KR960003805B1 - Manufacturing process of particle agricultural chemical-fertilizer - Google Patents

Abstract

The long-lasting pesticide fertilizer is prepared by coating more than one layers of the fertilizer granule, which consists of a single layer or multiple layers of fertilizer and pesticide, with basic coating agent by 1-40wt% with respect to the uttermost inner layer. The basic coating agent is obtained by dissolving 0.5-50wt% rosin in a solvent. Additionally the coating agent involves less than 70wt% rosin derivative , less than 20wt% polymeric substance or both of them.

Description

Manufacturing method of slow-release granular pesticide fertilizer

The present invention relates to a coated granular pesticide fertilizer which can improve the sustaining effect of fertilizers and pesticides and is easy to handle and store, and a method for producing the same.

More specifically, it consists of a fertilizer layer, pesticide layer, interlayer material, if the fertilizer layer or pesticide layer is a multi-layer coating at least one layer of the pesticide or fertilizer layer so that the desired fertilizer or pesticide components can be eluted at the required time, The present invention relates to a sustained-release granular agrochemical fertilizer which is easy to handle and store and optionally has a sustained effect by additionally coating a protective coating, and a method of manufacturing the same.

The use of fertilizers and pesticides is one of the most effective and rapid ways to maximize the yield of agricultural products per unit cultivated area. To date, the use of fertilizers and pesticides has contributed greatly to the improvement of agricultural productivity and the reduction of agricultural labor. Demand is expected to increase. However, many studies have been conducted to solve this problem because of the continuous pollution or excessive use of the environment and the need for labor to spray fertilizers and pesticides whenever necessary.

Since slow-release pesticide fertilizers are eluted into soil and water for a long time, they can reduce the number of times of use, which can reduce costs and labor compared to fast-acting pesticides or fertilizers. It is also possible to reduce the harm to the human body when using the development is urgently required.

Slow-release pesticide fertilizers come in both mixed and coated forms. The mixed type is made of pellets or briquettes by mixing chemically reacted urea such as isobutylidene diurea or nitrogen fertilizer such as oxamide melamine or compound fertilizer with pesticides and binders. Because it can be applied only in the case of fertilizers or pesticides, there is a disadvantage that cannot be applied to water-soluble fertilizers or pesticides.

The coating type includes a multi-layer coating of fertilizer particles with a crosslinked collagen or a crosslinking collagen with a coating agent containing a pesticide component, or a coating of particles prepared by mixing a fertilizer and a pesticide component with a polymer material. They are difficult to control the dissolution rate of the active ingredient or complicated coating process, the manufacturing cost is high, there is a problem that the polymer material used as the coating material remains in the soil after the active ingredient is eluted. In order to compensate for this, the soil decomposable polymer material may be used, but in such a case, the manufacturing price will be higher.

Applicants have studied to solve the above problems, and have developed a slow-acting agrochemical fertilizer and its manufacturing method which are excellent in effectiveness, easy in manufacturing process, and inexpensive without being accumulated in soil after use.

The present invention relates to a sustained-release pesticide fertilizer consisting of at least one layer of fertilizer, a pesticide layer and an interlayer material, and wherein at least one layer of the fertilizer layer or pesticide layer is coated with a rosin or a rosin mixture and a method for producing the same. Rosin mixtures are meant to contain rosin derivatives and / or polymers in addition to rosin.

In addition, the present invention is composed of one or more layers of fertilizer, pesticide layer and interlayer material, and base coating of one or more layers of fertilizer or pesticide layer with rosin or rosin mixture, and protecting the outer layer of the basic coated pesticide fertilizer with polymer material It relates to a coated sustained-release pesticide fertilizer and a method for producing the same.

Since the sustained-use pesticide fertilizer prepared by the method of the present invention can supply nutrients necessary for the growth of crops and prevent pests at the same time, it can reduce the amount and the number of pesticides and fertilizers. Reduce labor and reduce labor.

According to the present invention, cultivation of crops with single use by coating fertilizers, herbicides, fungicides, insecticides, plant growth regulators and the like in order to coat each layer containing fertilizers or pesticides so that each active ingredient is eluted at the required time. It can continue to supply the required fertilizers and pesticides.

The elution rate can be effectively controlled by separating one or more of each pesticide and fertilizer layer into rosin or rosin and / or rosin derivatives and / or base coatings containing the polymeric material as the main component.

In particular, in the present invention, since rosin, which is a natural substance, is used as the main component of the base coating, rosin is slowly decomposed in the soil or water after the active ingredient is eluted, and thus the coating material does not accumulate, thereby preventing environmental pollution.

In addition, according to the present invention, the final coating of the basic coated granular pesticide fertilizer with a protective film, there is no sticking and entanglement between the coated pesticide particles or damaged coating material, which is advantageous in handling and storage.

In addition, the process of the present invention is simpler than the conventional method for producing slow-acting pesticide fertilizer.

Fertilizers that can be used in the present invention are, for example, urea fertilizers or complex fertilizers.

Pesticides that can be used in the present invention are, for example, mixed with water-soluble herbicides, insecticides, plant growth regulators themselves or by weighting agents such as clay, talc, silica, diatomaceous earth, alumina, magnesia, CaO, bentonite, urea fertilizer, compound fertilizer, etc. It is a pesticide manufactured.

Examples of herbicides include dicamba, glufosinate, dimuron, triclopyr, fosamine-ammonium, 2,4-di-sodium oxadiazole, betazone, bromasil, glyphosate, methyl, propanyl, thio Bencarb, perfluidone, fenchlorim, dimethamethrin, simethrin and the like. Examples of fungicides include ivypi, pyroquilon, tricyclazole, kasugamycin, validamycin-, and examples of pesticides include diazinon, biphimci, pyradapention, metholcap, carbofuran, mono Crotoforce, Quinal force, Etofenprox, etc. are mentioned. Plant growth regulators include ansimides, ethylclozeates, chlormethol, choline chloride, and the like.

The method of the present invention is described in detail as follows.

First, the method of preparing the base-coated slow-release pesticide fertilizer of the present invention is dissolved 30-100% by weight of rosin, 0-70% by weight of rosin derivative and 0-20% by weight of high molecular material to 0.5-50% by weight in an organic solvent. The basic coating is prepared, and the basic coating consists of one or several basic coatings of 2-40% by weight of the fertilizer layer and / or the pesticide layer.

The base coating used in the present invention consists of a rosin and an organic solvent, and may optionally contain 70 wt% or less of rosin derivative and / or 20 wt% or less of polymer material. The coating process for basic coating is achieved by spraying rosin or rosin mixture in organic solvent with a pan-type rotating coater and spraying the pesticide and / or fertilizer particles.The drum rotation speed is 10-30rpm per minute and the air pressure of spray nozzle is 1-3Kg / cm ² , the temperature is maintained at 20-70 ℃.

After the coating, the pesticide particles finish the drying process in the drum of the coating machine. The temperature is 30-90 ℃ and the drying time is 1 minute-2 hours. The solvent is relatively easy to recover because it uses an organic solvent having a high volatility and a low boiling point, and the process is completed by drying the solvent without requiring a special heat treatment process.

The fertilizer layer and the pesticide layer may be monolayer or multilayer, respectively, and the layer order of each active ingredient will be determined according to the order to be eluted. It is not necessary to divide each layer into a base film, and the dissolution rate of each active ingredient can be controlled by adjusting the thickness of the base film. If necessary, the basic coating agent composed mainly of rosin and rosin derivatives may be divided into 1 to 10 times so that the content of the pesticide particles may be 2-40% by weight.

The base coating may optionally contain a fertilizer component.

The production method of the basic coating and protective coating of the sustained-release pesticide fertilizer according to the present invention is to prepare a basic coated pesticide fertilizer according to the production method of the basic-covered sustained-release pesticide fertilizer, the organic polymer material to 0.5-50% by weight in an organic solvent The protective coating prepared by melting is made of the protective coating of less than 30% by weight to the outer layer of the basic coating pesticide fertilizer.

The protective film is coated by spraying a coating solution obtained by dissolving an organic polymer compound in an organic solvent to the basic coating pesticide using the same fan-type rotary coating machine as in the rosin base coating. Drum rotation speed is 10-30rpm per minute, spray nozzle air pressure is 1-3Kg / cm, temperature is maintained at 20-70 ℃. As in the basic coating, the coating of the protective film may be divided into 1-10 times as necessary so that the total weight content of the protective coating is 0-30% for the basic coating pesticide fertilizer particles. After the process is finished, the coated pesticide particles are finished in the drum of the coater. The temperature is 30-90 ° C and the drying time is 1 minute-2 hours. The whole process is completed by the drying process without going through a special heat treatment process.

Since the coating material of the present invention has a smooth coating, high mechanical strength and flexibility, and the main ingredient is rosin, which is a natural resin, it has a merit that the coating material is gradually decomposed in the soil after the pesticide is eluted, and the coating material remains in the soil.

In the present invention, rosin includes gum rosin, wood rosin, tall oil rosin, and there are differences in softening temperature and components depending on the type and refining state, but their main components are all resinous resins such as abicic acid and slightly neutral. Contains substance. The effect is best when using gum rosin.

In the present invention, the rosin derivative means an ester of rosin, polymerized or dimerized rosin, hydrogenated rosin, rosin reacted with maleic anhydride or phenol-formaldehyde or an ester thereof.

They are effective in raising the melting point of rosin and increasing the durability, and particularly, the effect of the product obtained by reacting rosin reacted with maleic anhydride or esters of these with polyhydric alcohols such as glycerol and toluene diisocyanate. Several kinds of rosin derivatives may be used alone or in combination of two or more.

In the present invention, the polymer material refers to ethyl cellulose, benzyl cellulose, nitrocellulose, polyvinylacetate, polyacrylate, alkyd resin, copolymer of vinyl acetate and rosin, and the addition of such polymer material increases the sustaining effect and durability. Different polymer materials can be used alone or in combination of two or more. In particular, the effect of the copolymer of ethyl cellulose and nitrocellulose, polyvinylacetate, vinyl acetate and rosin is excellent.

Solvents that can be used in the present invention are organic solvents including alcohol solvents that can dissolve rosin, methanol, ethanol, isoprapanol, t-butanol, benzene, ether, methylene chloride, tetrahydrofuran, chloroform, acetone, methyl acetate , Ethyl acetate, acetonitrile, trichloroethane and the like, among which the effects of alcohols, acetone, ethers are excellent.

In the present invention, the organic polymer compound used for coating the protective film is ethyl cellulose, benzyl cellulose, nitro cellulose, polyvinylacetate, alkyd resin, copolymer of rosin and vinyl acetate, acrylate or copolymer of styrene and vinyl acetate, and the like. These may be used alone or in combination of two or more thereof. In particular, nitrocellulose or a copolymer of rosin and vinyl acetate shows an excellent effect in increasing the durability of the coated granular pesticides.

These organic solutions are prepared using alcohols such as ethanol, benzene, methylene chloride or acetone as solvents.

As used herein, "%" refers to weight percent unless otherwise noted.

The present invention will be described in more detail with reference to Examples.

These examples are intended to illustrate some of the scope of the invention and are not intended to limit the scope of the invention.

Example 1

Gum rosin was dissolved in ethanol to make a coating solution of 20% by weight. Using a fan type coater, a fertilizer particle having a thickness of 2.38-2.54 mm was coated at a temperature of 50 ° C. with an air pressure of 1.5 Kg / cm ² and a spray amount of 2 ml / min, so that the coating ratio was 5% by weight relative to the fertilizer particles. After the coating was finished, the pan was dried at the same temperature for 10 minutes to obtain a coated urea fertilizer.

The pesticide layer was coated by adding 20 g of pesticide while spraying 20 ml of water on it. At this time, the rotational speed of the fan was 70 rpm per minute, the air pressure of the spray nozzle was 1.5kg / cm ² , the temperature was maintained at 40 ℃. After the coating was finished, air heated to 50 ° C. in a rotating fan of the coating machine was blown and dried for 1 hour. The pesticides used are listed in Table 1. Using the gumozin solution prepared above, the fertilizer particles coated with the base coat and the pesticide layer were coated with a total coating rate of 10% by weight relative to the fertilizer particles.

After the drying process, the dissolution test was carried out, and the amount of the pesticide eluted was measured using high pressure liquid chromatography purchased from Verian. Table 1 shows the results of measuring the amount of pesticides and fertilizers eluted by coating the coated pesticide fertilizer in water at 30 ° C.

Among the pesticide fertilizers prepared, in particular glufosinate, fosamine-ammonium, 2,4-di-sodium, glyphosate, metomile, chlormethol, pyroquilon, kasugamycin, validamycin-A, metolcap, monochrom It was confirmed that the dissolution rate control effect by the coating was excellent in the case of agrochemicals having a high water solubility such as tophos.

[Table 1] Eluents of Pesticides and Fertilizers over Time

Example 2

The primary pesticide layer was coated by adding 20 g of clay mixed with 20% by weight of pyroquilon while spraying 20 g of water by the method of Example 1 onto 100 g of urea fertilizer particles having a diameter of 2.38-2.54 mm using a fan type coater. 100 g of gum rosin was melt | dissolved in 400 g of ethanol, and it coat | covered by the method of Example 1 so that the coating solution coverage may be set to 5 weight% with respect to fertilizer particle | grains.

20 g of clay mixed with 20% by weight monoclotophos was used to coat the secondary pesticide layer in the same manner as the primary pesticide layer coating. The pesticide fertilizer particles coated with the secondary pesticide layer were coated with a rosin base coating in the same manner as above using the gumrogin solution prepared above. In the same manner, a tertiary pesticide layer was coated with 20 g of glufosinate mixed in the same amount with urea. Finally, the rosin solution prepared above was used to coat 6%.

Table 2 shows the results of measuring the amount of pesticides and fertilizers eluted by putting the coated pesticide fertilizer into water at 30 ° C.

[Table 2] Dissolution Rate of Pesticides and Fertilizers over Time

Example 3

The rosin derivative was mixed with 30% by weight of gum rosin and dissolved in acetone to make a solution of 20% by weight. Table 3 shows the types of rosin derivatives used.

Example 1 In this method, 100 g of granular urea fertilizer was coated in the order of rosin base film, pesticide layer, and rosin base film, and the pesticide layer was coated with 20 g of clay mixed with 10% by weight of glufosinate. The primary coating was coated so that the coverage was 5% and the secondary coating was 10%.

Table 3 shows the results of measuring the amount of pesticides and fertilizers eluted by putting the coated pesticide fertilizer into water at 30 ° C.

[Table 3] Dissolution Rate of Pesticides and Fertilizers over Time

Example 4

Gum rosin was mixed with 10% by weight of polymer and dissolved in ether to form an ether solution having a concentration of 20% by weight. The polymer materials used are listed in Table 4. The coating process was carried out in the same manner as in Example 1, using this as a basic coating agent and using chloromethene as a pesticide.

Table 4 shows the dissolution rate of pesticides and fertilizers in water at 30 ℃.

[Table 4] Dissolution Rate of Pesticides and Fertilizers over Time

Example 5

In the method of Example 3, 100 g of granular urea fertilizer was coated with a rosin primary film at a coverage rate of 4.5%, and a pesticide layer was formed from 20 g of clay mixed with 40% by weight of valididamic acid-A, and at 9.5% coverage. After coating the secondary rosin coating, a protective coating was performed.

Dissolve the polymer material in an organic solvent to make 5% by weight or make an emulsion solution to prepare a protective film coating solution, and cover the pesticide particles at a spray nozzle air pressure of 1.5Kg / cm ² , spraying amount 2ml / min at a temperature of 50 ℃ I was. After the coating was finished, the pan was dried at the same temperature for 10 minutes.

Table 5 shows the results of measuring the amount of pesticides and fertilizers eluted by putting the coated pesticide fertilizer into water at 30 ° C.

[Table 5] Dissolution Rates of Pesticides and Non-yo

Example 6

The protective film was coated by the method of Example 5 to the coated pesticide fertilizer prepared by the methods of Examples 3 and 4. As a pesticide, a mixture of posamine-ammonium at 25% by weight was used. As the protective coating agent, ethyl cellulose dissolved in benzene at 10% by weight was used, and the coating was applied at a coverage of 2.5%.

Table 6 shows the dissolution rates of pesticides and fertilizers in water at 30 ° C.

[Table 6] Dissolution Rate of Pesticides with Time

Example 7

NPK composite fertilizer (15-15-15) having a diameter of 2.0-3.16 mm in the method of Example 1 was coated with ballidamic acid-A mixed with clay at 70% by weight, followed by wood rosin and tall oil, respectively. The coat was used to coat 10% coverage. The polyvinylacetate was dissolved in toluene to make a solution that was 5% by weight to prepare a protective coating solution, and was coated on the pesticide fertilizer by the method of Example 5. The coverage was 3% of the pesticide fertilizer particles, and the dissolution rate of the coated pesticide fertilizer in water at 30 ° C. is shown in Table 7.

[Table 7] Dissolution Rate of Pesticides and Fertilizers over Time

Example 8

In the same manner as in Example 3, 100 g of granular urea fertilizer was ground-coated at 10% by weight using a methanol solution containing 30% by weight of rosin, and 20g of glyphosinate mixed with 10% by weight of clay was added. The layer was coated with a pesticide layer and then secondary coated with a rosin base coating solution prepared at 9% coverage. Some of these were coated with 2% by weight nitrosel rate relative to the pesticide fertilizer. In order to investigate the durability, the two types of pesticide fertilizer prepared in each shaker (Model No. 1640 manufactured by KKIC) were shaken at a rate of 100 times / minute for 5 minutes, and then the dissolution rate of the pesticide fertilizer in water of 30 ℃ was measured. The measurement is shown in Table 8.

[Table 8] Dissolution Rate of Pesticides Untreated with Time

Example 9

The pesticide fertilizers made by the method of Example 8 were put into bags each made of polyethylene film 25 cm and 18 cm in width and length, respectively, and then weighted with a weight weighing 50 kg each for 10 days.

At this time, the pesticides coated only with rosin were severely entangled with the pesticide particles, but the pesticide fertilizer coated with rosin and protective film was not observed.

The pesticide dissolution rate in water at 30 ° C. is shown in Table 9.

[Table 9] Dissolution Rate of Pesticides and Fertilizers over Time

Claims (13)

A base coating material in which rosin is dissolved in an organic solvent at 0.5-50% by weight, wherein the base coating is coated at 1-40% by weight with respect to the innermost layer of at least one layer of pesticide fertilizer consisting of a single layer or a multilayer fertilizer layer and a pesticide layer. A process for producing sustained-release pesticide fertilizers. The rosin derivative according to claim 1, wherein the base coating agent further comprises 70% by weight or less of a rosin derivative; Or 20% by weight or less of a polymeric material; Or 70% by weight of a binary rosin derivative and 20% by weight or less of a polymeric material. The outermost layer of the pesticide fertilizer coated by the method of claim 1 or 2 is coated with a protective coating obtained by dissolving the organic polymer material in an organic solvent at 0.5-50% by weight to 30% by weight or less with respect to the innermost layer. A method for producing a sustained-release pesticide fertilizer. The method of claim 3, wherein the rosin is selected from the group consisting of wood rosin, gum rosin, tall oil rosin and mixtures thereof. 4. The rosin derivative according to claim 3, wherein the rosin derivative is an ester of rosin, polymerized or dimerized rosin, hydrogenated rosin, rosin with maleic anhydride, a product obtained by reacting them with glycerol or with toluene diisocyanate and their Method for producing a sustained-release pesticide fertilizer, characterized in that selected from the group consisting of a mixture. 4. The sustained-use pesticide fertilizer according to claim 3, wherein the high molecular material used in the basic coating is selected from the group consisting of ethyl cellulose, nitrocellulose, polyvinylacetate, copolymers of vinyl acetate and rosin, and mixtures thereof. Manufacturing method. The organic solvent used in the base coating is methanol, ethanol, isopropanol, t-butanol, benzene, ether, tetrahydrofuran, chloroform, acetone, methylene chloride, methyl acetate, ethyl acetate, acetonitrile. And trichloroethane. A process for producing a sustained-release pesticide fertilizer characterized in that it is selected from the group consisting of. The method of claim 3, wherein the organic polymer used in the protective coating is ethyl cellulose, benzyl cellulose, polyvinylacetate, nitrocellulose, vinyl acetate, copolymers of vinyl acetate and rosin, acrylates, styrene and mixtures thereof Method for producing a sustained-release pesticide fertilizer, characterized in that selected from the group consisting of. The method of claim 8, wherein the solvent used in the protective coating is selected from the group consisting of toluene, methanol, ethanol, isopropanol, benzene, acetone and methylene chloride. 4. The method for producing a sustained-release pesticide fertilizer according to claim 3, wherein the basic coating and the protective coating are divided and coated at a desired number of times. The method for producing a sustained-release pesticide fertilizer according to claim 3, wherein the base film contains fertilizer. A sustained-use pesticide fertilizer in which at least one layer of agrochemical fertilizer consisting of a single layer or a multi-layer fertilizer layer and a pesticide layer is coated with a base film containing rosin. At least one layer of pesticide fertilizer consisting of a single layer or a fertilizer layer and a pesticide layer is coated with a base coating containing rosin, and the outer layer of the fertilizer layer and the pesticide layer is protected with a protective coating containing a polymer compound. Pesticide fertilizer.