifunctional additive for a glyphosate dispersible oil suspending agent as well as a preparation method and application of the multifunctional additive. The multifunctional additive comprises an auxiliary rheological agent, polyamide wax, fatty acid, a surfactant and fatty acid ester, and the auxiliary rheological agent is urea and phosphate; the surface active agent comprises a non-ionic surface active agent and an anionic surface active agent. The multifunctional additive provided by the invention is good in applicability, green, environment-friendly and convenient to use; the glyphosate dispersible oil suspending agent has the functions of emulsification, dispersion, rheology, stabilization and synergism, can effectively improve the problem of layering of separated oil in normal-heat storage of glyphosate dispersible oil suspending agents with different contents, improves the normal-heat storage stability of the glyphosate dispersible oil suspending agent, prolongs the pesticide effect shelf life of the glyphosate dispersible oil suspending agent, also can significantly improve the weeding efficiency, and has a broad application prospect. Therefore, the utilization rate of the preparation is effectively improved, the pesticide consumption is reduced, the ecological environment is protected, and the application cost of the preparation is reduced.

Description

Technical Field

[0001] The invention relates to the technical field of pesticides, and in particular to a multifunctional adjuvant for a glyphosate dispersible oil suspension, a preparation method and an application thereof. Background Art

[0002] Glyphosate is a non-selective, lethal herbicide that is very effective against perennial rooted weeds and is widely used in rubber, mulberry, tea, orchards and sugarcane fields. In recent years, glyphosate has become the most commonly used and largest-volume herbicide in global agricultural production due to its advantages such as good weed control effect, low toxicity, low price, easy decomposition in soil, and environmental friendliness. In recent years, with the continuous commercialization of genetically modified crops, the application scope and usage of glyphosate will continue to expand in the future, especially in developing countries where the planting area of ​​genetically modified crops has steadily increased. The global demand for glyphosate will steadily increase, which provides a broad application market and development prospects for the development of various glyphosate formulations.

[0003] At present, the main processed formulation of glyphosate on the market is water-based solution, which is generally glyphosate isopropylammonium salt, ammonium salt, sodium salt, potassium salt, etc. Among them, synergistic adjuvants are indispensable, but the selection is relatively single, generally: tallow fatty amine ethoxylate, alkyl polysaccharide, fatty alcohol ethoxylate, silicone, betaine, etc., which have high weed control efficiency and low cost. However, the long-term continuous high-dose use of a single category has caused weeds to develop irreversible drug resistance and resistance to glyphosate water-based solution. The dosage has increased year by year, but the weed control effect is not ideal. In addition, the abuse, misuse, and over-range use of water-based solution have also caused certain negative impacts on the environment and soil pollution.

[0004] Studies have shown that glyphosate (acid) has herbicidal activity, and glyphosate ammonium salt releases glyphosate in water to have a weed-killing effect. Most herbicides require the addition of oily adjuvants during application to fully exert their effects, so dispersible oil suspension is one of the more suitable formulations for glyphosate herbicide products. Dispersible oil suspension has the advantages of good adhesion, good affinity to the target, and easy mechanized application, which meets the requirements of green development of pesticide formulations.

[0005] Glyphosate (acid) has a large particle size, and it is difficult to grind it finely with conventional grinding processes and time. After hot storage, the particles will aggregate and precipitate, resulting in serious oil separation and stratification. Therefore, at present, the original drug of glyphosate dispersible oil suspension is mostly glyphosate ammonium salt, which is mainly compounded with other original drugs, and single dosage is rare, mainly to improve the broad-spectrum and rapid effect of weed control. However, compounding not only increases the cost of application, but also whether there is antagonism between the action mechanisms of the drugs after combination and whether it will accelerate the resistance of weeds remains to be verified. In addition, conventional dispersible oil suspensions have many components. In addition to the dispersion medium, they mainly include emulsifiers, dispersants, rheological agents, stabilizers and synergists. They play the functions of emulsification, dispersion, thickening, stabilization and synergism in the system, and each performs its own duties. However, the compatibility requirements of these adjuvants are high. Improper handling will aggravate the hot storage instability of the preparation, thereby affecting the weed control efficiency of glyphosate. Among them, the dispersion medium is mostly plant oil ester, which is plant-based, low-cost, and has good permeability and quick-acting properties, but the effect is far from the efficacy of glyphosate aqueous solution. Therefore, when using plant oil ester as a dispersion medium, while solving the problems of low grinding efficiency and thermal storage instability of glyphosate dispersible oil suspension, it is necessary to significantly improve its herbicidal and increasing efficiency and reduce the application cost of the preparation. Summary of the invention

[0006] The purpose of the present invention is to provide a multifunctional adjuvant for glyphosate dispersible oil suspension, and a preparation method and application thereof.

[0007] In order to achieve the above object, the technical solution adopted by the present invention is:

[0008] A multifunctional adjuvant for a glyphosate dispersible oil suspension, comprising an auxiliary rheological agent, polyamide wax, fatty acid, a surfactant and fatty acid ester, wherein the auxiliary rheological agent is urea and phosphate; and the surfactant comprises a nonionic surfactant and an anionic surfactant.

[0009] The multifunctional auxiliary agent provided by the present invention has good applicability and can be used to prepare glyphosate dispersible oil suspension concentrates with different contents. After being uniformly stirred with glyphosate, the glyphosate dispersible oil suspension concentrate can be directly prepared by sand grinding, which is more convenient to use, simplifies the feeding operation of preparing the glyphosate dispersible oil suspension concentrate and shortens the grinding time of the preparation.

[0010] The auxiliary rheological agent in the multifunctional auxiliary agent can effectively improve the operating performance of the preparation grinding process after heating and temperature rise, and also has an antistatic effect, can reduce the flocculation and sedimentation caused by the mutual adsorption of the original drug particles after normal hot storage, and improve the dispersion stability of the preparation. It is mixed with polyamide wax, fatty acid and surfactant for heating and swelling, and then subjected to high-speed shearing, which can significantly improve the dispersibility and adhesion of various particles in the system, shorten the preparation sand grinding time, and reduce the preparation particle size; the compound use of polyamide wax, fatty acid and surfactant can significantly improve the herbicidal activity of glyphosate, and the synergistic function is significant. Therefore, the multifunctional auxiliary agent takes into account the emulsification, dispersion, rheology, stability and synergistic functions at the same time, can effectively improve the oil separation and stratification problem of the preparation during normal hot storage, improve the stability of the preparation during normal hot storage, and extend the shelf life of the preparation. It can also significantly improve the herbicidal effect of glyphosate, which is conducive to reducing the amount of preparation used and the cost of application, and is more environmentally friendly.

[0011] Preferably, the mass ratio of urea to phosphate is 1:(0.5-1.5), more preferably 1:(0.8-1.2), for example 1:0.8, 1:0.9, 1:1, 1:1.1, 1:1.2.

[0012] Preferably, the auxiliary rheological agent accounts for 2-6% of the total mass of the multifunctional additive, for example, 2%, 3%, 4%, 5%, 6%.

[0013] Preferably, the phosphate is monohydrogen phosphate.

[0014] In some embodiments, the phosphate is disodium hydrogen phosphate.

[0015] Preferably, the nonionic surfactant is selected from one or more of polyoxyethylene ethers, polyoxyethylene esters, polyoxyethylene amides, alkyl alcohol amides, polyols, and ethylene oxide adducts of polypropylene glycol.

[0016] Further preferably, the nonionic surfactant is selected from one or more of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and alkyl alcohol amide.

[0017] In some embodiments, the nonionic surfactant is castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether and coconut fatty acid diethanolamide (alkyl alcohol amide).

[0018] Furthermore, the mass ratio of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether and coconut fatty acid diethanolamide is 1:(1-1.5):(1.5-2), and more preferably 1:(1.1-1.4):(1.6-1.8).

[0019] Preferably, the anionic surfactant is selected from one or more of alkylbenzene sulfonates, α-olefin sulfonates, alkyl sulfonates, α-sulfomonocarboxylic acids and their derivatives, alkyl polyoxyethylene ether phosphate salts, fatty alcohol polyoxyethylene ether phosphates and their salts, and succinate sulfonates.

[0020] In some embodiments, the anionic surfactant is octanol polyoxyethylene ether phosphate and / or its sodium salt.

[0021] Preferably, the mass ratio of the nonionic surfactant to the anionic surfactant is (3-5):1, and more preferably (3.5-4.5):1.

[0022] Preferably, the surfactant accounts for 10-20% of the total mass of the multifunctional auxiliary agent, more preferably 13-20%, for example 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%.

[0023] Preferably, the fatty acid is selected from one or more of lauric acid, coconut oil fatty acid, palm oil fatty acid, oleic acid, linoleic acid, linolenic acid, tall oil fatty acid, castor oil fatty acid, soybean oil fatty acid, sunflower oil fatty acid, linseed oil fatty acid, corn oil fatty acid, rapeseed oil fatty acid, cottonseed oil fatty acid, hairy coconut acid, rice bran acid, isooleic acid, waste cooking oil fatty acid, and arachidonic acid.

[0024] Preferably, the fatty acid accounts for 3-10% of the total mass of the multifunctional additive, more preferably 3-8%, and even more preferably 5-8%.

[0025] Preferably, the fatty acid ester is selected from one or more of fatty acid methyl ester, fatty acid ethyl ester and fatty acid glyceride.

[0026] Preferably, based on the total mass of the multifunctional additive being 100%, the proportions of the components of the multifunctional additive are as follows:

[0027] Auxiliary rheological agent 2-6%;

[0028] Polyamide wax 1-3%;

[0029] Fatty acids 3-10%;

[0030] Surfactant 10-20%;

[0031] Fatty acid ester balance.

[0032] In some embodiments, based on the total mass of the multifunctional additive being 100%, the proportions of the components of the multifunctional additive are as follows:

[0033] Urea 1-3%;

[0034] Phosphate 1-3%;

[0035] Polyamide wax 1-3%;

[0036] Nonionic surfactant 5-9%;

[0037] Anionic surfactant 2-4%;

[0038] Amphoteric surfactant 3-7%;

[0039] Fatty acids 3-10%;

[0040] Fatty acid ester balance.

[0041] In some preferred embodiments, based on the total mass of the multifunctional additive being 100%, the proportions of the components of the multifunctional additive are as follows:

[0042] Urea 1.5-2.5%;

[0043] Phosphate 1.5-2.5%;

[0044] Polyamide wax 1.5-2.5%;

[0045] Nonionic surfactant 6-8%;

[0046] Anionic surfactant 2-4%;

[0047] Amphoteric surfactant 4-6%;

[0048] Fatty acids 5-10%;

[0049] Fatty acid ester balance.

[0050] The present invention also provides a method for preparing the multifunctional additive as described above, the method comprising the following steps:

[0051] S1, mixing the auxiliary rheological agent and the fatty acid ester under heating conditions to obtain a mixture A;

[0052] S2, mixing the polyamide wax with the mixture A, and obtaining a mixture B after heating, swelling, and shearing;

[0053] S3, mixing the surfactant and the fatty acid to obtain a mixture C;

[0054] S4, mixing the mixture B and the mixture C to obtain a multifunctional additive.

[0055] Preferably, the mixing temperature of S1 is 150-160°C.

[0056] Preferably, the swelling temperature of S2 is 60-65° C., and the swelling time is 1-3 hours.

[0057] Preferably, the shearing speed of S2 is 3000-3500 r / min.

[0058] Preferably, the mixing temperature of S4 is 60-65°C.

[0059] The present invention also provides a use of the multifunctional adjuvant as described above in preparing a glyphosate dispersible oil suspension, comprising mixing the multifunctional adjuvant with glyphosate, and grinding the mixture to prepare the glyphosate dispersible oil suspension.

[0060] Preferably, the grinding time is 90 to 100 minutes.

[0061] The present invention also provides a glyphosate dispersible oil suspension, comprising glyphosate and the multifunctional adjuvant as described above.

[0062] Preferably, the glyphosate accounts for 30-50% of the total mass of the glyphosate dispersible oil suspension concentrate.

[0063] Due to the application of the above technical solution, the present invention has the following advantages compared with the prior art:

[0064] The multifunctional adjuvant provided by the present invention is suitable for preparing glyphosate dispersible oil suspension concentrates with different contents, has good applicability, and can be directly sand-milled to obtain the glyphosate dispersible oil suspension concentrate after being uniformly stirred with glyphosate, thereby simplifying the feeding operation of the preparation and shortening the grinding time of the preparation, and making it more convenient to use;

[0065] Moreover, the multifunctional adjuvant has the functions of emulsification, dispersion, rheology, stabilization and synergism, and can effectively improve the oil separation and stratification problem of glyphosate dispersible oil suspensions with different contents during normal hot storage, improve the normal hot storage stability of the glyphosate dispersible oil suspension, and extend the shelf life of the glyphosate dispersible oil suspension. It can also significantly improve the herbicidal effect of glyphosate, which is beneficial to reducing the application amount and application cost of the preparation.

[0066] The multifunctional additive provided by the invention is green and environmentally friendly, safe to soil and has good application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0067] Figure 1 The actual pictures are of the oil separation and particle size change of the 30% glyphosate dispersible oil suspension of Example 1 and Comparative Example 1 of the present invention before and after normal storage and hot storage for 14 days;

[0068] Figure 2 The figure is a comparison chart of the field efficacy test results of some embodiments and comparative examples of the present invention. DETAILED DESCRIPTION

[0069] The present invention is further described below in conjunction with the examples. However, the present invention is not limited to the following examples. The implementation conditions used in the examples can be further adjusted according to the different requirements of specific use, and the implementation conditions not specified are conventional conditions in the industry. The technical features involved in each embodiment of the present invention can be combined with each other as long as they do not conflict with each other.

[0070] Unless otherwise specified, the reagents and instruments used in the following examples and comparative examples are all commercially available products, or can be prepared with reference to the prior art. Among them, polyamide wax was purchased from McLean, item number P916175; castor oil polyoxyethylene ether was purchased from Jiangsu Hai'an Petrochemical, brand EL-20; fatty alcohol polyoxyethylene ether was purchased from Jiangsu Hai'an Petrochemical, brand AEO-3; alkyl alcohol amide was purchased from Jiangsu Hai'an Petrochemical, brand 6501; octanol polyoxyethylene ether phosphate was purchased from Shandong Yousuo Chemical, brand ODEP-98; tall oil fatty acid was purchased from Shandong Yousuo Chemical; methyl oleate was purchased from Suzhou Fengbei.

[0071] Unless otherwise specified, the preparation method of the multifunctional additive comprises the following steps:

[0072] S1. Mix the auxiliary rheological agent and the fatty acid ester, heat to 150-160° C., and keep the temperature for 2 hours to obtain solution A.

[0073] S2. Add polyamide wax to the above solution A, heat and swell at 60-65° C. for 2 h, and shear at high speed (3000-3500 r / min) for 10-15 min after constant temperature to obtain solution B.

[0074] S3. Evenly mix the surfactant and fatty acid to obtain solution C.

[0075] S4. Mix solution B and solution C, heat with stirring at 60-65° C. for 2-3 h, and obtain a multifunctional additive at a constant temperature.

[0076] Unless otherwise specified, the preparation method of the glyphosate dispersible oil suspension concentrate hereinafter includes: adding glyphosate and a multifunctional adjuvant into a reaction kettle, stirring evenly, grinding in a vertical ball mill for 90 to 100 minutes, and discharging after naturally cooling to room temperature (25±5°C).

[0077] Example 1

[0078] The invention discloses a multifunctional auxiliary agent for a glyphosate dispersible oil suspension, which comprises the following components based on the total weight of the multifunctional auxiliary agent being 100%: 2% urea, 2% disodium hydrogen phosphate, 2% polyamide wax, 3% castor oil polyoxyethylene ether, 4% fatty alcohol polyoxyethylene ether, 5% alkyl alcohol amide, 3% octanol polyoxyethylene ether phosphate, 8% tall oil fatty acid and 71% methyl oleate. The multifunctional auxiliary agent is prepared according to a multifunctional auxiliary agent preparation method.

[0079] A glyphosate dispersible oil suspension, with the total weight of 100%, comprises: 30% glyphosate and the rest is made up by a multifunctional auxiliary agent.

[0080] Example 2

[0081] The invention discloses a multifunctional auxiliary agent for a glyphosate dispersible oil suspension, which comprises the following components based on the total weight of the multifunctional auxiliary agent being 100%: 1% urea, 1% disodium hydrogen phosphate, 2% polyamide wax, 3% castor oil polyoxyethylene ether, 4% fatty alcohol polyoxyethylene ether, 5% alkyl alcohol amide, 3% octanol polyoxyethylene ether phosphate, 8% tall oil fatty acid and 73% methyl oleate. The multifunctional auxiliary agent is prepared according to a multifunctional auxiliary agent preparation method.

[0082] A glyphosate dispersible oil suspension, with the total weight of 100%, comprises: 30% glyphosate and the rest is made up by a multifunctional auxiliary agent.

[0083] Example 3

[0084] The invention discloses a multifunctional auxiliary agent for a glyphosate dispersible oil suspension, which comprises the following components based on the total weight of the multifunctional auxiliary agent being 100%: 2% urea, 2% disodium hydrogen phosphate, 1% polyamide wax, 3% castor oil polyoxyethylene ether, 4% fatty alcohol polyoxyethylene ether, 5% alkyl alcohol amide, 3% octanol polyoxyethylene ether phosphate, 8% tall oil fatty acid and 72% methyl oleate. The multifunctional auxiliary agent is prepared according to a multifunctional auxiliary agent preparation method.

[0085] A glyphosate dispersible oil suspension, with the total weight of 100%, comprises: 30% glyphosate and the rest is made up by a multifunctional auxiliary agent.

[0086] Example 4

[0087] The invention discloses a multifunctional auxiliary agent for a glyphosate dispersible oil suspension, which comprises the following components based on the total weight of the multifunctional auxiliary agent being 100%: 2% urea, 2% disodium hydrogen phosphate, 2% polyamide wax, 3% castor oil polyoxyethylene ether, 4% fatty alcohol polyoxyethylene ether, 5% alkyl alcohol amide, 3% octanol polyoxyethylene ether phosphate, 3% tall oil fatty acid and 76% methyl oleate. The multifunctional auxiliary agent is prepared according to a multifunctional auxiliary agent preparation method.

[0088] A glyphosate dispersible oil suspension, with the total weight of 100%, comprises: 30% glyphosate and the rest is made up by a multifunctional auxiliary agent.

[0089] Example 5

[0090] The invention discloses a multifunctional auxiliary agent for a glyphosate dispersible oil suspension, which comprises the following components based on the total weight of the multifunctional auxiliary agent being 100%: 2% urea, 2% disodium hydrogen phosphate, 2% polyamide wax, 4% castor oil polyoxyethylene ether, 5% fatty alcohol polyoxyethylene ether, 7% alkyl alcohol amide, 4% octanol polyoxyethylene ether phosphate, 8% tall oil fatty acid and 66% methyl oleate. The multifunctional auxiliary agent is prepared according to a multifunctional auxiliary agent preparation method.

[0091] A glyphosate dispersible oil suspension, with the total weight of 100%, comprises: 30% glyphosate and the rest is made up by a multifunctional auxiliary agent.

[0092] Example 6

[0093] The invention discloses a multifunctional auxiliary agent for a glyphosate dispersible oil suspension, which comprises the following components based on the total weight of the multifunctional auxiliary agent being 100%: 2% urea, 2% disodium hydrogen phosphate, 2% polyamide wax, 3% castor oil polyoxyethylene ether, 4% fatty alcohol polyoxyethylene ether, 5% alkyl alcohol amide, 3% octanol polyoxyethylene ether phosphate, 8% tall oil fatty acid and 71% methyl oleate. The multifunctional auxiliary agent is prepared according to a multifunctional auxiliary agent preparation method.

[0094] A glyphosate dispersible oil suspension, with the total weight of 100%, comprises: 40% glyphosate and the rest is made up by a multifunctional auxiliary agent.

[0095] Example 7

[0096] A multifunctional adjuvant for a glyphosate dispersible oil suspension, which comprises the following components based on the total weight of the multifunctional adjuvant as 100%: 2% urea, 2% disodium hydrogen phosphate, 2% polyamide wax, 3% castor oil polyoxyethylene ether, 4% fatty alcohol polyoxyethylene ether, 5% alkyl alcohol amide, 3% octanol polyoxyethylene ether phosphate, 8% tall oil fatty acid, and 71% methyl oleate. The multifunctional adjuvant is prepared according to a multifunctional adjuvant preparation method;

[0097] A glyphosate dispersible oil suspension, with a total weight of 100%, comprises: 50% glyphosate and a multifunctional auxiliary agent as a supplement.

[0098] Comparative Example 1

[0099] A glyphosate dispersible oil suspension, based on 100% of the total weight, comprises the following components: 30% of glyphosate, 15% of an emulsifier (5% of tristyrylphenol polyoxyethylene ether, 5% of fatty alcohol polyoxyethylene ether, and 5% of benzene sulfonate), 2% of a dispersant (tristyrylphenol polyoxyethylene ether phosphate), 2% of organic bentonite, 1% of fumed silica, and the balance is methyl oleate;

[0100] The preparation method of the glyphosate dispersible oil suspension comprises the following steps:

[0101] (1) Weighing the following components in parts by weight: glyphosate, tristyrylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, benzene sulfonate, tristyrylphenol polyoxyethylene ether phosphate, organic bentonite, fumed silica, and methyl oleate;

[0102] (2) The materials in step (1) are uniformly stirred and ground in a vertical ball mill for 90 to 100 minutes to obtain a 30% glyphosate dispersible oil suspension.

[0103] Comparative Example 2

[0104] A multifunctional adjuvant for a glyphosate dispersible oil suspension, which comprises the following components based on the total weight of the multifunctional adjuvant as 100%: 2% polyamide wax, 3% castor oil polyoxyethylene ether, 4% fatty alcohol polyoxyethylene ether, 5% alkyl alcohol amide, 3% octanol polyoxyethylene ether phosphate, 8% tall oil fatty acid, and 75% methyl oleate. A mixed solution 1 is prepared according to a multifunctional adjuvant preparation method.

[0105] A glyphosate dispersible oil suspension, with a total weight of 100%, comprises: 30% glyphosate, supplemented by the above mixed solution 1.

[0106] Comparative Example 3

[0107] A multifunctional adjuvant for a glyphosate dispersible oil suspension, which comprises the following components based on the total weight of the multifunctional adjuvant being 100%: 2% urea, 2% disodium hydrogen phosphate, 3% castor oil polyoxyethylene ether, 4% fatty alcohol polyoxyethylene ether, 5% alkyl alcohol amide, 3% octanol polyoxyethylene ether phosphate, 8% tall oil fatty acid, and 73% methyl oleate. A mixed solution 2 is prepared according to a multifunctional adjuvant preparation method.

[0108] A glyphosate dispersible oil suspension, with a total weight of 100%, comprises: 30% glyphosate, supplemented by the above mixed solution 2.

[0109] Comparative Example 4

[0110] A multifunctional adjuvant for glyphosate dispersible oil suspension, which comprises the following components based on the total weight of the multifunctional adjuvant as 100%: 3% castor oil polyoxyethylene ether, 4% fatty alcohol polyoxyethylene ether, 5% alkyl alcohol amide, 3% octanol polyoxyethylene ether phosphate, 8% tall oil fatty acid, and 77% methyl oleate. A mixed solution 3 is prepared according to the multifunctional adjuvant preparation method.

[0111] A glyphosate dispersible oil suspension, with a total weight of 100%, comprises: 30% glyphosate, supplemented by the above mixed solution 3.

[0112] Comparative Example 5

[0113] A glyphosate dispersible oil suspension, based on 100% of the total weight, comprises the following components: 30% of glyphosate, 2% of urea, 2% of disodium hydrogen phosphate, 2% of polyamide wax, 15% of emulsifier (5% of tristyrylphenol polyoxyethylene ether, 5% of fatty alcohol polyoxyethylene ether, 5% of benzene sulfonate), 8% of tall oil fatty acid, and the balance is methyl oleate;

[0114] The preparation method of the glyphosate dispersible oil suspension comprises the following steps:

[0115] (1) Weigh the following substances according to their weight: glyphosate, urea, disodium hydrogen phosphate, polyamide wax, tristyrylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, benzene sulfonate, tall oil fatty acid, and methyl oleate;

[0116] (2) The materials in step (1) are uniformly stirred and ground in a vertical ball mill for 90 to 100 minutes to obtain a 30% glyphosate dispersible oil suspension.

[0117] Comparative Example 6

[0118] A multifunctional adjuvant for glyphosate dispersible oil suspension, which comprises the following components based on the total weight of the multifunctional adjuvant as 100%: 2% urea, 2% disodium hydrogen phosphate, 2% polyamide wax, 3% castor oil polyoxyethylene ether, 4% fatty alcohol polyoxyethylene ether, 5% alkyl alcohol amide, 3% octanol polyoxyethylene ether phosphate, and 79% methyl oleate. A mixed solution 4 is prepared according to the multifunctional adjuvant preparation method.

[0119] A glyphosate dispersible oil suspension, with a total weight of 100%, comprises: 30% glyphosate, supplemented by the above mixed solution 4.

[0120] Performance test of examples and comparative examples:

[0121] (1) Qualitative observation of samples under normal heat storage and particle size analysis

[0122] The 30% glyphosate dispersible oil suspension obtained after grinding was divided into 2 small bottles, and subjected to normal storage experiment (25°C, 14 days) and hot storage experiment (stored in a constant temperature box at 54±2°C for 14 days). The physical stability of the samples under normal temperature and hot storage experimental conditions was observed, and the change in glyphosate particle size before and after hot storage was detected by microscopic observation. The change in the content of the glyphosate active ingredient before and after hot storage was analyzed and detected by liquid chromatography analysis. The hot storage stability of the products prepared in the examples and comparative examples was detected according to "GB / T19136-2003 Method for Determining Hot Storage Stability of Pesticides", and the test results are shown in Table 1 below.

[0123] Table 1 Test results of physical properties of dispersible oil suspension at normal heat storage

[0124]

[0125] The data results in Table 1 show that the glyphosate dispersible oil suspension (Comparative Example 1) prepared by using emulsifiers, dispersants, etc. commonly used in dispersible oil suspensions and glyphosate has an oil separation rate of up to 19.79% and a large particle size after storage at room temperature for 14 days; after hot storage for 14 days, the oil separation rate is even higher, the particle size increases significantly, and the suspension performance and dispersion stability are poor.

[0126] The inventors configure a multifunctional auxiliary agent, mix the multifunctional auxiliary agent with the original drug evenly, and then directly grind the multifunctional auxiliary agent into a dispersible oil suspension, which is very convenient to use. More importantly, the multifunctional auxiliary agent of the present invention can effectively improve the normal heat storage stability of the dispersible oil suspension of glyphosate with a higher content, reduce the flocculation and sedimentation caused by the mutual adsorption of the original drug particles after normal heat storage, reduce the particle size, extend the storage period of the pesticide, and ensure the efficacy. Specifically refer to the embodiments of the present invention, after normal heat storage, all indicators are qualified. In addition, the multifunctional auxiliary agent of the present invention has good applicability and is suitable for configuring various concentrations of glyphosate dispersible oil suspensions.

[0127] By comparing Example 1 and Comparative Example 2, when no auxiliary rheological agent is added to the multifunctional adjuvant (Comparative Example 2), the glyphosate dispersible oil suspension prepared therefrom has a significantly increased particle size in the normal heat storage experiment, and the oil separation rate is significantly increased, especially the hot storage oil absorption rate is as high as 15% or more, and the hot storage stability needs to be improved. Further comparing Example 1 and Example 2, different amounts of auxiliary rheological agent will also affect the normal heat storage performance of the glyphosate dispersible oil suspension, and the amount in Example 1 is the best.

[0128] By comparing Example 1 and Comparative Example 3, when polyamide wax is not added to the multifunctional auxiliary agent (Comparative Example 3), the particle size of the glyphosate dispersible oil suspension prepared therefrom is significantly increased in the normal heat storage experiment, and the oil separation rate is significantly increased, the normal heat storage oil absorption rate is as high as 15% or more, and the normal heat storage stability needs to be improved. Further comparing Example 1 and Example 3, different amounts of polyamide wax will also affect the normal heat storage performance of the glyphosate dispersible oil suspension, and the amount in Example 1 is the best.

[0129] By comparing Example 1 and Comparative Example 5, when the surfactant in the multifunctional adjuvant is inappropriate, it will also affect the particle size and oil separation rate of the glyphosate dispersible oil suspension, and also affect the dispersion stability.

[0130] By comparing Example 1 and Comparative Example 6, when no fatty acid is added to the multifunctional adjuvant (Comparative Example 6), the particle size of the glyphosate dispersible oil suspension prepared therewith is significantly increased in the normal heat storage experiment, and the oil separation rate is significantly increased. The normal heat storage oil absorption rate is as high as more than 15%, and the normal heat storage stability needs to be improved.

[0131] (2) Determination of drug efficacy by indoor and actual field testing

[0132] (2.1) Indoor bio-test

[0133] The test of the efficacy of the samples of the embodiment and the comparative example on corn and ramie: the test plants are corn and ramie, and the greenhouse pot method is used to determine the control effect of the liquid medicine on the plants. The test plants are planted with 5 plants per pot, and the test temperature is a greenhouse (about 15-35°C during the day and about 10-15°C at night; relative humidity is about 60%). When the plants are 3-4 leaves, the stems and leaves are sprayed with a spray bottle according to the dosage designed in the experiment. The growth of the plants is observed and visually inspected 7d and 14d after spraying. The visual control effect is recorded 14d after the medicine is applied and the fresh weight of the aboveground part is counted. The fresh weight inhibition rate is calculated by the following formula:

[0134]

[0135] Wherein: R is the fresh weight inhibition rate (%); X0 is the plant weight of the control group 1 (g); X1 is the fresh weight of the plants in the treatment area (g).

[0136] The control group 1 was a 41% glyphosate ammonium salt solution (provided by Shanghai Taihe Chemical Co., Ltd.), with a water consumption of 30 liters / mu and a pesticide dosage of 150 g / mu. The actual application area was 0.2 m 2 The test results are shown in Table 2 below.

[0137] Table 2 Indoor fresh weight control effect determination

[0138]

[0139]

[0140] (2.2) Field efficacy test

[0141] Field efficacy test of samples of embodiments and comparative examples for the control of weeds in non-cultivated land: the test agent is a glyphosate dispersible oil suspension, and the control agent is a 41% glyphosate ammonium salt solution (provided by Shanghai Taihe Chemical Co., Ltd.). The application method and water consumption are as follows: during the weed-prosperous period, the water consumption is 30L / mu, the pesticide dosage is 180g / mu, and the actual application area is 20m 2 The test results can be found in Figure 2 .

[0142] From Table 2 and Figure 2The data show that the dispersible oil suspension of the embodiment of the present invention has a better control effect on corn and ramie, which is significantly better than the glyphosate aqueous solution, especially the best performance of embodiment 1. Furthermore, the increase efficiency of embodiments 6-7 on corn and ramie is more significant. The multifunctional adjuvant of the present invention can significantly improve the increase efficiency of the dispersible oil suspension of glyphosate with different contents, that is, the utilization rate of pesticide is higher, and the application amount can be reduced by 15% to 20%, thereby reducing the application cost of the preparation.

[0143] In summary, the multifunctional adjuvant of the present invention is suitable for preparing glyphosate dispersible oil suspensions with different contents, and can significantly control the increase of particle size after hot storage while promoting the dispersion and rheological properties of the system, effectively improve the hot storage oil absorption rate and stability of glyphosate dispersible oil suspensions with different contents, and extend the efficacy shelf life of the glyphosate dispersible oil suspension; in addition, the multifunctional adjuvant can significantly improve the weed control and increase efficiency, improve the utilization rate of pesticides, reduce the amount of pesticides used and the cost of application, and is beneficial to protecting the ecological environment.

[0144] The above detailed description of the present invention is intended to enable persons familiar with the art to understand the contents of the present invention and implement them. It does not limit the protection scope of the present invention. Any equivalent changes or modifications made according to the spirit of the present invention should be included in the protection scope of the present invention.

Claims

1. A multifunctional adjuvant for glyphosate dispersible oil suspension, characterized in that: The multifunctional additives include auxiliary rheological agents, polyamide wax, fatty acids, surfactants and fatty acid esters, wherein the auxiliary rheological agents are urea and phosphate; and the surfactants include nonionic surfactants and anionic surfactants.

2. The multifunctional adjuvant for glyphosate dispersible oil suspension according to claim 1, characterized in that: The mass ratio of urea to phosphate is 1:(0.5-1.5); and / or, The auxiliary rheological agent accounts for 2-6% of the total mass of the multifunctional additive; and / or, The phosphate is monohydrogen phosphate.

3. The multifunctional adjuvant for glyphosate dispersible oil suspension according to claim 1, characterized in that: The nonionic surfactant is selected from one or more of polyoxyethylene ethers, polyoxyethylene esters, polyoxyethylene amides, alkyl alcohol amides, polyols, and ethylene oxide adducts of polypropylene glycol; and / or, The anionic surfactant is selected from one or more of alkylbenzene sulfonates, α-olefin sulfonates, alkyl sulfonates, α-sulfomonocarboxylic acids and their derivatives, alkyl polyoxyethylene ether phosphates, fatty alcohol polyoxyethylene ether phosphates and their salts, and succinate sulfonates.

4. The multifunctional adjuvant for glyphosate dispersible oil suspension according to claim 3, characterized in that: The nonionic surfactant is selected from one or more of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and alkyl alcohol amide; The anionic surfactant is octanol polyoxyethylene ether phosphate and / or its sodium salt.

5. The multifunctional adjuvant for glyphosate dispersible oil suspension according to any one of claims 1, 3 and 4, characterized in that: The mass ratio of the nonionic surfactant to the anionic surfactant is (3-5):1; The surfactant accounts for 10-20% of the total mass of the multifunctional auxiliary agent.

6. The multifunctional adjuvant for glyphosate dispersible oil suspension according to claim 1, characterized in that: The fatty acid is selected from one or more of lauric acid, coconut oil fatty acid, palm oil fatty acid, oleic acid, linoleic acid, linolenic acid, tall oil fatty acid, castor oil fatty acid, soybean oil fatty acid, sunflower oil fatty acid, linseed oil fatty acid, corn oil fatty acid, rapeseed oil fatty acid, cottonseed oil fatty acid, hairy coconut acid, rice bran acid isooleic acid, kitchen waste oil fatty acid, and arachidonic acid; and / or, The fatty acid accounts for 3-10% of the total mass of the multifunctional auxiliary agent.

7. The multifunctional adjuvant for glyphosate dispersible oil suspension according to claim 1, characterized in that: The fatty acid ester is selected from one or more of fatty acid methyl ester, fatty acid ethyl ester and fatty acid glyceride.

8. The multifunctional adjuvant for glyphosate dispersible oil suspension according to claim 1, characterized in that: Taking the total mass of the multifunctional additive as 100%, the proportions of the components of the multifunctional additive are as follows: Auxiliary rheological agent 2-6%; Polyamide wax 1-3%; Fatty acids 3-10%; Surfactant 10-20%; Fatty acid ester balance.

9. The method for preparing a multifunctional adjuvant for a glyphosate dispersible oil suspension according to any one of claims 1 to 8, characterized in that: The preparation method comprises the following steps: S1, mixing the auxiliary rheological agent and the fatty acid ester under heating conditions to obtain a mixture A; S2, mixing the polyamide wax with the mixture A, and obtaining a mixture B after heating, swelling, and shearing; S3, mixing the surfactant and the fatty acid to obtain a mixture C; S4, mixing the mixture B and the mixture C to obtain the multifunctional auxiliary agent.

10. The preparation method according to claim 9, characterized in that: The mixing temperature of S1 is 150-160° C.; and / or, The swelling temperature of S2 is 60-65°C and the swelling time is 1-3h; and / or, The shearing speed of S2 is 3000-3500 r / min; and / or, The mixing temperature of S4 is 60-65°C.

11. Use of the multifunctional adjuvant according to any one of claims 1 to 8 in the preparation of a glyphosate dispersible oil suspension concentrate, characterized in that: The method comprises mixing the multifunctional adjuvant with glyphosate and grinding the mixture to prepare the glyphosate dispersible oil suspension.

12. The use according to claim 11, characterized in that: The grinding time is 90 to 100 minutes.

13. A glyphosate dispersible oil suspension, characterized in that: The invention comprises glyphosate and the multifunctional adjuvant according to any one of claims 1 to 8.

14. The glyphosate dispersible oil suspension according to claim 13, characterized in that: The glyphosate accounts for 30-50% of the total mass of the glyphosate dispersible oil suspension.

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