CN110583687A

CN110583687A - Glyphosate and triclopyr soluble solution

Info

Publication number: CN110583687A
Application number: CN201910890902.XA
Authority: CN
Inventors: 曹轩; 马碧峰; 刘乐; 李建群; 张建华
Original assignee: Hunan New Changshan Agriculture Development Ltd By Share Ltd
Current assignee: Hunan New Changshan Agriculture Development Ltd By Share Ltd
Priority date: 2019-09-23
Filing date: 2019-09-23
Publication date: 2019-12-20

Abstract

The invention relates to a herbicide soluble solution, the effective components of which are glyphosate and triclopyr, the mass ratio of the glyphosate to the triclopyr is 1: 0.16-1: 0.30; the other components are dimethylamine, triethylamine, cosolvent, surfactant and deionized water. The weeding composition has good control effect on non-cultivated land malignant weeds and resistant weeds, is simple in production process and stable in quality, and can effectively reduce the using amount of effective components.

Description

Glyphosate and triclopyr soluble solution

Technical Field

The invention belongs to the field of pesticides, and relates to a soluble solution compounded by glyphosate and triclopyr and a preparation method thereof.

Background

In the field of herbicides, soluble agents using water as a carrier are not only environment-friendly but also efficient. The compound preparation of glyphosate acid (glyphosate for short) and triclopyr has good effect on preventing and killing non-cultivated land weeds. At present, most of the commercially available glyphosate and triclopyr combined products are mainly solid dosage forms, and the dosage forms have high labor intensity, bring dust to production, equipment and environment and are inconvenient to use. The formulation of glyphosate and triclopyr compounded by taking water as a carrier has the advantages of complex process, complex operation, high requirement on equipment, high production cost, difficult control of the proportion of effective ingredients and no effective guarantee of product stability. The two compound preparations reported in the prior art have the following patent documents: CN108794526A, reacting triclopyr with organic base to obtain triclopyr salt; then adding glyphosate, stirring uniformly and then slowly adding organic base; finally, auxiliary agents such as cosolvent, surfactant, defoaming agent and the like are added to prepare the aqueous solution. CN104957171A, the raw medicines are mixed to prepare a composition, and the stability of the water aqua prepared by the method cannot be guaranteed. ③ CN104447862A, the mixture of glyphosate and triclopyr is prepared by the reaction of carboxylic acid group in triclopyr and dimethylamine salt of glyphosate.

Disclosure of Invention

In order to overcome the defects of the prior art, the invention provides a soluble solution of glyphosate and triclopyr and a preparation method thereof.

The glyphosate soluble solution and the triclopyr soluble solution have two active ingredients, namely glyphosate and triclopyr respectively, and the mass ratio of the glyphosate to the triclopyr is 1: 0.16-1: 0.30; other components include: triethylamine, dimethylamine, cosolvent, surfactant and deionized water. The dosage of the cosolvent is 3-10% of the total mass of the soluble agent, preferably 3-8%, and is selected from one or more of the following: ethylene glycol, propylene glycol, isopropanol, ethanol, polyethylene glycol, preferably both ethylene glycol and polyethylene glycol are employed. The dosage of the surfactant is 3-10% of the total mass of the soluble agent, preferably 5-6%, and is selected from one or more of the following: alkyl glycoside, fatty alcohol-polyoxyethylene ether sodium sulfate, tallow amine polyoxyethylene ether and fatty alcohol-polyoxyethylene ether, preferably alkyl glycoside and fatty alcohol-polyoxyethylene ether are adopted simultaneously. The balance being deionized water.

The invention also discloses a preparation method of the glyphosate and triclopyr soluble solution, which comprises the following steps: respectively carrying out salt forming reaction on the glyphosate and the triclopyr with triethylamine and dimethylamine, then mixing the reacted liquid, adding a cosolvent, a surfactant and deionized water, and fully and uniformly stirring. The method specifically comprises the following steps:

1) weighing a proper amount of deionized water to fully wet the glyphosate, slowly adding triethylamine while stirring until the mixed solution is a light yellow transparent liquid, controlling the pH value of the system to be 5.5-6.0 as a reaction end point, and controlling the temperature of the system to be lower than 55 ℃.

2) Weighing a proper amount of deionized water to moisten the triclopyr, slowly adding a dimethylamine aqueous solution while stirring until the mixed solution is a transparent liquid, controlling the pH value of the system to be 8.0-9.0, and controlling the temperature of the system to be lower than 50 ℃.

3) Mixing the liquids obtained after the reaction in the step 1) and the step 2), adding a cosolvent, a surfactant and the balance of water, and fully and uniformly stirring to obtain the homogeneous stable glyphosate-triclopyr soluble solution.

The preparation method of the glyphosate and triclopyr soluble solution provided by the invention has the following advantages: 1. the glyphosate and the triclopyr react with triethylamine and dimethylamine respectively to form salts, the salt has high compatibility and good stability, the influence of strong base on the stability of single salt is effectively avoided, and the product stability is high. 2. The process is simple to operate, the key processing technical points are easy to control, and mass production and implementation are easy to realize. 3. Inorganic alkali is not used in the production process, the production equipment is friendly, the requirement on the type selection of the production equipment is not high, and the cost control is low.

Detailed Description

In order to make the technical solutions of the present invention better understood by those skilled in the art, the technical solutions in the embodiments of the present invention will be clearly and completely described below, but the present invention is not limited thereto.

Example 1: 35% glyphosate-triclopyr soluble solution

This example contains 30 mass% of glyphosate, 5 mass% of triclopyr as an active ingredient. Other components: 25 mass% of triethylamine; 3.5 mass% of dimethylamine (40% aqueous solution), 4 mass% of alkyl glycoside, 3 mass% of glycol, 3 mass% of polyethylene glycol, 1.5 mass% of fatty alcohol-polyoxyethylene ether, and the balance of deionized water.

Putting glyphosate raw drug into a sealable mixing tank, weighing a certain amount of deionized water to fully wet the glyphosate. The dosage of the deionized water is not strictly required, and the deionized water is preferably fully wetted and is about 1/4-1/2 of the mass of glyphosate technical product. And (3) slowly adding triethylamine while stirring until the mixed solution is light yellow transparent liquid, controlling the temperature of the system to be lower than 55 ℃ and the pH value of the system to be 5.5-6.0 as a reaction end point, and cooling to room temperature.

Adding the triclopyr raw drug into a sealable mixing tank, weighing quantitative deionized water, and wetting the triclopyr. The dosage of the deionized water is not strictly required, and the deionized water is preferably fully wetted and is about 1/3-2/3 of the mass of the triclopyr original drug. Slowly adding dimethylamine aqueous solution while stirring until the mixed solution is transparent liquid, controlling the temperature of the system to be lower than 50 ℃ and the pH value of the system to be 8.0-9.0, cooling to room temperature, and transferring to a storage tank for later use.

Slowly adding the triclopyr reaction solution in a storage tank into a mixing tank for glyphosate salt forming reaction, uniformly stirring, then sequentially adding ethylene glycol, polyethylene glycol, the balance of water, alkyl glycoside and fatty alcohol-polyoxyethylene ether, and fully and uniformly stirring to obtain the homogeneous transparent 35% glyphosate-triclopyr soluble solution.

Example 2: 37% glyphosate-triclopyr soluble solution

30 mass percent of glyphosate serving as an effective component and 7 mass percent of triclopyr serving as an effective component; other components: 25 mass% of triethylamine, 5 mass% of dimethylamine (40% aqueous solution), 4 mass% of alkyl glycoside, 3 mass% of ethylene glycol, 1.5 mass% of polyethylene glycol, 1.5 mass% of fatty alcohol-polyoxyethylene ether, and the balance of deionized water. The preparation method is the same as example 1.

Example 3: 39% glyphosate-triclopyr soluble solution

30 mass percent of glyphosate serving as an effective component and 9 mass percent of triclopyr serving as an effective component; other components: 25 mass% of triethylamine, 6.5 mass% of dimethylamine (40% aqueous solution), 4 mass% of alkyl glycoside, 1.5 mass% of ethylene glycol, 2 mass% of polyethylene glycol, 1.5 mass% of fatty alcohol-polyoxyethylene ether, and the balance of deionized water.

The preparation method is the same as example 1.

Example 4: dilution stability, Low temperature, Heat storage tests and assays were performed on the samples of examples 1-3

Dilution stability: 5mL of the sample is diluted by 20 times with standard hard water and is kept stand in a water bath at 30 +/-2 ℃ for 1 h.

Low-temperature stability: the samples were placed in 100mL conical centrifuge tubes with graduations and stored at 0 ℃ for 7 days. Heat storage stability: the samples were placed in ampoules, sealed, and the total mass recorded before and after thermal storage at 54 ℃ for 14 days.

TABLE 1 physical stability and Main physicochemical indices

"+ +" indicates that the sample or dilution was homogeneous, free of precipitate, free of oil, free of insoluble matter, and free of separation.

TABLE 2 Main technical indices

As can be seen from Table 2, the soluble solution of the present invention is equivalent or superior to the comparative examples in the indexes of water-insoluble matter, low temperature stability and heat storage stability, and the extremely slow decomposition rate of the effective ingredient indicates that the effect of the product can be better maintained and the shelf life can be prolonged.

Example 5: field test of glyphosate and triclopyr compounded soluble agent

TABLE 2 field test fresh weight control effect (30 days after application)

The test result shows that: the soluble solution compounded by the glyphosate and the triclopyr has stronger weed killing activity on non-cultivated land weeds, can effectively reduce the dosage, has more prominent control effect on resistant weeds such as erigeron breviscapus, hairyvein agrimony, black nightshade and the like, and is obviously superior to single glyphosate and triclopyr.

Claims

1. The soluble solution of glyphosate and triclopyr has two active ingredients, namely glyphosate and triclopyr, wherein the mass ratio of the glyphosate to the triclopyr is 1: 0.16-1: 0.30; other components include: triethylamine, dimethylamine, cosolvent, surfactant and deionized water; the cosolvent is used in an amount of 3-10% by mass and is selected from one or more of the following: ethylene glycol, propylene glycol, isopropanol, ethanol, polyethylene glycol; the amount of the surfactant is 3-10% by mass, and is selected from one or more of the following: alkyl glycoside, fatty alcohol-polyoxyethylene ether sodium sulfate, tallow amine polyoxyethylene ether and fatty alcohol-polyoxyethylene ether

The soluble solution of glyphosate and triclopyr is prepared by the following method: respectively carrying out salt forming reaction on the glyphosate and the triclopyr with triethylamine and dimethylamine, then mixing the reacted liquid, adding a cosolvent, a surfactant and deionized water, and fully and uniformly stirring.

2. The solubles of glyphosate and triclopyr according to claim 1 wherein said co-solvent comprises both ethylene glycol and polyethylene glycol.

3. The solubles of glyphosate and triclopyr according to claim 1 or 2 wherein the amount of co-solvent is between 3 and 8% of the total mass of the solubles.

4. The glyphosate and triclopyr soluble solution of claim 1 wherein the surfactant includes both an alkyl glycoside and a fatty alcohol polyoxyethylene ether.

5. The solubles of glyphosate and triclopyr according to claim 1 or 4 wherein the amount of said surfactant is from 5 to 6% of the total mass of said solubles.

6. The soluble solution of glyphosate and triclopyr according to claim 1 wherein the mass ratio of glyphosate and triclopyr is 30: 5, 30: 7 or 30: 9.

7. A solubles of glyphosate and triclopyr according to claim 1 prepared by the following method:

1) weighing a proper amount of deionized water to fully wet glyphosate, slowly adding triethylamine while stirring until the mixed solution is a light yellow transparent liquid, controlling the pH value of the system to be 5.5-6.0 as a reaction end point, and controlling the temperature of the system to be lower than 55 DEG C

2) Weighing a proper amount of deionized water to wet triclopyr, slowly adding a dimethylamine aqueous solution while stirring until the mixed solution is a transparent liquid, controlling the pH value of the system to be 8.0-9.0 and the temperature of the system to be lower than 50 DEG C

3) Mixing the liquids obtained after the reactions in the steps 1) and 2), adding a cosolvent, a surfactant and the balance of water, and fully and uniformly stirring to obtain the glyphosate and triclopyr soluble solution.