An auxiliary agent for effectively preventing oxazolidinone from caking

Abstract

The present application relates to the technical field of functional additives, in particular to an additive for effectively preventing the agglomeration of oxadiazole, comprising the following raw materials in parts by weight: 100-130 parts of hydroxyethyl cellulose, 80-90 parts of sodium alginate, 15-30 parts of polyethylene glycol, 20-40 parts of inorganic powder, and 30-50 parts of surfactant. The additive for effectively preventing the agglomeration of oxadiazole of the present application is used for oxadiazole, and the additive for effectively preventing the agglomeration of oxadiazole is dissolved in water and sprayed on the surface of oxadiazole, and an isolation film is formed on the surface of oxadiazole, so that the water exchange between oxadiazole and the atmosphere is hindered, and the channel for water propagation is cut off. The agglomeration rate of oxadiazole obtained after 10 days of agglomeration experiment is as low as 5.1-0.6%, and the agglomeration rate after 20 days of agglomeration experiment is as low as 5.6-0.7%, which greatly improves the anti-caking effect of oxadiazole.

Description

Technical Field

[0001] The present application relates to the technical field of functional additives, and in particular to an additive that can effectively prevent caking of mefenamic acid. Background Art

[0002] The mainstream methods to solve soil-borne diseases are root irrigation, root showering and broadcasting. Root irrigation and root showering are labor-intensive, costly, and can easily cause pesticide damage if used improperly, so farmers are generally reluctant to irrigate the roots and usually do it out of necessity. Broadcasting generally uses fungicide granules, which have the advantages of saving labor, time, and a long lasting effect. The fungicide granules currently used are mostly oxazolidinone granules.

[0003] Methaclay is a new generation of methaclay developed by agricultural plant protection experts. It is a systemic high-efficiency pesticide fungicide, soil disinfectant, and also a plant growth regulator. It has unique efficacy, high efficiency, low toxicity, and is pollution-free. It is a green, environmentally friendly, high-tech product. Methaclay can effectively inhibit the normal growth of pathogenic fungal mycelium or directly kill pathogens, and promote plant growth; it also promotes the growth and development of crop roots, rooting and seedling growth, and improves the survival rate of crops. Methaclay has a very high penetration rate. It can move to the stem in two hours and move to the whole plant in 20 hours.

[0004] During the storage and transportation of oxazolidinone, changes in temperature, humidity, pressure and other factors will cause the surface of the crystal to repeatedly dissolve-crystallize-redissolve-recrystallize, forming crystal bridges and thus causing agglomeration. Agglomerated oxazolidinone must be crushed before use, which not only increases the workload but also poses a potential safety risk, bringing great inconvenience to the use of the product. Summary of the invention

[0005] In order to reduce the probability of powdered medicines agglomerating, the present application provides an auxiliary agent that effectively prevents the agglomeration of oxadiazine.

[0006] In the first aspect, the present application provides an auxiliary agent for effectively preventing oxazolidinone from agglomerating, using the following technical solution:

[0007] An auxiliary agent for effectively preventing oxadipazole from caking comprises the following raw materials in parts by weight: 100-130 parts of hydroxyethyl cellulose, 80-90 parts of sodium alginate, 15-30 parts of polyethylene glycol, 20-40 parts of inorganic powder and 30-50 parts of surfactant.

[0008] By adopting the above technical solution, the inorganic powder has the characteristics of fine particles, low density, strong adhesion, and has the function of mechanical isolation and absorbing moisture on the surface of particles, which can prevent the formation of connection points between grains and effectively prevent powder agglomeration. However, if the inorganic powder is used to prevent agglomeration of oxadone, the dosage is large, and the effect of using it alone is poor, which will cause the dust content of oxadone to increase.

[0009] Hydroxyethyl cellulose is a derivative of cellulose, prepared by etherification reaction of alkaline cellulose and ethylene oxide, and belongs to the class of non-ionic soluble cellulose ethers. Hydroxyethyl cellulose has good film-forming properties and a wide range of solubility. It is non-ionic and can coexist with other water-soluble polymers such as surfactants in a wide range, interacting to form a complex, so that the properties of the two are modified, the surface activity of the aqueous solution system is improved, and the dispersibility of the surfactant is enhanced.

[0010] Hydroxyethyl cellulose is firmly bonded to the outside of oxadipazole to form a tough solid film, which cuts off the channel for water transmission and mechanically isolates the oxadipazole particles, hindering the water exchange between oxadipazole and the atmosphere, thereby inhibiting the dissolution and recrystallization process on the crystal surface, preventing the formation of crystal bridges, and thus improving the anti-caking performance of the product. In addition, hydroxyethyl cellulose is a water-absorbing substance. Once there is more water on the surface of oxadipazole, it will absorb the water, thereby avoiding the redissolution of oxadipazole crystals.

[0011] Hydroxyethyl cellulose is used as the main film-forming substance, compounded with sodium alginate and polyethylene glycol, to form a film on the surface of the oxadiazine particles, promote the film-forming process, improve the film-forming quality and efficiency, and embed the inorganic powder and surfactant in the film during the film-forming process, so that the inorganic powder can be evenly dispersed outside the oxadiazine and cooperate with the surfactant to prevent the oxadiazine from agglomerating.

[0012] Furthermore, the inorganic powder includes one or more of talc, kaolin, bentonite, and diatomaceous earth.

[0013] By adopting the above technical scheme, talcum powder has good lubricity and dispersibility, can reduce the friction between powders, and reduce the agglomeration of powders during storage and transportation. Kaolin is a fine-grained clay mineral with good adsorption and dispersibility. In terms of powder anti-caking, kaolin can absorb moisture on the surface of the powder, reduce the adhesion between powder particles, and thus prevent agglomeration. Bentonite is a clay mineral with high water absorption and swelling, and its main component is montmorillonite. In terms of powder anti-caking, bentonite can absorb moisture and swell to form an isolation layer to prevent direct contact between powder particles, thereby reducing agglomeration. Diatomaceous earth is a porous material composed of diatom fossils with high porosity and large specific surface area. In terms of powder anti-caking, diatomaceous earth can provide additional surface area, adsorb moisture and grease on the surface of the powder, reduce adhesion between particles, and prevent agglomeration. These inorganic powders can all be used in the anti-caking agent in this application to reduce the probability of agglomeration of oxadiazon.

[0014] Furthermore, the inorganic powder comprises talc and bentonite in a weight ratio of 2:(3-5).

[0015] Furthermore, the particle size of the talc is 0.5-1.5 μm, and the particle size of the bentonite is 3-5 μm.

[0016] By adopting the above technical solution, the types and particle size distribution of the inorganic powder are limited, thereby further improving the anti-caking effect of oxazolidinone.

[0017] Furthermore, the surfactant includes at least one of sodium dodecylbenzene sulfonate and ammonium octadecanoate.

[0018] Furthermore, the surfactant comprises sodium dodecylbenzene sulfonate and ammonium octadecanoate in a weight ratio of (2-3):1.

[0019] By adopting the above technical solution, sodium dodecylbenzene sulfonate can improve the smoothness of the coating film, reduce the friction between particles, and adjust the hygroscopicity of the particles to prevent the particles from absorbing too much water and causing agglomeration. Ammonium octadecanoate is a surfactant that can form a hydrophobic protective film on the surface of the particles. This film can reduce the mutual attraction between the particles and reduce the adhesion of the particles, thereby preventing agglomeration. The combination of the two can further enhance the anti-caking effect of oxadiazon.

[0020] Furthermore, the hydroxyethyl cellulose is modified hydroxyethyl cellulose, and the modification method thereof is as follows:

[0021] The hydroxyethyl cellulose is dispersed in the dispersion, and a sodium hydroxide solution is added to completely swell the hydroxyethyl cellulose, and then octadecane bromide is added to react at 80-85° C. After the reaction is completed, the mixture is cooled, and the product is soaked in n-hexane, and then filtered to obtain a precipitate, which is washed and dried to obtain modified hydroxyethyl cellulose.

[0022] Furthermore, the weight ratio of the hydroxyethyl cellulose to octadecane bromide is 10:(7-9).

[0023] By adopting the above technical solution, a long carbon chain is grafted onto hydroxyethyl cellulose, and the hydroxyethyl cellulose is hydrophobically modified, so that the hydroxyethyl cellulose contains both hydrophilic groups and hydrophobic groups, and can form nano micelles with a core-shell structure in an aqueous solution through self-assembly technology. The content of ether bonds and alkane structures in the polymer is increased, the hydrophobic effect of the polymer is improved, the micelle structure formed by the polymer dispersed in water is more compact, the particle size is reduced, the self-assembly ability of the polymer is improved, and the encapsulation capacity of the oxazolidinone is improved.

[0024] In a second aspect, the present application provides an application of an auxiliary agent for effectively preventing the agglomeration of oxadipazole, using the following technical solution;

[0025] The invention discloses an auxiliary agent for effectively preventing caking of oxadipazole, which is applied to oxadipazole.

[0026] Furthermore, the auxiliary agent for effectively preventing the agglomeration of oxadone is dissolved in water to obtain a mixed solution, the mixed solution is sprayed on the surface of oxadone, and then dried, so that the auxiliary agent for effectively preventing the agglomeration of oxadone forms a film and wraps around the surface of oxadone.

[0027] By adopting the above technical solution, an effective wrapping film is formed outside the oxazolidinone, thereby improving the anti-caking effect of the oxazolidinone.

[0028] In summary, this application has the following beneficial effects:

[0029] 1. A compound of hydroxyethyl cellulose, sodium alginate and polyethylene glycol is used as a film-forming substance, and an inorganic powder and a surfactant are used as functional additives to prepare an auxiliary agent for effectively preventing the agglomeration of oxadzeb; the auxiliary agent for effectively preventing the agglomeration of oxadzeb is used for oxadzeb to form an isolation film outside the oxadzeb, and the agglomeration rate of the obtained oxadzeb after 10 days of the agglomeration experiment is as low as 5.1-0.6%, and the agglomeration rate after 20 days of the agglomeration experiment is as low as 5.6-0.7%, which greatly improves the anti-caking effect of oxadzeb.

[0030] 2. Hydroxyethyl cellulose was modified with octadecane bromide to further improve the anti-caking effect of oxadiazon. The caking rate of oxadiazon was as low as 1.9-0.6% after 10 days of the caking experiment and as low as 2.1-0.7% after 20 days of the caking experiment, which greatly improved the anti-caking effect of oxadiazon. DETAILED DESCRIPTION

[0031] The present application is further described in detail below with reference to the embodiments.

[0032] Raw materials and intermediate preparation examples

[0033] raw material

[0034] The raw materials in the examples of this application can be obtained from the market:

[0035] Hydroxyethyl cellulose, analytical grade, molar substitution 1.8;

[0036] Sodium alginate, analytical grade;

[0037] Polyethylene glycol, molecular weight 2000, analytical grade.

[0038] Preparation Example

[0039] Preparation Example 1

[0040] A modified hydroxyethyl cellulose, the preparation method of which is as follows:

[0041] 1. Weigh 1 kg of hydroxyethyl cellulose and disperse it in 6 L of isopropanol solution by ultrasonic dispersion. Stir it in a water bath with magnetic stirring at 25°C for 30 min to obtain a hydroxyethyl cellulose dispersion.

[0042] 2. Under nitrogen protection, 0.05 kg of sodium hydroxide solution was added to water to prepare a saturated sodium hydroxide solution, and the saturated sodium hydroxide solution was added dropwise to the hydroxyethyl cellulose dispersion, and magnetic stirring was performed for 24 hours to completely swell the hydroxyethyl cellulose to obtain a mixed solution;

[0043] 3. Disperse 0.7 kg of octadecane bromide in 2 L of isopropanol solution to obtain octadecane bromide dispersion, add the octadecane bromide dispersion dropwise into the above mixed solution, and stir and react at 80°C for 5 h;

[0044] 4. After the reaction is completed, the reaction system is cooled to room temperature, the product is soaked in n-hexane overnight, and then filtered to obtain a precipitate. The precipitate is soaked and filtered with acetone solution for 3 times. The final product is adjusted to pH 7 with glacial acetic acid and vacuum dried at 45°C for 12 hours to obtain modified hydroxyethyl cellulose.

[0045] Preparation Example 2

[0046] The difference from Preparation Example 1 is that the amount of octadecane bromide used in Preparation Example 2 is 0.8 kg.

[0047] Preparation Example 3

[0048] Different from Preparation Example 1, the amount of octadecane bromide used in Preparation Example 3 is 0.9 kg.

[0049] Preparation Example 4

[0050] Different from Preparation Example 1, the amount of octadecane bromide used in Preparation Example 4 is 1 kg. Example

[0051] Examples 1-3

[0052] An auxiliary agent for effectively preventing oxazolidinone from caking, and a preparation method thereof is as follows:

[0053] According to the raw material ratio in Table 1, hydroxyethyl cellulose, sodium alginate, polyethylene glycol, inorganic powder and surfactant are mixed to obtain an auxiliary agent that effectively prevents caking of oxadipate.

[0054] Table 1 Raw material ratios in Examples 1-3 (kg)

[0055]

[0056] The inorganic powder is talcum powder with a particle size of 0.5-1.5 μm, and the surfactant is sodium dodecylbenzene sulfonate and ammonium octadecanoate in a weight ratio of 2:1.

[0057] Example 4

[0058] Different from Example 2, the inorganic powder in Example 4 is bentonite with a particle size of 3-5 μm.

[0059] Example 5

[0060] Different from Example 2, the inorganic powder in Example 5 is talcum powder and bentonite in a weight ratio of 2:4, wherein the particle size of the talcum powder is 0.5-1.5 μm, and the particle size of the bentonite is 3-5 μm.

[0061] Example 6

[0062] Different from Example 2, the inorganic powder in Example 6 is talcum powder, kaolin and bentonite in a weight ratio of 1:1:2, wherein the particle sizes of talcum powder, kaolin and bentonite are all 0.5-1.5 μm.

[0063] Example 7

[0064] Different from Example 5, the surfactant in Example 7 is sodium dodecylbenzene sulfonate.

[0065] Example 8

[0066] Different from Example 5, the surfactant in Example 8 is ammonium octadecanoate.

[0067] Examples 9-12

[0068] Different from Example 5, in Examples 9-12, hydroxyethyl cellulose is replaced by an equal amount of modified hydroxyethyl cellulose from Preparation Examples 1-4, respectively.

[0069] Comparative Example

[0070] Comparative Example 1

[0071] The difference from Example 1 is that in Comparative Example 1, an equal amount of hydroxyethyl cellulose is used to replace sodium alginate.

[0072] Comparative Example 2

[0073] The difference from Example 1 is that in Comparative Example 1, an equal amount of hydroxyethyl cellulose is used to replace polyethylene glycol.

[0074] Comparative Example 3

[0075] Different from Example 1, in Comparative Example 3, equal amounts of hydroxyethyl cellulose were used to replace sodium alginate and polyethylene glycol.

[0076] Comparative Example 4

[0077] Different from Example 1, in Comparative Example 4, the surfactant was replaced by an equal amount of inorganic powder.

[0078] Comparative Example 5

[0079] Different from Example 1, in Comparative Example 5, an equal amount of surfactant is used to replace the inorganic powder.

[0080] Comparative Example 6

[0081] Different from Example 1, in Comparative Example 6, the surfactant and the inorganic powder were replaced by an equal amount of hydroxyethyl cellulose.

[0082] Performance Testing

[0083] The performance of the films of the anti-caking agents obtained in Examples 1-12 and Comparative Examples 1-3 after film formation was tested according to the following method. The test results are shown in Table 2.

[0084] The additive that effectively prevents the caking of oxadipate was dissolved in water at a weight ratio of 1:30. 20 mL of the anti-caking agent solution was cast on a culture dish with a diameter of 10 cm and dried in an oven at 60 °C. After cooling, the mechanical properties were measured using a mechanical universal testing machine. Before the test, the sample was cut into rectangles (80 mm long and 10 mm wide), the gauge length was fixed at 30 mm, and the speed of the pneumatic clamp was 5 mm / min.

[0085] Table 2 Performance test results

[0086]

[0087] Combining Examples 1-12 with Comparative Examples 1-6 and Table 2, it can be seen that the mechanical properties of the films obtained in Examples 1-12 are better than those of Comparative Examples 1-6, which indicates that the coating film obtained by the auxiliary agent of the present application that effectively prevents the agglomeration of oxadiazine has better mechanical properties.

[0088] Combining Example 1 with Comparative Examples 1-3 and Table 2, it can be seen that in Example 1, hydroxyethyl cellulose, sodium alginate, and polyethylene glycol are compounded as film-forming substances to prepare coating films; in Comparative Example 1, hydroxyethyl cellulose and polyethylene glycol are compounded as film-forming substances to prepare coating films; in Comparative Example 2, hydroxyethyl cellulose and sodium alginate are compounded as film-forming substances to prepare coating films; in Comparative Example 3, strong and cellulose silk are used as film-forming substances to prepare coating films; the mechanical properties of the coating films in Example 1 are significantly better than those in Comparative Examples 1-3, which shows that the coating films obtained by compounding hydroxyethyl cellulose, sodium alginate, and polyethylene glycol as film-forming substances have better performance. This may be because hydroxyethyl cellulose has good film-forming properties. Using hydroxyethyl cellulose as the main film-forming substance, compounded with sodium alginate and polyethylene glycol, sodium alginate and polyethylene glycol can be well cross-linked with hydroxyethyl cellulose, dispersed evenly, promote the film-forming process, and improve the film-forming quality and efficiency.

[0089] Combining Example 5 with Examples 9-12 and Table 2, it can be seen that the mechanical properties of the coating film obtained in Examples 9-12 are better than those in Example 5, which shows that the modification of hydroxyethyl cellulose with long-chain carbon can further improve the performance of the coating film. This may be because the long carbon chain is grafted onto hydroxyethyl cellulose, the content of ether bonds and alkane structures in the polymer is increased, and the hydrophobic effect of the polymer is improved. Nano-micelles with a core-shell structure can be formed in an aqueous solution through self-assembly technology, so that the micelle structure formed by the polymer dispersed in water is more compact, the particle size is reduced, and the self-assembly ability of the polymer is improved, thereby improving the encapsulation capacity of oxazolidinone.

[0090] Application Examples

[0091] Application Example 1

[0092] An application of an auxiliary agent for effectively preventing caking of oxadipazole in oxadipazole comprises the following steps:

[0093] The auxiliary agent for effectively preventing the agglomeration of oxadone obtained in Example 1 was dissolved in water at a weight ratio of 1:30 to obtain a mixed solution, and the mixed solution was sprayed on the surface of oxadone, and then dried at 50°C, so that the auxiliary agent for effectively preventing the agglomeration of oxadone formed a film and was wrapped on the surface of oxadone.

[0094] Application Example 2-12

[0095] Different from Application Example 1, the auxiliary agents that effectively prevent the agglomeration of oxazolidinone in Application Examples 2-12 are from Examples 2-12, respectively.

[0096] Comparative Application Examples

[0097] Comparative Application Examples 1-3

[0098] Different from Application Example 1, the auxiliary agents that effectively prevent the agglomeration of oxazolidinone in Comparative Application Examples 1-3 come from Comparative Examples 4-6, respectively.

[0099] Performance Testing

[0100] The anti-caking performance of the oxadiazine obtained in the corresponding use case and the comparative application example was tested according to the following method. The test results are shown in Table 3.

[0101] The anti-caking oxadipate was sealed in a bag and placed in an oven. The temperature was kept at 60°C during the day and dropped to 25°C at night. The relative humidity was 70%. The caking condition was checked on the 10th and 20th days, and the caking rate was determined. The caking rate was determined by dropping the sample from a height of 1 m on both sides once, unpacking it, sieving it with a standard sieve, and then weighing the total mass of oxadipate and the mass of caking oxadipate after sieving, and calculating the caking rate:

[0102] ;

[0103] In the formula, m is the mass of agglomerated compound fertilizer after screening, g; m0 is the total mass of compound fertilizer, g.

[0104] Table 3 Performance test results

[0105]

[0106] Combining Application Examples 1-12 with Comparative Application Examples 1-6 and Table 3, it can be seen that the caking rate of oxazolidinone in Application Examples 1-12 is lower than that in Comparative Application Examples 1-6, which indicates that the auxiliary agent for effectively preventing oxazolidinone from caking prepared in the present application has a better anti-caking effect on oxazolidinone.

[0107] Combining Application Example 1 with Comparative Application Examples 1-3 and Table 3, it can be seen that in Example 1, inorganic powder and surfactant are added to the coating film formed by hydroxyethyl cellulose, in Comparative Application Example 1, inorganic powder is added to the coating film formed by hydroxyethyl cellulose, in Comparative Application Example 2, surfactant is added to the coating film formed by hydroxyethyl cellulose, and in Comparative Application Example 3, no other raw materials are added to the coating film formed by hydroxyethyl cellulose. The caking rate of oxadiazine in Example 1 is significantly lower than that in Comparative Application Examples 1-3, among which the caking rate in Comparative Application Example 3 is the highest, which indicates that the addition of inorganic powder and surfactant to the coating film formed by hydroxyethyl cellulose can further improve the anti-caking performance of oxadiazine. This may be because the addition of inorganic powder and surfactant regulates the surface properties of the hydroxyethyl cellulose film and further improves the anti-caking effect of oxadiazine.

[0108] Combining Application Example 2 with Application Examples 4-6 and Table 3, it can be seen that the type of inorganic powder and the particle size distribution will affect the anti-caking performance of oxazolidinone. Among them, the anti-caking performance is better when talcum powder and bentonite are compounded in a weight ratio of 2:4 as inorganic powder, wherein the talcum powder particle size is 0.5-1.5μm and the bentonite particle size is 3-5μm.

[0109] Combining Application Example 5 with Application Examples 9-12 and Table 3, it can be seen that the caking rate of oxadiazon in Application Examples 9-12 is lower than that in Application Example 5, which indicates that the anti-caking effect of oxadiazon can be improved by modifying hydroxyethyl cellulose. This may be because grafting a long carbon chain on hydroxyethyl cellulose can regulate the quality of film formation, improve the mechanical properties of the film, and better play its anti-caking effect, which can also be confirmed by combining Table 2.

[0110] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make modifications to the present embodiment without any creative contribution as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.

Claims

1. An auxiliary agent for effectively preventing oxazolidinone from caking, characterized in that: The method comprises the following raw materials in parts by weight: 100-130 parts of hydroxyethyl cellulose, 80-90 parts of sodium alginate, 15-30 parts of polyethylene glycol, 20-40 parts of inorganic powder, and 30-50 parts of surfactant; The inorganic powder comprises talc and bentonite in a weight ratio of 2:(3-5); The particle size of the talc is 0.5-1.5 μm, and the particle size of the bentonite is 3-5 μm; The hydroxyethyl cellulose is modified hydroxyethyl cellulose, and the modification method thereof is as follows: Dispersing hydroxyethyl cellulose in a dispersion, adding a sodium hydroxide solution to completely swell the hydroxyethyl cellulose, then adding octadecane bromide, reacting at 80-85° C., cooling after the reaction, soaking the product with n-hexane, then filtering to obtain a precipitate, washing and drying the precipitate to obtain modified hydroxyethyl cellulose; The weight ratio of the hydroxyethyl cellulose to octadecane bromide is 10:(7-9).

2. The auxiliary agent for effectively preventing oxazolidinone from agglomerating according to claim 1, characterized in that: The surfactant includes at least one of sodium dodecylbenzene sulfonate and ammonium octadecanoate.

3. The auxiliary agent for effectively preventing caking of oxamexazole according to claim 2, characterized in that: The surfactant includes sodium dodecylbenzene sulfonate and ammonium octadecanoate in a weight ratio of (2-3):

1.

4. An application of an auxiliary agent for effectively preventing caking of oxamexazole according to any one of claims 1 to 3, characterized in that: It is applied to oxadiazine.

5. The use of an auxiliary agent for effectively preventing caking of oxamexazole according to claim 4, characterized in that: The auxiliary agent for effectively preventing the agglomeration of oxadone is dissolved in water to obtain a mixed solution, the mixed solution is sprayed on the surface of oxadone, and then dried, so that the auxiliary agent for effectively preventing the agglomeration of oxadone forms a film and wraps the surface of oxadone.

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