Preparation method and application of nano plant growth regulator

Abstract

The invention relates to a preparation method and application of a nano plant growth regulator, in particular to a nano plant growth regulator containing mepiquat chloride and prohexadione calcium, which is prepared from the following raw materials in 1000 parts by weight: 50 to 300 parts by weight of mepiquat chloride, 30 to 150 parts by weight of prohexadione calcium, 40 to 400 parts by weight of auxiliaries and the balance of water. Wherein the weight ratio of mepiquat chloride to prohexadione calcium is 2: 1. The nano plant growth regulator provided by the invention reduces the particle size of pesticide, enhances the permeability of the pesticide, is beneficial to crop absorption, reduces the usage amount of the pesticide, improves the pesticide effect, is safe to crops, has a very good promotion effect on wheat yield increase, and also can improve the quality of wheat.

Description

Technical Field

[0001] The present invention belongs to the technical field of pesticides, and particularly relates to a preparation method and application of a nano plant growth regulator. The regulator contains calcium cyclanilide, mepiquat chloride, an auxiliary agent and water, and is made into a suspension concentrate. Background Art

[0002] Calcium cyclanilide, with the chemical name of calcium 3,5-dioxo-4-propionylcyclohexanecarboxylate, is a plant growth regulator. The pure product is a white amorphous solid, and the technical material appears as a beige or light yellow amorphous solid without odor. It is relatively stable to light and air, easily decomposes in acidic media, is stable in alkaline media, and has good thermal stability. Calcium cyclanilide is a calcium salt of cyclohexanecarboxylic acid, and the really effective component is cyclanilide. When calcium cyclanilide is sprayed on plants, it can be quickly absorbed by the leaf cells of crops. The part where plants synthesize gibberellin is in the leaves, so it can directly act on the target, thus having the characteristic of high activity. At the same time, the half-life of calcium cyclanilide is very short, and in the soil rich in microorganisms, the half-life does not exceed 24 hours. Moreover, the final metabolic products of calcium cyclanilide are carbon dioxide and water, so calcium cyclanilide is a low-toxic and residue-free green product.

[0003] Mepiquat chloride is a new type of plant growth regulator and has good systemic conduction effect on plants. It can promote the reproductive growth of plants; inhibit the excessive growth of stems and leaves, control lateral branches, shape an ideal plant type, increase the number and vitality of roots, increase the weight of fruits and improve the quality. It is widely used in crops such as cotton, wheat, rice, peanut, corn, potato, grape, vegetable, bean, flower, etc.

[0004] The applicant found through experiments that when mepiquat chloride and calcium cyclanilide with different action mechanisms are mixed in a weight ratio of 2:1, it has a very good effect on increasing the yield of wheat, and can also improve the quality of wheat, especially can improve the protein content, soluble sugar content and starch content of wheat. Summary of the Invention

[0005] The purpose of the present invention is to provide a preparation method and application of a nano plant growth regulator. According to a certain ratio and dosage, the regulator has a very good synergistic effect on increasing the yield of wheat, can also improve the protein content, soluble sugar content and starch content of wheat, and is safe for the environment.

[0006] The technical solution of the present invention is as follows:

[0007] A preparation method and application of a nano plant growth regulator, characterized in that: the effective active ingredients of the nano plant growth regulator are calcium cyclanilide and mepiquat chloride. The effective active ingredients are added with an auxiliary agent and water to make a suspension concentrate, wherein the weight ratio of mepiquat chloride to calcium cyclanilide is 2:1.

[0008] Further, the auxiliary agent is selected from one or more of hyperbranched dispersants, wetting agents, defoaming agents, preservatives, pH regulators, and thickeners.

[0009] Further, the hyperbranched dispersant is selected from one or more of styrene maleic anhydride polymers and polyoxyethylene polyoxypropylene polyetheramine graft copolymers; the wetting agent is selected from one or more of alkyl sulfonates, alkyl naphthalene sulfonates, fatty alcohol polyoxyethylene ethers, alkyl glycosides, trisiloxane polyoxyethylene ethers, polyaryl phenol polyoxyethylene ethers, and castor oil polyoxyethylene ethers; the antifreeze agent is selected from one or more of ethylene glycol, propylene glycol, glycerol, polyethylene glycol, allantoin, and sorbitol; the thickener is selected from one or more of xanthan gum, polyvinyl alcohol, magnesium aluminum silicate, sodium carboxymethyl cellulose, sodium alginate, and guar gum; the defoaming agent is a silicone defoaming agent, a C10-20 saturated fatty acid compound, or a C8-10 fatty alcohol; the pH regulator is selected from one or more of citric acid and glacial acetic acid; the preservative is benzoic acid and its sodium salt, isothiazolinone, sorbic acid and its sodium or potassium salt.

[0010] Further, the weight ratio of the effective active ingredient to the hyperbranched dispersant is 1:1 to 8:1, optionally 1:1 to 5:1.

[0011] Further, the total weight of mepiquat chloride and calcium cyclohexanedicarboxylate in the regulator is 90 to 510 g / L, optionally 300 g / L.

[0012] Further, based on 1000 parts by weight, the regulator is composed of the following components in the following contents:

[0013] 60 to 340 parts by weight of mepiquat chloride, 30 to 170 parts by weight of calcium cyclohexanedicarboxylate, 10 to 150 parts by weight of hyperbranched dispersant, 20 to 80 parts by weight of wetting agent, 0 to 60 parts by weight of antifreeze agent, 2 to 25 parts by weight of thickener, 0.5 to 15 parts by weight of defoaming agent, 0.05 to 5 parts by weight of pH regulator, 0 to 20 parts by weight of preservative, and the balance being water.

[0014] Further, based on 1000 parts by weight, the regulator is composed of the following components in the following contents:

[0015] 60 to 340 parts by weight of mepiquat chloride, 30 to 170 parts by weight of calcium cyclohexanedicarboxylate, 10 to 100 parts by weight of dispersant, 20 to 50 parts by weight of wetting agent, 30 to 60 parts by weight of antifreeze agent, 2 to 10 parts by weight of thickener, 0.5 to 8 parts by weight of defoaming agent, 0.05 to 2 parts by weight of pH regulator, 2 to 8 parts by weight of preservative, and the balance being water.

[0016] Further, the preparation method of the nano regulator is as follows: First, water, wetting agent, hyperbranched dispersant, and defoamer are put into a stirring tank and sheared at high speed. After sufficient dispersion, mepiquat chloride technical and prohexadione-calcium technical are added and sheared at high speed to form a primary dispersion liquid; then it is transported to two sand mills connected in series by a diaphragm pump for sand grinding. The feeding speed of the sand grinding is adjusted to control the fineness of the sand grinding within 3 - 5 μm, and then it is transported to a turnover kettle by a diaphragm pump for stirring; this slurry is filtered through a 200 - mesh filter and then sand - ground with a nano - sand mill, and the particle size D 50 is controlled to be less than 100 nanometers, and the particle size D 90 is controlled to be less than 300 nanometers. Finally, the slurry is transported to a modulation kettle, thickening agent and defoamer are added to adjust the viscosity of the material, and samples are taken for quality inspection to obtain the finished product.

[0017] Further, the application of the nano regulator in regulating the growth of wheat.

[0018] The advantages of the present invention are as follows: (1) Compared with single agents, it has a good synergistic effect on increasing wheat yield; (2) It is low - toxic and highly efficient, reducing the amount of pesticide used, decreasing the residue of pesticides on crops, having a short safe interval period, and being safe for wheat; (3) It can significantly improve the quality of wheat, increasing the protein content, soluble sugar content, and starch content of wheat. Specific Embodiments

[0019] The following further illustrates the present invention with reference to embodiments. The percentages in the embodiments are all weight percentages, but the present invention is not limited thereto.

[0020] Application Example 1: Preparation Example of Nano - Suspension

[0021] The following example is calculated based on 1000 parts by weight and contains the following components, and a 400 g / L clothianidin·lufenuron suspension is prepared according to the preparation method claimed in the present invention:

[0022]

[0023]

[0024] Application Example 2: Main Technical Indicators of the Embodiment

[0025]

[0026] It can be seen that the particle size of the nano - suspension in the embodiment of the present invention is significantly smaller than that of the control example.

[0027] Application Example 3:

[0028] Report on the Joint Toxicity Determination Test of Mepiquat Chloride and Prohexadione - Calcium in Regulating Wheat Growth Indoors

[0029] Test target: Wheat, variety "Taimai 198".

[0030] Test method: Stem and leaf spraying method

[0031] Test basis: Refer to NY / T 2061.2-2011 and NY / T 2061.5-2016

[0032] 1 Test purpose

[0033] Using mepiquat chloride and calcium cyclohexanecarboxylate as test agents, at the initial jointing stage of wheat, spray treatment was adopted to determine the best ratio through indoor combined action screening after mixing, so as to determine its formula, provide a basis for the rational mixing of the two agents, and develop an effective agent for regulating wheat growth. The test results are reported as follows.

[0034] 2 Cultivation conditions

[0035] Wheat was cultivated by the potting method.

[0036] 3 Test design

[0037] 3.1 Reagents

[0038] 98% mepiquat chloride technical, provided by the applicant;

[0039] 88% calcium cyclohexanecarboxylate technical, provided by the applicant;

[0040] Emulsifier: Tween 80.

[0041] 3.2 Test treatments

[0042] 3.2.1 Dose setting

[0043] The mepiquat chloride technical was formulated into a 2.5×10 3 mg / L stock solution with distilled water for standby.

[0044] Calcium cyclohexanecarboxylate is poorly soluble in water and insoluble in most organic solvents. In the laboratory, it was first processed into a 10% suspension by a sand mill and then diluted into a 2.5×10 3 mg / L stock solution for standby.

[0045] Referring to the respective action activities of the two agents and combining the characteristics of indoor determination, on the basis of the preliminary test, the dosages of mepiquat chloride and calcium cyclohexanecarboxylate were set as different mixing combinations, as shown in Table 1, with a total of 35 groups designed.

[0046] An aqueous solution containing no agent, the same solvent and emulsifier was used as the blank control, and indoor bioassays were carried out separately.

[0047] Table 1 Experimental agent dosage design

[0048]

[0049] 3.2.2 Test repetition

[0050] For each concentration treatment of the test agent, it was divided into 4 repetitions, with 20 pots per repetition and 1 wheat plant per pot.

[0051] 3.3 Treatment method

[0052] The medicine was applied at the early jointing stage of wheat, with a total of 1 application.

[0053] 4 Data investigation and statistical analysis

[0054] 4.1 Result investigation time and method

[0055] At the harvest stage, the absolute value (numerical measurement) investigation method was adopted. Randomly select 10 pots per repetition to investigate the plant height and single ear weight of wheat.

[0056] 4.2 Data statistical analysis

[0057] Use the Gowing method to calculate the theoretical inhibition rate (growth rate) E0 of each treatment mixture combination (E0 = X + Y - X * Y / 100), and then compare it with the measured inhibition rate (growth rate) (E) to evaluate the combined effect of the two when mixed on wheat.

[0058] When the value of E - E0 is greater than 10%, it is a synergistic effect; when the value of E - E0 is less than -10%, it is an antagonistic effect; when the value of E - E0 is between -10% and 10%, it is an additive effect. Determine the optimal ratio based on factors such as the actual drug effect, the characteristics of the two agents, and the balance of the formulation.

[0059] In the formula, X is the plant height inhibition rate / single ear increase rate of wheat when the dosage of mepiquat chloride is P; Y is the plant height inhibition rate / single ear increase rate of wheat when the dosage of prohexadione-calcium is Q.

[0060] 5 Results and analysis

[0061] Table 2 Determination of the combined effect of mepiquat chloride and prohexadione-calcium on wheat in the laboratory (Gowing method)

[0062]

[0063]

[0064] It can be seen from the results in Table 2 that after the test agents were mixed, for the treatment of mepiquat chloride 160 mg / L + prohexadione-calcium 80 mg / L (the ratio is 2:1), the value of E - E0 for the single ear weight increase rate of wheat was 10.13, which was greater than 10%, showing a synergistic effect. The value of E - E0 for the plant height inhibition rate was between -10% and 10%, showing an additive effect.

[0065] Observation during the experiment showed that both agents and their respective formulation dosages were safe for the growth of the experimental wheat and caused no phytotoxicity.

[0066] Application Example 4: Field Efficacy Experiment of 300 g / L Mepiquat Chloride · Prohexadione Calcium Suspension Concentrate (Examples 1 - 3) on Regulating Wheat Growth

[0067] 1 Experimental Objectives

[0068] To verify the regulating effect, appropriate application period, recommended dosage, and safety for wheat growth of the 300 g / L mepiquat chloride · prohexadione calcium suspension concentrate (Examples 1 - 3) developed by the applicant, and to provide a basis for the registration of this product.

[0069] 2 Materials and Methods

[0070] Application Method: Spraying method, with a water consumption of 450 - 750 L / ha.

[0071] Experiment Conduct Time: 2022, 2023.

[0072] 2.1 Experimental Agent Treatments

[0073] Table 3 Test Agent Treatments

[0074]

[0075] 2.2 Test Objects and Crops

[0076] Test Object: Wheat, with good growth after emergence.

[0077] 2.3 Application Method

[0078] Application Time: Spray once at the early jointing stage of wheat.

[0079] 2.4 Investigation Methods

[0080] Phytotoxicity Investigation: Observe whether wheat shows phytotoxicity 3, 5, and 7 days after application.

[0081] Investigate plant height 15 days after application;

[0082] Investigate plant height, lengths of the first and second basal internodes 30 days after application;

[0083] At wheat harvest, investigate the number of effective spikes per square meter and the number of grains per spike;

[0084] After wheat is dried, measure the 1000 - grain weight and yield, and calculate the yield increase rate.

[0085] And conduct quality determinations such as protein content, soluble sugar content, and starch content on the grains of wheat in each plot.

[0086] Quality detection method: Randomly select 50 g of wheat seeds from each plot, divide them into four equal parts on average, determine the protein content by Coomassie brilliant blue method, determine the starch content by enzymatic hydrolysis method, and determine the soluble sugar content by anthrone colorimetric method.

[0087] 2.5 Calculation and analysis methods

[0088] Yield increase rate (%) = [(yield in the medicament treatment area - yield in the blank control area) / yield in the blank control area] × 100

[0089] 3 Results and analysis

[0090] Statistically analyze the experimental data by Duncan's new multiple range (DMRT) method.

[0091] Table 4 Experimental results of the effects of 300 g / L mepiquat chloride·prohexadione-calcium suspension and control on wheat yield and quality

[0092]

[0093]

[0094] 4 Conclusions

[0095] Suitable application period and dosage: The test drug, 300 g / L mepiquat chloride·prohexadione-calcium suspension, is applied once during the jointing stage of wheat. It has a significant inhibitory effect on wheat plant height. At the same time, the effective ear number, grains per ear, 1000-grain weight, and yield are all significantly increased. The effect of the test drug is significantly better than that of the control single agent. By analyzing the wheat quality, it is found that the protein content, soluble sugar content, and starch content of wheat treated with the test drug are all higher than those of the water control and single-agent control. Each medicament treatment has no adverse effects on wheat quality and non-target organisms.

[0096] The above content is a further detailed description of the present invention in combination with specific preferred embodiments. It cannot be determined that the specific implementation of the present invention is only limited to these descriptions. For those of ordinary skill in the technical field to which the present invention belongs, without departing from the concept of the present invention, several simple deductions or substitutions can still be made, which should all be regarded as belonging to the protection scope of the present invention.

Claims

1. A preparation method and application of a nano plant growth regulator, characterized in that: The effective active ingredients of the nano plant growth regulator are calcium cyclaconate and mepiquat chloride. The effective active ingredients are added with auxiliaries and water to form a suspension agent, wherein the weight ratio of mepiquat chloride to calcium cyclaconate is 2:

1.

2. The preparation method according to claim 1, characterized in that: The auxiliaries selected from one or more of hyperbranched dispersants, wetting agents, defoaming agents, preservatives, pH regulators, thickeners.

3. The preparation method according to claim 1 or 2, characterized in that: The hyperbranched dispersants selected from one or more of styrene maleic anhydride polymers, polyoxyethylene polyoxypropylene polyetheramine graft copolymers.

4. The preparation method according to claim 3, characterized in that: The weight ratio of the effective active ingredients to the hyperbranched dispersant is 1:1 to 8:1, optionally the weight ratio is 1:1 to 5:

1.

5. The preparation method according to any one of claims 1 to 4, characterized in that: The total weight of mepiquat chloride and calcium cyclaconate in the regulator is 90 to 510 g / L, optionally the total content is 300 g / L.

6. The preparation method according to claim 5, characterized in that: Taking 1000 parts by weight of the regulator, the components with the following contents Composition: 60 - 340 parts by weight of mepiquat chloride, 30 - 170 parts by weight of calcium cyclaconate, 10 - 150 parts by weight of hyperbranched dispersant, 20 - 80 parts by weight of wetting agent, 0 - 60 parts by weight of antifreeze, 2 - 25 parts by weight of thickener, 0.5 - 15 parts by weight of defoaming agent, 0.05 - 5 parts by weight of pH regulator, 0 - 20 parts by weight of preservative, and the balance of water.

7. The preparation method according to claim 6, characterized in that: Taking 1000 parts by weight of the regulator, the components with the following contents Composition: 60 - 340 parts by weight of mepiquat chloride, 30 - 170 parts by weight of calcium cyclaconate, 10 - 100 parts by weight of dispersant, 20 - 50 parts by weight of wetting agent, 30 - 60 parts by weight of antifreeze, 2 - 10 parts by weight of thickener, 0.5 - 8 parts by weight of defoaming agent, 0.05 - 2 parts by weight of pH regulator, 2 - 8 parts by weight of preservative, and the balance of water.

8. The preparation method according to claim 1, characterized in that: First, water, wetting agent, hyperbranched dispersant, and defoamer are put into a stirring tank and subjected to high-speed shearing. After sufficient dispersion, mepiquat chloride technical and prohexadione-calcium technical are added and subjected to high-speed shearing to form a primary dispersion liquid. Then, it is transported to two sand mills connected in series by a diaphragm pump for sanding. The sanding feed rate is adjusted to control the sanding fineness within 3 - 5 μm, and then it is transported to a turnover kettle by a diaphragm pump for stirring. This slurry is sanded by a nano sand mill after being filtered through a 200-mesh sieve, and the particle size D 50 is controlled to be less than 100 nanometers, and the particle size D 90 is controlled to be less than 300 nanometers. Finally, the slurry is transported to a modulation kettle, a thickening agent and a defoamer are added, the viscosity of the material is adjusted, and a sample is taken for quality inspection to obtain the finished product.

9. The application according to claim 1, wherein: Application of the regulator in regulating the growth of wheat.

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