Picloram triethanolamine salt aqueous auxiliary agent and preparation method thereof

Abstract

The invention discloses an picloram triethanolamine salt water agent auxiliary agent and a preparation method thereof. The auxiliary agent is prepared from the following components in percentage by weight: 20-45% of dihydrogenated tallow dimethyl ammonium chloride, 10-20% of triethanolamine, 10-20% of sodium chloride, 5-10% of sodium chloride, 5-10% of sodium chloride and the balance of water. 15 to 30% of hydrogenated tallow amine acetate; 10 to 20% of hexadecyl dimethyl allyl ammonium chloride; 1-2% of dioctyl sodium sulfosuccinate; and the balance water. The picloram triethanolamine ammonium salt aqueous solution processed by the method is not easy to solidify at low temperature, has the characteristics of high efficiency, high environmental and biological safety, good preparation stability and the like, is particularly suitable for northern use, and has a good application prospect.

Description

Technical Field

[0001] The invention belongs to the application field of agricultural chemicals, and particularly relates to an amiloride triethanolammonium salt solution synergistic adjuvant. Background Art

[0002] Amloprid is a new type of pyridine carboxylic acid herbicide developed by Tao Nongke. It is widely used for weed control in mountainous areas, grasslands, plantations and non-cultivated lands. It is currently being researched and developed for weed control in rapeseed and cereal crops. The agent has the characteristics of low toxicity, no teratogenicity, mutagenicity, carcinogenicity, no side effects on endocrine and reproduction, and low toxicity to humans. In addition to the production of CO2, no other products that affect soil and water quality have been found in metabolism. The acute and chronic toxicity to mammals, birds, fish, and aquatic invertebrates are low.

[0003] Amlopyralid is a synthetic hormone herbicide. It can be quickly absorbed by the stems, leaves and roots of plants, and induce an upward reaction in sensitive plants, resulting in plant growth stagnation and rapid necrosis. The agent has a long lasting effect and can be used to control annual and perennial broadleaf weeds in pastures such as blunt-leaved sorrel, wrinkled sorrel, field thistle, European thistle, hemp, dandelion, dandelion and chickweed, and has good selectivity.

[0004] Since the long-term application of herbicides with a single mode of action will inevitably lead to the evolution of herbicide-resistant weed populations, resistant weeds continue to increase. Slowing down the development of amiloride-resistant weeds, increasing the weed-killing speed of amiloride and expanding the weed-killing spectrum will become the future development trend.

[0005] Amlodipine has long residual activity and is likely to cause residual phytotoxicity to the next crop. The next crop of sensitive crops should be planted 12-18 months apart.

[0006] Existing amiloride herbicides, such as the compound pesticide composition, preparation and application containing amiloride or its salts with application number 201210223900.3, have the defects of poor rapid effect, high cost, insufficient long-lasting control effect, and easy precipitation at low temperature.

[0007] When used, although amlodipine triethanolammonium salt has better control effect on general broadleaf weeds and grass weeds than amlodipine potassium salt and amlodipine monoethanolamine salt, amlodipine triethanolammonium salt is unstable at low temperatures and easily solidifies, so it is not suitable for use in the north. Summary of the invention

[0008] The object of the present invention is to overcome the above-mentioned shortcomings and provide a high-efficiency auxiliary agent for a triethanolammonium amitraz salt solution. The aqueous solution obtained by using the auxiliary agent is not easy to solidify at low temperature, is environmentally friendly, has a small dosage, has obvious synergy, is low in cost, and can significantly increase the preparation stability of the triethanolammonium amitraz salt solution.

[0009] In order to achieve the above-mentioned invention object, the specific technical scheme is as follows:

[0010] A synergistic auxiliary agent for amloprotial acid triethanolammonium salt solution, which is prepared from the following components in percentage by weight:

[0011]

[0012] Preferred:

[0013] The described amloprotinic acid triethanolammonium salt solution synergistic aid is made of the following components in percentage by weight:

[0014]

[0015] Most preferred:

[0016] The described amloprotinic acid triethanolammonium salt solution synergistic aid is made of the following components in percentage by weight:

[0017]

[0018]

[0019] The auxiliary agent of the present invention is particularly suitable for amiloride triethanolammonium salt solution with an active ingredient content of about 240 g / L.

[0020] The dosage of the above-mentioned auxiliary agent in the composite aqueous solution is 5%-25%, and the preferred dosage is 10%.

[0021] The preparation method of the triethanolammonium salt solution synergistic aid of amloprotilinic acid comprises the following steps: adding water and sodium diisooctyl sulfosuccinate into a reaction kettle, starting stirring, adding dihydrogenated tallow dimethyl ammonium chloride, heating to 40-50° C. and stirring evenly, then adding hydrogenated tallow amine acetate and stirring evenly, and finally adding hexadecyl dimethyl allyl ammonium chloride and stirring evenly.

[0022] The sodium diisooctyl sulfosuccinate surfactant added in the formula of the present invention can effectively improve the permeability and strength, spreadability and physical sealing effect of the triethanolammonium salt preparation of amlodipine, and improve the efficacy without increasing the dosage. Dihydrogenated tallow dimethyl ammonium chloride can be strongly adsorbed on the surface of the pesticide active material particles, while providing electrostatic repulsion and steric hindrance. Hydrogenated tallow amine acetate has strong salt resistance. As an anionic surfactant, it can enhance the adhesion of the liquid medicine in the formula of the present invention and improve the utilization rate of the pesticide. Hexadecyl dimethyl allyl ammonium chloride can synergistically wet and disperse the surface of the original drug particles and improve the efficacy. The formula of the present invention prevents the entire preparation system from precipitation at low temperatures.

[0023] Compared with the prior art, the present invention has the following advantages:

[0024] The sodium acifluorfen salt solution processed by the present invention has obvious synergistic effect, is not easy to solidify at low temperature, can improve the lasting effect, delay the generation of weed resistance, reduce the number of repeated use of pesticides, reduce the amount of pesticides used, and reduce agricultural costs. It has the characteristics of good formulation stability, high efficiency, high environmental and biological safety, and has good application prospects. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 These are photos of Example 7 amiloride triethanolammonium saline solution (left) and commercially available 240 g / L amiloride triethanolammonium saline solution (right) before application.

[0026] Figure 2 This is a comparison photo of the efficacy of the amloprothiolane triethanolammonium saline solution (left) of Example 7 and the commercially available 240g / L amloprothiolane triethanolammonium saline solution (right) (third day after application)

[0027] Figure 3 This is a comparison photo of the efficacy of the amloprothiolane triethanolammonium saline solution (left) of Example 7 and the commercially available 240g / L amloprothiolane triethanolammonium saline solution (right) (seventh day after application)

[0028] Figure 4 The stability comparison photographs of the amiloride triethanolammonium saline solution of Example 8 (left) and the amiloride triethanolammonium saline solution of Example 11 (right) after cold storage (0±1° C.) for 14 days are shown. DETAILED DESCRIPTION

[0029] The technical solution of the present invention is further described in detail below in conjunction with several preferred embodiments and drawings. This embodiment is implemented on the premise of the technical solution of the invention, and a detailed implementation method and specific operation process are given, but the protection scope of the present invention is not limited to the following embodiments.

[0030] The experimental methods described in the following examples, unless otherwise specified, are conventional methods and are performed according to the techniques or conditions described in the literature in the art or according to the product instructions.

[0031] Unless otherwise specified, the materials and reagents described in the following examples can be obtained from commercial sources. Among them, dihydrogenated tallow dimethyl ammonium chloride was purchased from Shanghai Gewu Chemical Co., Ltd., hydrogenated tallow amine acetate was purchased from Zhangjiagang Hanbadu Chemical Co., Ltd., hexadecyl dimethyl allyl ammonium chloride was purchased from Shandong Polyfa Biotechnology Co., Ltd., and sodium diisooctyl sulfosuccinate was purchased from Hai'an Petrochemical Plant in Jiangsu Province.

[0032] Example 1

[0033] formula:

[0034]

[0035] Example 2

[0036] formula:

[0037]

[0038]

[0039] Example 3

[0040] formula:

[0041]

[0042] Example 4

[0043] formula:

[0044]

[0045] Example 5

[0046] formula:

[0047]

[0048] The preparation method of the auxiliary agent of Example 1-5 is as follows: add water and sodium diisooctyl sulfosuccinate to a reaction kettle, start stirring, add dihydrogenated tallow dimethyl ammonium chloride, heat to 40-50°C and stir evenly, then add hydrogenated tallow amine acetate, stir evenly, and finally add hexadecyl dimethyl allyl ammonium chloride and stir evenly.

[0049] Comparative Example 1

[0050]

[0051] The preparation method is as follows: add water into a reaction kettle, start stirring, add dihydrogenated tallow dimethyl ammonium chloride, heat to 40-50°C and stir evenly, then add hydrogenated tallow amine acetate, stir evenly, and finally add hexadecyl dimethyl allyl ammonium chloride and stir evenly.

[0052] Comparative Example 2

[0053]

[0054] The preparation method is as follows: add water and sodium diisooctyl sulfosuccinate into a reaction kettle, start stirring, add dihydrogenated tallow dimethyl ammonium chloride, heat to 40-50° C. and stir evenly, finally add hexadecyl dimethyl allyl ammonium chloride and stir evenly.

[0055] Comparative Example 3

[0056]

[0057] The preparation method is as follows: add water and sodium diisooctyl sulfosuccinate into a reaction kettle, start stirring, add styrylphenol polyoxyethylene ether, heat to 40-50°C and stir evenly, then add hydrogenated tallow amine acetate and stir evenly, and finally add hexadecyl dimethyl allyl ammonium chloride and stir evenly.

[0058] Comparative Example 4

[0059]

[0060] Preparation method: Add water and sodium diisooctyl sulfosuccinate into a reaction kettle, start stirring, add dihydrogenated tallow dimethyl ammonium chloride, heat to 40-50°C and stir evenly, then add sodium dodecyl sulfate and stir evenly, finally add hexadecyl dimethyl allyl ammonium chloride and stir evenly.

[0061] Comparative Example 5

[0062]

[0063] Preparation method: Add water and sodium diisooctyl sulfosuccinate into a reaction kettle, start stirring, add dihydrogenated tallow dimethyl ammonium chloride, heat to 40-50°C and stir evenly, then add hydrogenated tallow amine acetate, stir evenly, and finally add fatty alcohol polyoxyethylene ether and stir evenly.

[0064] Example 6 (Application Example 1)

[0065] The preparation process of amiloride triethanolammonium salt solution is as follows: first, amiloride raw powder and water are added into a reaction kettle, and triethanolamine is dripped from the hole (12.04g of triethanolamine with a mass concentration of 78% is dripped for every 100g of amiloride). After the dripping is completed, stirring is carried out at a constant temperature of 50°C for about 1 hour, and an auxiliary agent (prepared by the method of Example 1) with a mass% of the aqueous solution is added, and stirring is carried out for about 30 minutes. The prepared aqueous solution contains 20.69% of amiloride, that is, 240g / L of amiloride triethanolammonium salt solution.

[0066] The prepared aqueous solution has the appearance of a light yellow, transparent, non-viscous liquid. There is no stratification or precipitation when cold-stored (0±1°C) or hot-stored (54±2°C) for 14 days, respectively, and the cold and hot storage stability is good.

[0067] Example 7 (Application Example 2)

[0068] The preparation process of amloprotinic acid triethanolammonium salt solution is the same as that of Example 6, except that the auxiliary agent is prepared by the method of Example 2. The prepared aqueous solution has a light yellow transparent non-viscous liquid appearance, and has no stratification or precipitation after cold storage (0±1°C) and hot storage (54±2°C) for 14 days, respectively, and has good cold and hot storage stability.

[0069] Example 8 (Application Example 3)

[0070] The preparation process of amloprotinic acid triethanolammonium salt solution is the same as that of Example 6, except that the auxiliary agent used is prepared by the method of Example 3. The prepared aqueous solution has a light yellow transparent non-viscous liquid appearance, and has no stratification or precipitation after cold storage (0±1°C) and hot storage (54±2°C) for 14 days, respectively, and has good cold and hot storage stability.

[0071] Example 9 (Application Example 4)

[0072] The preparation process of amloprotinic acid triethanolammonium saline solution is the same as that of Example 6, except that the auxiliary agent used is prepared by the method of Comparative Example 1.

[0073] The prepared aqueous solution showed no stratification or precipitation when stored cold (0±1°C) or hot (54±2°C) for 14 days, and had good stability during cold and hot storage.

[0074] The field efficacy experiment shows that the addition of sodium diisooctyl sulfosuccinate to the formula of the present invention has a significant synergistic effect, a stronger quick effect, and a faster weed killing effect.

[0075] Example 10 (Application Example 5)

[0076] The preparation process of triethanolammonium ammonium salt solution of amloprothiolane is the same as that of Example 6. The difference is that the auxiliary agent used is prepared by the method of Comparative Example 2. The prepared aqueous solution has no stratification or precipitation during cold storage (0±1°C) and hot storage (54±2°C) for 14 days, and has good cold and hot storage stability.

[0077] The comparison of the efficacy experiments in the field shows that the addition of hydrogenated tallow amine acetate to the formula of the present invention has a significant preventive effect and a good persistence of efficacy.

[0078] Example 11 (Application Example 6)

[0079] The preparation process of amloprotinic acid triethanolammonium salt solution is the same as that of Example 6, except that the auxiliary agent used is prepared by the method of Comparative Example 3.

[0080] The prepared aqueous solution precipitated when stored in cold (0±1°C), but did not stratify when stored in hot (54±2°C) for 14 days.

[0081] Example 12 (Application Example 7)

[0082] The preparation process of amloprotinic acid triethanolammonium salt solution is the same as that of Example 6, except that the auxiliary agent used is prepared by the method of Comparative Example 4.

[0083] The prepared aqueous solution precipitated when stored in cold (0±1°C), but did not stratify when stored in hot (54±2°C) for 14 days.

[0084] Field efficacy experiment

[0085] Test reagents: Example 7-11 amiloride triethanolammonium saline solution, commercially available 240g / L amiloride triethanolammonium saline solution,

[0086] Target plants for control: Solanum nigrum, Amaranthus tricolor, Ragweed, etc.

[0087] Test method: Select 6 10 2 For wasteland with uniform grass phase, six test grasslands were treated with amlodipine triethanolammonium salt solution treatment A of Example 7, amlodipine triethanolammonium salt solution treatment B of Example 8, amlodipine triethanolammonium salt solution treatment C of Example 9, amlodipine triethanolammonium salt solution treatment D of Example 10 and amlodipine triethanolammonium salt solution treatment E of Example 11, and commercially available amlodipine triethanolammonium salt solution F with a concentration of 240 g / L.

[0088] The fields were randomly arranged and the effective ingredient of amloprotien was 0.6 kg / hm 2 , add 600L of water per hectare for spraying, and observe the efficacy before treatment, on the third day after application, and on the seventh day after application. Record the fresh weight prevention effect after 7 days.

[0089] Control effect = (Weed mass in control area - Weed mass in treatment area) / Weed mass in control area × 100% The results of the efficacy observation on the third day after application are shown in Table 1:

[0090] Table 1

[0091]

[0092]

[0093] The results of the efficacy and control effect on the seventh day after application are recorded in Table 2:

[0094] Table 2

[0095]

[0096] From the above data results obtained from the field efficacy test, it can be seen that the 240g / L amiloride triethanolammonium salt solution prepared by the present invention has obvious protective effect 7 days after application, better rapidity, and long lasting effect, compared with the existing commercially available 240g / L amiloride triethanolammonium salt solution, which can reduce the amount of pesticide used and agricultural costs, significantly reduce costs, and is safer for the environment.

Claims

1. A synergistic aid for amloprotinic acid triethanolammonium salt solution, characterized in that The additive is made of the following components in percentage by weight:

2. The synergistic aid of amloprothiolane triethanolammonium salt solution according to claim 1, characterized in that The additive is made of the following components in percentage by weight:

3. The synergistic aid of amloprothiolane triethanolammonium salt solution according to claim 1, characterized in that The additive is made of the following components in percentage by weight:

4. The synergistic aid of triethanolammonium salt solution of amloprothiolane according to claim 1, 2 or 3, characterized in that The dosage of the auxiliary agent in the compound water agent is 5%-25%.

5. The synergistic aid of triethanolammonium salt solution of amloprothiolane according to claim 4, characterized in that The dosage of the auxiliary agent in the composite aqueous solution is 10%.

6. A method for preparing the synergistic aid of triethanolammonium salt solution of amloprothiolane according to claim 1, 2 or 3, characterized in that The method comprises the following steps: adding water and sodium diisooctyl sulfosuccinate into a reaction kettle, starting stirring, adding dihydrogenated tallow dimethyl ammonium chloride, heating to 40-50° C. and stirring evenly, then adding hydrogenated tallow amine acetate and stirring evenly, and finally adding hexadecyl dimethyl allyl ammonium chloride and stirring evenly.

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