Preparation method of anionic vesicle tank mixing auxiliary agent

Abstract

The invention relates to the technical field of tank mixing aids, and particularly discloses a preparation method of an anion vesicle tank mixing aid. Comprising the following operation steps: S1, adding 40wt% of an alkali solution into a component A, carrying out heating reaction, carrying out heat preservation aging, removing moisture, cooling to 20-25 DEG C, adding ethanol, and uniformly mixing, so as to obtain a component B; s2, in a nitrogen atmosphere, heating fatty acid monoglyceride to 80-85 DEG C, adding sulfamic acid and a catalyst, uniformly mixing, heating to 120-125 DEG C, reacting for 3-3.5 hours, adding propylene glycol, and uniformly mixing to obtain a component C; and S3, uniformly mixing the component A, the component B, the component C and the component D, and adjusting the pH value with sodium dihydrogen phosphate and disodium hydrogen phosphate to obtain the anion vesicle tank mix additive.

Description

Technical Field

[0001] The invention relates to the technical field of barrel-mixing additives, and in particular to a method for preparing an anionic vesicle barrel-mixing additive. Background Art

[0002] With the popularization of agricultural mechanization, pesticides of different varieties and dosage forms are often mixed and used in actual use, and are often used through secondary dilution. The dilution multiple during the first dilution is small, so flocculation and precipitation often occur, clogging the spray nozzles.

[0003] Tank-mixed adjuvants are directly poured into the diluted water together with the pesticide formulation and stirred evenly. They are a kind of adjuvant product that can be mixed and used immediately. Since they do not need to be added to the pesticide formulation, they are not restricted by content, miscibility with pesticides, and mutual influence and decomposition, so the selection range is wider. Not only can surfactants be used to improve the adhesion, distribution, and penetration of the liquid on the target, but also by adding ingredients with biological functions to improve the metabolic transport of pesticides in plants, and even have a regulatory effect to improve the efficacy.

[0004] At present, the tank-mix adjuvants on the market are still at the stage of directly transferring adjuvants for pesticide formulations to tank-mix adjuvants, or simply mixing bioactive ingredients (oils, lecithin, hormones, etc.) with surfactants for use. There is no further in-depth research and development through systematic physiological and biochemical reactions of plants and animals, and the market prospects are broad.

[0005] In summary, the preparation of an anionic vesicle barrel mix additive is of great significance. Summary of the invention

[0006] The object of the present invention is to provide a method for preparing an anionic vesicle barrel mix auxiliary agent to solve the problems raised in the above background technology.

[0007] In order to solve the above technical problems, the present invention provides the following technical solutions: A method for preparing an anionic vesicle barrel mix auxiliary agent comprises the following steps: S1: adding 40wt% alkali solution to component A, heating for reaction, heat preservation for aging, removing moisture, cooling to 20℃~25℃, adding ethanol and mixing evenly to obtain component B; S2: In a nitrogen atmosphere, monoglyceride is heated to 80°C-85°C, aminosulfonic acid and a catalyst are added, mixed evenly, heated to 120°C-125°C for reaction for 3-3.5 hours, propylene glycol is added and mixed evenly to obtain component C; S3: Component A, component B, component C, and component D are uniformly mixed, and the pH is adjusted with sodium dihydrogen phosphate and disodium hydrogen phosphate to obtain an anionic vesicle barrel mix auxiliary agent.

[0008] In the scheme, the heating reaction is carried out until the alkali reaction is complete and then the thermal aging is carried out.

[0009] More optimally, the anionic vesicle barrel mix auxiliary agent includes the following components: by mass percentage, component A and component B total 70%~80%, 5%~10% component C, and 15%~20% component D.

[0010] More optimally, 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; the component D is one or more of dodecylbenzene sulfonate, Tween 80, fatty acid amide propyl betaine, and alkyl glycoside.

[0011] More optimally, the molar ratio of the fatty acid to the fatty acid salt is 2:(1-1.2).

[0012] More preferably, 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.

[0013] Preferably, the alkali in the alkali solution is one of sodium hydroxide, potassium hydroxide, isopropylamine, dimethylamine, monoethanolamine, and ethylamine; and the molar ratio of component A to the alkali is 1:(0.95-1).

[0014] More optimally, the molar ratio of the monoglyceride, aminosulfonic acid and catalyst is 1:(0.9~1):(0.3~0.5).

[0015] In the scheme, the catalyst is crushed urea.

[0016] More optimally, in S1, the temperature of the heating reaction is 70°C to 80°C; in S2, the pH is 6.5 to 7.5.

[0017] Compared with the prior art, the beneficial effects achieved by the present invention are: The anionic vesicle barrel mix adjuvant of the present invention can self-assemble into stable multilayer vesicles in water at a pH of 5 to 8. Since the vesicles are amphiphilic, they can encapsulate lipophilic and hydrophilic substances, so that the mixed pesticides and fertilizers are respectively encapsulated in different vesicles to avoid flocculation and sedimentation caused by mutual interaction. The vesicles can also form a layer of membrane on the surface of plants, seal and oil the cell wall, promote the absorption of water in the liquid medicine by the plant, and then promote drug metabolism. DETAILED DESCRIPTION

[0018] The following is a preferred implementation of the embodiment of the present invention. Obviously, the described embodiment is only a part of the embodiment of the present invention, not all of the embodiments. For ordinary technicians in this technical field, all other embodiments obtained by ordinary technicians in this field without creative work without departing from the principle of the embodiment of the present invention are within the scope of protection of the present invention.

[0019] In this embodiment, it should be noted that the purchase manufacturers of all raw materials involved in the present invention are not subject to any special restrictions, and exemplary examples include: diuron and thidiazuron (suspension concentrate) were purchased from Henan Changjiang Biotechnology Co., Ltd., 40% ethephon (aqueous solution) was purchased from Hubei Iprole Biotechnology Co., Ltd., S-isopropylamine (emulsifiable concentrate) was purchased from Shandong Binnong Technology Co., Ltd., thifensulfuron-methyl (wettable powder) was purchased from Shaanxi Shanggezhilu Bioscience Co., Ltd., amino oligosaccharides (aqueous solution) was purchased from Dalian Kaifei Chemical Co., Ltd., and alkyl ethyl sulfonate was purchased from Nanjing Taihua Chemical Co., Ltd. Example

[0020] Add 30 g of component A (oleic acid) into a 250 mL three-necked round-bottom flask, install a condenser, turn on magnetic stirring, add 14.57 g of 40 wt% potassium hydroxide aqueous solution in batches, heat to 80°C until the alkali reacts completely, keep warm and age for 1 hour, remove the condenser, heat and evaporate the water, cool to 25°C, add 34.04 g of ethanol and stir evenly to obtain component B, which is a 50 wt% potassium oleate ethanol solution. Example

[0021] Add 50 g of monoolein into a 250 mL three-necked round-bottom flask, install a condenser and a nitrogen gas guide tube, turn on magnetic stirring, heat to 80 ° C under a nitrogen atmosphere, add 13.62 g of aminosulfonic acid and 3.37 g of catalyst (crushed urea), heat to 125 ° C, stir and react for 3 hours, add 63.6 g of propylene glycol and stir until completely dissolved, cool to obtain component C, which is a propylene glycol solution of 50 wt% olein ammonium sulfate. Example

[0022] 35 g of oleic acid (component A), 39.72 g of 50 wt% potassium oleate ethanol solution (component B), 6 g of 50 wt% oleyl glycerol ammonium sulfate propylene glycol solution (component C), 10 g of sodium dodecylbenzene sulfonate and 8.98 g of APG0810 (component D) were uniformly mixed, and the pH was adjusted to 6.9 with 0.2 g of sodium dihydrogen phosphate and 0.1 g of sodium dihydrogen phosphate to obtain an anionic vesicle barrel mix auxiliary agent. Example

[0023] 15 mL of suspension concentrate (540 g / L diuron + thidiazuron), 100 mL of aqueous solution (40% ethephon), 60 mL of anionic vesicle barrel mix auxiliary agent, and 40 kg of water were uniformly mixed to obtain treatment 1; there was no obvious floating or sinking within 30 minutes. Example

[0024] Evenly mix 30 mL of emulsifiable concentrate (960 g / L S-isopropylamine), 0.6 g of wettable powder (75% thifensulfuron-methyl), 60 mL of aqueous solution (2% amino oligosaccharides), 20 mL of anionic vesicular barrel mix adjuvant, and 2 L of water.

[0025] Comparative Example 1: 15 mL of suspension concentrate (540 g / L diuron + thidiazuron), 100 mL of aqueous solution (40% ethephon), 60 mL of 288 g / L alkyl ethyl sulfonate, and 40 kg of water were uniformly mixed to obtain treatment 2; there was no obvious floating or sinking within 30 minutes.

[0026] Comparative Example 2: Evenly mix 30 mL of emulsifiable concentrate (960 g / L S-isopropylamine), 0.6 g of wettable powder (75% thifensulfuron-methyl), 60 mL of aqueous solution (2% amino oligosaccharides), 20 mL of 63% polyol-type nonionic surfactant, and 2 L of water.

[0027] Detection experiment: (1) Experimental design: A film with 4 rows, a 30+60cm wide and narrow row pattern, and a plant spacing of 9cm were used. The experiment set up two groups, Example 4 and Comparative Example 1, and one group without adding a barrel-mixed adjuvant as a control group CK. Each treatment area was 1 mu, and the total experimental land was 3 mu; 5 points were selected in each plot using the diagonal method, and 10 cotton plants were continuously selected at each point, and they were marked with a sign before spraying; the spray volume was 40L / mu, and mechanical spraying was uniformly adopted; Treatment 1 was Example 4, and Treatment 2 was Comparative Example 1, as shown in Table 1.

[0028] (2) Sampling and measurement: The total boll number and boll opening number of each treatment 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. The total number of leaves, total number of bolls and boll opening number of cotton plants were recorded, and the shedding rate and boll opening rate were calculated. The per mu yield at harvest was measured, as shown in Table 2 and Table 3. The specific calculation formula is as follows: Defoliation rate = (number of leaves before application - number of leaves during investigation) / number of leaves before application × 100%; The rate of unfurling before drug administration = the number of unfurling / the total number of bolls × 100%; The rate of boll opening after drug application = the number of boll opening after drug application / the total number of bolls before drug application × 100%.

[0029]

[0030] Table 1

[0031] Table 2 Conclusion: After spraying the defoliant, the defoliation rate increased continuously and the leaf hanging rate decreased with the increase of the application time; the defoliation rate of treatment 1 was higher than that of treatment 2 at each time; the defoliation rates of treatments 1 and 2 were significantly higher than those of CK at each time after application; the results showed that defoliant tank-mixed adjuvants play an important role in cotton defoliation technology, and the defoliation effect of treatment 1 was better than that of treatment 2.

[0032]

[0033] Table 3 Conclusion: The boll opening rates of each treatment were similar 7 days before application. 7 days after application, the boll opening rates of treatments 1 and 2 were slightly higher than those of CK. 15 days after application, the boll opening rates of each treatment were higher than those of CK, and treatment 1 was significantly better than treatment 2. 20 days and 30 days after application, treatment 1 was slightly better than treatment 2, and both were significantly better than CK. Treatment 1 had the best boll opening effect.

[0034] In summary, the barrel-mixed synergist is significantly helpful for cotton defoliation and boll opening, and the anionic vesicle barrel-mixed synergist is significantly better than the 288g / L alkyl ethyl sulfonate commonly used on the market.

[0035]

[0036] Table 4 Conclusion: Compared with the 63% polyol nonionic surfactant commonly used in the market, the anionic vesicle barrel mix additive has better anti-flocculation and precipitation effects under the dosage form compounding and secondary dilution method.

[0037] Finally, it should be noted that the above is only a preferred embodiment of the present invention, but the protection scope of this application is not limited thereto. Any changes or substitutions that can be easily thought of by any technician familiar with the technical field within the spirit and principle of the present invention and within the technical scope disclosed in this application should be included in the protection scope of this application; in the absence of conflict, the embodiments of this application and the features in the embodiments can be combined with each other. Therefore, the protection scope of this application shall be based on the protection scope of the claims.

Claims

1. A method for preparing an anionic vesicle barrel mix auxiliary agent, characterized in that: The steps include: S1: adding 40wt% alkali solution to component A, heating for reaction, heat preservation for aging, removing moisture, cooling to 20℃~25℃, adding ethanol and mixing evenly to obtain component B; S2: In a nitrogen atmosphere, monoglyceride is heated to 80°C-85°C, aminosulfonic acid and a catalyst are added, mixed evenly, heated to 120°C-125°C for reaction for 3-3.5 hours, propylene glycol is added and mixed evenly to obtain component C; S3: Component A, component B, component C, and component D are uniformly mixed, and the pH is adjusted with sodium dihydrogen phosphate and disodium hydrogen phosphate to obtain an anionic vesicle barrel mix auxiliary agent.

2. The method for preparing an anionic vesicle barrel mix auxiliary agent according to claim 1, characterized in that: The anionic vesicle barrel mix auxiliary agent includes the following components: by mass percentage, component A and component B total 70% to 80%, 5% to 10% component C, and 15% to 20% component D.

3. The method for preparing an anionic vesicle barrel mix auxiliary agent according to claim 1, characterized in that: The component B is a 50wt% fatty acid salt ethanol solution; the component A is a fatty acid; the component C is a 50wt% fatty acid glyceride ammonium sulfate propylene glycol solution; the component D is one or more of dodecylbenzene sulfonate, Tween 80, fatty acid amide propyl betaine, and alkyl glycoside.

4. The method for preparing an anionic vesicle barrel mix auxiliary agent according to claim 3, characterized in that: The molar ratio of the fatty acid to the fatty acid salt is 2:(1-1.2).

5. The method for preparing an anionic vesicle barrel mix auxiliary agent according to claim 3, 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.

6. The method for preparing an anionic vesicle barrel mix auxiliary agent 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).

7. The method for preparing an anionic vesicle barrel mix auxiliary agent according to claim 1, characterized in that: The molar ratio of the monoglyceride, aminosulfonic acid and catalyst is 1:(0.9-1):(0.3-0.5).

8. The method for preparing an anionic vesicle barrel mix auxiliary agent according to claim 1, characterized in that: In S1, the temperature of the heating reaction is 70°C to 80°C; in S2, the pH is 6.5 to 7.5.

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