FI59014C - Process for making disinfectants. - Google Patents

Description

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Patent- och raglttarttyraltan 'Anaekan titlagd och utl.skrMtwi publlcand .Όέ.οι (32) (33) (31) Requested MU «Utwi — 8« | ird prlorit · * (71) (72) Johan Alfred Olof Johansson, Ejdervägen lU , 2U0 1 ^ Veberöd, Sweden-Sverige (SE) (7U) Berggren Oy Ab (5¾.) Method for preparing the disinfectant - Förfarande för framställning av disinfektionsmedel

The invention relates to a method called for the preparation of an iodophor-type disinfectant.

Iodine in water / alcohol solution has long been used as a disinfectant. Iodine has a good and fast-acting antimicrobial potency, has a broad spectrum and does not cause the development of resistance. However, iodine in this form has several disadvantages, e.g. poor stability, high chemical reactivity, unpleasant odor, etc., and also causes staining, irritation, and often damage when handling biological tissues such as wounds and skin.

Attempts have been made to overcome the disadvantages of such water / alcohol solutions of iodine by binding the iodine complex to a water-soluble organic carrier such as polyvinylpyrrolidone. Water-soluble complexes of this type have long been known (see, e.g., Swedish Patent 191,385, German Patent 1,171,112, and French Patent 2,128,082) and lack some of the disadvantages of iodine solutions while retaining antimicrobial activity.

2 59014

Although water-soluble iodophores have represented significant progress over conventional iodine solutions, they nevertheless have numerous disadvantages and limitations in both manufacture and use. The water-solubility of the products thus makes it difficult to purify them during manufacture, as precipitation methods must be used, resulting in lower yields and costly solvent recovery. In connection with wound and skin disinfection, soluble iodophores can also cause skin and wound irritation. In addition, soluble iodophores release iodine far too quickly for most applications, with iodine being consumed far too quickly due to its tendency to react with other substances. Therefore, in many cases, a transient disinfecting and sterilizing effect is obtained too quickly.

When disinfecting and sterilizing with water-soluble iodophores, these are usually dissolved in a treatment liquid which is introduced into the object to be disinfected. Once the disinfecting and sterilizing effect of the iodophor has occurred through the release of iodine, the concept liquid and the remaining carrier, possibly containing unused iodine, are discarded, resulting in high costs and environmental problems. In many cases, the liquid form itself limits the use of soluble iodophores.

Attempts have also been made to absorb / adsorb water-soluble iodophores on various soluble or insoluble inorganic materials, such as metal salts, clay, talc, etc., in order to obtain iodophores in powder form (see, e.g., Danish Patent Publication 89-57). However, the inorganic materials used are physiologically unsuitable (see, for example, Deutsche Medizinische Wochenschrift, Vol. 76, pp. 39-397), and the disadvantages and limitations otherwise mentioned above for soluble iodophores remain.

According to another attempt to improve water-soluble iodophores (see e.g. DT-OS 1 570 668), iodophores are encapsulated in a polyethylene or polypropylene polymer. By encapsulating this soluble iodophor, it is possible to prevent the release of iodine, so that a longer-lasting disinfection and sterilization effect is achieved. However, the above-mentioned disadvantages of soluble iodophores, especially those related to the preparation, remain, the further encapsulated polyethylene or polypropylene polymer is not hydrophilic and, in addition, is foreign to tissues, which greatly limits the use of iodophor in capsules.

Thus, there is a great need for a new formulation of iodine which makes it possible to take advantage of the excellent disinfecting properties of iodine, but which lacks the disadvantages of known iodine solutions or water-soluble iodophores, respectively. To this end, the present invention proposes a new type of iodophores which is versatile, storage-resistant, simple to prepare and handle, and which allows a controlled release of iodine, and which is also odorless and can be regenerated after use.

The invention thus relates to a process for preparing a disinfectant containing iodine in a complex bond, and the process is characterized in that the hydrophilic organic carrier is treated with iodine to form an iodine complex containing at least 100 ppm iodine, the carrier forming a cohesive three-dimensional network of covalent bonds has the ability to swell in water to form a gel and is prepared from a polymerization product obtained by crosslinking a polyhydroxyl-containing organic material with a bifunctional organic crosslinking agent of the type Z-R-Y, wherein Z and Y represent epoxy groups or halogen atoms and R is an aliphatic .

The water-insoluble but gel-forming carriers used in the preparation of the iodophores according to the invention are either known in the art or can be prepared analogously to such known gel-forming carriers. The preparation takes place in principle by polymerizing by crosslinking a polyhydroxyl group-containing organic substance in a reaction with a bifunctional organic crosslinking agent of the type Y to R-Z, in which Y and Z denote epoxy groups or halogen atoms, and R is an organic residue. In this polymerization reaction, the functional groups Y and Z each react with their own hydroxyl group in a polyhydroxyl group-containing starting material to form ether bonds. In the polymerization reaction, bifunctional glycerol derivatives such as epichlorohydrin, dichlorohydrin, epibromohydrin, dibromohydrin and the like, but also other bifunctional ether bridging agents, such as 1,2; diepoxypropyl ethers and the like can be used. In general, aliphatic epoxy or anti-halogen epoxy compounds containing carbon, hydrogen, oxygen and lacking dissociable groups are suitable for use. If, for example, epichlorohydrin is used as the crosslinking agent, the reaction procedure is as follows R1 - O - H + CH2 - CH - CH2 -Cl + H-O-R2 + NaOH - X0 / -> R] - 0 - CH2 - CH (OH) - CH2 - 0 - R 2 + NaCl + H 2 O where R 1 and R 2 here denote the molecules of the starting material from which the hydroxy group has been reduced.

In order to obtain a water-insoluble but water-forming carrier, a large number of such bridging bonds is generally required, but the degree of crosslinking required also depends, of course, on the particular starting material used, in which case the molecular weight is decisive.

As the polyhydroxyl group-containing organic starting material, many different types of organic material can be used, the molecular weight of which varies, which contains several hydroxy groups and which has the ability to form a water-insoluble but water-swellable gel by forming intermolecular ether bridges. Starch of different average molecular weights and its various degradation products have proven to be quite suitable starting materials, but other polysaccharides such as dextran, dextrin, cellulose and the like can also be used advantageously, as well as synthetic polyhydroxyl group-containing polymers such as polyvinyl onion. also with very good results from low molecular weight polyhydroxyl-containing substances, e.g. mono- and disaccharides such as sucrose, maltose, lactose, etc., or sugar alcohols such as sorbitol. The polyhydroxyl group-containing starting material can also be substituted with anionic, cationic or nonionic groups, and by suitable substitution it is possible to prepare carriers (and thus also iodophores) having ion exchange properties. Examples of suitable substituents for this purpose are carboxylic and sulfonic acid groups or amino groups. Dextranane, dextrin and starch substituted with carboxymethyl, hydroxyethyl, hydroxypropyl, diethylaminoethyl groups and the like are examples of suitable substituted starting materials. These substituents can also be introduced into a finished, crosslinked support in a known manner (see, e.g., Swedish Patent Publication 204,906). The ion exchange capacity of the support or iodophor, respectively, can be up to about 5 meq / g.

The polymerization reaction is suitably carried out in a solvent which dissolves one or more of the reactants, preferably in an aqueous medium. The reaction is catalyzed by an alkali, and as alkali catalysts, for example, alkali metal hydroxides or alkaline earth metal hydroxides can be used. Examples of other time catalysts include quaternary and tertiary amines. When, for example, halohydrins are used as the bifunctional organic substance, which form hydrogen halide in the reaction, the amount of alkali-reactive substance must be sufficient to neutralize the hydrogen halide formed.

In order to accelerate the reaction, it is preferable to work at an elevated temperature, a suitable temperature range being about 50-90 ° C. The reaction may be carried out as a bulk polymerization or as an emulsion polymerization in an inert solvent, e.g. toluene. In the emulsion polymerization, a two-phase system is formed from the reaction mixture and the inert solvent, respectively, whereby the particle size of the prepared support can be adjusted by varying e.g. the stirring rate, the stabilizer content and the shape of the reaction vessel. In pulp polymerization, the particle size is controlled mainly by mechanical comminution, e.g. grinding.

The support is suitably cleaned, e.g. by washing, suction filtration or centrifugation. The washing is then preferably carried out with water or an organic solvent, e.g. ethanol. Since the carrier in an impermeable state often mechanically encloses contaminants, it is convenient to use some swelling agent, preferably water, to swell the carrier so that the contaminants can diffuse from the carrier particles.

The swelling capacity of the support (and at the same time the iodophor prepared therefrom) can be adjusted by varying the reaction conditions and by the choice of starting material. Swelling, which indicates the ability of a carrier or iodophor to bind a swelling agent such as water, is defined in this specification as the gel volume (in ml) obtained when 1 g of dry carrier or iodophor, respectively, is allowed to swell completely in a corresponding swelling agent. Otherwise, under standard conditions, the swelling capacity of the prepared carrier is directly proportional to the solvent content and inversely proportional to both the amount of bifunctional organic crosslinking agent (i.e., degree of crosslinking) and the molecular weight of the polyhydroxyl group-containing starting material. The swelling ability in water can be reduced by substituting the hydroxyl groups of the carrier with nonionic groups such as hydroxyethyl and hydroxypropyl groups. The swelling capacity in organic solvents, such as ethanol, then increases at the same time. The swelling capacity of the iodophores according to the invention or of the carriers used in the preparation, respectively, can vary between about 2 and about 100 ml / g.

In addition to the properties of the carrier used, the properties of the iodophor produced also depend on its iodine content. The ability of the carrier to reversibly complex bind iodine and the ability of the iodophor to release iodine, respectively, will vary depending primarily on the particular carrier used, its swelling ability, degree of substitution and type of substituents, iodine content in complex formation and particle size. Low swelling capacity of the carrier, i.e. the large number of ether bridges formed therein prevents the carrier's ability to complexally bind iodine, since the molecular chains are then largely chemically bound. Using the same type of carrier, the ability to complexally bind iodine can be increased by increasing the swelling capacity and decreasing the particle size, and vice versa. Most carrier types can complex up to about 5 ~ 10% iodine based on the dry weight of the iodophor, which is sufficient in most applications ». However, by using a carrier of suitable material with a high swelling capacity and ensuring high iodine contents in the complexation, iodophores with a substantially higher iodine content, e.g. up to about 50 ?, can be prepared.

As mentioned above, the preparation of the novel iodophor according to the invention can be carried out on a commercially available support, but the formation of the complex can also be carried out in connection with the preparation of the support. If a dried support is used as a starting material, this must be swollen, e.g. in water, before complexation to facilitate the diffusion of iodine into the support particles. Preferably, 7,501014 larger amounts of water are used than are required for complete swelling of the carrier to facilitate homogenization and complexation reaction. As mentioned above, swelling agents other than water may also be used, but the reaction mixture preferably contains at least some water.

Although it is possible to add iodine as a solid or gas to the complexation reaction in a cascade of carrier and iodine, iodine is most preferably dissolved in a suitable solvent, preferably an ethanol / water mixture. Any solvent that dissolves iodine (partially or completely) and is inert to the carrier can be used. The preparation of the iodine solution must use as little organic solvent as possible, as such solvents can shrink the carrier and make it difficult for the iodine to diffuse into the carrier particles. Since the complex dosing reaction takes place very easily and at room temperature and normal pressure, these conditions are most preferably used for simplicity. However, the reaction can be accelerated by slight heating, but temperatures above about 50 ° C must be avoided. The preferred temperature range is about 0-50 ° C, especially about 15-40 ° C.

Upon completion of complexation, the iodophor formed is separated from the reaction mixture in a suitable manner, e.g. by suction filtration. The iodophor gel can optionally also be washed and / or dried in the usual way and optionally also mechanically comminuted and screened to the desired particle size. By waiving the washing of the iodophor or, alternatively, by performing only a gentle wash, the iodophor also contains iodine which is only adsorbed / absorbed into the support and is easily released therefrom. The iodophores according to the invention, which contain both complexed and adsorbed / absorbed iodine, can be advantageously used when it is desired to obtain a high initial concentration of iodine.

An interesting feature of the iodophores of the invention is that they contain iodine reversibly complexed to a carrier that is insoluble in water. Thus, it is possible to regenerate the support complex by binding new iodine to it after the original iodine has been used. The regeneration can be carried out analogously to the preparation of iodophers, e.g. by treating iodine-depleted iodophor with an iodine solution.

r · 8 59014

As can be seen from the above description and also from the following specific examples, the physical and chemical properties of the iodophores can be varied substantially within the basic idea of the invention, and thus it is possible to adapt the properties of the iodophor to the needs and wishes in each specific case. The novel iodophores can also be used either in dry form or as a gel of variable viscosity made of dry iodophor with a suitable swelling agent.

The novel iodophores according to the invention can be used as disinfectants for a wide variety of cosmetic and medical as well as technical purposes. For example, powdered iodophores can be used to spray-infect large surfaces, such as various room spaces and hard-to-reach surfaces in general. Due to the hydrophilic properties of iodophers, they have the ability to absorb water and moisture, and due to this property, powdered iodophor adheres to the treated surface and its germicidal activity acts on it for a long time due to the gradual release of iodine. For example, water-swollen iodophores according to the invention can be used, for example, to disinfect microbially contaminated water, e.g. in swimming pools, cooling tower systems or the like, and to disinfect equipment for the production, transport and storage of products such as milk, wine and beer. In such technical applications, the articles to be disinfected can be treated with a liquid, such as water, containing an effective amount of iodophor. After treatment, the support, possibly containing residual iodine, can be recovered by passing the treatment liquid through a filter, whereby the water-insoluble support can be recovered and regenerated. Alternatively, the treatment liquid can be passed through an iodophor gel filter, from which iodine is gradually released into the treatment liquid. When used as filters, the iodophores preferably have a relatively large particle size, e.g. a dry particle size of up to about 1 mm or even larger, in order to reduce the flow resistance through the filter. The iodophores according to the invention can also be used for the same purposes as the carrier used as starting material, e.g. for performing ion exchange or gel chromatography, in which case the substance to be treated is at the same time disinfected.

The iodophores of the invention can also be advantageously used as anti-microbial ingredients in technochemical, cosmetic and pharmaceutical preparations such as baby powder, foot powder, body deodorants, various types of cleansing compositions, skin creams and the like.

The iodophores according to the invention can also be used with very good results for the disinfection of skin and wounds and the so-called For the prevention of nosocomial infections. Because the iodophores of the invention are hydrophilic and fluid-absorbing, they are particularly suitable for disinfecting fluid-forming wounds, such as burns. Iodophores in the form of a viscous gel are particularly suitable for disinfecting hard-to-reach infected areas, such as wound cavities and fistula canals and e.g. vaginal infections. ' When used for cosmetic or pharmaceutical purposes, iodophores preferably have a relatively small particle size, e.g. from about 0.01 to about 0.50 mm / l.

Because the optimal antimicrobial effect of iodine occurs at a slightly acidic pH, it is preferred in many cases to use iodophores substituted with acidic groups. Suitable substituents in cosmetic and pharmaceutical applications include, for example, carboxymethyl groups which give the iodophor a weakly acidic nature. In purely technical applications, it may in some cases be advantageous to use iodophores which have a strong cation exchanger character and which are substituted by groups such as, for example, sulfoethyl groups. Weakly acidic iodophores are particularly useful for treating skin, wounds, and other alkaline surfaces.

It is, of course, also possible to use the iodophores according to the invention in combination with a suitable acidic component.

The iodine content and iodine release are naturally adjusted in each according to need and desire. As a general rule, for example, a relatively low iodine content (e.g. from about 100 ppm to about 0.5%) is usually sufficient for skin and wound disinfection, while for many technical applications a higher iodine content, released as evenly as possible over a long period of time, is cheaper.

The new iodophores according to the invention can be used in virtually any situation in which it is desired to obtain an effective disinfecting effect. Thus, in addition to the applications specifically mentioned above, many other applications will be apparent to those skilled in the art.

10 5901 4

The invention is described in more detail in the following specific embodiments, which are intended only to illustrate it without in any way limiting the scope of the invention. The stabilizer solution solution mentioned in the examples is a mixture of mono- and diesters of orthophosphoric acid (GAC PE 510, supplied by GAP Corporation, USA) in toluene. The solution contains 14 g of orthophosphoric acid esters per kg of toluene. The total iodine content was determined by the standard Schöninger method. Iodine release was determined by an aid method in which water was added to a certain amount of dry iodophor to form a 100 ml mixture which was shaken for 2 hours. After sedimentation, the iodine content was determined from the supernatant and the amount of iodine released was calculated (expressed as% by weight of the total amount of iodine). In some cases, this procedure was repeated, re-adding water (to 100 ml) to the settled gel after each extraction. In each example, the amount of dry iodophor used, the number of extractions, and the percentage of iodine released in each extraction are reported.

Example 1 500 g of commercial dextrin was dissolved in 500 ml of 3.10 N sodium hydroxide containing 5 g of sodium borohydride. 700 ml of stabilization solution was introduced into a 2-liter 3-neck flask. The stirring speed was adjusted to 200 rpm, and the dextrin solution was added slowly. After 30 minutes, 100 ml of epichlorohydrin was added and the reaction was allowed to proceed for 5 hours at 70 ° C. As a reaction product, a gel was obtained, which was purified as follows: 8 L of water was added to the reaction product with stirring. After the water-insoluble gel product settled, the supernatant solution containing a small amount of non-settling product was decanted off. 8 L of water was added again with stirring, and the mixture was neutralized with 2N HCl to pH 6.5. The product was allowed to settle and the supernatant was decanted. The washing procedure was repeated 3 times with the same amount of water. After the last wash, the product was isolated by suction filtration. To the drip-dry gel was added 1 liter of acetone, then the gel was treated with 4 g of iodine in 50 ml of ethanol (95 vol-56). The reaction mixture was stirred at room temperature (23 ° C) for 60 minutes. The resulting iodophor gel was suction filtered and then dried for 15 h at room temperature and 48 h at 40 ° C.

Yield: 485 g- Analysis: 0.33% iodine and 4.9% moisture; swelling capacity: 6.6 ml / g.

li 5901 4

Example 2

The procedure of Example 1 was repeated using 400 g of dextrin, 400 ml of 3.10 N sodium hydroxide, 5 g of sodium borohydride, 700 ml of stabilizer solution, 80 ml of epichlorohydrin and 25 g of iodine in 200 ml of ethanol.

Yield: 352 g. Analysis: 1.22% iodine and 5.52% moisture; swelling capacity: 6.0 ml / g; extraction test: 3.01 g; 1st edition - 31% 2nd edition - 12.3% 3rd edition - 4.1%

Particle size distribution:> 500 ^ 14% 300 - 500 / U 41% 100 - 300 ^ u 33% <100 / U 12%

Example 3

The procedure of Example 1 was repeated using 400 g of starch (average molecular weight 44,000), 500 ml of 2,4-sodium hydroxide, 3 g of sodium borohydride, 800 ml of stabilizer solution, 80 ml of epichlorohydrin and 5 g of iodine in 50 ml of ethanol.

Yield: 393 g. Analysis: 0.46% iodine and 6.6% moisture; swelling capacity: 5.0 ml / g; extraction test: 4.00 g - 1st extraction - 53%.

Example 4

The procedure of Example 1 was repeated using 400 g of sodium carboxymethyl starch (degree of substitution: 0.25 carboxymethyl groups per unit of Gluose), 500 ml of 2.12 N sodium hydroxide, 1000 ml of stabilizer solution, 80 ml of epichlorohydrin and 10 g of iodine in 100 ml of ethanol.

Yield: 401 g. analysis: 0.55% iodine and 3.72% moisture; swelling capacity: 5.6 ml / g; ion exchange capacity: 1.26 mq / g; extraction test: 4.01 g - 1st extraction 41%.

Prior to reaction with iodine, the support was converted to the acid form by treatment with HCl.

Cr. 1 character 5

The procedure of Example 4 was repeated using 400 g of carboxymethyl starch, 500 ml of 4.65 sodium hydroxide, 1000 ml of stabilizer solution, 225 g of 1,3-dibromohydrin and 2.5 g of iodine in 25 ml of ethanol.

12 5901 4

Yield: 408 g. Analysis: 0.31% iodine and 9.19% moisture; swelling capacity: 5.6 ml / g; ion exchange capacity: 1.23 meq / g; extraction test: 4.01 g - 1st extraction - 71% ·

Prior to reaction with iodine, the support was converted to the acid form by treatment with HCl.

Example 6

The procedure of Example 1 was repeated using 100 g of sorbitol (Merck, Sorbit Griessform DAB 7), 80 g of sodium hydroxide solution (50% by weight), 150 ml of stabilizer solution, 75 ml of epichlorohydrin and 5 g of iodine in 50 ml of ethanol.

Yield: 33 g. Analysis: 0.46% iodine and 5.32% moisture; swelling capacity: 11.4 ml / g; extraction test: 2.01 g - 1st extraction 28%.

Example 7

The procedure of Example 1 was repeated using 100 g of sucrose, 124 ml of 8.1 N sodium hydroxide, 200 ml of stabilizer solution, 75 ml of epichlorohydrin and 4 g of iodine in 50 ml of ethanol.

Yield: 75 g. Analysis: 0.63% iodine and 9.28% moisture; swelling capacity: 8.0 ml / g; extraction test: 3.01 g - 1st extraction - 46%.

Example 8

The procedure of Example 1 was repeated using 44.6 g of polyvinyl alcohol having an average molecular weight of 72,000 (Polyviol W 28/20, supplied by Wacker-Chemie, Federal Republic of Germany), 270 ml of 0.5 N sodium hydroxide, 300 ml of stabilizer solution, 12, 5 g 1.2; 3,4-Diepoxybutane and 5 g of iodine in 50 ml of ethanol.

Yield: 22 g. Analysis: 0.25% iodine and 3.90% moisture; swelling capacity: 10.6 ml / g; extraction test: 2.37 g - 1st extraction - 16%.

Example 9 750 g of a commercially available dextran gel (Sephadex® G-25, Pharmacia Pine Chemicals, Uppsala, Sweden) with a particle size of 100-300 and a swelling capacity of 2.47 g / g were swollen with stirring in 5750 ml of water. To the swollen gel was added 62.5 g of iodine dissolved in 500 ml of ethanol. The reaction mixture was stirred for 2 hours at 35 ° C. The resulting iodophor was separated by suction filtration, washed with 600 ml of water and dried first at room temperature for 15 hours and then at 40 ° C for 48 hours.

Yield: 755 g. Analysis: 2.39% iodine and 10.03% moisture; swelling capacity: 5.0 ml / g; extraction test: 5.01 g - 1st extraction - 15.3.

«59014

Example 10

The procedure of Example 9 was repeated using 225 g of Sephade®-G-25, 1075 ml of water, 600 ml of acetone and 5 g of iodine in 50 ml of ethanol.

Yield: 222 g. Analysis: 0.20% iodine and 4.44% moisture; swelling capacity: 5.2 ml / g.

Example 11 100 g of a commercially available dextran gel (SephadeiP® G-150, Pharmacia Fine Chemicals, Uppsala, Sweden) with a particle size of 40-120 and a swelling capacity of 15 g / g were swollen in 1500 ml of water and 500 ml of acetone. To the swollen gel was added 8.35 g of iodine dissolved in 100 ml of ethanol. The reaction mixture was stirred for 30 minutes at room temperature. The product was filtered off with suction and dried at room temperature for 15 h and then at 40 ° C for 48 h.

Yield: 102 g. Analysis: 0.53% iodine and 8.88% moisture; swelling capacity: 41 ml / g; extraction test: 1.01 g - 1st extract - 85% -

Example 12 100 g of a commercially available dextran gel substituted with diethylaminoethyl groups (DEAE - Spehadex® A-25, Pharmacia Fine Chemicals, Uppsala, Sweden) with a particle size of 40-120 and an anion exchange capacity of 3.5 meq / g were allowed to swell 600 in ml of water and in 200 ml of acetone. To the swollen gel was added with stirring 7 g of iodine in 100 ml of ethanol. Stirring was continued for 60 minutes at 35 ° C. The resulting iodophor gel was separated by suction filtration and dried at room temperature for 12 h and then at 40 ° C for 48 h.

Yield: 105 g · Analysis: 6.12% iodine and 10.90% moisture; ion exchange capacity: 3.1 meq / g; swelling capacity: 6.6 ml / g; extraction test: 2.00 g of iodophor.

1st extract: 1,9% iodine 2nd extract: 2,0% iodine 3rd extract: 2,0% iodine 4th extract: 1,4% iodine 5th extract: 1,4% iodine 6th extract: 1 .5% iodine 7th extract: 1.4% iodine.

Example 13 100 g of a commercially available carboxymethyl-substituted dextran gel (CM-SephadesfS'C-25, Pharmacia Fine Chemicals, Uppsala, Sweden) having a particle size of 40-120 and a cation exchanger capacity of 4.6 meq / g were allowed to swell 600 in 1 ml of water and 200 ml of acetone. To the swollen gel was added with stirring 10 g of iodine in 100 ml of ethanol. Stirring was continued at room temperature for 60 minutes. The resulting iodophor gel was separated by suction filtration and dried at room temperature for 16 hours and then at 40 ° C for 48 hours.

Yield: 98 g. Analysis: 0.25% iodine and 9.58% moisture; cation exchanger capacity: 7.5 ml / g; extraction test: 3.01 g - 1st extraction - 56%.

Example 14

A disinfectant skin and wound ointment was prepared by mixing the following ingredients: 3 g of the iodophor of Example 3 (particle size <100), swollen in 28 g of water 31 g of paraffin 10 g of lanolin 10 g of petrolatum 24 g of silicone oil 2 g of wool fatty alcohols 1 g cetanol 1 g zinc oxide_24 g total 103 g

Example 15

A viscous suspension for disinfection of wound pockets and fistula passages was prepared as follows: 5 g of iodophor prepared according to Example 2 (screened for particle size <100 μl) was allowed to swell in 25 ml of saline. The resulting suspension was suitably used for treatment with a syringe cannula.

Example 16

The iodophor prepared according to Example 10 (particle size 100-300) was used (clinically) to disinfect open wounds. Iodophor powder was applied to the wounds with a salt spreader. Wound healing progressed without any undesirable side effects being observed.

15 5901 4

Example 17

Diethylaminoethyl-hydroxypropyl-starch gel prepared analogously to the gel prepared in Example 3 had the following properties:

Nitrogen content: 4.57%

Hydroxypropyl substitution: DS = 0.05

Swelling capacity: 13.0 ml / g

Humidity: 5.59% 70 g of this gel was allowed to swell in a mixture of 200 ml of acetone and 600 ml of water at 22 ° C with stirring for 60 minutes. The pH was adjusted to 4.1. A solution of 14 g of iodine in 100 ml of 99.5% ethanol was added and the mixture was stirred at 22 ° C for 30 minutes. The resulting iodophor gel was suction filtered and dried. Yield: 32 g. Analysis: 14.9% iodine and 3.9% moisture; swelling capacity 11.1 ml / g; extraction test: 1st extraction 2.7% ·

Example 18

Diethylaminoethyl starch gel, prepared according to Example 3, had the following properties:

Nitrogen content: 5.62%

Swelling capacity: 5.4 ml / g

Moisture: 3.72% 100 g of this gel was allowed to swell in 1000 ml of 60 methanol at 23 ° C with stirring for 30 minutes. The pH was adjusted to 4.5. The gel was suction filtered and the gel sucked dry was treated as a filter with a solution of 30 g of iodine in 2000 ml of 70% ethanol. The gel sucked dry was diluted with 500 ml of 60% methanol. 30 g of iodine in 300 ml of 99.5% ethanol were added with stirring. Stirring was continued for 30 minutes. The resulting iodophor gel was suction filtered and dried.

Yield: 142 g. Analysis: 32.2% iodine and 1.12% moisture; swelling capacity: 3.6 ml / g.

Claims (7)

5901 4 16 A process for preparing a disinfectant containing iodine in a complex bond, characterized in that the hydrophilic organic carrier is treated with iodine to form an iodine complex containing at least 100 ppm iodine, the carrier forming a three-dimensional network of covalent bonds and insoluble in water but having water insolubility forming a gel and prepared from a polymerization product obtained by crosslinking a polyhydroxyl group-containing organic material with a bifunctional organic crosslinking agent of the type Z to R to Y, wherein Z and Y represent epoxy groups or halogen atoms and R is an aliphatic organic residue lacking. Process according to Claim 1, characterized in that the complexation is carried out in the presence of a liquid medium capable of swelling the carrier and at a temperature which does not rise above about 50 ° C. Process according to Claim 1 or 2, characterized in that a larger amount of liquid reaction medium is present than is required for complete swelling of the support. Process according to Claim 1, 2 or 3, characterized in that the reaction medium contains water. Process according to one of Claims 1 to 4, characterized in that the iodine is added in the form of a solution in a solvent which is at least partially capable of dissolving the iodine and is inert to the support. Process according to one of Claims 1 to 5, characterized in that a carrier is used which has a swelling capacity such that 1 g of dry carrier in complete swelling in water forms a gel with a volume of 2 to 100 ml. Process according to one of Claims 1 to 6, characterized in that a support which is substituted by anionic, cationic or nonionic groups, preferably ion exchange groups such as carboxymethyl or diethylaminoethyl groups, is used.