Preformed pesticide product, dispersible in water, and method thereof

 

(57) Abstract:

Pelletized pesticidal composition, despergiruemaya in water with the formation of particles with a size of 1-3 microns, includes 30-40 wt.% pesticide with so pl. of not less than 100oC 3-7% surfactant, polyvinylpyrrolidone 20-40 wt.%, cellulose - 10-30 wt. %, silicon dioxide and magnesium stearate as additives is 0.5 to 1.0 and 0.05-2.0 wt.% respectively. The way to obtain this drug is that the active ingredient is subjected to predominantly wet grinding, and the resulting suspension is mixed with other ingredients, followed by granulating and pelletizing the mixture. 2 S. and 6 C.p. f-crystals.

The invention relates to metering devices (metered tool). It is also concerned with a method of formation of the dosing device and to a method of processing products or the local places.

According to the first aspect of the present invention, a method of manufacturing a metering device, which includes:

mixing at least one active ingredient, which is at the 25oC is in solid form and which has an average particle size less than 5 microns, with dezintegriraat agent received/P> This method can include grinding the active ingredient, which is in a solid form and having an average particle size greater than 5 microns, in order to obtain particles with an average size of less than 5 microns. The active ingredient can be quite crushed to particles with an average size of 1 to 3 μm. In one of the embodiments of this invention, the grinding can be carried out dry grinding of the active ingredient, for example, by micronisation, to particles of the desired size. Then milled active ingredient may be mixed in the form of particles with dezintegriraat agent. Another embodiment of the present invention is that the grinding can be carried out by preparing a suspension concentrate active ingredient in a suitable liquid carrier in which the active ingredient is insoluble or sparingly soluble, and wet grinding suspension concentrate to produce particles of active ingredient desired size. Then the suspension concentrate can be mixed with dezintegriraat agent by absorbing it in dezintegriraat agent. However, if desired, crushed suspension concentrate can be dried by spraying and then si ingredient, such as a therapeutic tool, antihelminthic agent, pigment or dye, and the like, the applicant believes that this method will especially be used, but this is not necessarily the only, in the manufacture of the metering devices in which the active ingredient is a pesticide, such as insecticide, herbicide, fungicide, and the like.

A pesticide may be a pesticide, which is moderately soluble in water, so water can be used as a liquid medium during the formation of the suspension concentrate, and concentration of the pesticide in water, a suspension concentrate, therefore higher than the limit of solubility of the pesticide in water. The pesticide may have a solubility in water at 25oC less than 1000 mg/l, preferably less than 50 mg/L. Preferably, the pesticide had a melting point above 70oC.

A pesticide may be a herbicide such as atrazine (atrazine), simazine (simazine), cyanazine (cyanazin), tributyltin (terbuthylazine, Diuron (diuron), chlorsulfuron (chlorsulphuron), metsulfuron (metsulfuron), tralkoxydim (tralkoxydin) or 2-/2-chloro-4-methylbenzoyl/-cyclohexane-1,3-dione; insecticide such as deltamethrin (with deltamethrin), lindane (lindane), carbaryl (carbaryl), endosulfan (endosulfan compounds), or uconazole (hexaconazole), CHLOROTHALONIL (chlorothalonil), chlorosis copper, Captan or thiram (thiram); or acaricide, such as hexythiazox (hexythiazox), cyhexatin (cyhexatin) or amitraz (amitraz).

The metering device may contain, based on the weight of the parts:

Active ingredient 5 60

Disintegrity agent 20 70

Disintegrity agent is able to disintegrate through a rapid evolution of gas or swelling upon contact with water. If he is able to swell in contact with water, it can be crosslinked polyvinylpyrrolidone, which behaves as a binder. For example, crosslinked polyvinylpyrrolidone can be one that is available under the trademark POLYPLASDONE XL, produced by GAF corp. or the one available under the trade name KOLLIDON CL, manufactured by BASF. However, you may instead be any other suitable disintegrity agent that is able to swell in contact with water, such as gum, modified cellulose, such as that available under the trade name AC-DI-SOL, manufactured by FMC Corporation, or the sodium glycolate starch, such as that available under the trade name EXPLOTAB produced Protea Chemical Services. In those cases, when disintegrity agent is able to rapidly select gases in contact Nate or bicarbonate of an alkali metal, for example, sodium bicarbonate.

The method may include mixing at least one additional substance with the active ingredient before and/or after the grinding. So, in those cases where the form of suspension concentrate, the method may include adding at least one dispersant for suspension concentrate until its wet grinding. When conducting wet grinding, the dispersant can be added before or after grinding. The dispersant may be a surfactant, such as that typically used in the preparation of wettable powder or a suspension concentrate, for example, sodium lignosulphonate; condensate sodium salt naphthalenesulfonate and formaldehyde; alkylarylsulfonate sodium; the condensate of Nonylphenol and accelerated, such as a condensate of Nonylphenol with ethylene oxide or Nonylphenol with ethylene oxide/propylene oxide; laurilsulfate sodium, which behaves as a wetting agent, like the one available under the trade name EMPICOL LZ produced by Lankro; condensate sodium salt naphthalenesulfonate and formaldehyde, as that available under the trade name TAMOL NNO, produced by BASF; phosphate ethoxylated polyarylene, which is lenc under the trade name SOPROPHOR FL; dipropylenetriamine sodium, which behaves as a wetting agent, like the one available under the trade name AEROSOL OS manufactured by Cyanamid; and the like.

Additional substance may otherwise be, or can include one or more of the following components:

absorption media, such as colloidal silica, for example AEROSIL 200 (trade name), diatomaceous earth or clay, such as attapulgite (attapulgite);

binder, such as powdered cellulose, such as that available under the trade name ELCEMA P100, produced by Degussa, and which also acts as a filler and disintegrity agent; or monohydrate lactose, which, for example, get under the trade name LUDIPRESS (BASF) and which is directly additive at the pelletizing;

a lubricant such as magnesium stearate;

an agent that improves the fluidity, such as absorption silicon dioxide, for example, SIPERNAT 22 S (trade name) manufactured by Degussa, which is a silica, milled and spray dried, and which behaves as a substance that promotes the free flow and preventing sintering;

water-soluble memo can contain, wt.

Active ingredient 5 60

The binder 10 30

An agent that improves the fluidity of 0.5 to 10

Wetting/dispersing agent, 0.5 to 5

Disintegrity agent 3 50

Grease 0,05 2

Filler 2 30

The invention also extends to a dosing device which is manufactured according to the method of the first aspect of this invention.

According to the second aspect of the present invention proposed dosing device, which is an extruded individual sample and which contains a mixture of active ingredient, which is at the 25oC is in solid form and an average particle size less than 5 microns, with dezintegriraat agent.

According to a third aspect of the present invention, a method for processing products or the local place, which includes:

the introduction of metering devices that are the subject of the present invention, in a pre-set amount of water, and the volume of water such that the concentration of active ingredient in water is higher than the limit of solubility of the active ingredient in water;

decay (disintegration) of the dosing device, leading to the formation of suspense the process.

Below will be described the present invention with non-limiting examples, all proportions are given in parts by weight):

Example 1

Stage 1.

Suspension concentrate having the following composition was made by mixing the following components:

As the active ingredient, technical methylthiophene (purity 93% equivalent 40,08 parts of active ingredient) 43,10

As a dispersing agent, TAMOL NNO 3,50

As an additional dispersing agent, TERIC 200 (trade name), which is a condensate of Nonylphenol and accelerated produced by ICI, Australia 1,50

As additives that prevent foaming, SILCOLAPSE 5000A (trade name), which is a silicone that prevents foaming, and obtained from ICI 0.04

Water 51,86.

The suspension concentrate was ground, passing it twice through a horizontal ball mill (laboratory model KDL Dyno-mill) to obtain the solid particles, the average size of which was 2 µm.

Stage 2.

Was shaped tablets having the following composition:

Suspension concentrate from stage 1 (equivalent to 35.0 parts of active ingredient) 87,32

As a researcher who dezintegriruetsja agent, POLYPLASDONE XL 40,9

As the binder, ELCEMA P100 15,4

As the lubricant, magnesium stearate 0,1.

In order to manufacture tablets were carried out following stages:

/i/ Suspension concentrate was absorbed dezintegriraat agent.

/ii/ This mixture was granulated by passing it through a sieve (British Standard Sieve of 16 mesh.).

/iii/ Then these granules were dried in a vacuum oven at 70oC.

/iv/ Remaining components were mixed with the dried granules.

/v/ and the Mixture was pressed into tablets weighing 2.5 g at a pressure of 1 t

Therefore, each tablet contained 0,875 g of the active ingredient. When used, add 1 tablet to 1 litre of water with ambient temperature, for example 25oC. the Tablet is destroyed for 30 s with the formation of suspensions of the active ingredient in the water. The study of suspension under the microscope showed that the majority of suspended particles have a size in the range of 1 to 3 μm.

Example 2

Stage 1.

Suspension concentrate having the composition below was prepared, and crushed as described in example 1.

Technical hexaconazole (purity of 87.3% is equivalent to 20 parts of the active ingredient having a composition, below, according to the method of example 1, except that the dispersing agent was added to the milled suspension concentrate before it was absorbed dezintegriraat agent.

Suspension concentrate from stage 1 (the equivalent of 30 pieces of active ingredient) 150,0

POLYPLASDONE XL (disintegrity agent) 58,4

SOPROPHOR FL (dispersing agent) 3,1

Magnesium stearate is 0.1.

When the obtained tablets were dispersible in standard hard water containing 340 ppm calcium as calcium carbonate, and the concentration of the active ingredient of 0.005% after 30 min, the suspension was passed 88% solids.

Example 3

Stage 1.

Suspension concentrate having the composition specified below was prepared and milled as described in example 1.

Technical deltamethrin (purity, 98% is equivalent to 64 parts of active ingredient) 65,31

TERIC 200 2,73

SILCOLAPSE 5000A 0,08

Water 31,47.

Stage 2.

Were made tablets having the composition shown below, according to the method of example 1, except that the mixture was granulated, and extruded immediately after drying, using industrial press MANESTY.

Suspensioned) 24,25

ELCEMA P100 (binder) 30,60

EMPICOL LZ (wetting) 2,0

SIPERNAT 22 S (agent, improves fluidity) 0,50

Magnesium stearate 0,10

Tablets were evaluated dispersive them in water at the rate of 1 tablet weighing 2.5 g/1 g active ingredient/ 5 l of water, i.e., 0.2 g of active ingredient per 1 liter of water. The solubility of deltamethrine in water at 20oC is less than 2 µg/l of water. Tablets were disintegrated for 30 s

Tested for ability to form a suspension show that after 30 min of stay in an ordinary hard water, containing 340 ppm calcium as calcium carbonate, 65% of the active ingredient was still in suspension.

Example 4

Stage 1.

Suspension concentrate having the composition specified below was prepared, and crushed as described in example 1.

Technical atrazine (purity, 98%) 50,0

TERIC 200 2,5

SILCOLAPSE 5000A 0,1

Water 47,4.

Stage 2.

Using the methodology described in example 1, there were prepared tablets, the composition of which is specified below:

Suspension concentrate from stage 1 (equivalent 36,45 parts of active ingredient) 74,4

KOLLIDON CL 27,9

ELCEMA P100 28,4

EMPICOL LZ 4,0

SIPERNAT 22 S 0,5

Magnesium stearate is 0.1.

Tablet, the surface. The obtained tablets were tested for hardness, exposing the individual tablets are increasing the load on the edge of the sample. Tablets withstand pressure up to 5 kg of destruction was determined by placing a separate tablet at approximately 2 l of water at room temperature, and weakly mixing. The test tablet was completely destroyed 30 C. Study the resulting suspension under the microscope showed that the majority of the suspension particles have a size in the range of 1 to 3 μm.

Example 5.

Tablets weighing 2.5 g was prepared by homogeneous mixing of the components listed below, and pressing at a pressure of 1.5 t mixture:

Technical deltamethrin 40,0

EMPICOL LZ (wetting agent) 2,0

TAMOL NNO (dispersing agent) 5,0

KOLLIDON CL (disintegrity agent) 25,0

ELCEMA P100 (binder) 27,4

SIPERNAT 22 S (agent, improves fluidity) 0,5

Magnesium stearate (lubricant) of 0.1.

Before mixing with other components, deltamethrin is subjected to dry grinding, to obtain particles deltamethrin, the average size of which would be less than 5 microns. For example, it may be in micronized form as deltamethrin produced Roussel Uelag at which 50% of particles (by weight) kolocany powder to mix with the remaining ingredients, as specified above.

When tablets were placed in water (1 tablet per 5 l of water), they were destroyed for 1 min Examination under the microscope showed that the majority of the particles in suspension have a size of about 2 microns.

The applicant was found that the application of active pesticides that require very low doses of drug abuse, usually of the order of a few grams per hectare, it is desirable for the effective, proper and uniform distribution of pesticides to use very small particles of pesticides, usually having an average size less than 5 microns, dispersed in a prescribed liquid medium, usually water. Moreover, the smaller the particle size, the more surface area, which promotiom the selection of the pesticide after application on the local site or the substrate. To date, however, there was a problem with the application of pesticides in the form of tablets, because the presence of too small particles of pesticide leads to unsatisfactory velocity dispersion tablets in liquid media. However, it has been unexpectedly found that it is possible to obtain a high speed destruction tablets and dispersing them using the method and dosing device presents the image is camping tablets have sufficient strength, that allows you to work with them in the field, and when the dispersion tablets have excellent suspension properties.

Dosing devices presents of the invention provide a good medium for such pesticides, because they are compact and therefore easy to transport and store, and they are in the form in which they are safe when working with them. Moreover, there is no problem arising from the use of large containers of pesticides. In addition, their (pesticides) it is easy to spread and apply effectively and properly, as previously described, i.e., with small losses. Moreover, it has been unexpectedly found that after the disintegration of tablets in water average particle size of the active ingredient was desired value 1 3 microns in spite of the fact that after the active ingredient was ground to a particle size of less than 5 μm, it is then extruded from dezintegriraat agent in tablets, the result would be expected agglomeration of particles of large size. However, as indicated, it has been unexpectedly found that the resulting suspensions average particle size of the active ingredient was still in the range of 1 to 3 μm.

1. Tabletime and dispersing agent, swelling in water disintegrity agent, media agent that increases the fluidity, characterized in that as pesticide-active substances it contains a pesticide, little soluble in water, with TPLnot less than 100oWith a particle size of 1 to 3 μm, as dezintegriruetsja agent is polyvinylpyrrolidone, and optionally contains a lubricating agent in the following ratio, wt.

Active substances 30 40

SURFACTANT 3 7

Disintegrity agent 20 40

The carrier 10 30

The agent that increases the fluidity 0,5 10,0

Lubricating agent is 0.05 to 2.0

and when you make in a certain amount of water ensures the dispersion of the active component in a particle size of 1 to 3 microns.

2. The drug under item 1, characterized in that the active substances it contains a herbicide, insecticide, acaricide, fungicide.

3. The drug under item 1, characterized in that as a herbicide contains atrazine.

4. The drug PCP. 1 and 2, characterized in that as an insecticide contains deltamethrin.

5. The drug PCP. 1 and 2, characterized in that as a fungicide contains thiophanate-methyl.

6. A method of obtaining a preformed pesticide preparation, including becoming, media, lubricating agent, substances for improving the fluidity and pressing, characterized in that the active substance use pesticide solubility in water of less than 1000 mg/l and TPLnot less than 100oWith that crushed to particle size of 1 to 3 μm, as dezintegriruetsja agent polyvinylpyrrolidone and the components are mixed in the quantities of the components of the total weight of the composition, wt.

Active substance 30 40

SURFACTANT 3 7

Disintegrity agent 20 40

The carrier 10 30

The agent that increases the fluidity 0,5 10,0

Lubricating agent is 0.05 to 2.0

7. The method according to p. 6, characterized in that the active ingredient is subjected to wet grinding in aqueous suspension.

8. The method according to PP. 6 and 7, characterized in that crushed in the form of suspensions of the active agent is mixed with dezintegriraat agent.

 

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