DE967860C - Process for the production of solutions of fragrances in solid bodies - Google Patents

Description

Process for the preparation of solutions of odoriferous substances in solid Bodies The invention relates to a method for producing solutions of fragrances in solid bodies.

The method consists in that one in the production of high molecular weight Substances through polymerization, copolymerization or polycondensation to the reaction mixture suitable solid or liquid before the start of the reaction or during the reaction Adding fragrances. Surprisingly, high molecular weight Manufacture substances which, although they are solid, are larger quantities of originally liquid Contain fragrances.

From French patent 981 831 it is known to a Plasticizer or a plastic that can be plasticized without additives, fragrances to add to the unpleasant odor that adheres to some plastics or plasticizers to cover. The fragrance is always incorporated into the finished plastic. It is also known, in water-soluble polyvinyl alcohol with an average Use a molecular weight of 3,000 up to 100,000 as a carrier substance for fragrances, wherein the fragrance is adsorbed by the finished polyvinyl alcohol.

In contrast, the solutions according to the invention are used for fragrances Made in solids by going into the manufacture of high molecular weight substances by polymerizing or condensing the mixture of starting materials before beginning the implementation or during the implementation of odoriferous substances added, and indeed in large quantities larger amounts than according to the French patent mentioned. Also come only those high molecular weight substances that do not have an unpleasant odor.

The high molecular weight solutions of fragrances according to the invention in Solid substances are insoluble in water and go beyond the odorous substance longer period than, for example, solutions of fragrances in alcohol, soaps, save or wax or talc powder of the same odorant concentration, d. That is, the fragrances are strong in the bodies prepared according to the invention fixed.

The solutions of odoriferous substances in solid prepared according to the invention Bodies can be added to cosmetic preparations in finely ground form. But it can also be done depending on the choice of the starting products and the special implementation of the process produce solid, compact bodies that are both mechanically and can be thermoplastically processed into a wide variety of everyday objects can.

The production of the body according to the invention by polycondensation can in principle be carried out with all substances capable of this reaction, Of course, only those are suitable for the method according to the invention that are after the polycondensation do not have any unpleasant odor. The condensation can depending on the starting materials used are made so that the odorous substance either before the start of the reaction or only after the condensation has started is treated. If a condensation is carried out with formalin solution, it is expedient to add the fragrances only when the condensation has already started advanced and most of the water formed in the reaction is removed is. If, however, a condensation with paraformaldehyde or other formaldehyde delivering solids carried out, then it is appropriate to the fragrance before Add the beginning of the reaction.

Surprisingly, solid bodies can be produced by this method produce that contain up to 40% of liquid fragrance (cf. lead example I).

Leave depending on the choice of working conditions and raw materials produce porous, easily pulverizing or compact masses, the latter either mechanically by sawing, drilling, milling and the like, or by using a thermoplastic technique can be further processed. There is also the possibility of using the polycondensates for as long they are still highly viscous, to be poured into molds and then hardened.

The polycondensation are preferably carried out at moderate temperatures, at a maximum of 60 to 700.

In the production of the bodies according to the invention by polymerization the fragrance is added to the monomer and the polymerization is known per se Way by UV radiation and / or heat and / or the addition of accelerating catalysts set in motion. It has been found to be advantageous to carry out the polymerization in closed Carry out vessels. Depending on the test conditions and the amount of odorant added Here, too, it is possible to produce compact or easily pulverizable polymers. The latter are particularly suitable for powder preparation; With the according to the invention Process, natural and synthetic fragrances can be used. lead the selection of suitable fragrance compositions must be taken into account that each depending on the nature of the polymerizing or condensing starting material Components of the composition participate in the implementations and thereby their value as fragrances can lose or change the fragrance of the entire composition. Examples are: Aldehydes in the production of phenoplasts and aminoplasts and olefins or polyenes in the production of polymers. This difficulty can be circumvented by either avoiding the addition of such components or add a larger amount to make up for the loss.

Example I 2.5 g of urea are dissolved in 37.5 g of formaldehyde and 1 cc of 250 per cent HC1 was added. When condensation starts, this is indicated by the fact that The initially clear solution begins to become cloudy when heated, the liquid becomes Fragrance (20 ccm) added quickly with vigorous stirring.

The mass hardens in a short time and still has a faint odor for formaldehyde.

By heating the condensate to 600 for 2 to 3 hours in the closed Vessel this smell disappears. The hard mass is powdered several times with Water and then washed with ether and dried in a desiccator.

Example 2 10 g of rennet casein are mixed with 10 cc of a n / 10 sodium carbonate solution swelled and processed into a plastic mass by kneading. To this crowd 1.5 g of liquid fragrance, which is a slurry of 0.8 g of paraformaldehyde contains, added and incorporated homogeneously into the plastic mass. The hardening in the closed vessel at 400 is finished after 5 days. It will be a dry one Granules obtained, which were powdered in a ball mill and then dried.

Example 3 30 g of urea and 3 g of hexamethylenetetramine are in 75 g of 40% formaldehyde dissolved.

After refluxing for 4 hours, the water is turned in vacuo distilled off. In the viscous mass 1.5 g of fragrance with the addition of 0.5 g Dissolved NH4SCN and poured the polycondensate into molds at a temperature of 400. After 24 hours the synthetic resin has solidified and can be mechanically milled.

Process drilling, cutting, etc. well.

Example 4 60 g of urea are dissolved in 150 g of 40% formaldehyde, the one with 0.5 g of soda is weakly alkaline was made, solved and on Reflux heated to boiling. 10 g of broxy acid were then added to this solution and the reaction mixture was refluxed for 3 hours. After distilling off the In the vacuum, 2 g of fragrance are dissolved in the reaction mixture, the mass then poured into molds and then hardened through at 650.

Example 5 30 g of vinyl acetate are sealed with 1 g of fragrance in a Quartz glass exposed to UV radiation with gentle heating to 35 to 400. The resulting polymer is colorless and transparent. It can be used according to known Process procedures in a wide variety of ways.

Example 6 a) 30 g of acrylonitrile are mixed with 0.5 g of fragrance and the solution in a sealed, suitable vessel under UV irradiation in stages warmed up. For example: 6 hours at 350, 6 hours at 750 and another 10 hours at 1200.

The block polymer can be processed by conventional methods and in be brought into the desired shape. b) 30 g of acrylonitrile are mixed with 2 g of fragrance added and the solution is gradually warmed in a closed vessel, 12 hours at 350, 12 hours at 750 and another 12 hours at 100 to I200. After that has a polymer with a waxy consistency is formed. The same thing was squeezed out. The squeezed out liquid, the fragrance, monomeric and low-polymer acrylonitrile can be used for a new polymerization. The press residue was washed several times with ether. The polymer is fine as dust and can can be used directly for powder preparation.

Claims (4)

PATENT CLAIMS. I. Process for the preparation of solutions of fragrances in solid Bodies, characterized in that one in the production of high molecular weight substances by polymerization. Mixed polymerization or polycondensation before the reaction mixture Beginning of the implementation or solid or liquid fragrances during the implementation clogs. 2. The method according to claim I, characterized in that at Condensation with formalin solution does not affect the odorous substances until some time after the start of the Condensation adds after most of the water formed in the reaction away. 3. The method according to claim I, characterized in that the polymerization the monomers used in a known manner by irradiation with ultraviolet Light and / or accelerated by heat and / or by the addition of catalysts will. 4. The method according to claim I, characterized in that the polymerization takes place in closed vessels. Documents considered: German Patent No. 825 293; French patent specification No. 98I 83I.