JPS6020359B2 - 1'-Ethoxycarbonyloxyethyl ester of valbroic acid and its production method - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a coated fertilizer whose surface is treated to prevent water repellency and a method for producing the coated fertilizer.

More specifically, it relates to a fertilizer in which powder particles and a surfactant are attached to the surface of a fertilizer coated with a coating material containing resin, and a method for adhering them.The purpose is to impart permanent hydrophilicity to the surface of the coated fertilizer. It is an object of the present invention to provide a coated fertilizer that prevents floating due to water repellency when fertilizing paddy fields or in ditch water, and a method for producing the same. A coated fertilizer has been developed in which granular fertilizer is coated with a water-resistant film to control the dissolution of fertilizer components.

This type of fertilizer is made by covering a hydrous fertilizer such as urea, ammonium sulfate, or sulfurized ammonium with a coating material such as resin or sulfur, but all coating materials have poor affinity for water and are not water repellent. Because it is strong, it has the disadvantage that it tends to float when applied to rice fields or when flooded, for example. In addition, even when applied to fields, it has the disadvantage that it is easily exposed to the soil surface by irrigation or rainfall. However, there is currently no research to eliminate this drawback. It can be inferred from the literature that in order to impart hydrophilicity to highly water-repellent materials such as coating materials, it is sufficient to spray or apply a surfactant, but in this method, once placed in water or soil, the surfactant is It washes away, and the lasting effect of hydrophilicity disappears.

Also, when a surfactant is added to the coating material, some effect is observed, but it is insufficient or sufficient. The inventors have completed the present invention through repeated research into a treatment method that has a long-term and complete effect of preventing floating due to vertical water properties.

The present invention resides in a fertilizer in which powder particles and a surfactant are attached to the surface of a granular fertilizer coated with a resin-containing coating material, and a method for attaching the same.

The resin referred to in this) is not particularly limited, but thermoplastic resins such as JP-A-50-9 Shikiniri Hakama Sekisho 51
Resin compositions containing one or more of polyolefins, ethylene vinyl acetate copolymers, and vinylidene chloride resins as shown in Japanese Patent Publication No. 175674, 1975-265, and thermosetting resins, such as those disclosed in Japanese Patent Publication No. 40-128927. Preferred examples include coating compositions obtained by uniformly dispersing talc, charcoal, metal oxides, sulfur, etc. in the relatively soft resin oil-dicyclobentadiene copolymer shown above and their resin compositions. However, in the case of thermosetting resin, the effect is not durable unless the surface treatment is performed immediately before the completion of curing of the resin before coating is completed. The present invention can be applied to any type of coating material as long as it is carried out under conditions where powder adheres to the surface.
Preferred surfactants for the present invention have an HLB of 6 to 16. If the HLB is too high, the surfactant has poor affinity with the resin component, so the surfactant tends to diffuse unevenly onto the resin surface, and substances attached to the powder tend to transfer to the aqueous phase, resulting in a sustained effect. lacking in sex. On the other hand, if it is too low, the affinity with water will be poor and the effect of preventing vertical water will be insufficient. These surfactants can be used alone or as a mixture. The amount used is 0.01 to 20% by weight of the resin weight, preferably 0.05 to 20% by weight.
If the amount is less than 0.01% by weight, which is 1% by weight, the water repellency prevention effect is insufficient, and if it is added more than 2% by weight, there is no advantage. Furthermore, the surfactant used in the present invention can be either nonionic or ionic. For example, polyoxyethylene alkyl ethers, polyoxyethylene alkyl phenyl ethers, esters of polyoxyethylene glycol and fatty acids, polyoxyethylene amines, higher alcohol sulfates, etc. However, nonionic ones that do not require consideration of solution pH etc. are easier to use. In the present invention, the characteristic powders to be attached to the surface of the coating material include activated carbon, diatomite, iron oxide, clay, bentonite, silicic acid, etc., but porous activated carbon, diatomite, and iron oxide are the most It is a preferable powder and is effective in a range of 0.01% by weight or more based on the coated fertilizer.

If the amount is less than 0.01%, the effect of preventing vertical water formation is insufficient, and it is usually difficult to deposit more than 0.5%.

The reason why the surface of the product of the present invention is highly hydrophilic is: (1) The surface of the fertilizer particle has a porous powder attached to it, forming an uneven structure with acute angles; In this case, the contact with water becomes less than 4, and as a result, it becomes easier to leak into water.
■Because surfactants are adsorbed on the surface of the powder, it becomes easy to peel, and water sinks into the powder, resulting in a water film layer on the surface and loss of water repellency. Conceivable.

The reason for the effectiveness of the product of the present invention is: (1) Part of the surfactant used penetrates into the coating of the coated fertilizer during processing and storage.
When the soil is retained and fertilizer is applied to the soil, the surfactant is released from the coating, and the surfactant is more concentrated and more strongly adsorbed on the adhering powder than on the surface of the resin coating layer. Therefore, it is thought that the product of the present invention retains the surfactant for a longer period of time than when the surfactant is applied to the surface of the coated fertilizer to which no particles adhere, and therefore the effect lasts for a longer period of time. The product of the present invention is a coated fertilizer in which powder particles are attached to the surface of the coating, and is different from coated fertilizers in which fillers such as talc and metal oxides are dispersed inside the coating.

In other words, when powder particles are dispersed within the coating, the type of powder particles,
The surface is smooth regardless of the amount added, and the surface of this coating is highly hydrophobic unless the surface treatment shown in the table of the present application is carried out. The production of the fertilizer of the present invention consists of two steps: (1) a step of adhering the characteristic powder to a coating; and (2) a step of adding a surfactant.

A preferable method for adhering fine powder according to the present invention is a method in which the coated particles are fluidized or jetted using a fluid such as air in which the powder is dispersed, so that the coated particles are uniformly adhered to the surface.

In this case, it is important that the coating surface and the fine powder adhere firmly; if the adhesion is weak, part of the fine powder will separate from the surface when the surface absorbs water, and the water repellency prevention effect will not be achieved. It will be enough. A factor that enhances this adhesion is the surface temperature of the particle coating, requiring the adhesion to operate at temperatures close to the fusion point. This temperature varies depending on the type of resin and mixture composition, and if it is carried out in a temperature range above the brooding point, parts of the resin covering the fertilizer particles will fuse together, and when they separate, film defects will occur. As a result, the effectiveness of the coating is impaired, so it is important to appropriately determine the surface temperature of the coating upon adhesion of the powder by experiment. An example of a method for selecting this temperature will be described below.

First, a surfactant is made to coexist with coated fertilizer particles to which powder has been attached at a specific particle temperature using the method described in the section on adding a surfactant, and it is confirmed whether or not they actually float.
If a large number of particles float in this step, a similar confirmation test may be performed by changing the particle temperature to find the point at which they do not float, and this temperature can be used as the adhesion temperature. An example of the determination is shown below. Place tens or hundreds of coated fertilizer particles into a container such as a petri dish, place them on the wall of the container, and check whether the particles float when water is gently poured into the container. If the whole amount floats to the surface. Items that do not have a lasting effect will not float to the surface at first, but if the water is removed and water is poured in the same way again, they will float to the surface, so sustainability can be determined through this repeated test. The addition of the surfactant in the present invention is not limited to a specific method, and various methods can be used.

For example, when a surfactant is applied to the surface of a coating material and then powder is attached, the surfactant may be in the form of a liquid or in the form of a solution. When adding a solid surfactant, it may be melted by heating and liquefied before being added, or it may be dissolved in a solvent and added in the form of a solution. In order to uniformly apply these surfactants to the particle surfaces, any of various particle mixing methods such as fluidized bed, spouted bed, rotating drum, rotating pan, etc. can be used. When adding a surfactant after adhering the powder to the surface of the coating, it is important to add the surfactant uniformly in the form of a spray, and to ensure uniformity, it is necessary to spray the surfactant next to each other in the form of a solution. It is more preferable. In this case as well, the powder-adhering particles are maintained in various mixed states, such as jetting, fluidization, rolling, etc., and a necessary amount is added in the form of mist for surface treatment. In general, the surfactant adsorption method on the coated powder is used to adsorb the surfactant on the coated powder and make the coated fertilizer particles adhere to the surface of the coated fertilizer particles to prevent the surface from becoming watery. It can be adsorbed by the method of adsorbing organic compounds to.

For example, a preferred method is to dissolve a surfactant in a solvent, immerse the surfactant in the solution to absorb it, and then dry it. In this case, the fine powder can be attached to the surface of the coated particles in the same way as the fine powder to which no surfactant is adsorbed, by the above-mentioned attachment method. The coated fertilizer treated according to the present invention has excellent fluidity and does not have caking properties, and is not only preferable as a mechanically applied fertilizer, but also especially when applied to paddy fields, since floating due to water repellency can be prevented, the coated fertilizer This is an indispensable treatment method when applied to paddy fields.

Example 1 This example shows a method for attaching fine powder to the surface of a coated fertilizer. FIG. 1 shows a jet device used for attaching fine powder in this example.

Reference numeral 1 denotes a jet tower with a diameter of 25 m, a height of 200 m, an air outlet diameter of 5 m, and a fertilizer inlet 2 and an exhaust gas outlet 3.

The jet air is sent from the blower 7, passes through the orifice flow meter 6 and the heat exchanger 5, and reaches the jet tower.The flow rate is controlled by the flow meter, the temperature is controlled by the heat exchanger, and the exhaust gas is sent from the outlet to the outside of the tower. guided by. The coated fertilizer that undergoes surface treatment is introduced through the input port while a predetermined amount of air is allowed to flow. When the coated fertilizer particles to be treated reach a predetermined temperature, the fine powder contained in the fine powder hopper 8 is fed by the micro feeder 9 to one fine powder disperser. The special powder disperser has a structure that blows out high-velocity air at the part where it comes into contact with the fine powder. It comes into contact with the surface and adheres to it. When a predetermined amount of adhesion is reached, the microfeeder is stopped, the pressurized air and the blower are stopped, and the product is extracted from the extraction port 4. In this example, processing was carried out while maintaining the following basic conditions.

Hot air volume: 4/min Coated granular fertilizer input amount: 10k9 fertilizer particle size
5-7 mesh (coated spherical urea with coverage rate of 5 wt%)
Powder supply speed: 5 mm/min In Fig. 1, 11 is a mist nozzle, 12 is a pump, and 13 is a tank, but these are for feeding the surfactant, and from Example 2 onwards. When a surfactant was added in any case, it was added through this nozzle.

Example 2 This example shows a method of searching for a preferable temperature at which the powder is deposited.

In Example 1, as a covering material, polyethylene 9-goku,
A surfactant (hexaoxyethylene nonyl phenyl ether) (1% by weight of the coating) was applied to the granular urea coated with a coating material consisting of 1 anchor portion of ethylene vinyl acetate copolymer to the particles in the jet stream.

As a powder, 3 females of Diabetes japonica (0.3% by weight relative to the fertilizer) were attached to the particles at the particle temperature shown in Table 1. Two females (approximately 600 particles) were treated at each particle temperature with a diameter of 15. &mosquito,
After placing it in a petri dish with a height of 3 skins, water was poured gently along the wall of the dish and the ratio of the number of particles that floated (floating rate) was determined. After this test, it was left overnight) and then all the water was extracted. The test to determine the levitation rate of the aircraft was repeated 10 times, 3 times each time. Table 1 shows the test results of this example.

In all cases where the particle temperature at the time of deposition is 75° C. or higher, sustainability of floating prevention is observed. For comparison, a sample coated with only a surfactant did not float until the first coat, but after the second coat there was no lasting effect because the surfactant on the surface was washed away. Moreover, the untreated one had no effect from the first time. Furthermore, the adhesion temperature is 120qo
In this case, part of the coated fertilizer particle film fuses with each other, and when they separate due to particle movement, part of the fused film is damaged and lacquer oozes out from the defective part, resulting in early elution. has increased. Therefore, in this example, the appropriate temperature range for the treatment of the coated fertilizer used is 75 to 80q○. In addition, the dissolution rate in water for 2 hours in Table 1 is 1 female coated particle to 3 pi○20 in water.
This figure shows the weight percent of nitrogen dissolved into water when the sample was warmed and left at that temperature for 2 hours.

Table 1 Example 3 This example describes the relationship between the amount of the characteristic powder added and the sustained flotation prevention effect.

In the characteristic powder adhesion method of Example 2, 0, 0.01, 0.5, 1.0% by weight of the coated fertilizer was used instead of diatoms.
Iron oxide powder corresponding to the amount of the coated fertilizer was maintained at 7% and 0) and adhered to the surface, and the floating rate was determined by the floating rate measuring method shown in Example 2. Table 2 shows the 4th ascent rate. In Table 2, the adhesion rate of iron oxide was determined by increasing the weight of the attached particles, and in this example, it was 0.3 to 0.4wt.
% is the limit of the adhesion rate, and it is thought that the excess amount escaped from the system without being attached.

Example 4 This example describes the amount and effect of surfactant.

In the powder adhesion method of Example 2, the weight of the coated portion was 0, 0.01, 0.05, and 1.05, respectively. Activated carbon powder corresponding to 0.3% was supplied to the coated fertilizer coated with 0.3% surfactant and adhered to the surface of the coated fertilizer.

The fourth levitation rate, which was measured using the method of Example 2, was as shown in Table 3. Table 3 Example 5 This example shows that even if a surfactant is added after the powder is attached to the surface of the coated fertilizer, it has an anti-floating effect.

In the surface treatment method of Example 2, firstly, 0.00% of the coating fertilizer was applied. t% of powder was supplied and adhered to the surface.

Thereafter, one layer of the surfactant used in Example 2 was used.
A product of the present invention was obtained by exposing a solution (solvent: trichlorethylene) at dawn while maintaining the temperature at which the powder was deposited. Table 4 shows the composition of the coating film, the deposition temperature, the amount of surfactant added, and the results of measuring the flying rate in this example.

In all cases, the levitation rate was 0 and sustainability was observed. In addition, in this example, tests were conducted in which the amount of surfactant was changed and added to the coating by 0, 1, 10, and 2 wt%, respectively.
% flotation, but the flotation rate of the one to which a surfactant was added remained 0 even after 10 injection tests. Fourth Example 6 This example is provided to show that it is also effective to apply a surfactant to the powder and adhere it to the surface of the coated fertilizer.

The surfactant used in Example 2 was dissolved in methanol (1%) and activated carbon powder was added to 1/10th of the solution.
The activated carbon powder was soaked in an amount of 0.3 wt % to the granular coated fertilizer used in Example 2 and applied at 80 qo according to the application method of Example 2.

This surface-treated product was tested by the flying rate measurement method of Example 2, and it was found that the flying rate preventing effect was sustained.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flow sheet showing a schematic vertical cross-sectional view of the jet device used in Example 1 to attach the powder to the surface of the coated fertilizer.

FIG. 2 is an enlarged sectional view of the powder supply section. 1...
... Jet tower, 2 ... Fertilizer inlet, 3 ...
・Exhaust gas exhaust port, 4... Exhaust port, 5...
・Heat exchanger, 6... Orifice flow meter, 7...
... Prower, 8 ... Powder hopper, 9
...Ficro feeder, 10...Characteristic powder disperser, 11...Nozzle.

Sai/Picture of the outside of the box

Claims (1)

[Scope of Claims] 1. A fertilizer coated with a resin-containing coating material and having fine powder and a surfactant having an HLB of 6 to 16 adhered to the surface of the granular fertilizer. 2. A surfactant with an HLB of 6 to 16 is added to the surface of granular fertilizer coated with a coating material containing resin, and the coated fertilizer is fluidized or jetted in hot air, and the temperature of the coated fertilizer is adjusted to the temperature of the coating. A coating that imparts hydrophilicity and prevents flotation, characterized by adhering the fine powder to the surface of the coated granular fertilizer by feeding and dispersing the fine powder in hot air while maintaining the temperature near the fusion temperature. Fertilizer manufacturing method. 3. Fluidize or jet the granular fertilizer coated with a resin-containing coating material in hot air, and feed the fine powder into the hot air while maintaining the temperature of the coated fertilizer near the melting temperature of the coating. The fine powder is attached to the surface of the coated granular fertilizer by dispersion, and a surfactant having an HLB of 6 to 16 is added to the surface to impart hydrophilicity and prevent floating. Method for producing coated fertilizer. 4 A granular fertilizer coated with a resin-containing coating material is fluidized or jetted in hot air, and while the temperature of the coated fertilizer is raised and maintained near the melting temperature of the coating, a surfactant is added in advance. A hydrophilic fertilizer characterized in that fine powder containing a surfactant with an HLB of 6 to 16 is adhered to the surface of the coated granular fertilizer by feeding the adhered fine powder into hot air and dispersing it. A method for producing a coated fertilizer that prevents floating when applied.