A method of obtaining a protective coating

 

(57) Abstract:

Use: for applying a protective coating of pH-sensitive polymers for drug and/or nutritional active ingredients. The inventive pre-exercise emulsion copolymerization of 1 mol of vinylpyridine and 2 mol of styrene in the presence of 3 wt.% the sodium oleate. Then add 10 to 70 wt. including the resulting aqueous emulsion of a copolymer of 30 to 90 wt. including stearic acid and 0.4 to 1.5 vol.% 10% aqueous sodium hydroxide solution at 150 to 1000 ml of water. The resulting composition is sprayed on the granules of methionine and/or lysine. table 1.

The invention relates to a method of applying a protective coating of pH-sensitive polymer to the active components. It refers, in particular, to a method for producing a pH-sensitive polymer in the emulsion and to its use for applying a protective coating for medicinal and/or nutritional active ingredients.

Known coating active ingredients using a pH-sensitive polymers, if necessary mixed with a hydrophobic substance such as stearic acid and/or water-insoluble polymer, such as ethylcellulose. Put protective the pH-sensitive polymer, pre-synthesized and selected, which is then dissolved for applying a protective coating in one or more organic solvents, such as halogenated solvents, alcohols or ethers. This method provides an easy and homogeneous dispersion of one or more pH-sensitive polymers and additives. The disadvantages of the method: the need to allocate the polymer; the need to introduce a significant amount of solvent is about 20 to 100 g of the solvent for dissolving 1 g of the pH-sensitive polymer. In products intended for animal nutrition, you must enter the solvents emissions are known.

The invention made it possible to carry out the synthesis of the polymer and to use it for applying a protective coating without the intermediate stage of selection. This method allows the application of a protective coating on the active components, such as amino acids or vitamins, avoiding the selection of polymer and use at the stage of applying a protective coating of organic solvents that are not compatible with biological means.

The method of applying a protective coating using a composition based on pH-sensitive polymer on leku the copolymerization of 1 mol of vinylpyridine and 2 mol of styrene in the presence of 3 wt. oleate sodium, then add on 10-70 wt.h. the resulting aqueous emulsion copolymer 30-90 wt.h. stearic acid and 0.4-1.5 on. 10% aqueous sodium hydroxide solution at 150-1000 ml of water and the resulting composition is sprayed on the granules of methionine and/or lysine. Medicinal and/or nutritional active ingredients that cause the protective coating, are used preferably in the form of granules, especially spherical or egg-shaped, having a diameter of 0.3-3 mm Protective coatings based on aqueous emulsion polymerization lead to significant savings, as it avoids the selection of the polymer, applying a solvent to re-dissolve the polymer and, accordingly, the use of plants for the recovery of expensive solvents.

Obtaining the emulsion copolymer is carried out in the presence of surfactant and initiator of polymerization. As surface-active substances are used the sodium salt of oleic acid. The polymerization initiator is selected among the soluble initiators are usually used in emulsion methods, in particular, prefer to use the sodium persulfate. During polymerization, the pH is fixed, preferably between 10 and 14, in particular between 11 and 13. This is a high polymer are extremely interesting for feeding ruminants, because they have little decay or not decay when moving through the first chamber of the stomach of ruminants and released in the abomasum (fourth division of the stomach and/or intestines of ruminants. The granules obtained after applying a protective coating of a thickness of 5-100 μm, are used as additional food or for medicinal treatment of ruminants.

P R I m e R 1. For the preparation of an emulsion copolymer of 2-vinylpyridine) - derivatives and styrene are mixed with 150 g of styrene and 350 g of fresh 2-vinylpyridine) - derivatives. This mixture is washed twice by 160 ml of 5% aqueous sodium hydroxide solution, then twice through 320 ml of demineralized water. Treated in this way the monomers are loaded into the reactor for polymerization, nitrogen purged. In another bowl, prepare the basic solution of sodium oleate, Prilepa 15,25 g of oleic acid in 736 g of demineralized water in which is dissolved in 7.7 g of sodium hydroxide in the form of tablets. Prelivanje oleic acid is carried out for 10 min at room temperature and moderate stirring.

Thus obtained solution oleate injected into the reactor for polymerization and mixed with the monomers. Diluted zobrazovania emulsion. Rinsed thoroughly system, barbotine it nitrogen, and start to heat up. When the temperature of the emulsion is stabilized at 50aboutWith, poured for 2 min, 100 g of a 5% aqueous solution of sodium persulfate. Heating at a temperature of 50aboutC and the stirring is maintained for 5 minutes After polymerization, emulsion clear of light fractions steam to remove traces of residual monomers. Thus receive the aqueous emulsion copolymer, its concentration on a dry residue is 20,75 wt. and its pH is 13.

To characterize the formed polymer, a sample is taken of the emulsion. As a result of coagulation upon acidification of the sample, the polymer is separated by filtration through ritterband glass and dried in a drying Cabinet after several rinses with demineralized water.

The dried polymer in powder form has the following characteristics:

characteristic viscosity, measured at a temperature of 25aboutWith, for a solution containing 0.5 g of the copolymer in 100 ml of dimethylformamide, equal to 1.33 decal/g;

molecular weight determined by the GPC method (helpanimals chromatography) in N-organic, relative to the standards of politicality in a glass vessel with a volume of 2 l load 420 g of demineralized water and 1.8 ml of 10% aqueous sodium hydroxide solution (p/v). This mixture is heated to a temperature of 84aboutWith moderate stirring, poured in 1 min and 106 g of the emulsion of a copolymer prepared before that. To this mixture, maintained at a temperature of 80aboutWith added 88 g of stearic acid, sold by the company "UNICHEMA" called PRIFAC 2981, previously placed in the addition funnel, and heated to a temperature of 90aboutWith using electrical heating winding. Prelivanje carried out in approximately 2 min, while the mixture is vigorously stirred by the device transmitter station, rotating with a speed of 11 tech. about./minutes After prilipanie support mixing for another 2 minutes thus Receive the emulsion, which is maintained at a temperature exceeding 70aboutWith moderate stirring (magnetic stirrer). The content of the extract in this emulsion 20.4%

In this example, the emulsion for applying a protective coating on the granules of amino acids was used in half an hour after its preparation. In a device for coating by pulverizing the UNIGLATT, equipped with a WURSTER system, load 500 g of spherical granules with a mean diameter of 2 mm, containing 57% of lysine hydrochloride and 16% methionine. Emulsion, you is Olami. The sputtering conditions are the following: the number of sprayable emulsion approximately 320 g; air flow to create a fluidized bed 130 m3/h; the temperature of the air to create the fluidized bed (output) 37aboutC; air pressure for spraying 1.5 bar; air temperature for spraying 85aboutWith; the emulsion flow rate 9 ml/min; duration sputtering 41 minutes

The degree of protection created by the protective film of coating applied in this way, estimated in accordance with the test in vitro, which consists in mixing a certain quantity of granules with a protective coating in an aqueous buffer solution with pH=6, maintained at a temperature of 40aboutC. Conduct a measurement of the amount of lysine hydrochloride released into the solution after 6 hours and after 24 hours is also estimated from the pH-sensitivity of the protective coating with the help of test in vitro, which consists in mixing a certain quantity of granules with a protective coating in an aqueous buffer solution with pH=2, maintained at a temperature of 40aboutC. Determine the number of lysine hydrochloride released into the water after 15 min and 30 min, respectively. The results are given in the table. These results reveal a high level of protection at pH=6 and fast speed Iegotovlenna before this, reproduce example 1, varying only the duration of storage of the emulsion for applying a protective coating. The latter, instead of to use almost immediately, first store within 48 hours at a temperature of 72aboutWith before subjected to dispersion in a fluidized bed of granules. Amino acids are coated with a protective coating assessed in accordance with the tests described in example 1. The results in the table show characteristics of protection at pH= 6, and release at pH=2, a fully satisfactory for the application.

P R I m e R 3. Proceed from the emulsion copolymer with a primary environment, prepared in example 1. Reproduce example 1, changing only the dry matter content of the emulsion for applying a protective coating. Moving from 20,4 to 30,2% using 236 g of demineralized water instead of 420 g for diluting the copolymer with the primary environment.

P R I m e R 4. Proceed as in examples 1 and 3. Change just the amount of demineralized water used for dilution of the emulsion copolymer with the primary environment at the first stage of preparation of the emulsion for applying a protective coating. This example used a 130 g of water, which led to the final emulsion content Ustilago polymer granules from methionine and/or lysine, wherein the pre-exercise emulsion copolymerization of 1 mole of vinylpyridine and 2 moles of styrene in the presence of 3 wt.% oleate sodium, then add 10 to 70 wt.h. the resulting aqueous emulsion of a copolymer of 30 to 90 wt.h. stearic acid and 0.4 to 1.5 vol.% 10% aqueous sodium hydroxide solution at 150 to 1000 ml of water and the resulting composition is sprayed on the granules of methionine and/or lysine.

 

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