CN115581240A

CN115581240A - Preparation method of high-adhesion cypermethrin microcapsule suspending agent

Info

Publication number: CN115581240A
Application number: CN202211308049.4A
Authority: CN
Inventors: 邢刚; 张龙; 张伟; 张阳洋; 任雯雯
Original assignee: Jiangsu Aijin Crop Technology Group Co ltd
Current assignee: Jiangsu Aijin Crop Technology Group Co ltd
Priority date: 2022-10-25
Filing date: 2022-10-25
Publication date: 2023-01-10

Abstract

The invention discloses a preparation method of a high-adhesion cypermethrin microcapsule suspending agent, which comprises the steps of preparing dopamine aqueous solution; adding metered water, emulsifier and cypermethrin benzene oil into a reaction kettle, and dispersing; adding gelatin water solution, adjusting pH, dispersing, and microencapsulating; adding dopamine aqueous solution and stirring; adding xanthan gum and a dispersing agent, and stirring to obtain a cypermethrin microcapsule suspending agent; the invention has simple processing technology without high temperature and high pressure, simple processing equipment without temperature control equipment, nontoxic and environment-friendly capsule materials, stronger adhesion effect and higher adhesiveness on the leaf surfaces of crops after modification of the microcapsule dopamine, can reduce bounce in the process of contacting the liquid medicine with the leaf surfaces of the crops in the pesticide application process, effectively improves the retention rate of the leaf surfaces of the pesticides, has longer lasting effect and has very wide application prospect.

Description

Preparation method of high-adhesion cypermethrin microcapsule suspending agent

Technical Field

The invention belongs to the technical field of pesticide preparation, and particularly relates to a preparation method of a high-adhesion cypermethrin microcapsule suspending agent.

Background

Microcapsules refer to a micro-container or package having a polymer or inorganic wall. The microcapsule granulation technology is a technology for embedding and sealing solid, liquid or gas in a microcapsule to form a solid particle product. At present, the common production process is complex, so that the equipment investment is large, the process operation method is discontinuous, the linked production is not facilitated, and the waste is not easy to recycle when the waste is produced in the capsule.

The cypermethrin has the effects of stomach toxicity, contact poisoning and the like, can be used for preparing pesticide insecticides, has the characteristics of high efficiency and high speed, and has good insecticidal effect on cotton, fruit trees, vegetables, tobacco, tea trees, soybeans, corns, flowers and other plants.

Meanwhile, in actual use, due to the influence of conditions such as wind blowing, rainfall, dew, sunshine and the like, the adhesion of the cypermethrin on the surface of the plant is further reduced, particularly, the pesticide effect is obviously reduced when the plant meets the rainfall after the pesticide is applied, and the pesticide effect period is shortened.

Dopamine is a polyphenol which can self-polymerize in a weakly alkaline solution and is finally oxidized into polydopamine to coat the surface of other substances. Polydopamine is used as an oxidation polymer of dopamine, and has been widely applied to the fields of energy, environment, photoelectric sensing and the like according to rich groups, good hydrophilicity, adhesiveness and biocompatibility. In addition, the polydopamine phenol catechol can react with hydroxyl or sulfhydryl to form covalent bonds with biological mucosa, and has strong adhesion effect on animal and plant surfaces.

The common processing method of the cypermethrin microcapsule suspending agent at present is an interface method, and the cypermethrin microcapsule suspending agent has no special performance. The processing technology is complex, the processing energy consumption is high, in the using process, the adhesion on the surface of a plant body is poor, the liquid medicine is more lost, and the liquid medicine is not resistant to water washing, so that the drug effect is poor, and therefore, a cypermethrin product with good adhesion and high adhesion needs to be developed.

Disclosure of Invention

The invention aims to provide a preparation method of a high-adhesion cypermethrin microcapsule suspending agent, which aims to solve the problems in the background technology.

In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a high-adhesion cypermethrin microcapsule suspending agent based on dopamine modification comprises the following steps:

(1) Preparing dopamine aqueous solution

a. Preparing 0.01 mol/L dopamine tris-HCl buffer solution.

1) 121.1 g Tris was weighed into a 1L beaker.

2) Deionized water at about 800 ml was added and dissolved with sufficient agitation.

3) Adding concentrated hydrochloric acid to adjust pH value to 8.3-8.8.

4) The solution was made to volume of 1L to prepare stock solution a.

5) 10ml of the stock solution A was taken and the volume of the solution was set to 1L.

6) Storing at room temperature for later use.

b. 1mol/L dopamine aqueous solution

1.2636g of 98% dopamine hydrochloride is weighed and added into the prepared tris-Hcl buffer solution of 1L0.01 mol/L dopamine to prepare 1mol/L dopamine aqueous solution for later use.

(2) Preparation of high-adhesion cypermethrin microcapsule suspending agent

a. Preparing the A type gelatin into a 5% aqueous solution, preparing the cypermethrin into 60% benzene oil, and preparing the xanthan gum into a 1% aqueous solution for later use.

b. Adding metered water, emulsifier and cypermethrin benzene oil into a reaction kettle, and opening a dispersion head to disperse for 10 minutes at the rotating speed of 1200 r/min.

c. Adding 5%A gelatin water solution, adjusting pH to 7-9, dispersing at 600r/min for 50 min, and making into microcapsule.

d. Adding 1mol/L dopamine aqueous solution and continuously stirring for 30-45 minutes at the rotating speed of 600 r/min.

e. 1% xanthan gum and dispersant were added and stirred at 300r/min for 30 minutes.

f. And discharging and detecting.

Preferably, in step (1), the Tris-HCl buffer is prepared by cooling the solution to room temperature and then adjusting the pH, since the pH of the Tris solution varies greatly with temperature, and the pH of the solution decreases by about 0.03 unit for every 1 ℃ rise in temperature; the 5%A aqueous gelatin solution was added and the agitation speed was reduced as required before adjusting the PH.

The invention has the technical effects and advantages that: the high-adhesion cypermethrin microcapsule suspending agent disclosed by the invention is prepared by coating the active ingredients of a pesticide with specific gelatin at normal temperature and modifying the formed microcapsule with dopamine. Compared with the conventional cypermethrin microcapsule suspending agent on the market at present, the cypermethrin microcapsule suspending agent has the advantages of simple processing technology, no need of high temperature and high pressure, simple and convenient processing equipment, no need of temperature control equipment, and no toxicity and environmental protection of capsule materials. After the microcapsule dopamine is modified, the microcapsule dopamine has a stronger adhesion effect and higher adhesiveness on the crop leaf surfaces, can reduce bounce in the process that the liquid medicine contacts the crop leaf surfaces in the pesticide application process, effectively improves the leaf surface retention rate of the pesticide, has longer lasting effect and has very wide application prospects.

Detailed Description

The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

A preparation method of a high-adhesion cypermethrin microcapsule suspending agent comprises the following steps:

1. preparing dopamine aqueous solution

a. Preparing 0.01 mol/L dopamine tris-HCl buffer solution.

121.1 g Tris was weighed into a 1L beaker.

Deionized water at about 800 ml was added and dissolved with sufficient agitation.

The pH is adjusted to 8.3-8.8 by adding concentrated hydrochloric acid, and the pH is adjusted after cooling the solution to room temperature, since the pH of Tris solutions varies greatly with temperature, and decreases by about 0.03 unit for every 1 ℃ rise in temperature.

The solution was brought to 1L to prepare stock solution a.

10ml of the stock solution A was taken and the volume of the solution was set to 1L.

Storing at room temperature for later use.

b. 1mol/L dopamine aqueous solution

2. Preparation of high-adhesion cypermethrin microcapsule suspending agent

Preparing 5% aqueous solution of type A gelatin, 60% benzene oil of cypermethrin, and 1% aqueous solution of xanthan gum;

adding metered water, emulsifier and cypermethrin benzene oil into a reaction kettle, and opening a dispersion head to disperse for 10 minutes at the rotating speed of 1200 r/min;

adding 5%A type gelatin aqueous solution, adjusting pH to 7-9, adding 5%A type gelatin aqueous solution, adjusting pH, reducing stirring speed, dispersing at 600r/min for 50 min, and microencapsulating;

adding 1mol/L dopamine aqueous solution and continuously stirring for 30-45 minutes at the rotating speed of 600 r/min;

adding 1% xanthan gum and a dispersing agent, and stirring for 30 minutes at the rotating speed of 300 r/min;

and discharging and detecting.

Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims

1. A preparation method of a high-adhesion cypermethrin microcapsule suspending agent is characterized by comprising the following steps: the method comprises the following steps:

s1: preparing a dopamine aqueous solution;

s2: adding metered water, emulsifier and cypermethrin benzene oil into a reaction kettle, and dispersing;

s3: adding gelatin water solution, adjusting pH to 7-9, dispersing, and microencapsulating;

s4: adding the dopamine aqueous solution in the step S1 and stirring;

s5: adding xanthan gum and a dispersing agent, and stirring to obtain a cypermethrin microcapsule suspending agent;

s6: and (6) detecting.

2. The preparation method of the high-adhesion type cypermethrin microcapsule suspending agent according to claim 1, characterized in that: in step S1, the dopamine aqueous solution is 1mol/L dopamine aqueous solution, and the preparation method of the dopamine aqueous solution is as follows:

a. preparing tris-HCl buffer solution of dopamine:

weighing Tris and placing in a beaker;

adding deionized water, and fully stirring for dissolving;

adding concentrated hydrochloric acid to adjust pH value to 8.3-8.8.

3. Fixing the volume of the solution to the required volume, and preparing a preparation solution A;

taking 10ml of the prepared solution A, and fixing the volume of the solution to 1L;

storing at room temperature for later use;

b. preparing a dopamine aqueous solution;

and adding dopamine hydrochloride into a prepared tris-HCl buffer solution of dopamine to prepare a dopamine aqueous solution.

4. The preparation method of the high-adhesion type cypermethrin microcapsule suspending agent according to claim 2, characterized in that: in step a, a tris-HCl buffer was prepared by cooling the solution to room temperature at the time of pH adjustment and then adjusting the pH.

5. The preparation method of the high-adhesion type cypermethrin microcapsule suspending agent according to claim 1, characterized in that: in step S3, the stirring speed is reduced as required before the aqueous gelatin solution is added to adjust the pH.

6. The preparation method of the high-adhesion type cypermethrin microcapsule suspending agent according to claim 1, characterized in that: in step S2, the cypermethrin benzene oil is 60% of benzene oil prepared from cypermethrin, and is dispersed for 10 minutes at the rotating speed of 1200r/min by a dispersion head.

7. The preparation method of the high-adhesion type cypermethrin microcapsule suspending agent according to claim 1, characterized in that: in step S3, the gelatin aqueous solution is 5%A type gelatin aqueous solution, and the dispersion is carried out for 50 minutes at a rotation speed of 600 r/min.

8. The preparation method of the high-adhesion type cypermethrin microcapsule suspending agent according to claim 1, characterized in that: in step S4, the stirring is continued for 30-45 minutes at a rotation speed of 600 r/min.

9. The preparation method of the high-adhesion type cypermethrin microcapsule suspending agent according to claim 1, characterized in that: in step S5, 1% xanthan gum is adopted as the xanthan gum, and stirring is carried out for 30 minutes at a rotating speed of 300 r/min.