CN115868496A - A kind of brassinolide composition and preparation method thereof - Google Patents

Abstract

The invention belongs to the technical field of pesticide preparations, and particularly relates to a brassinolide composition and a preparation method thereof. The invention mainly aims at the characteristic that brassinolide needs to be diluted by tens of thousands of times in the application process, the diluted liquid medicine is sprayed on the super-hydrophobic plant leaves and is easy to rebound, sputter and deposit, and the like, the ammonium super-spreading agent with higher solubility in water is selected, the dosage of the ammonium super-spreading agent is increased to 56-72%, and the agricultural emulsion solubilizing surfactant is used as an auxiliary, the composition is prepared into a stable and transparent soluble liquid through a high-shear emulsifying machine, the preparation method is simple, the ejection and sputtering of the sprayed liquid drops on the super-hydrophobic plant leaves can be effectively inhibited after the ammonium super-spreading agent is diluted to the use concentration, the purposes of depositing, wetting, spreading and the like on the super-hydrophobic plant leaves can be achieved, and the pesticide utilization rate and the like can be effectively improved.

Description

A kind of brassinolide composition and preparation method thereof

technical field

The invention belongs to the technical field of pesticide preparations, and in particular relates to a brassinolide composition and a preparation method thereof.

Background technique

Brassinolide is a new type of green and environmentally friendly plant growth regulator. It can promote the growth of vegetables, melons, fruits, grains and other crops by soaking seeds with appropriate concentration of brassinolide and spraying stems and leaves, and improve the quality. Increase yield and be more resistant to storage.

At present, the brassinolide preparations are in the form of soluble agents, water agents, soluble granules, etc., wherein the content of auxiliary agents such as surfactants is generally about 10-20%, and it needs to be diluted 2000-100000 times when used. At such a dilution factor, the content of all additives will be less than 0.01%, which is very unfavorable for the deposition of spray droplets on superhydrophobic blades, because the low additive content cannot suppress ejection and sputtering. The minimum additive content required for the deposition on the superhydrophobic leaves reported so far is above 0.1%, which will lead to a large amount of rebound and splash when the brassinolide is sprayed on the superhydrophobic plant leaves. Injection, causing a lot of losses, the utilization rate of pesticides is not high. At the same time, as a systemic drug, most of the adjuvants cannot help it penetrate into the plant body, and the effect is even worse. Therefore, it is necessary to develop a brassinolide preparation capable of efficient deposition and spreadable wetting on superhydrophobic plant leaves.

Contents of the invention

In view of the deficiencies of the existing formulations, the inventors provide a brassinolide composition and a preparation method thereof, by enhancing the deposition and spreading of the systemic plant growth regulator brassinolide on the superhydrophobic leaf surface and wetting effect, so that brassinolide can conduct, absorb and take effect in plants better and faster, thereby completing the present invention.

In one aspect, the present invention provides a brassinolide composition, which comprises a brassinolide compound, a super-spreading agent, an emulsifying solubilizer and an antifreeze agent, and optionally Micronutrient fertilizers, insecticides, fungicides, herbicides.

Further, the mass ratio of the super-spreading agent to the brassinolide compound is 560-720:1, preferably 640:1.

Further, the mass ratio of the emulsifying solubilizer to the brassinolide compound is 80-150:1, preferably 100:1.

Further, the brassinolide compound is selected from the group consisting of 24-epibrassinolide, 28-epihomobrassinolide, 28-homobrasinolide and other brassinolide compounds or more.

Further, the superspreading agent is not a silicone additive in the traditional sense, but a surfactant that can inhibit water droplets from bouncing and sputtering on a superhydrophobic surface at a lower concentration, such as bis-octyl dimethyl bromide One of ammonium, didecyl dimethyl ammonium bromide, didodecyl dimethyl ammonium bromide, dihexadecyl dimethyl ammonium bromide or two or more in any proportion, preferably bis Decyl Dimethyl Ammonium Bromide.

Further, the emulsifier is one of Nongru 300#, Nongru 400#, Nongru 1601# or two or more in any proportion, preferably Nongru 400#.

Further, the antifreezing agent is one of ethylene glycol, urea, propylene glycol, glycerin, and methanol, or two or more of them in any proportion.

Further, the trace element fertilizer is selected from one of ammonium molybdate, sodium molybdate, chelated zinc, chelated iron, chelated manganese, and chelated copper, or two or more in any proportion. The chelated iron may be iron edetate.

The insecticide is selected from carbamates (such as carbaryl, carbofuran, etc.), pyrethroids (such as fenvalerate, deltamethrin, etc.) and organic nitrogen (such as chlordimeform, Dimehypo, etc.), preferably carbaryl, fenvalerate, deltamethrin, chlordimeform and dimehypo.

The bactericide is selected from benzimidazoles (such as carbendazim, thiabendazole, thiophanate) and benzamides (such as metalaxyl, imacarb, hymexazol), or azoxystrobin, Preferred are carbendazim, thiabendazole and thiophanate.

The herbicide is selected from one of glyphosate, oxadiazone, oxyfluorfen, amiloride, toxachlor, propannil, metazachlor, and alachlor, or two or more in any proportion.

It should be noted that the selected added trace element fertilizers, insecticides, fungicides, and herbicides do not affect the activity of the brassinolide compound itself, and the wettability and deposition of the brassinolide composition.

Further, in terms of mass, the brassinolide composition comprises 0.1% of 2,4-epibrasinolide, 64% of didecyldimethylammonium bromide, 10% of agricultural milk 400#, 5% ethylene glycol and the balance water.

In another aspect, the present invention provides a method for preparing the above-mentioned brassinolide composition, the method comprising:

(1) Pre-mixing treatment

Accurately weigh the brassinolide compound, super-spreading agent, emulsifying solubilizer, and antifreeze according to the proportion, then transfer it to a beaker, fill it up to a predetermined amount with ultrapure water, and stir until the system has no obvious solids to obtain a premix;

(2) Shear emulsification treatment

Transfer the pre-mixture into a shear emulsifier, set the rotation speed at 3000-4000r/min, suspend the operation of the shear emulsifier for 3 minutes every 10 minutes, repeat four times, and obtain the brassinolide composition.

Further, in the step (1), the orcinolactone compound and the superspreading agent can be mixed first, and then mixed with an emulsifier, an antifreeze and other optional trace element fertilizers, insecticides, and fungicides Mix the mixture.

Further, in the step (2), the rotational speed of the shear emulsifier is 3000r/min.

In the invention, the composition is sheared and emulsified by a high-shear emulsifier, solubilized by an emulsifying solubilizer, and a super-spreading agent is assisted to help deposit and increase efficiency, and finally form a stable and transparent system. The preparation method is simple and the cost is low.

Beneficial effect

The present invention obtains the brassinolide composition by selecting and optimizing the type and amount of superspreading agent and emulsifier, and has achieved the following beneficial effects:

First, the super-spreading agent in the present invention can effectively reduce the surface tension of droplets, can reduce the rebound and sputtering of droplets on superhydrophobic plant leaves, and improve the deposition rate;

Second, even if the present invention is diluted 10,000 to 100,000 times, it can still be completely deposited on the super-hydrophobic surface, and the practical application effect is good

Third, in the present invention, the super-spreading agent helps the brassinolide to spread and infiltrate the superhydrophobic plant leaves, so that the brassinolide can be quickly absorbed on the plant leaves to produce drug effect;

In addition, the preparation method of the present invention is simple, the cost is low, and the obtained composition has high stability. Using this new type of super-spreading surfactant and other pesticide adjuvants, the super-hydrophobic leaf has strong wettability, high deposition rate, and environmental protection. A brassinolide pesticide composition with the same advantages.

Description of drawings

Fig. 1 is the photo of the contact angle of the brassinolide preparation product diluted 10000 times on the superhydrophobic substrate on the market.

Fig. 2 is a photograph of the droplet deposition and contact angle measurement of the composition of Example 1 of the present invention diluted 10,000 times.

Fig. 3 is a photograph of the contact angle measurement of the droplet deposition of the composition diluted 100,000 times in Example 1 of the present invention.

Specific embodiments

Example 1

Preparation of mixture A: Add 64g of bisdecyldimethylammonium bromide and 0.1g of 24-epibrassinolide into a beaker, and mix well to obtain mixture A;

Preparation of mixture B: weigh 10g Nongru 400#, 5g ethylene glycol, and mix to obtain mixture B;

Preparation of brassinolide composition: Slowly add mixture B to mixture A and mix evenly, add ultrapure water to 100g. After adjusting the elevator to a suitable height, put the mixed product into the shear emulsifier, set the rotation speed at 3000r/min, stop the operation of the shear emulsifier for 3 minutes every 10 minutes, and repeat the process four times to complete the process to obtain brassinolide combination.

Example 2

Preparation of mixture A: Add 56g dihexadecyldimethylammonium bromide, 0.1g 24-epibrassinolide, 0.5g ferric edetate (fertilizer) into a beaker, mix well, and then Obtain mixture A;

Preparation of mixture B: weigh 10g Nongru 300#, 5g ethylene glycol, and mix to obtain mixture B;

Preparation of brassinolide composition: Slowly add mixture B to mixture A and mix evenly, add ultrapure water to 100g. After adjusting the elevator to a suitable height, put the mixed product into the shear emulsifier, set the rotation speed at 3600r/min, stop the operation of the shear emulsifier for 3 minutes every 10 minutes, and complete the process after repeating four times to obtain brassinolide combination.

Example 3

Premix product A preparation: 72g didecyl dimethyl ammonium bromide, 0.1g 24-epibrassinolide, fungicide (azoxystrobin), 10g agricultural milk 1601#, 5g ethylene glycol were added to the beaker After adding water to 100g and mixing evenly, the premixed product A is obtained.

Preparation of the brassinolide composition: after adjusting the elevator to a suitable height, put the mixed premixed product A into the shear emulsifier, set the speed at 4000r/min, stop the shear emulsifier for 3min every 10min, repeat four times After finishing the treatment, the brassinolide composition is obtained.

Example 4-10

The preparation method of Examples 4-10 is the same as that of Example 1, and the raw materials and feed amounts are shown in Table 1 below.

Table 1

Test Example 1

Materials and methods: contact angle tester, high-speed camera, surface tensiometer, wheat leaves

Experimental Design: The brassinolide composition prepared in Example 1 and the emulsifiable concentrate (Apree, 0.01% emulsifiable concentrate preparation) product on the market are diluted 10,000 times and 100,000 times after deposition and contact angle tests, and the substrate is selected as The average contact of water droplets on the surface of the superhydrophobic substrate coated with hydrophobic nano-silica/n-hexane superhydrophobic liquid is 152.4°.

results and analysis:

The market product was diluted 10,000 times for contact angle measurement and deposition test. The contact angle was similar to the contact angle of a water droplet on a superhydrophobic surface (Figure 1A); and observed by a high-speed camera, the sprayed droplet bounced off the superhydrophobic wheat leaf. , and cannot spread (Figure 1B).

When the composition of Example 1 was diluted 10,000 times for deposition test and contact angle measurement, the droplets could not only deposit on superhydrophobic wheat leaves, but also spread completely on the substrate 120ms after impact, achieving the expected effect, as shown in Figure 2A and 2B.

When the composition of Example 1 is diluted to 100,000 times, the wetting performance is still good, as shown in FIG. 3 .

The data of the 0ms contact angle and the surface tension of the diluent after diluting the composition of Example 1 by 1w times and 10w times are shown in Table 2 below.

Table 2

As can be seen from Table 2, the diluent of the composition in Example 1 has a low surface tension and a very small contact angle on a superhydrophobic surface, which can give play to the super-spreading agent's advantages in enhancing deposition and spreading wetting on a superhydrophobic surface, and can be used in agricultural production. In the process, the ejection and sputtering losses of the sprayed droplets are minimized, and it helps the agent to spread and wet, which is conducive to absorption and penetration, and effectively improves the use efficiency of pesticides.

The above is only a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto, other modifications or equivalent replacements made by those skilled in the art to the technical solution of the present invention, as long as they do not depart from the technology of the present invention The spirit and scope of the scheme should be included in the claims of the present invention.

Claims (10)

1. A brassinolide composition comprises a brassinolide compound, a super-spreader, an agricultural milk solubilizer, an antifreezing agent, and optional trace element fertilizers, bactericides, insecticides and herbicides.

2. The brassinolide composition according to claim 1, wherein the mass ratio of the hyper-spreader to the brassinolide compound is 560-720:1, preferably 640:1.

3. the brassinolide composition according to claim 1, wherein the mass ratio of the agricultural milk solubilizing agent to the brassinolide compound is 80-150:1, preferably 100:1.

4. the brassinolide composition according to claim 1, wherein the brassinolide compound is selected from one or more of 24-epibrassinolide, 28-homobrassinolide and other brassinolide compounds.

5. The brassinolide composition according to claim 1 wherein the superspreading agent is one or more of dioctyldimethylammonium bromide, didecyldimethylammonium bromide, didodecyldimethylammonium bromide and dihexadecyldimethylammonium bromide in an arbitrary ratio.

6. The brassinolide composition according to claim 1, wherein the emulsifier is one or more of Nongru 300#, nongru 400# and Nongru 1601#, preferably Nongru 400#.

7. The brassinolide composition according to claim 1, wherein the antifreeze is one or more of ethylene glycol, urea, propylene glycol, glycerin and methanol at any ratio.

8. The brassinolide composition according to claim 1, wherein the brassinolide composition comprises 0.1% by mass of 2, 4-epibrassinolide, 64% by mass of didecyldimethylammonium bromide, 10% by mass of Nongru No. 400, 5% by mass of ethylene glycol and the balance of water.

9. A method of making the brassinolide composition of any one of claims 1-8, the method comprising:

(1) Pre-mixing treatment

Accurately weighing brassinolide compound, super-spreading agent, emulsifier and antifreeze according to proportion, then transferring to a beaker, supplementing to a predetermined amount with ultrapure water, and stirring until the system has no obvious solid to obtain a premix;

(2) Shear emulsification treatment

And (3) transferring the premix into a shearing emulsifying machine, setting the rotating speed to be 3000-4000r/min, pausing the operation of the shearing emulsifying machine every 10min for 3min, and repeating for four times to obtain the brassinolide composition.

10. The method of claim 9, wherein the shear emulsifier is rotated at 3000 to 4000r/min.

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