A method for preparing an anionic vesicular bucket-mixing aid

Abstract

The application relates to the technical field of barrel-mixed auxiliary agents, and particularly discloses a preparation method of an anionic vesicular barrel-mixed auxiliary agent. The method comprises the following operation steps: S1: adding a 40wt% alkali solution into component A, heating and reacting, aging, removing water, cooling to 20-25 DEG C, adding ethanol and uniformly mixing to obtain component B; S2: under a nitrogen atmosphere, heating monoglyceride to 80-85 DEG C, adding sulfamic acid and a catalyst, uniformly mixing, heating to 120-125 DEG C and reacting for 3-3.5 hours, adding propylene glycol and uniformly mixing to obtain component C; and S3: uniformly mixing component A, component B, component C and component D, adjusting the pH by using sodium dihydrogen phosphate and disodium hydrogen phosphate to obtain the anionic vesicular barrel-mixed auxiliary agent.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of barrel mixing adjuvant, in particular to a preparation method of anionic vesicle barrel mixing adjuvant. BACKGROUND

[0002] With the popularization of agricultural mechanization, different varieties and different types of pesticides are often mixed and used through secondary dilution in actual use, and the dilution multiple is small in the first dilution, so that flocculation, precipitation and other phenomena often occur, and the spray nozzle is blocked.

[0003] The barrel mixing adjuvant is directly poured into the diluted water together with the pesticide preparation for stirring, which is a kind of adjuvant product for mixing and using at present; since it does not need to be added to the pesticide preparation, it is not limited by the content, mutual solubility and mutual influence and decomposition, and the selection range is wider. Not only can the surface active agent be used to improve the adhesion, spreading and penetration of the pesticide liquid on the target, but also the biological functional components can be added to improve the metabolism and transport of the pesticide in the plant body, and even the pesticide itself has a regulating effect to improve the efficacy.

[0004] At present, the barrel mixing adjuvant on the market is still in the stage of directly transporting the pesticide preparation adjuvant to the barrel mixing adjuvant, or simply mixing the biological active components (oil, lecithin, hormone, etc.) with the surface active agent, without further research and development through the systematic physiological and biochemical reactions of animals and plants, so the market prospect is broad.

[0005] In view of the above, it is of great significance to prepare an anionic vesicle barrel mixing adjuvant. SUMMARY

[0006] The present application aims to provide a preparation method of an anionic vesicle barrel mixing adjuvant to solve the problems in the background art.

[0007] In order to solve the above technical problems, the present application provides the following technical scheme:

[0008] A preparation method of an anionic vesicle barrel mixing adjuvant, comprising the following operation steps:

[0009] S1: 40wt% alkali solution is added to component A, heated and reacted, aged, water is removed, and cooled to 20℃~25℃, ethanol is added and uniformly mixed to obtain component B;

[0010] S2: under the atmosphere of nitrogen, monoglyceride is heated to 80℃~85℃, aminosulfonic acid and a catalyst are added and uniformly mixed, the temperature is raised to 120℃~125℃ and reacted for 3~3.5 hours, and propylene glycol is added and uniformly mixed to obtain component C;

[0011] S3: uniformly mixing component A, component B, component C and component D, adjusting pH with sodium dihydrogen phosphate and disodium hydrogen phosphate to obtain an anionic vesicle bucket mixed aid.

[0012] In the scheme, the reaction is heated to complete the base reaction and then aged.

[0013] More preferably, the anionic vesicle bucket mixed aid comprises the following components: 70-80% of component A and component B, 5-10% of component C and 15-20% of component D by mass percentage.

[0014] More preferably, the component A is a fatty acid; the component B is a 50wt% fatty acid salt ethanol solution; the component C is a 50wt% fatty acid glyceride ammonium sulfate propylene glycol solution; and the component D is one or more of dodecyl benzene sulfonate, Tween 80, fatty acid amide propyl betaine and alkyl glycoside.

[0015] More preferably, the molar ratio of the fatty acid to the fatty acid salt is 2:(1-1.2).

[0016] More preferably, the molecular formula of the fatty acid salt in the component B is CH3(CH2) m COOR, m=7-16; the molecular formula of the component A is CH3(CH2) m COOH, m=7-16; and the molecular formula of the component C is CH3(CH2) n COOC-C(OH)-COSO3NH4, n=10-16.

[0017] More preferably, the base in the base solution is one of sodium hydroxide, potassium hydroxide, isopropylamine, dimethylamine, monoethanolamine and ethylamine; and the molar ratio of the component A to the base is 1:(0.95-1).

[0018] More preferably, the molar ratio of the single fatty acid glyceride, sulfamic acid and catalyst is 1:(0.9-1):(0.3-0.5).

[0019] In the scheme, the catalyst is pulverized urea.

[0020] More preferably, in S1, the temperature of the heating reaction is 70-80°C; and in S2, the pH is 6.5-7.5.

[0021] Compared with the prior art, the present application has the following beneficial effects:

[0022] The anionic vesicle bucket mixing aid of the present application can self-assemble into stable multilayer vesicles in water at pH 5-8, since the vesicles have amphiphilicity, they can wrap lipophilic and hydrophilic substances, so that the mixed pesticide and chemical fertilizer are wrapped in different vesicles, avoiding flocculation and settlement caused by mutual interaction. The vesicles can also form a film on the surface of plants, sealing and oiling the cell wall, promoting the absorption of water in the drug solution by plants, and further promoting drug metabolism. DETAILED DESCRIPTION

[0023] The following describes preferred embodiments of the present application. It is obvious that the described embodiments are only part of the embodiments of the present application, but not all the embodiments. For ordinary skilled in the art, all other embodiments obtained without creative labor under the premise of not departing from the principles of the embodiments of the present application, belong to the scope of protection of the present application.

[0024] In this embodiment, it should be noted that there is no special restriction on the purchase manufacturer of all raw materials involved in the present application, which exemplarily includes: diuron and thifensulfuron-methyl (suspension agent) purchased from Henan Common Biological Technology Co., Ltd., 40% ethephon (aqueous agent) purchased from Hubei Yipule Biological Technology Co., Ltd., precision isopropyl methylamine (emulsion) purchased from Shandong Binagro Technology Co., Ltd., thifensulfuron-methyl (wettable powder) purchased from Shaanxi Shanggelu Biological Science Co., Ltd., amino oligosaccharide (aqueous agent) purchased from Dalian Kaifei Chemical Co., Ltd., and alkyl ethyl sulfonate purchased from Nanjing Taihua Chemical Co., Ltd. EMBODIMENT

[0025] 30g of component A (oleic acid) was added to a 250mL three-necked round-bottom flask, a condenser tube was installed, magnetic stirring was started, 14.57g of 40wt% potassium hydroxide aqueous solution was added in batches, heated to 80℃, until the base completely reacted, aged for 1 hour, the condenser tube was removed, heated to evaporate the water, cooled to 25℃, 34.04g of ethanol was added and stirred uniformly to obtain component B, which was a 50wt% potassium oleate ethanol solution.

[0026] 50g of monoolein was added to a 250mL three-necked round-bottom flask, a condenser tube and a nitrogen gas inlet tube were installed, magnetic stirring was started, heated to 80℃ under nitrogen atmosphere, 13.62g of sulfamic acid and 3.37g of catalyst (powdered urea) were added, the temperature was raised to 125℃, and the reaction was stirred for 3 hours, 63.6g of propylene glycol was added and stirred until completely dissolved, and then cooled to obtain component C, which was a 50wt% oleic acid glycerol solution of ammonium sulfate.

[0027] Mix 35 g of oleic acid (component A), 39.72 g of 50 wt% potassium oleate ethanol solution (component B), 6 g of 50 wt% glyceryl oleate ammonium sulfate propylene glycol solution (component C), 10 g of sodium dodecylbenzenesulfonate, and 8.98 g of APG0810 (component D) uniformly, adjust the pH to 6.9 with 0.2 g of sodium dihydrogen phosphate and 0.1 g of disodium hydrogen phosphate, to obtain an anionic vesicle tank-mix adjuvant.

[0028] Mix 15 mL of a suspension agent (540 g / L of diuron + thidiazuron), 100 mL of a water agent (40% ethephon), 60 mL of an anionic vesicle tank-mix adjuvant, and 40 kg of water uniformly to obtain treatment 1; no obvious floating or sinking is observed for 30 minutes.

[0029] Mix 30 mL of an emulsifiable concentrate (960 g / L of s-metolachlor), 0.6 g of a wettable powder (75% thifensulfuron-methyl), 60 mL of a water agent (2% oligosaccharide), 20 mL of an anionic vesicle tank-mix adjuvant, and 2 L of water uniformly.

[0030] Comparative Example 1:

[0031] Mix 15 mL of a suspension agent (540 g / L of diuron + thidiazuron), 100 mL of a water agent (40% ethephon), 60 mL of 288 g / L of an alkyl ethyl sulfonate, and 40 kg of water uniformly to obtain treatment 2; no obvious floating or sinking is observed for 30 minutes.

[0032] Comparative Example 2:

[0033] Mix 30 mL of an emulsifiable concentrate (960 g / L of s-metolachlor), 0.6 g of a wettable powder (75% thifensulfuron-methyl), 60 mL of a water agent (2% oligosaccharide), 20 mL of 63% polyol nonionic surfactant, and 2 L of water uniformly.

[0034] Test experiment: (1) Experimental design:

[0035] A film 4 rows, 30+60 cm wide and narrow row mode, plant spacing 9 cm, test set example 4 and comparative example 1 two groups, one without tank-mix adjuvant as a control group CK, each treatment area is 1 mu, and the test land is 3 mu; adopt the diagonal line method to select 5 points in each plot, and continuously select 10 cotton plants for each point; mark before spraying; the spraying amount is 40 L / mu, and the mechanical spraying is uniformly adopted; treatment 1 is example 4, and treatment 2 is comparative example 1, as shown in Table 1.

[0036] (2) Sampling and determination:

[0037] The total number of bolls and the number of bolls shedding were investigated 7 days before spraying, and the marked plants were investigated on the day of spraying and 7 days, 15 days, 20 days and 30 days after spraying, respectively. The total number of leaves, the total number of bolls and the number of bolls shedding were recorded, and the shedding rate and the shedding rate were calculated. The yield per mu at harvest was measured, as shown in Tables 2 and 3. The specific calculation formula is as follows:

[0038] Leaf shedding rate = (number of leaves before spraying - number of leaves at the time of investigation) / number of leaves before spraying x 100%;

[0039] Pre-spraying shedding rate = number of bolls shedding / total number of bolls x 100%;

[0040] Post-spraying shedding rate = number of bolls shedding after spraying / total number of bolls before spraying x 100%.

[0041]

[0042] Table 1

[0043]

[0044] Table 2

[0045] Conclusion: After spraying the defoliation agent, the leaf shedding rate increases continuously with the increase of spraying time, and the leaf hanging rate decreases. The leaf shedding rate of treatment 1 at each time is higher than that of treatment 2. The leaf shedding rate of treatment 1 and treatment 2 at each time after spraying is significantly higher than that of CK. The results show that the bucket-mixed adjuvant plays an important role in the defoliation technology of cotton, and the defoliation effect of treatment 1 is better than that of treatment 2.

[0046]

[0047] Table 3

[0048] Conclusion: The shedding rate of cotton in each treatment is equivalent 7 days before spraying. 7 days after spraying, the shedding rate of cotton in treatment 1 and treatment 2 is slightly higher than that of CK. 15 days after spraying, the shedding rate of each treatment is higher than that of CK, and treatment 1 is significantly better than treatment 2. 20 days and 30 days after spraying, treatment 1 is slightly better than treatment 2, and both are significantly better than CK. The shedding effect of treatment 1 is the best.

[0049] In summary, the bucket-mixed synergist is obviously helpful for cotton defoliation and shedding, and the anionic vesicle bucket-mixed adjuvant is significantly better than the commonly used 288 g / L alkyl ethyl sulfonate on the market.

[0050]

[0051] Table 4

[0052] Conclusion: Compared with the commonly used 63% polyol nonionic surfactant on the market, the anionic vesicle bucket-mixed adjuvant has better anti-flocculation and precipitation effect under the mode of multiple dosage forms and secondary dilution.

[0053] Finally, it should be noted that the above only describes the preferred embodiments of the present application, but the protection scope of the present application is not limited thereto, any person skilled in the art can easily think of changes or replacements within the technical range disclosed by the present application, as long as they are within the spirit and principles of the present application, and should be covered within the protection scope of the present application; the embodiments and features in the embodiments can be combined with each other without conflict. Therefore, the protection scope of the present application should be subject to the protection scope of the claims.

Claims

1. A process for the preparation of an anionic vesicular bucket-mixing aid, characterized by: The method comprises the following steps: S1: adding 40wt% alkali solution into component A, heating reaction, aging, removing water, cooling to 20-25℃, adding ethanol and mixing to obtain component B; S2: under nitrogen atmosphere, heating monoglyceride to 80-85℃, adding sulfamic acid and catalyst, mixing, heating to 120-125℃ and reacting for 3-3.5 hours, adding propylene glycol and mixing to obtain component C; S3: mixing component A, component B, component C and component D, adjusting pH with sodium dihydrogen phosphate and disodium hydrogen phosphate to obtain anionic vesicle barrel mixing aid; The component B is 50wt% fatty acid salt ethanol solution; the component A is fatty acid; the component C is 50wt% fatty acid glyceride ammonium sulfate propylene glycol solution; and the component D is dodecyl benzene sulfonate and alkyl glycoside.

2. A process for the preparation of an anionic vesicle bucket mix adjuvant according to claim 1, characterized in that: The anionic vesicle barrel mixing aid comprises the following components: 70-80% component A and component B, 5-10% component C and 15-20% component D by mass percentage.

3. A process for the preparation of an anionic vesicle bucket mix adjuvant according to claim 1, characterized in that: The molar ratio of the fatty acid to the fatty acid salt is 2:(1-1.2).

4. A process for the preparation of an anionic vesicle bucket mix aid according to claim 1, characterized in that: The molecular formula of the fatty acid salt in component B is CH3(CH2) m COOR, m = 7~16; the molecular formula of component A is CH3(CH2) m COOH, m = 7~16; the molecular formula of component C is CH3(CH2) n COOC-C(OH)-COSO3NH4, n = 10~16.

5. A process for the preparation of an anionic vesicle bucket mix adjuvant according to claim 1, characterized in that: The alkali in the alkali solution is one of sodium hydroxide, potassium hydroxide, isopropylamine, dimethylamine, monoethanolamine and ethylamine; and the molar ratio of the component A to the alkali is 1:(0.95-1).

6. A process for the preparation of an anionic vesicle bucket mix adjuvant according to claim 1, characterized in that: The molar ratio of the monoglyceride, sulfamic acid and catalyst is 1:(0.9-1):(0.3-0.5).

7. A process for the preparation of an anionic vesicle bucket mix adjuvant according to claim 1, characterized in that: In S1, the heating reaction temperature is 70-80℃; and in S2, the pH is 6.5-7.5.

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