Composite moroxydine hydrochloride water dispersible granule and preparation method thereof
Through the preparation of composite morpholin guanidine hydrochloride water dispersing granules, the combination of morpholin guanidine hydrochloride and aminooligosaccharide and porous structure design are used to solve the problems of weak targeting and poor stability of virus prevention and control agents, and the advantages of high efficiency and low toxicity, environmentally friendly virus prevention and control effects, good stability and convenient use are achieved.
Patent Information
- Application Number
- CN202510464760.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-15
- Publication Date
- 2025-07-29
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
Existing virus prevention and control agents have problems such as weak targeting, unstable effects, great impact on the environment, poor stability of microbial antiviral substances and inconvenient use.
Complex morpholin guanidine hydrochloride water dispersing granules are used to combine morpholin guanidine hydrochloride with amino oligosaccharide, and the guanidine and imino groups in morpholin guanidine hydrochloride are used to connect the amino and hydroxyl groups in amino oligosaccharide, and combine dispersants, wetting agents, disintegrants, binders and fillers to form a porous structure of water dispersing granules, which promote the uniform dispersion and rapid disintegration of amino oligosaccharide and morpholin guanidine hydrochloride, and improve stability and viral targeting.
It has achieved efficient and low-toxicity and environmentally friendly virus prevention and control effects, and the plants' resistance to viruses is enhanced. The water-dispersed granules are stable during transportation and are convenient to use.
Abstract
Description
Technical Field
[0001] The present application relates to the field of fungicides, and more specifically, to a compound moroxydine hydrochloride water dispersible granule and a preparation method thereof. Background Art
[0002] Currently, in the field of plant disease control, especially for diseases caused by viruses, it has a serious impact on the growth of plants. Traditional control measures mainly use chemically synthesized insecticides to indirectly inhibit the virus transmission vector, or cultivate virus-resistant crop varieties through genetic improvement; however, the long-term use of chemically synthesized drugs is likely to cause environmental pollution and damage the ecological balance. Although the transgenic technology to synthesize new species is effective, its acceptance is limited, and the development cycle is long.
[0003] Therefore, the existing control means have problems such as weak pertinence, unstable effect, and great environmental impact. Currently, for the control strategy based on biotechnology, generally, natural active substances produced by microorganisms can be used to fight against viruses. However, the antiviral substances of microorganisms have problems such as poor stability, inconvenient use, and difficulty in large-scale production and application.
[0004] Therefore, with the increasing pursuit of green and sustainable agriculture by people, how to prepare a new virus control agent with the advantages of high efficiency, low toxicity, environmental friendliness, strong virus pertinence, good stability, and convenient use is a problem to be solved. Summary of the Invention
[0005] In order to prepare a new virus control agent with the advantages of high efficiency, low toxicity, environmental friendliness, strong virus pertinence, good stability, and convenient use, the present application provides a compound moroxydine hydrochloride water dispersible granule and a preparation method thereof.
[0006] In the first aspect, the present application provides a compound moroxydine hydrochloride water dispersible granule, adopting the following technical solution: A compound moroxydine hydrochloride water dispersible granule contains the following raw materials in parts by weight: 1 - 3 parts of amino-oligosaccharides, 75 - 80 parts of moroxydine hydrochloride, 15 - 20 parts of dispersant, 5 - 15 parts of wetting agent, 4 - 8 parts of disintegrant, 20 - 35 parts of binder solution, and 50 - 60 parts of filler.
[0007] By adopting the above technical solution, moroxydine hydrochloride and oligosaccharins are combined. The guanidine group and imino group in moroxydine hydrochloride are connected with the amino group and hydroxyl group in oligosaccharins to improve the stability of the water dispersible granule. When moroxydine hydrochloride enters the plant body, it inhibits or destroys the nucleic acid and lipoprotein for virus replication, thereby blocking the replication chain of the virus. After oligosaccharins contact with the virus, the cation in the oligosaccharin molecule combines with the anion on the virus cell wall, thus blocking virus reproduction. By inhibiting virus replication and reproduction, the effect of controlling the virus is achieved, and the damage of the virus to the plant is reduced. At the same time, as a sugar signal activator, oligosaccharins can stimulate the defense response in the plant body, thereby indirectly promoting the production of disease-resistant substances in the plant, such as phenolic compounds, lignin, phytoalexins and other substances, further improving the plant's resistance to the virus and further reducing the damage of the virus to the plant. Moroxydine hydrochloride and oligosaccharins are of low toxicity, making the finished water dispersible granule have the advantages of high efficiency, low toxicity, environmental friendliness and strong virus targeting at the same time.
[0008] By utilizing the dispersion effect of the dispersant, it is convenient for oligosaccharins and moroxydine hydrochloride to be evenly dispersed. Combining with the filling and supporting effect of the filler, it further promotes the formation of a porous and loose structure inside the water dispersible granule. Combining with the water disintegration effect of the disintegrant, it can quickly disintegrate when the water dispersible granule is used. Combining with the water wetting effect of the wetting agent, it is beneficial for water to penetrate into the water dispersible granule, thereby further promoting the release of oligosaccharins and moroxydine hydrochloride, inhibiting the virus and improving the antiviral effect of the plant. At the same time, combining with the binding liquid can promote the formation of water-dispersible granules and also improve the stability of the water dispersible granule, and it is not easy to break or crack due to collision during transportation, ensuring the storage stability and transportation integrity of the water dispersible granule, and also having the advantage of convenient use.
[0009] Preferably, the filler is composed of modified sepiolite, diatomite and coconut shell fiber with a mass ratio of 1:1 - 3:0.5 - 1.
[0010] By adopting the above technical solution, modified sepiolite, diatomite and coconut shell fiber are combined. Using the porous structures of sepiolite, diatomite and coconut shell fiber as carriers, it is convenient to adsorb oligosaccharins and moroxydine hydrochloride, ensuring the granulation and forming effect of oligosaccharins and moroxydine hydrochloride, and improving the stability of the water dispersible granule, and it is not easy to lose oligosaccharins and moroxydine hydrochloride due to transportation collision, ensuring the medicinal property of the water dispersible granule. And sepiolite, diatomite and coconut shell fiber all have good adsorption effects, and can adsorb the virus to move and migrate towards the filler surface, thereby promoting the contact between the virus in the soil and oligosaccharins and moroxydine hydrochloride, inhibiting the virus, and cooperating with the control of the virus by oligosaccharins and moroxydine hydrochloride to prevent the virus from reproducing, migrating and spreading in the soil, thereby protecting the health of the plant.
[0011] During the disintegration of the water dispersible granule, the water absorption effect of sepiolite and diatomite is utilized in combination with the water diversion effect of coconut shell fiber, enabling water to quickly penetrate to the central position inside the water dispersible granule, thereby accelerating the disintegration of the water dispersible granule.
[0012] Preferably, the modified sepiolite is prepared by immersing sepiolite in an amino sulfonic acid solution and then bonding a polyacrylamide solution on its surface. The mass ratio of sepiolite to the polyacrylamide solution is 1:0.1 - 0.2.
[0013] By adopting the above technical solution, after being treated with the amino sulfonic acid solution, the surface porosity of sepiolite increases and its surface hydrophilicity enhances. Then, the polyacrylamide solution is bonded. By using the amide group in polyacrylamide in combination with the amino group and sulfonic acid group in the amino sulfonic acid solution, the toughness and hydrophilicity of the modified sepiolite are further increased. During the transportation of the water dispersible granule, by utilizing the toughness of the modified sepiolite and the cross - linking bonding stability between the modified sepiolite and the binder in the bonding liquid, the stability of the water dispersible granule is further improved, and it is not easy to appear fragmented or chipped due to collision during transportation, ensuring the integrity of the water dispersible granule during transportation.
[0014] Sepiolite has a certain adsorption effect, making it convenient for the bacteria on the surface of plant leaves to contact the amino sulfonic acid solution. By utilizing the good disease - resistant activity of the amino sulfonic acid solution, the control effect of the amino sulfonic acid solution on plant diseases is improved. And the amino sulfonic acid solution can also increase the nutrient components required by plants, such as elements like nitrogen and sulfur, improving the plant's antiviral property. When the amino sulfonic acid solution is combined with amino - oligosaccharin and moroxydine hydrochloride, it can also inhibit the replication and spread of viruses, thereby inhibiting virus activity. At the same time, the amino sulfonic acid solution can also trigger the plant's defense response and enhance the plant's resistance to viruses.
[0015] Preferably, the diatomite is prepared from diatomite microparticles and hydroxyethyl cellulose solution with a mass ratio of 1:0.1 - 0.3.
[0016] By adopting the above technical solution, by utilizing the viscosity of the hydroxyethyl cellulose solution, it is convenient to form a binding film layer through cross - linking connection with the bonding liquid and the polyacrylamide on the surface of the modified sepiolite, improving the stability of the diatomite microparticles and sepiolite in the water dispersible granule, and it is not easy to have problems such as being knocked and fragmented or chipped during transportation, ensuring the integrity of the water dispersible granule.
[0017] Preferably, the coconut shell fiber is prepared from coconut shell fiber filaments, sodium alginate solution and oat protein powder with a mass ratio of 1:0.1 - 0.2:0.1 - 0.2.
[0018] By adopting the above technical solution, the oat protein powder is adhered to the surface of the coconut shell fiber filaments by the viscosity of the sodium alginate solution. Utilizing the water absorption effect of the oat protein powder and in combination with the water-soluble effect of sodium alginate, during the preparation of the water dispersible granule, it is convenient to cooperate with the binder solution to form a film layer in which the coconut shell fiber, modified sepiolite, and diatomite are cross-linked and connected, sealing the oligosaccharin and moroxydine hydrochloride. With the flexibility of the film layer, the stability and transportation integrity of the water dispersible granule are further protected.
[0019] Oat protein and sodium alginate contain nutritional components, which can promote plant growth, induce the production of disease-resistant active ingredients in plants, improve the immune ability of plants, enhance the resistance of plants to pests and diseases. Moreover, oat protein and sodium alginate can also make the coconut shell fiber adhere to the surface of crops, extend the action time of oligosaccharin and moroxydine hydrochloride, and further improve the resistance of crops to virus diseases.
[0020] Preferably, the binder solution is prepared from fucoidan, hydroxypropyl-β-cyclodextrin and water with a mass ratio of 1:0.5 - 1:100 - 200.
[0021] By adopting the above technical solution, fucoidan and hydroxypropyl-β-cyclodextrin have good water-soluble viscosity. In combination with the hydroxyl groups of fucoidan and the hydroxyl groups in hydroxypropyl-β-cyclodextrin, it is convenient to tightly connect the oligosaccharin and moroxydine hydrochloride with the filler. The stable binding effect, combined with the film layer formed by the cross-linking of fucoidan, hydroxypropyl-β-cyclodextrin, hydroxyethyl cellulose, sodium alginate, and polyacrylamide, further seals the oligosaccharin and moroxydine hydrochloride, ensuring the transportation integrity and storage stability of the water dispersible granule.
[0022] Preferably, the dispersant is composed of sodium dodecylbenzenesulfonate and sodium hexametaphosphate with a mass ratio of 1:1 - 2.
[0023] By adopting the above technical solution, sodium dodecylbenzenesulfonate and sodium hexametaphosphate are combined. Utilizing their good dispersion effect, water dispersible granules with uniform dispersion can be prepared, enabling the water dispersible granules to have a rapid disintegration effect while having good forming effect and stability.
[0024] Preferably, the wetting agent is composed of glycerol and fatty alcohol polyoxyethylene ether with a mass ratio of 1:0.2 - 0.4.
[0025] By adopting the above technical solution, the plasticizing effect of glycerol can further promote the connection between modified sepiolite, diatomite and coconut shell fiber. The hydrophilic groups on the surface of the filler are connected to form a flexible film layer; in combination with fatty alcohol polyoxyethylene ether to promote the uniform dispersion of oligosaccharin and moroxydine hydrochloride, thus preparing a stably dispersed water dispersible granule, ensuring its rapid disintegration while having good stability and transportation integrity.
[0026] Preferably, the disintegrant is composed of carboxymethyl starch, citric acid and microcrystalline cellulose filaments with a mass ratio of 1:1 - 3:0.5 - 1.
[0027] By adopting the above technical solution, the rapid water absorption and swelling effects of carboxymethyl starch and citric acid are utilized to promote the rapid disintegration of the water dispersible granules. During the water absorption process, the microcrystalline cellulose filaments have a good flow guiding effect, which can promote the rapid migration of water into the interior of the water dispersible granules, further accelerating the disintegration of the water dispersible granules.
[0028] In a second aspect, the present application provides a method for preparing a compound moroxydine hydrochloride water dispersible granule, adopting the following technical solution: A method for preparing a compound moroxydine hydrochloride water dispersible granule, comprising the following steps: S1. Mix and stir uniformly amino-oligosaccharins, moroxydine hydrochloride, a dispersant, a wetting agent, a disintegrant and a filler to obtain a preliminary mixture; S2. Add a binding liquid to the preliminary mixture and stir evenly to obtain a mixed material; S3. Knead, granulate, dry and screen the mixed material to obtain the finished water dispersible granule.
[0029] By adopting the above technical solution, the water dispersible granule has the advantages of high efficiency, low toxicity, environmental friendliness, strong virus targeting, good stability and convenient use.
[0030] In summary, the present application has the following beneficial effects: 1. Moroxydine hydrochloride and amino-oligosaccharins are combined. The guanidine group and imino group in moroxydine hydrochloride are connected to the amino group and hydroxyl group in amino-oligosaccharins to improve the stability of the water dispersible granule; when moroxydine hydrochloride enters the plant body, it inhibits or destroys the nucleic acid and lipoprotein for virus replication, thereby blocking the virus replication chain. After cooperating with amino-oligosaccharins to contact the virus body, the cation in the amino-oligosaccharin molecule combines with the anion on the virus cell wall, thereby blocking virus reproduction. By inhibiting virus replication and reproduction, the effect of controlling the virus is achieved, reducing the damage of the virus to plants. Amino-oligosaccharins and moroxydine hydrochloride are of low toxicity, making the finished water dispersible granule have the advantages of high efficiency, low toxicity, environmental friendliness and strong virus targeting.
[0031] 2. Oligochitosan is a low-toxic bactericidal component, which has a strong inhibitory effect on pathogenic bacteria, can affect the germination of fungal spores, induce hyphal variation, and cause internal changes in spores. Moreover, it also has a significant antiviral effect, enabling plants to have a better antiviral disease effect. Oligochitosan itself contains rich carbon and nitrogen elements, which can be directly absorbed and utilized by crops after being decomposed by microorganisms. This can not only provide nutrients for crops, but also enhance the growth potential of crops, improve their resistance to viruses. And moroxydine hydrochloride also has a good antiviral effect on tomatoes, peppers, cucumbers and other plants.
[0032] 3. Modified sepiolite, diatomite and coconut shell fiber are combined. Using the porous structures of sepiolite, diatomite and coconut shell fiber as carriers, it is convenient to adsorb oligochitosan and moroxydine hydrochloride, ensure the granulation forming effect of oligochitosan and moroxydine hydrochloride, and improve the stability of the water dispersible granule. It is not easy to lose oligochitosan and moroxydine hydrochloride due to transportation collision, ensuring the medicinal properties of the water dispersible granule. And sepiolite, diatomite and coconut shell fiber all have good adsorption effects, which can adsorb viruses to move and migrate towards the filler surface, thereby promoting the contact between viruses in the soil and oligochitosan and moroxydine hydrochloride, inhibiting the viruses, and cooperating with the control of viruses by oligochitosan and moroxydine hydrochloride to prevent the reproduction, migration and diffusion of viruses in the soil, thus protecting the health of plants. Specific embodiments
[0033] The following further elaborates on this application with reference to the embodiments.
[0034] The following raw materials are all commercially available.
[0035] Preparation examples of modified sepiolite Preparation example 1: Modified sepiolite is prepared by the following method: Put 1 kg of sepiolite into 5 kg of sulfamic acid solution, soak and disperse it for 1 min under the condition of 20 kHz, then evenly spray 0.15 kg of polyacrylamide solution on the surface, and after drying and dispersing until the sepiolite does not adhere and agglomerate with each other, the finished modified sepiolite is obtained; the sepiolite passes through a 325-mesh sieve; the sulfamic acid solution is an aqueous solution of sulfamic acid with a mass fraction of 1%; the polyacrylamide solution is an aqueous solution of polyacrylamide with a mass fraction of 1%.
[0036] Preparation example 2: The difference between this preparation example and preparation example 1 is as follows: Put 1 kg of sepiolite into 5 kg of sulfamic acid solution, soak and disperse it for 1 min under the condition of 20 kHz, then evenly spray 0.1 kg of polyacrylamide solution on the surface, and after drying and dispersing until the sepiolite does not adhere and agglomerate with each other, the finished modified sepiolite is obtained.
[0037] Preparation example 3: The difference between this preparation example and preparation example 1 is as follows: Put 1 kg of sepiolite into 5 kg of sulfamic acid solution, soak and disperse it for 1 min under the condition of 20 kHz, then evenly spray 0.2 kg of polyacrylamide solution on the surface, and after drying and dispersing until the sepiolite does not adhere and agglomerate with each other, the finished modified sepiolite is obtained.
[0038] Preparation example of diatomite Preparation example 4: Diatomite was prepared by the following method: Evenly spray 0.2 kg of hydroxyethyl cellulose solution on the surface of 1 kg of diatomite particles. The hydroxyethyl cellulose solution is an aqueous solution of hydroxyethyl cellulose with a mass fraction of 1%. After drying and dispersing until the diatomite particles do not adhere and agglomerate with each other, the finished diatomite is obtained; the diatomite particles pass through a 325-mesh sieve, and the average open pore porosity is 85%.
[0039] Preparation example 5: The difference between this preparation example and preparation example 4 is that: Evenly spray 0.1 kg of hydroxyethyl cellulose solution on the surface of 1 kg of diatomite particles. The hydroxyethyl cellulose solution is an aqueous solution of hydroxyethyl cellulose with a mass fraction of 1%. After drying and dispersing until the diatomite particles do not adhere and agglomerate with each other, the finished diatomite is obtained.
[0040] Preparation example 6: The difference between this preparation example and preparation example 4 is that: Evenly spray 0.3 kg of hydroxyethyl cellulose solution on the surface of 1 kg of diatomite particles. The hydroxyethyl cellulose solution is an aqueous solution of hydroxyethyl cellulose with a mass fraction of 1%. After drying and dispersing until the diatomite particles do not adhere and agglomerate with each other, the finished diatomite is obtained.
[0041] Preparation example of coconut shell fiber Preparation example 7: Coconut shell fiber was prepared by the following method: Evenly apply 0.15 kg of sodium alginate solution on the surface of 1 kg of coconut shell fiber filaments, then add 0.15 kg of oat protein powder. The addition rate of the oat protein powder is 60 g / min. During the addition process, continuously stir under the condition of 200 r / min. After drying and dispersing until the coconut shell fiber filaments do not adhere and agglomerate with each other, the finished coconut shell fiber is obtained; the average length of the coconut shell fiber filaments is 40 μm, the sodium alginate solution is an aqueous solution of sodium alginate with a mass fraction of 1%, the average particle size of the oat protein powder is 5 μm, and the coconut shell fiber passes through a 200-mesh sieve.
[0042] Preparation example 8: The difference between this preparation example and preparation example 7 is that: Evenly apply 0.1 kg of sodium alginate solution on the surface of 1 kg of coconut shell fiber filaments, then add 0.1 kg of oat protein powder. The addition rate of the oat protein powder is 60 g / min. During the addition process, continuously stir under the condition of 200 r / min. After drying and dispersing until the coconut shell fiber filaments do not adhere and agglomerate with each other, the finished coconut shell fiber is obtained.
[0043] Preparation Example 9: This preparation example differs from Preparation Example 7 in that: 0.2 kg of sodium alginate solution is evenly applied on the surface of 1 kg of coconut shell fiber, and then 0.2 kg of oat protein powder is added at a rate of 60 g / min. During the addition process, stirring is continuously performed at 200 r / min. The coconut shell fiber is dried and dispersed until the coconut shell fiber does not stick to each other and agglomerate, thereby obtaining a finished coconut shell fiber.
[0044] Preparation example of adhesive solution Preparation Example 10: The adhesive solution was prepared by the following method: 1 kg of fucoidan, 1 kg of hydroxypropyl-β-cyclodextrin and 150 kg of water were mixed and stirred uniformly to obtain a bonding liquid.
[0045] Preparation Example 11: This preparation example differs from Preparation Example 10 in that: 1 kg of fucoidan, 0.5 kg of hydroxypropyl-β-cyclodextrin and 100 kg of water were mixed and stirred uniformly to obtain a bonding liquid.
[0046] Preparation Example 12: This preparation example differs from Preparation Example 10 in that: 1 kg of fucoidan, 1 kg of hydroxypropyl-β-cyclodextrin and 200 kg of water were mixed and stirred uniformly to obtain a bonding liquid. Example
[0047] Example 1: A composite morpholinoguanidine hydrochloride water dispersible granules: 2kg of amino oligosaccharides, 78kg of morpholinoguanidine hydrochloride, 18kg of dispersant, 10kg of wetting agent, 6kg of disintegrant, 28kg of binding liquid, and 55kg of filler; the dispersant is composed of sodium dodecylbenzenesulfonate and sodium hexametaphosphate in a mass ratio of 1:1; the wetting agent is composed of glycerol and fatty alcohol polyoxyethylene ether in a mass ratio of 1:0.3; the disintegrant is composed of carboxymethyl starch, citric acid, and microcrystalline cellulose in a mass ratio of 1:2:1; the binding liquid is the binding liquid prepared in Preparation Example 10; the filler is composed of modified sepiolite prepared in Preparation Example 1, diatomaceous earth prepared in Preparation Example 4, and coconut shell fiber prepared in Preparation Example 7 in a mass ratio of 1:2:1; The preparation method is as follows: S1. Mixing and stirring the amino oligosaccharide, morpholinoguanidine hydrochloride, dispersant, wetting agent, disintegrant and filler to obtain a primary mixture; S2, adding the binder to the primary mixture and stirring evenly to obtain a mixture; S3. The mixture is kneaded, granulated, dried and sieved to obtain finished water-dispersible granules with an average particle size of 2-3 mm.
[0048] Example 2: This example differs from Example 1 in that: 1 kg of oligosaccharins, 75 kg of moroxydine hydrochloride, 15 kg of dispersant, 5 kg of wetting agent, 4 kg of disintegrant, 20 kg of binder solution, 50 kg of filler; the dispersant is composed of sodium dodecyl benzene sulfonate and sodium hexametaphosphate with a mass ratio of 1:1; the wetting agent is composed of glycerol and fatty alcohol polyoxyethylene ether with a mass ratio of 1:0.2; the disintegrant is composed of carboxymethyl starch, citric acid and microcrystalline cellulose filaments with a mass ratio of 1:1:0.5; the binder solution is the binder solution prepared in Preparation Example 11; the filler is composed of modified sepiolite prepared in Preparation Example 2, diatomaceous earth prepared in Preparation Example 5 and coconut shell fiber prepared in Preparation Example 8 with a mass ratio of 1:1:0.5.
[0049] Example 3: The difference between this example and Example 1 is that: 3 kg of oligosaccharins, 80 kg of moroxydine hydrochloride, 20 kg of dispersant, 15 kg of wetting agent, 8 kg of disintegrant, 35 kg of binder solution, 60 kg of filler; the dispersant is composed of sodium dodecyl benzene sulfonate and sodium hexametaphosphate with a mass ratio of 1:2; the wetting agent is composed of glycerol and fatty alcohol polyoxyethylene ether with a mass ratio of 1:0.4; the disintegrant is composed of carboxymethyl starch, citric acid and microcrystalline cellulose filaments with a mass ratio of 1:3:1; the binder solution is the binder solution prepared in Preparation Example 12; the filler is composed of modified sepiolite prepared in Preparation Example 3, diatomaceous earth prepared in Preparation Example 6 and coconut shell fiber prepared in Preparation Example 9 with a mass ratio of 1:3:1.
[0050] Example 4: The difference between this example and Example 1 is that: The filler is diatomaceous earth.
[0051] Example 5: The difference between this example and Example 1 is that: In the filler, modified sepiolite is replaced with sepiolite of the same mass, coconut shell fiber is replaced with coconut shell fiber filaments of the same mass, the diatomaceous earth is ordinary commercially available diatomaceous earth, and hydroxyethyl cellulose is not added.
[0052] Example 6: The difference between this example and Example 1 is that: Hydroxypropyl-β-cyclodextrin is not added during the preparation of the binder solution.
[0053] Example 7: The difference between this example and Example 1 is that: Glycerol is not added to the wetting agent.
[0054] Example 8: The difference between this example and Example 1 is that: Microcrystalline cellulose is not added to the disintegrant.
[0055] Comparative Example Comparative Example 1: The difference between this comparative example and Example 1 is that: Oligosaccharins are not added to the raw materials.
[0056] Performance detection test 1. Disintegration detection The water dispersible granules were prepared by the methods of Examples 1 - 6 and 8 respectively. By using the graduated cylinder method, 1 g of the sample was weighed and quickly poured into a 200 mL stoppered graduated cylinder containing 180 mL of hard water. Then the cylinder mouth was stoppered, and it was rotated around the center of the graduated cylinder at a speed of 8 r / min. The stopwatch was used to record the time required for 99% complete disintegration of the granules. If the disintegration time was less than 3 min, it was qualified, and the data was recorded.
[0057] 2. Control effect detection The water dispersible granules were prepared by the methods of Examples 1 - 6 and Comparative Example 1 respectively; the water dispersible granules were added with water until they were completely disintegrated to obtain a suspension; the concentration of the active ingredient was controlled to be 33 mg / kg to obtain the medicament; Method for preparing the virus: Fresh tomato leaves infected with virus disease were collected, and buffer solution (phosphate buffered saline (PBS), pH = 7) was added according to the ratio of fresh diseased leaves: buffer solution = 1:3 (g:ml). The above mixture was placed into a sterilized mortar, quartz sand was added, and it was ground into a homogenate, filtered through sterilized gauze, and the virus was inoculated by the friction inoculation method; Control effect of tomato virus disease: Field prevention experiment: The experiment was carried out in the tomato plantation of Yimu Farm in Jinan City; when the tomato seedlings had the first true leaf (breaking the heart), the medicament was sprayed. 100 tomato seedlings were sprayed for each treatment, and then it was sprayed once every 7 days for 3 consecutive times. Each treatment was repeated 4 times and arranged randomly. After the medicament was sprayed, tomato virus was inoculated. The disease condition was investigated 10 days after inoculation, and the disease index and prevention effect were calculated; the application method of the medicament was spraying after diluting with water, and the water consumption per mu was 45 kg; Field treatment experiment: When the first inflorescence of the tomato seedlings showed buds, the virus was inoculated, and the inoculation method was the same as above. The medicament was sprayed 48 hours after inoculation, and the medicament treatment and spraying method were the same as above. The disease condition was investigated before each spraying and 7 days after the 3rd spraying, and the disease index and treatment effect were calculated; When investigating tomato virus disease, it was required to investigate all the plants in the investigation plot and record the disease occurrence situation by grading; Grade 0: No symptoms; Grade 1: Bright veins in the heart leaves, or mild mosaic; Grade 3: Mosaic in the heart leaves and middle leaves, and sometimes necrotic spots appeared on the leaves; Grade 5: Mosaic on most leaves, a few leaves were deformed and wrinkled, sometimes necrotic spots appeared on the leaves or stems, or short strip spots appeared on the stems; Grade 7: Severe mosaic, most leaves were deformed and slender, or systemic necrosis occurred in the stems and leaf veins, and the plants were dwarfed; Grade 9: The plants had severe systemic mosaic and deformity, or sometimes severe systemic necrosis, and the plants were severely dwarfed or even died; The disease index was investigated before applying the medicament, the control effect was investigated every 7 days during the application interval, and the control effect was investigated 14 days after the 3rd application; Disease index = ∑(number of diseased leaves at each level × relative level value) / total number of leaves surveyed × highest disease level × 100% Control effect = (control disease index - disease index of medicament treatment) / control disease index × 100%.
[0058] 3. Stability test The water-dispersible granules were prepared by the methods of Examples 1-7 respectively. During transportation, they were shaken for 30 min under the condition of 2000 Hz to simulate the shaking and extrusion during transportation. Then, the mass of the crushed powder of the water-dispersible granules was weighed and the data were recorded. The crushed powder was the powder passing through an 80-mesh sieve.
[0059] Table 1 Performance test table (in the table, " / " represents that the corresponding example or comparative example did not detect this item, so there is no data) Project Disintegration time / s Prevention and control effect / % Powder quality / g Example 1 88 92.65 1.8 Example 2 92 92.04 2.1 Example 3 95 92.87 1.6 Example 4 108 91.02 3.2 Example 5 100 91.44 2.8 Example 6 96 92.53 2.5 Example 7 / / 2.3 Example 8 95 / / Comparative Example 1 / 85.26 / Combined with Examples 1-3 and Table 1, it can be seen that the water-dispersible granules prepared in this application have the advantages of rapid dissolution, good control effect on virus diseases, and are not prone to fragmentation and caking during transportation, with good stability and integrity.
[0060] Combined with Example 1 and Examples 4-8 and Table 1, it can be seen that the filler of Example 4 is diatomite. Compared with Example 1, the disintegration time of the water-dispersible granules prepared in Example 4 is longer than that of Example 1, the control effect is worse than that of Example 1, and the mass of the crushed powder is greater than that of Example 1. It shows that the addition of modified sepiolite and coconut shell fiber not only increases the hydrophilicity of the water-dispersible granules, but also the porous water absorption of sepiolite cooperates with the water diversion effect of coconut shell fiber to further promote the rapid disintegration of the water-dispersible granules, and can also improve the stability and transportation integrity of the water-dispersible granules, and at the same time improve the control effect of plants on virus diseases.
[0061] In Example 5, the modified sepiolite was replaced with sepiolite of the same mass, the coconut shell fiber was replaced with coconut shell fiber filaments of the same mass, the diatomite was ordinary commercially available diatomite, and hydroxyethyl cellulose was not added. Compared with Example 1, the disintegration time of the water-dispersible granules prepared in Example 5 is longer than that of Example 1, the control effect is worse than that of Example 1, and the mass of the crushed powder is greater than that of Example 1. It shows that the surface-treated sepiolite, diatomite and coconut shell fiber can promote the cross-linking connection between the filler and the binder solution, ensure the stability and integrity of the water-dispersible granules during transportation; and can increase the hydrophilicity of the filler, further accelerate the disintegration of the water-dispersible granules; and can also improve the control effect of plants on virus diseases.
[0062] In Example 6, hydroxypropyl-β-cyclodextrin was not added during the preparation of the binder solution. Compared with Example 1, the disintegration time of the water dispersible granules prepared in Example 6 was longer than that in Example 1, the control effect was worse than that in Example 1, and the crushed powder quality was greater than that in Example 1. This shows that hydroxypropyl-β-cyclodextrin has good hydrophilic effect, can further promote the rapid dissolution of water dispersible granules, and hydroxypropyl-β-cyclodextrin can connect with fucoidan, hydroxyl, carboxyl, and amide substances on the surface of the filler to cooperate with the film-forming effect, further improving the internal structure stability of water dispersible granules, and it is not easy to have problems such as fragmentation and slagging of water dispersible granules during transportation.
[0063] In Example 7, glycerol was not added as the wetting agent. Compared with Example 1, the crushed powder quality of the water dispersible granules prepared in Example 7 was greater than that in Example 1. This shows that glycerol has good plasticizing effect, can promote the connection between the filler and the binder solution to form a tough film layer, and protect the water dispersible granules from fragmentation and slagging during transportation.
[0064] In Example 8, microcrystalline cellulose was not added as the disintegrant. Compared with Example 1, the disintegration time of the water dispersible granules prepared in Example 8 was longer than that in Example 1. This shows that microcrystalline cellulose has a certain guiding and draining effect on water, can accelerate the rapid dissolution of granular water dispersible granules, and is not easy to have problems such as the dissolution of the outer surface of water dispersible granules while the inside is not dissolved. At the same time, it has good hydrophilic effect and further accelerates the rapid dissolution effect of water dispersible granules.
[0065] Combined with Example 1 and Comparative Example 1 and Table 1, it can be seen that in Comparative Example 1, aminooligosaccharide was not added to the raw materials. Compared with Example 1, the control effect of the water dispersible granules prepared in Comparative Example 1 was worse than that in Example 1. This shows that aminooligosaccharide and moroxydine hydrochloride cooperate to improve the control effect of water dispersible granules on plant virus diseases.
[0066] This specific embodiment is only an explanation of the present application, and it does not limit the present application. Those skilled in the art can make modifications without creative contributions to this embodiment after reading this specification, but as long as it is within the scope of the claims of the present application, it is protected by the patent law.
Claims
1. A compound moroxydine hydrochloride water dispersible granule, characterized in that, It contains the following raw materials in parts by weight: 1 - 3 parts of amino - oligosaccharins, 75 - 80 parts of moroxydine hydrochloride, 15 - 20 parts of dispersant, 5 - 15 parts of wetting agent, 4 - 8 parts of disintegrant, 20 - 35 parts of binding liquid, and 50 - 60 parts of filler.
2. The compound moroxydine hydrochloride water dispersible granule according to claim 1, wherein: The filler is composed of modified sepiolite, diatomaceous earth, and coconut shell fiber with a mass ratio of 1:1 - 3:0.5 - 1.
3. A compound moroxydine hydrochloride water dispersible granule according to claim 2, characterized in that, The modified sepiolite is prepared by soaking sepiolite in an amino - sulfonic acid solution and then bonding a polyacrylamide solution on its surface. The mass ratio of sepiolite to the polyacrylamide solution is 1:0.1 - 0.
2.
4. The compound moroxydine hydrochloride water dispersible granule according to claim 2, characterized in that, The diatomaceous earth is prepared from diatomaceous earth microparticles and hydroxyethyl cellulose solution with a mass ratio of 1:0.1 - 0.
3.
5. A compound moroxydine hydrochloride water dispersible granule according to claim 2, characterized in that, The coconut shell fiber is prepared from coconut shell fiber filaments, sodium alginate solution, and oat protein powder with a mass ratio of 1:0.1 - 0.2:0.1 - 0.
2.
6. A compound moroxydine hydrochloride water dispersible granule according to claim 1, characterized in that, The binding liquid is prepared from fucoidan, hydroxypropyl - β - cyclodextrin, and water with a mass ratio of 1:0.5 - 1:100 - 200.
7. A compound moroxydine hydrochloride water dispersible granule according to claim 1, characterized in that, The dispersant is composed of sodium dodecyl benzene sulfonate and sodium hexametaphosphate with a mass ratio of 1:1 - 2.
8. The compound moroxydine hydrochloride water dispersible granule according to claim 1, characterized in that, The wetting agent is composed of glycerol and fatty alcohol polyoxyethylene ether with a mass ratio of 1:0.2 - 0.
4.
9. A compound moroxydine hydrochloride water dispersible granule according to claim 1, characterized in that, The disintegrant is composed of carboxymethyl starch, citric acid, and microcrystalline cellulose filaments with a mass ratio of 1:1 - 3:0.5 - 1.
10. A preparation method of a compound moroxydine hydrochloride water dispersible granule according to any one of claims 1-9, characterized in that, It includes the following steps: S1. Mix and stir evenly amino - oligosaccharins, moroxydine hydrochloride, dispersant, wetting agent, disintegrant, and filler to obtain a preliminary mixture. S2. Add the binding liquid to the preliminary mixture and stir evenly to obtain a mixed material. S3. Knead, granulate, dry, and screen the mixed material to obtain the finished product of water - dispersible granules.