CN115777701A - Thiacloprid-containing nano suspending agent and preparation method thereof - Google Patents
Thiacloprid-containing nano suspending agent and preparation method thereof Download PDFInfo
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Abstract
The invention provides a suspending agent and a preparation method thereof, belonging to the field of pesticides. The suspending agent comprises thiacloprid, a wetting agent, a dispersing agent, a thickening agent, an antifreezing agent and water; the wetting agent is selected from one, two or three of isopropyl naphthalene sulfonate 4075, block polyether HDB-500 and sulfosuccinate SP-4099, and the dispersant is selected from at least two of carboxylate dispersant RD-95, phosphate dispersant 3016, phosphate dispersant EMULSON AG TRST and polycarboxylate dispersant SP-2728. The suspending agent has small particle size, low viscosity, good particle size stability and good application prospect.
Description
Technical Field
The invention relates to the field of pesticides, and particularly relates to a thiacloprid-containing nano suspending agent and a preparation method thereof.
Technical Field
Thiacloprid is a novel chloronicotinyl insecticide. The mechanism of action of thiacloprid is different from that of other conventional insecticides. It mainly acts on insect nerve junction posterior membrane, and is combined with nicotine acetylcholine receptor to interfere normal conduction of insect nervous system, and cause block of nerve channel, and result in accumulation of acetylcholine, thereby causing insect abnormal excitation, general spasm, paralysis and death. Has stronger functions of systemic absorption, contact killing and stomach toxicity, has no cross resistance with the conventional insecticides such as pyrethroids, organophosphorus and carbamates, can be used for resistance control, has good crop safety and outstanding environmental compatibility, and has excellent control effect on important pests on pome fruits, cotton, vegetables and potatoes. The pesticide is also effective to various beetles (such as potato beetle, sterculia littoralis and rice weevil) and lepidoptera pests such as leaf miner and codling moth on apple trees, is suitable for all corresponding crops, and is a first-choice product in a vegetable and fruit pollution-free base.
Thiacloprid has been used in domestic markets for many years, has excellent effect and safe use, is consistently praised by broad farmers, has gradually found the insect-preventing and yield-increasing effects on different crops along with the popularization of the application in recent years, develops the traditional suspending agent into a nano-scale (the grain diameter D98 is less than 1.000 mu m) suspending agent, improves the bioavailability and is a good research direction.
However, the inventors have found that when thiacloprid and its adjuvant ingredients are ground to a particle size D98 < 1.000 μm, a problem of thickening and creaming is likely to occur and a problem that the particle size cannot be stabilized for a long time is likely to occur.
Therefore, a suspending agent containing thiacloprid with small particle size, small viscosity and good particle size stability is still needed.
Disclosure of Invention
In order to solve the above technical problems, the present invention provides the following technical solutions.
In a first aspect, the present invention provides a suspension concentrate.
A suspension concentrate, comprising: thiacloprid, wetting agent, dispersant, thickening agent, antifreezing agent and water; the wetting agent is selected from one, two or three of isopropyl naphthalene sulfonate 4075, block polyether HDB-500 and sulfosuccinate SP-4099, and the dispersant is selected from at least two of carboxylate dispersant RD-95, phosphate dispersant 3016, phosphate dispersant EMULSON AG TRST and polycarboxylate dispersant SP-2728.
In some embodiments, the thiacloprid is 30.00wt% to 50.00wt%, the wetting agent is 3.00wt% to 6.00wt%, the dispersant is 5.00wt% to 15.00wt%, the thickener is 0.05wt% to 1.00wt%, the antifreeze is 3.00wt% to 6.00wt%, and the water is 22.00wt% to 58.95wt%, based on the total mass of the suspending agent.
In some embodiments, the thiacloprid is 30.00wt% to 50.00wt%, the wetting agent is 3.00wt% to 6.00wt%, the dispersant is 5.00wt% to 15.00wt%, the thickener is 0.05wt% to 1.00wt%, the antifreeze is 3.00wt% to 6.00wt%, and the balance is water, based on the total mass of the suspending agent.
In some embodiments, the thiacloprid is 40.00wt%, the wetting agent is 3.00wt% to 6.00wt%, the dispersant is 12.00wt%, the thickener is 0.10wt% to 0.50wt%, the antifreeze is 5.00wt%, and the balance is water, based on the total mass of the suspending agent.
In some embodiments, the wetting agent is isopropyl naphthalene sulfonate 4075 and the dispersants are phosphate dispersant 3016 and carboxylate dispersant RD-95.
In some embodiments, the wetting agent is sulfosuccinate SP-4099 and the dispersants are polycarboxylate dispersants SP-2728 and carboxylate dispersant RD-95.
In some embodiments, the wetting agents are block polyether HDB-500 and isopropyl naphthalene sulfonate 4075, and the dispersants are phosphate dispersant EMULSON AG TRST and polycarboxylate dispersant SP-2728.
In some embodiments, the wetting agents are block polyether HDB-500 and sulfosuccinate SP-4099, and the dispersants are phosphate dispersant 3016 and polycarboxylate dispersant SP-2728.
In some embodiments, the suspending agent is selected from one or both of magnesium aluminum silicate, xanthan gum.
In some embodiments, the anti-freeze agent is selected from one or both of propylene glycol, ethylene glycol.
In some preferred embodiments, the wetting agent is isopropyl naphthalene sulfonate 4075, and the dispersants are phosphate dispersant 3016 and carboxylate dispersant RD-95; the antifreezing agent is ethylene glycol; the thickening agent is magnesium aluminum silicate; calculated by the total mass of the suspending agent, the content of the thiacloprid is 40.00wt%, the content of the wetting agent is 6.00wt%, the content of the phosphate dispersant 3016 is 6.00wt%, the content of the carboxylate dispersant RD-95 is 6.00wt%, the content of the thickening agent is 0.50wt%, the content of the antifreezing agent is 5.00wt%, and the balance is water. By adopting the technical scheme, the particle size stability of the obtained suspending agent is favorably improved, the viscosity of the obtained suspending agent is favorably reduced, and the grinding efficiency is favorably improved.
In some embodiments, the wetting agent is sulfosuccinate SP-4099, the dispersants are polycarboxylate dispersants SP-2728 and carboxylate dispersant RD-95; the antifreezing agent is ethylene glycol; the thickening agent is aluminum magnesium silicate; calculated by the total mass of the suspending agent, the content of the thiacloprid is 40.00wt%, the content of the wetting agent is 4.50wt%, the content of the polycarboxylate dispersant SP-2728 is 4.00wt%, the content of the carboxylate dispersant RD-95 is 8.00wt%, the content of the thickening agent is 0.50wt%, the content of the antifreezing agent is 5.00wt%, and the balance is water.
In some embodiments, the wetting agent is block polyether HDB-500 and isopropyl naphthalene sulfonate 4075, the dispersant is phosphate dispersant EMULSON AG TRST and polycarboxylate dispersant SP-2728; the antifreezing agent is ethylene glycol; the thickening agent is xanthan gum; calculated by the total mass of the suspending agent, the content of the thiacloprid is 40.00wt%, the content of the block polyether HDB-500 is 1.50wt%, the content of the isopropyl naphthalene sulfonate 4075 is 1.50wt%, the content of the phosphate dispersant EMULSON AG TRST is 6.00wt%, the content of the polycarboxylate dispersant SP-2728 is 6.00wt%, the content of the thickening agent is 0.10wt%, the content of the antifreezing agent is 5.00wt%, and the balance is water. By adopting the technical scheme, the particle size stability of the obtained suspending agent is favorably improved, and the viscosity of the obtained suspending agent is favorably reduced.
In some embodiments, the wetting agent is a block polyether HDB-500 and a sulfosuccinate SP-4099, the dispersant is a phosphate dispersant 3016 and a polycarboxylate dispersant SP-2728; the antifreezing agent is ethylene glycol; the thickening agent is xanthan gum; based on the total mass of the suspending agent, the content of the thiacloprid is 40.00wt%, the content of the block polyether HDB-500 is 1.50wt%, the content of the sulfosuccinate SP-4099 is 4.50wt%, the content of the phosphate dispersant 3016 is 6.00wt%, the content of the polycarboxylate dispersant SP-2728 is 6.00wt%, the content of the thickening agent is 0.10wt%, the content of the antifreezing agent is 5.00wt%, and the balance is water.
In some embodiments, the particle size D98 of the material in the suspending agent is < 1.000 μm.
In some embodiments, the particle size D98 of the material in the suspending agent is less than or equal to 0.700 μm.
In some embodiments, the particle size D98 of the material in the suspending agent is from 0.600 μm to 1.000 μm.
In some embodiments, the particle size D98 of the material in the suspending agent is from 0.600 μm to 0.700. Mu.m.
In a second aspect, the present invention provides a process for the preparation of the suspension formulation of the first aspect.
A method for preparing the suspending agent of the first aspect, comprising:
step S1: mixing one third of wetting agent and all dispersing agent in the suspending agent with water to obtain mixed solution 1;
step S2: mixing the thickening agent with water to obtain a mixed solution 2;
and step S3: mixing thiacloprid with the mixed solution 1, and homogenizing and dispersing to obtain a mixed solution 3;
and step S4: taking the mixed solution 3, carrying out coarse grinding by adopting grinding beads with the particle size of 0.6-0.8 mm until the material particle size D98 in the mixed solution 3 is 7.0-8.0 mu m, adding one third of wetting agent in the suspending agent, and grinding to obtain a mixed solution 4;
step S5: grinding the mixed solution 4 by using grinding beads with the particle size of 0.15mm-0.20mm, adding the rest wetting agent when the mixed solution is ground until the particle size D98 of the material is 1.0-1.5 mu m, continuing grinding until the particle size D98 of the material is less than or equal to 0.700 mu m, and obtaining mixed solution 5;
step S6: and mixing the mixed solution 5 with the antifreezing agent and the mixed solution 2, and stirring to obtain the suspending agent.
In some embodiments, the content of the thickener in the mixed solution 2 is 1.5wt% to 3.0wt% based on the total mass of the mixed solution 2.
In some embodiments, the content of the thickener in the mixed solution 2 is 2.0wt% based on the total mass of the mixed solution 2.
In some embodiments, the amount of water added in step S1 is the remaining amount of the total mass of water in the suspension minus the mass of water used in step S2.
Advantageous effects
Compared with the prior art, one embodiment provided by the invention has at least one of the following beneficial effects:
(1) Compared with other wetting agents or other wetting agent combinations, the wetting agent or the wetting agent combination provided by the invention is more favorable for improving the particle size heat storage stability of the thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 mu m and reducing the viscosity of the thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 mu m.
(2) Compared with other dispersants or other dispersant combinations, the dispersant combination provided by the invention is more favorable for improving the particle size heat storage stability of the thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 mu m, and is more favorable for reducing the viscosity of the thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 mu m.
(3) Compared with other formulas in the prior art, the formula provided by the invention is more favorable for improving the particle size heat storage stability of the thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 mu m and reducing the viscosity of the thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 mu m.
(4) The preferred technical scheme of the invention is as follows:
a suspension concentrate, comprising: thiacloprid, wetting agent, dispersant, thickening agent, antifreezing agent and water; the wetting agent is isopropyl naphthalene sulfonate 4075, and the dispersing agent is phosphate dispersing agent 3016 and carboxylate dispersing agent RD-95; the antifreezing agent is ethylene glycol; the thickening agent is magnesium aluminum silicate; calculated by the total mass of the suspending agent, the content of the thiacloprid is 40.00wt%, the content of the wetting agent is 6.00wt%, the content of the phosphate dispersant 3016 is 6.00wt%, the content of the carboxylate dispersant RD-95 is 6.00wt%, the content of the thickening agent is 0.50wt%, the content of the antifreezing agent is 5.00wt%, and the balance is water. Or
A suspension concentrate, comprising: the wetting agent is block polyether HDB-500 and isopropyl naphthalene sulfonate 4075, and the dispersant is phosphate dispersant EMULSON AG TRST and polycarboxylate dispersant SP-2728; the antifreezing agent is ethylene glycol; the thickening agent is xanthan gum; calculated by the total mass of the suspending agent, the content of the thiacloprid is 40.00wt%, the content of the block polyether HDB-500 is 1.50wt%, the content of the isopropyl naphthalene sulfonate 4075 is 1.50wt%, the content of the phosphate dispersing agent EMULSON AG TRST is 6.00wt%, the content of the polycarboxylate dispersing agent SP-2728 is 6.00wt%, the content of the thickening agent is 0.10wt%, the content of the antifreezing agent is 5.00wt%, and the balance is water.
The suspending agent obtained by the preferable technical scheme has better particle size heat storage stability and smaller viscosity.
(5) Compared with the method of adding the wetting agent all at once, the wetting agent is added three times at different grinding stages, which is more favorable for improving the particle size heat storage stability of the obtained thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 mu m.
(6) Compared with the method that only one kind of grinding beads (such as only 0.15mm-0.20mm grinding beads) is adopted, the method adopts different grinding beads to grind in different grinding stages, firstly one third of wetting agent is added, 0.6mm-0.8mm grinding beads are adopted to grind roughly until the grain diameter D98 of the material is 7.0 mu m-8.0 mu m, then one third of wetting agent is added to grind continuously, then 0.15mm-0.20mm grinding beads are used to grind finely, when the grain diameter D98 of the material is 1.0 mu m-1.5 mu m, the rest wetting agent is added to grind continuously until the grain diameter D98 of the material is less than or equal to 0.700 mu m, and the grain diameter heat storage stability of the thiacloprid-containing suspending agent with the grain diameter D98 of less than 1.000 mu m is improved.
Definition of terms
The terms "above", "below", "within" and the like are to be understood as including the instant numbers, e.g., two or more means ≧ two.
The term "and/or" should be understood to mean any one of the options or a combination of any two or more of the options.
The term "wt%" means mass percent.
The term "plurality" means at least two, such as 2, 3, 4 or 5, and the like.
The term "room temperature" means ambient temperature, typically 20 ℃ to 30 ℃ or 25 ℃.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
The short names of the auxiliary materials adopted in the embodiment of the invention are corresponding full names and manufacturers thereof:
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, some non-limiting examples are further disclosed below to further explain the present invention in detail.
The reagents used in the present invention are either commercially available or can be prepared by the methods described herein.
The term "hot storage" means that the pesticide sample is sealed in a glass bottle, stored in an incubator at 54 ℃. + -. 2 ℃ for 14 days, taken out, put into a desiccator, and cooled to room temperature.
Example 1-example 4: preparation of the suspending agent
Prescription: see table 1.
Table 1: formulations of the suspending agents of examples 1-4
The preparation method comprises the following steps:
step S1: mixing one third of wetting agent and all dispersing agent in the suspending agent with water (the adding amount of the water in the step is the residual amount of the total water in the suspending agent minus the mass of the water used in the step S2) to obtain a mixed solution 1;
step S2: mixing a thickening agent with water to obtain a mixed solution 2, wherein the content of the thickening agent in the mixed solution 2 is 2.0wt% calculated by the total mass of the mixed solution 2;
and step S3: mixing thiacloprid with the mixed solution 1, and homogenizing and dispersing to obtain a mixed solution 3;
and step S4: coarse grinding: taking the mixed solution 3, carrying out coarse grinding by adopting grinding beads with the particle size of 0.6-0.8 mm until the material particle size D98 in the mixed solution 3 is 7.0-8.0 mu m, adding one third of wetting agent in the suspending agent, and continuously grinding for 5min to obtain a mixed solution 4;
step S5: fine grinding: grinding the mixed solution 4 by using grinding beads with the particle size of 0.15mm-0.20mm, adding the rest wetting agent when the particle size D98 of the material is 1.0 mu m-1.5 mu m, continuing grinding until the particle size D98 of the material is less than or equal to 0.700 mu m, and obtaining mixed solution 5;
step S6: and mixing the mixed solution 5 with the antifreezing agent and the mixed solution 2, and stirring to obtain the suspending agent.
Comparative example 1 to comparative example 3: examination of wetting Agents
Prescription: a review of the wetting agents was made based on the formulation of example 1, the detailed formulation is given in Table 2.
Table 2: wetting agent prescription
The preparation method comprises the following steps: the preparation method is the same as that of example 1.
Comparative example 4-comparative example 10: investigation of dispersant formulation: a review of the dispersant was made based on the formulation of example 1, the detailed formulation is given in Table 3.
Table 3: examination of dispersant
The preparation method comprises the following steps: the preparation method is the same as that of example 1.
Comparative example 11: investigation of the formulation of the suspension (cf. Example 2 of CN107439540A, but with particle size ground to below 0.7 μm)
Prescription: comprises the following components in percentage by mass: 40wt% of thiacloprid, 5wt% of wetting dispersant, 3wt% of synergist, 1wt% of thickener, 0.5wt% of preservative, 5wt% of antifreeze, 0.5wt% of defoamer and the balance of water. The wetting dispersant consists of sp-2700 and PEAS03 in a mass ratio of 4:1, the synergist is a mixture of silicone BQ-809F and silicone T1118 in a mass ratio of 3:1, the thickening agent consists of xanthan gum and magnesium aluminum silicate in a mass ratio of 1:1, the defoaming agent is AF1501, the antifreezing agent is ethylene glycol, and the preservative is kason.
The preparation method of the thiacloprid suspending agent comprises the following steps:
a) Adding 70% of formula amount of water and wetting dispersant into a reaction vessel, and uniformly stirring;
b) Adding thiacloprid into a reaction container, homogenizing for 25min by a homogenizer, pumping into a sand mill, carrying out coarse grinding by using grinding beads with the particle size of 0.6-0.8 mm until the particle size D98 is less than or equal to 4 mu m, and then grinding by using grinding beads with the particle size of 0.15-0.20 mm until the particle size D98 is less than or equal to 0.700 mu m to obtain a ground substance;
c) And (3) uniformly mixing the rest water, the synergist, the thickener, the defoaming agent, the preservative and the antifreezing agent, homogenizing for 10min by using a homogenizer, adding the ground substance while stirring, and uniformly stirring to obtain the thiacloprid suspending agent.
Comparative example 12: examination of wetting agent addition mode (one-shot addition)
Prescription: the components and component ratios of comparative example 12 were the same as in example 1.
The preparation method comprises the following steps:
step S1: mixing all wetting agents, all dispersing agents and water (the adding amount of the water in the step is the residual amount of the total water in the suspending agent minus the mass of the water used in the step S2) to obtain a mixed solution 6;
step S2: mixing a thickening agent with water to obtain a mixed solution 7, wherein the content of the thickening agent in the mixed solution 7 is 2.0wt% based on the total mass of the mixed solution 7;
and step S3: mixing thiacloprid with the mixed solution 6, homogenizing and dispersing to obtain a mixed solution 8;
and step S4: taking the mixed solution 8, and carrying out coarse grinding by adopting grinding beads with the particle size of 0.6-0.8 mm until the particle size D98 of the material in the mixed solution 8 is 7.0-8.0 mu m to obtain a mixed solution 9;
step S5: grinding the mixed solution 9 by using grinding beads with the particle size of 0.15mm-0.20mm, adding the rest wetting agent when the mixed solution is ground until the particle size D98 of the material is 1.0 mu m-1.5 mu m, continuing grinding until the particle size D98 of the material is less than or equal to 0.700 mu m, and obtaining mixed solution 10;
step S6: and mixing the mixed solution 10 with the antifreezing agent and the mixed solution 7, and stirring to obtain the suspending agent.
Comparative example 13: examination of grinding means (using only 0.15mm-0.20mm grinding beads)
Prescription: the components and component ratios of comparative example 13 were the same as in example 1.
The preparation method comprises the following steps:
step S1: mixing one third of wetting agent and all dispersing agent in the suspending agent with water (the adding amount of the water in the step is the residual amount of the total water in the suspending agent minus the mass of the water used in the step S2) to obtain a mixed solution 11;
step S2: mixing a thickening agent with water to obtain a mixed solution 12, wherein the content of the thickening agent in the mixed solution 12 is 2.0wt% based on the total mass of the mixed solution 12;
and step S3: mixing thiacloprid with the mixed solution 11, and homogenizing and dispersing to obtain a mixed solution 13;
and step S4: coarse grinding the mixed solution 13 by using grinding beads of 0.15mm-0.20mm until the particle size D98 of the material in the mixed solution 13 is 7-8 μm, adding one third of wetting agent in the suspending agent, and continuously grinding for 5min to obtain a mixed solution 14;
step S5: continuously grinding the mixed solution 14 by using grinding beads with the diameter of 0.15-0.20 mm, adding the rest wetting agent when the grain diameter D98 of the material is 1-1.5 mu m, continuously grinding until the grain diameter D98 of the material is less than or equal to 0.700 mu m, and obtaining a mixed solution 15;
step S6: and mixing the mixed solution 15 with the antifreezing agent and the mixed solution 12, and stirring to obtain the suspending agent.
Example 5: performance detection
The suspensions obtained in examples 1 to 4 and comparative examples 1 to 13 were taken, respectively, and the time required for grinding was measured, and the particle diameter D98 and viscosity of the obtained suspension were measured for 0 day, and the particle diameter D98 was measured for 14 days by heat storage at 54 ℃ and the results are shown in tables 4 to 6.
Table 4: results of testing the Properties of the suspending agents obtained in examples 1 to 4
Table 5: results of testing the Properties of the suspensions obtained in comparative examples 1 to 3 and 11 to 13
Table 6: results of testing the Properties of the suspensions obtained in comparative examples 4 to 10
And (4) conclusion:
(1) Compared with other wetting agents or other wetting agent combinations, the wetting agent or the wetting agent combination provided in the embodiment 1 to the embodiment 4 is more favorable for improving the particle size heat storage stability of the obtained thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 mu m, and is more favorable for reducing the viscosity of the obtained thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 mu m.
(2) Compared with other dispersants or other dispersant combinations, the dispersant combination provided in examples 1 to 4 is more favorable for improving the particle size heat storage stability of the thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 μm, and is more favorable for reducing the viscosity of the thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 μm.
(3) Compared with other formulas in the prior art, the formulas provided in the embodiments 1 to 4 are more favorable for improving the particle size heat storage stability of the thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 mu m and reducing the viscosity of the thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 mu m.
(4) Compared with example 2 and example 4, more preferable examples 1 and 3 are, the particle size of examples 1 and 3 has better heat storage stability and smaller viscosity.
(5) Compared with the method of adding the wetting agent all at once, the wetting agent is added three times at different grinding stages, which is more favorable for improving the particle size heat storage stability of the obtained thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 mu m.
(6) Compared with the method that only grinding beads with one particle size (such as only grinding beads with 0.15mm-0.20 mm) are adopted, different grinding beads are adopted for grinding in different grinding stages, one third of wetting agent is added firstly, grinding beads with 0.6mm-0.8mm are adopted for coarse grinding until the particle size D98 of the material is 7.0 mu m-8.0 mu m, then one third of wetting agent is added for continuous grinding, then grinding beads with 0.15mm-0.20mm are used for fine grinding, when the particle size D98 of the material is 1.0 mu m-1.5 mu m, the rest of wetting agent is added for continuous grinding until the particle size D98 of the material is less than or equal to 0.700 mu m, and the particle size heat storage stability of the thiacloprid-containing suspending agent with the particle size D98 of less than 1.000 mu m is improved.
While the methods of the present invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications of the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of the present invention within the context, spirit and scope of the invention. Those skilled in the art can modify the process parameters appropriately to achieve the desired results with reference to the disclosure herein. It is expressly intended that all such similar substitutes and modifications which would be obvious to those skilled in the art are deemed to be included within the invention.
Claims (9)
1. A suspension concentrate, comprising: thiacloprid, wetting agent, dispersant, thickening agent, antifreezing agent and water; the wetting agent is selected from one, two or three of isopropyl naphthalene sulfonate 4075, block polyether HDB-500 and sulfosuccinate SP-4099, and the dispersant is selected from at least two of carboxylate dispersant RD-95, phosphate dispersant 3016, phosphate dispersant EMULSON AG TRST and polycarboxylate dispersant SP-2728.
2. The suspending agent according to claim 1, wherein the content of thiacloprid is 30.00wt% to 50.00wt%, the content of wetting agent is 3.00wt% to 6.00wt%, the content of dispersing agent is 5.00wt% to 15.00wt%, the content of thickening agent is 0.05wt% to 1.00wt%, the content of anti-freezing agent is 3.00wt% to 6.00wt%, the content of water is 22.00wt% to 58.95wt% or the balance is water.
3. The suspending agent according to any one of claims 1 to 2, wherein the content of thiacloprid is 40.00wt%, the content of the wetting agent is 3.00wt% to 6.00wt%, the content of the dispersing agent is 12.00wt%, the content of the thickening agent is 0.10wt% to 0.50wt%, the content of the anti-freezing agent is 5.00wt%, and the balance is water, calculated on the total mass of the suspending agent.
4. The suspension concentrate according to any of claims 1-3, wherein the wetting agent is isopropyl naphthalene sulfonate 4075, the dispersants are phosphate dispersant 3016 and carboxylate dispersant RD-95; or
The wetting agent is sulfosuccinate SP-4099, and the dispersing agent is polycarboxylate dispersing agent SP-2728 and carboxylate dispersing agent RD-95; or
The wetting agent is block polyether HDB-500 and isopropyl naphthalene sulfonate 4075, and the dispersant is phosphate dispersant EMULSON AG TRST and polycarboxylate dispersant SP-2728; or
The wetting agent is block polyether HDB-500 and sulfosuccinate SP-4099, and the dispersant is phosphate dispersant 3016 and polycarboxylate dispersant SP-2728.
5. A suspending agent as claimed in any of claims 1 to 4, wherein the suspending agent is selected from one or both of magnesium aluminium silicate, xanthan gum; and/or
The antifreezing agent is one or two of propylene glycol and ethylene glycol.
6. The suspension concentrate of any one of claims 1-5, wherein the wetting agent is isopropyl naphthalene sulfonate 4075, and the dispersants are phosphate dispersant 3016 and carboxylate dispersant RD-95; the antifreezing agent is ethylene glycol; the thickening agent is magnesium aluminum silicate; calculated by the total mass of the suspending agent, the content of the thiacloprid is 40.00wt%, the content of the wetting agent is 6.00wt%, the content of the phosphate dispersant 3016 is 6.00wt%, the content of the carboxylate dispersant RD-95 is 6.00wt%, the content of the thickening agent is 0.50wt%, the content of the antifreezing agent is 5.00wt%, and the balance is water; or
The wetting agent is sulfosuccinate SP-4099, and the dispersing agent is polycarboxylate dispersing agent SP-2728 and carboxylate dispersing agent RD-95; the antifreezing agent is ethylene glycol; the thickening agent is magnesium aluminum silicate; calculated by the total mass of the suspending agent, the content of the thiacloprid is 40.00wt%, the content of the wetting agent is 4.50wt%, the content of the polycarboxylate dispersant SP-2728 is 4.00wt%, the content of the carboxylate dispersant RD-95 is 8.00wt%, the content of the thickening agent is 0.50wt%, the content of the antifreezing agent is 5.00wt%, and the balance is water; or
The wetting agent is block polyether HDB-500 and isopropyl naphthalene sulfonate 4075, and the dispersant is phosphate dispersant EMULSON AG TRST and polycarboxylate dispersant SP-2728; the antifreezing agent is ethylene glycol; the thickening agent is xanthan gum; calculated by the total mass of the suspending agent, the content of the thiacloprid is 40.00wt%, the content of the block polyether HDB-500 is 1.50wt%, the content of the isopropyl naphthalene sulfonate 4075 is 1.50wt%, the content of the phosphate dispersant EMULSON AG TRST is 6.00wt%, the content of the polycarboxylate dispersant SP-2728 is 6.00wt%, the content of the thickening agent is 0.10wt%, the content of the antifreezing agent is 5.00wt%, and the balance is water; or
The wetting agent is block polyether HDB-500 and sulfosuccinate SP-4099, and the dispersant is phosphate dispersant 3016 and polycarboxylate dispersant SP-2728; the antifreezing agent is ethylene glycol; the thickening agent is xanthan gum; calculated by the total mass of the suspending agent, the content of the thiacloprid is 40.00wt%, the content of the block polyether HDB-500 is 1.50wt%, the content of the sulfosuccinate SP-4099 is 4.50wt%, the content of the phosphate dispersant 3016 is 6.00wt%, the content of the polycarboxylate dispersant SP-2728 is 6.00wt%, the content of the thickener is 0.10wt%, the content of the antifreeze is 5.00wt%, and the balance is water.
7. A suspension concentrate according to any of claims 1-6, wherein the particle size D98 of the material in the suspension concentrate is < 1.000 μm, or the particle size D98 of the material in the suspension concentrate is < 0.700 μm; or the particle size D98 of the materials in the suspending agent is 0.600-1.000 μm; or the particle size D98 of the materials in the suspending agent is 0.600-0.700 mu m.
8. A process for the preparation of a suspension concentrate as claimed in any of claims 1 to 7 which comprises:
step S1: mixing one third of wetting agent and all dispersing agent in the suspending agent with water to obtain mixed solution 1;
step S2: mixing the thickening agent with water to obtain a mixed solution 2;
and step S3: mixing thiacloprid with the mixed solution 1, and homogenizing and dispersing to obtain a mixed solution 3;
and step S4: taking the mixed solution 3, carrying out coarse grinding by adopting grinding beads with the particle size of 0.6-0.8 mm until the material particle size D98 in the mixed solution 3 is 7.0-8.0 mu m, adding one third of wetting agent in the suspending agent, and grinding to obtain a mixed solution 4;
step S5: grinding the mixed solution 4 by using grinding beads with the particle size of 0.15mm-0.20mm, adding the rest wetting agent when the particle size D98 of the material is 1.0-1.5 mu m, continuing grinding until the particle size D98 of the material is less than or equal to 0.700 mu m, and obtaining mixed solution 5;
step S6: and mixing the mixed solution 5 with the antifreezing agent and the mixed solution 2, and stirring to obtain the suspending agent.
9. The preparation method according to claim 8, wherein the content of the thickener in the mixed solution 2 is 1.5wt% to 3.0wt% or 2.0wt% based on the total mass of the mixed solution 2; and/or
The amount of water added in step S1 is the remaining amount of the total mass of water in the suspending agent minus the mass of water used in step S2.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115997761A (en) * | 2023-03-23 | 2023-04-25 | 惠州市银农科技股份有限公司 | Compound nano suspending agent and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101629038A (en) * | 2009-08-19 | 2010-01-20 | 郭振荣 | Production method of aqueous nanometer color past for digital ink jet and container with ultrasonic generator |
| CN101669466A (en) * | 2009-10-13 | 2010-03-17 | 深圳诺普信农化股份有限公司 | Pymetrozine-containing suspension agent composition |
| CN111392731A (en) * | 2020-04-08 | 2020-07-10 | 江苏新效新材料科技有限公司 | Preparation method of nano silica sand mill by taking polyvinylpyrrolidone as dispersing agent |
| US20210076670A1 (en) * | 2018-02-23 | 2021-03-18 | Nouryon Chemicals International B.V. | Pesticide suspension concentrate and fertilizer composition therewith |
| CN112742551A (en) * | 2020-12-22 | 2021-05-04 | 安徽儒特实业有限公司 | Fine grinding equipment for nano pesticide |
| AU2021106568A4 (en) * | 2021-08-23 | 2021-11-11 | Institute of grain crops, Henan Academy of Agricultural Sciences | High-yield production method of Astragalus sinicus seeds |
-
2022
- 2022-12-20 CN CN202211639809.XA patent/CN115777701B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101629038A (en) * | 2009-08-19 | 2010-01-20 | 郭振荣 | Production method of aqueous nanometer color past for digital ink jet and container with ultrasonic generator |
| CN101669466A (en) * | 2009-10-13 | 2010-03-17 | 深圳诺普信农化股份有限公司 | Pymetrozine-containing suspension agent composition |
| US20210076670A1 (en) * | 2018-02-23 | 2021-03-18 | Nouryon Chemicals International B.V. | Pesticide suspension concentrate and fertilizer composition therewith |
| CN111392731A (en) * | 2020-04-08 | 2020-07-10 | 江苏新效新材料科技有限公司 | Preparation method of nano silica sand mill by taking polyvinylpyrrolidone as dispersing agent |
| CN112742551A (en) * | 2020-12-22 | 2021-05-04 | 安徽儒特实业有限公司 | Fine grinding equipment for nano pesticide |
| AU2021106568A4 (en) * | 2021-08-23 | 2021-11-11 | Institute of grain crops, Henan Academy of Agricultural Sciences | High-yield production method of Astragalus sinicus seeds |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115997761A (en) * | 2023-03-23 | 2023-04-25 | 惠州市银农科技股份有限公司 | Compound nano suspending agent and preparation method thereof |
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