Suspending agent containing D-limonene and sophocarpidine and preparation method thereof

Abstract

The invention relates to the technical field of pesticide formulations, and provides a suspending agent containing D-limonene and sophocarpidine and a preparation method thereof.The suspending agent containing D-limonene and sophocarpidine is prepared from, by weight, 0.002%-0.1% of D-limonene, 0.002%-0.1% of sophocarpidine, 1%-5% of wetting agents, 0.5%-2% of defoaming agents, 0.05%-0.2% of thickening agents, 4%-8% of auxiliaries, 1%-5% of antifreeze agents, 1%-3% of stabilizers and the balance solvents, the auxiliary agent comprises an aminoanisole sulfonic acid compound and / or N-hydroxymethyl acetamide. According to the technical scheme, the problems of low stability and poor dispersibility of the suspending agent in the prior art are solved.

Description

Technical Field

[0001] The invention relates to the technical field of pesticide formulations, and in particular to a suspension concentrate containing D-limonene and matrine and a preparation method thereof. Background Art

[0002] In the agricultural field, suspension concentrate is a common formulation used to suspend pesticide particles in water so that they can be sprayed on the surface of crops or soil to achieve the purpose of preventing and controlling pests and diseases. However, there are also certain problems with the use of suspension concentrates. When the suspension concentrate is in a static state, the solid particles will settle to the bottom of the container, resulting in the particles being unable to be effectively dispersed in the liquid, affecting the uniformity of spraying. Frequent stirring is required to maintain a uniform suspension state, especially when spraying over a large area, which may increase the complexity of the operation and consume more time. Therefore, the development of a highly stable and highly dispersible suspension concentrate is an urgent problem to be solved. Summary of the invention

[0003] The invention provides a suspension containing D-limonene and matrine and a preparation method thereof, which solves the problems of low stability and poor dispersibility of the suspension in the related art.

[0004] The technical scheme of the present invention is as follows: The present invention proposes a suspension containing D-limonene and matrine, comprising the following raw materials in weight percentage: 0.002%~0.1% of D-limonene, 0.002%~0.1% of matrine, 1%~5% of wetting agent, 0.5%~2% of defoaming agent, 0.02%~0.5% of thickener, 4%~8% of auxiliary agent, 1%~5% of antifreeze agent, 1%~3% of stabilizer, and the balance is solvent, wherein the auxiliary agent comprises anisole aminosulfonic acid compound and / or N-hydroxymethylacetamide.

[0005] As a further technical solution, the mass ratio of D-limonene to matrine is 1-10:1.

[0006] As a further technical solution, when the auxiliary agent consists of anisole sulfonic acid compound and N-methylolacetamide, the mass ratio of the anisole sulfonic acid compound to the N-methylolacetamide is 2-4:1.

[0007] As a further technical solution, the mass ratio of the aminoanisole sulfonic acid compound to N-hydroxymethylacetamide is 3:1.

[0008] As a further technical solution, the anisole sulfonic acid compound includes one or more of p-anisole-2-sulfonic acid, o-anisole-4-sulfonic acid, and p-anisole-3-sulfonic acid.

[0009] As a further technical solution, the aminoanisole sulfonic acid compound is preferably p-aminoanisole-3-sulfonic acid.

[0010] As a further technical solution, the wetting agent is octanol polyoxyethylene ether.

[0011] As a further technical solution, the thickener includes one or more of xanthan gum, sodium alginate, and magnesium aluminum silicate.

[0012] As a further technical solution, the antifreeze agent includes one or both of glycerol and propylene glycol.

[0013] As a further technical solution, the stabilizer includes one or more of propyl gallate, p-aminobenzoic acid, and sorbitol.

[0014] As a further technical solution, the defoaming agent includes one or both of n-octanol and isooctyl alcohol.

[0015] As a further technical solution, the solvent is water.

[0016] The invention also provides a method for preparing a suspension containing D-limonene and matrine, comprising the following steps: weighing the raw materials, mixing and dispersing them uniformly, and then sand-grinding to obtain the suspension.

[0017] As a further technical solution, the particle size of the suspending agent after sand grinding is 1-5 μm.

[0018] The working principle and beneficial effects of the present invention are: In the present invention, anisole sulfonic acid compound and / or N-hydroxymethyl acetamide are added as auxiliary agents to enhance the dispersibility and stability of the suspension. The amino group in the anisole sulfonic acid compound has hydrophilicity, can increase the affinity of the suspension to water, is conducive to the mixing and dispersibility of the suspension with water, the ether bond maintains the dispersed state of the particles and the stability of the suspension by reducing the surface tension, and the sulfonic acid group enhances the dispersibility of the suspension by increasing the electrostatic repulsion and steric hindrance effect between the particles; the amide functional group in the N-hydroxymethyl acetamide has a higher bond energy and good thermal stability, and the hydroxyl group not only increases the hydrophilicity of the molecule and improves the dispersibility of the suspension, but also can be adsorbed on the surface of the pesticide particles to form a hydration film to prevent direct contact between the particles and help maintain the dispersed state of the pesticide component, thereby increasing the stability of the suspension. DETAILED DESCRIPTION

[0019] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0020] In the following examples and comparative examples: Octanol polyoxyethylene ether: model DE-6, manufacturer Jiangsu Maoheng Chemical Co., Ltd.; Xanthan gum: industrial grade, effective substance content is 99%, manufacturer is Zhengzhou Yuxiang Chemical Products Co., Ltd.

[0021] Example 1 A suspension containing D-limonene and matrine is composed of the following substances in percentage by weight: 0.002% D-limonene, 0.002% matrine, 1% octanol polyoxyethylene ether, 0.5% n-octanol, 0.02% xanthan gum, 4% p-anisole sulfonic acid compound, 1% glycerol, 1% propyl gallate, and the balance is water, wherein the p-anisole sulfonic acid compound is p-anisole-2-sulfonic acid.

[0022] Weigh D-limonene, matrine, octanol polyoxyethylene ether, n-octanol, xanthan gum, p-aminoanisole sulfonic acid compound, glycerol, propyl gallate, and water, mix and disperse them fully, and after uniform dispersion, add a sander to grind until 90% of the particle size is 1-5 μm to obtain a suspension.

[0023] Example 2 A suspension containing D-limonene and matrine is composed of the following substances in percentage by weight: 0.0158% D-limonene, 0.0028% matrine, 3% octanol polyoxyethylene ether, 1% n-octanol, 0.1% sodium alginate, 6% p-aminoanisole sulfonic acid compound, 3% propylene glycol, 2% aminobenzoic acid, and the balance is water, wherein the p-aminoanisole sulfonic acid compound is p-aminoanisole-2-sulfonic acid.

[0024] Weigh D-limonene, matrine, octanol polyoxyethylene ether, n-octanol, sodium alginate, p-aminoanisole sulfonic acid compound, propylene glycol, aminobenzoic acid, and water, mix and disperse them fully, and after uniform dispersion, add a grinder to grind until 90% of the particle size is 1-5 μm to obtain a suspension.

[0025] Example 3 A suspension containing D-limonene and matrine is composed of the following substances in percentage by weight: 0.1% D-limonene, 0.1% matrine, 5% octanol polyoxyethylene ether, 2% isooctyl alcohol, 0.2% magnesium aluminum silicate, 8% p-anisidine sulfonic acid compound, 5% propylene glycol, 3% sorbitol, and the balance is water, wherein the p-anisidine sulfonic acid compound is p-anisidine-2-sulfonic acid.

[0026] Weigh D-limonene, matrine, octanol polyoxyethylene ether, isooctyl alcohol, magnesium aluminum silicate, p-aminoanisole sulfonic acid compound, propylene glycol, sorbitol, and water, mix and disperse them fully, and after uniform dispersion, add a sander to grind until 90% of the particle size is 1-5 μm to obtain a suspension.

[0027] Example 4 Compared with Example 2, Example 4 is different in that p-aminoanisole-2-sulfonic acid is replaced by an equal amount of p-aminoanisole-3-sulfonic acid.

[0028] Example 5 Compared with Example 2, Example 5 is different in that p-aminoanisole-2-sulfonic acid is replaced by an equal amount of o-aminoanisole-4-sulfonic acid.

[0029] Example 6 Compared with Example 2, Example 6 is different in that p-aminoanisole-2-sulfonic acid is replaced by an equal amount of N-hydroxymethylacetamide.

[0030] Example 7 Compared with Example 4, the difference of Example 7 is that, by weight percentage, 6% of p-aminoanisole-3-sulfonic acid is replaced by 3% of p-aminoanisole-3-sulfonic acid and 3% of N-hydroxymethylacetamide.

[0031] Example 8 Compared with Example 4, the difference of Example 8 is that, by weight percentage, 6% of p-aminoanisole-3-sulfonic acid is replaced by 4% of p-aminoanisole-3-sulfonic acid and 2% of N-hydroxymethylacetamide.

[0032] Example 9 Compared with Example 4, the difference of Example 9 is that, by weight percentage, 6% of p-aminoanisole-3-sulfonic acid is replaced by 4.5% of p-aminoanisole-3-sulfonic acid and 1.5% of N-hydroxymethylacetamide.

[0033] Example 10 Compared with Example 4, the difference of Example 10 is that, by weight percentage, 6% of p-aminoanisole-3-sulfonic acid is replaced by 4.8% of p-aminoanisole-3-sulfonic acid and 1.2% of N-hydroxymethylacetamide.

[0034] Embodiment 11 Compared with Example 4, the difference of Example 11 is that, by weight percentage, 6% of p-aminoanisole-3-sulfonic acid is replaced by 5% of p-aminoanisole-3-sulfonic acid and 1% of N-hydroxymethylacetamide.

[0035] Comparative Example 1 Compared with Example 2, the difference in Comparative Example 1 is that no p-aminoanisole sulfonic acid compound is added.

[0036] The suspension prepared in Examples 1 to 11 and Comparative Example 1 was tested as follows: 1. Suspension rate: According to the test method 2 specified in GB / T 14825-2006 "Determination of suspension rate of pesticides", the suspension rate of the test sample is diluted 10 times with water and then left to stand for 2 hours.

[0037] 2. Hot storage suspension rate: According to the test method specified in GB / T 19136-2021 "Test method for hot storage stability of pesticides", the hot storage suspension rate of the sample is tested. The test conditions are: 54°C, 20d, and the change rate of hot storage suspension rate = suspension rate before hot storage - suspension rate after hot storage.

[0038] The test results are shown in the following table: Table 1 Performance test results of the suspension prepared in Examples 1 to 11 and Comparative Example 1

[0039] Compared with Comparative Example 1, Example 2 adds p-aminoanisole sulfonic acid compound. As a result, the suspension rate and heat storage stability of Example 2 are better than those of Comparative Example 1, indicating that the addition of p-aminoanisole sulfonic acid compound can improve the dispersibility and stability of the suspending agent.

[0040] Compared with Example 2, Example 4 replaces p-aminoanisole-2-sulfonic acid with an equal amount of p-aminoanisole-3-sulfonic acid, and Example 5 replaces p-aminoanisole-2-sulfonic acid with an equal amount of o-aminoanisole-4-sulfonic acid. As a result, the suspension rate and hot storage stability of Example 4 are better than those of Example 2 and Example 5, indicating that when the o-aminoanisole sulfonic acid compound added is p-aminoanisole-3-sulfonic acid, the dispersibility and stability of the suspending agent can be further improved.

[0041] Compared with Example 4 and Example 6, Examples 7 to 11 simultaneously added anthranilic acid compound and N-hydroxymethylacetamide. As a result, the suspension rate and heat storage stability of Examples 7 to 11 were better than those of Examples 4 and 6, indicating that the anthranilic acid compound and N-hydroxymethylacetamide played a synergistic role, and the obtained suspension had better dispersibility and stability.

[0042] Compared with Example 7, Examples 8 to 11 added different proportions of anisole sulfonic acid compound and N-hydroxymethylacetamide. As a result, the suspension rate and hot storage stability of Examples 8 to 10 were better than those of Examples 7 and 11, indicating that when the mass ratio of anisole sulfonic acid compound to N-hydroxymethylacetamide was 2 to 4:1, and the preferred ratio was 3:1, the obtained suspension had the best dispersibility and stability.

[0043] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A suspension containing D-limonene and matrine, characterized in that: The following raw materials are included in weight percentage: D-limonene 0.002%-0.1%, matrine 0.002%-0.1%, wetting agent 1%-5%, defoaming agent 0.5%-2%, thickener 0.05%-0.2%, auxiliary agent 4%-8%, antifreeze agent 1%-5%, stabilizer 1%-3%, and the balance is solvent, wherein the auxiliary agent includes aminoanisole sulfonic acid compound and / or N-hydroxymethylacetamide.

2. A suspension concentrate containing D-limonene and matrine according to claim 1, characterized in that, When the auxiliary agent consists of anisole sulfonic acid compound and N-hydroxymethylacetamide, the mass ratio of the anisole sulfonic acid compound to the N-hydroxymethylacetamide is 2-4:

1.

3. A suspension concentrate containing D-limonene and matrine according to claim 1, characterized in that, The anisole sulfonic acid compound includes one or more of p-anisole-2-sulfonic acid, o-anisole-4-sulfonic acid, and p-anisole-3-sulfonic acid.

4. A suspension concentrate containing D-limonene and matrine according to claim 1, characterized in that, The wetting agent is octanol polyoxyethylene ether.

5. A suspension concentrate containing D-limonene and matrine according to claim 1, characterized in that, The thickener includes one or more of xanthan gum, sodium alginate, and magnesium aluminum silicate.

6. A suspension concentrate containing D-limonene and matrine according to claim 1, characterized in that, The antifreeze agent includes one or both of glycerol and propylene glycol.

7. A suspension concentrate containing D-limonene and matrine according to claim 1, characterized in that, The stabilizer includes one or more of propyl gallate, p-aminobenzoic acid, and sorbitol.

8. A suspension concentrate containing D-limonene and matrine according to claim 1, characterized in that, The defoaming agent includes one or two of n-octanol and isooctyl alcohol.

9. A method for preparing a suspension concentrate containing D-limonene and matrine according to any one of claims 1 to 8, characterized in that: The method comprises the following steps: weighing the raw materials, mixing and dispersing them uniformly, and then sand-milling them to obtain a suspension.

10. The method for preparing a suspension concentrate containing D-limonene and matrine according to claim 9, characterized in that: The particle size of the suspending agent after sand milling is 1-5 μm.

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