NL8007006A - PROCESS FOR PREPARING PERFUMED DETERGENTS - Google Patents

Abstract

The aim of the invention is to achieve long-termed durability of scent of powdered detergents, especially during long storing, and to decrease the amount of perfume added to the detergent. The aim is achieved by sorption of the perfume on a porous carrier which is mixed directly with the powdered detergent and uniformly distributed therein. A sorbent with large active surface is used as a porous carrier, which sorbent is on the basis of polyacrylates, polyvinyl chloride and polyalkyl methacrylate and other similar compounds. The invention can be used in the production of pre- washing and soaking agents and detergents and in the production of perfumed cosmetic preparations and deodorants in powdered form.

Description

,. 1's- Λ -Γ N.0. 29,702

Process for the preparation of perfumed detergents

The invention relates to a process for the preparation of perfumed detergents, in particular of powdered detergents and cleaning agents, which process stabilizes the perfume component in these products during storage by reducing their volatility and by increasing the resistance to resolves chemical changes *

The heretofore known powdered detergents and cleaning agents are mixed by mixing an atomized aqueous suspension of surfactants, predominantly of an anionic type, and additives such as, for example, alkaline polyphosphates, alkaline silicates, sodium sulfate, borax, sodium carbonate, organic chelate. molding agents based on the sodium salts of nitrilotriacetic acid or ethylenediamine tetraacetic acid, carboxymethyl cellulose, optical brighteners and the like, prepared in spray drying towers in the heat or in the cold. The dry intermediate is then homogenized in mixers with other powdered, optionally liquid, components, such as, for example, with sodium peroxyborate, polyphosphates, alkaline proteases and amylsaen, nonionic surfactants, and the like, usually in water and with dry water. became less stable at fairly high temperatures; optionally it is economically more advantageous to add these directly to the product without prior dissolving in water. The powdered detergent prepared in this way is usually perfumed on the mixed product by spraying a liquid perfume preparation in the final stage of production.

A similar principle is based on hitherto known processes for the preparation of detergents, wherein the higher content of inorganic additives, which are capable of removing the water from the solution or suspension, is advantageously used in the drying of the atomized solution or suspension. to bind; the dry product, usually in the form of a powder of different particle structure and shape, is sprayed with a. atomized or dispersed form of the perfume composition perfumed. A drawback of this process for the preparation of detergents is that partial volatilization of the fragrances already takes place in the atmosphere during production and that by the direct spraying of the powder 8007006 ". 2 -shaped detergent with the perfume preparation no uniform homogeneity of the products with regard to the perfume content due to the different sorption capacity of the individual components of the detergents can be obtained * 5 A further drawback is that the perfume losses during storage are evident by volatilization thereof are increased »possibly also by the action of chemical changes of a separate component», which may lead to a change in the nature and intensity of the original odor. These facts result in a significantly less effective use of the perfume in powder detergents. In order to maintain the desired useful properties of detergents after a rather long storage time, it is necessary to add a larger amount of perfume and this means an uneconomical application of a higher perfume content in the actual products.

Powdered detergents are known having an increased perfume stability, which is achieved by the presence of an amorphous silica hydrate in the powdered detergent, which is added with the perfume in the usual and known manner · The residual content of the perfume after six months storage with these detergents is about 30 to 50% by weight compared to a detergent without an additive which increases the stability of the perfume, after which a residual content of about 10% by weight was found after the same space of time. The disadvantages of such deter 25 gens and the process for their preparation are similar to the aforementioned preparation methods, because the perfume is again sprayed on the powder detergent, which additionally contains the amorphous silicic acid hydrate, which ensures no definable, controllable and reduced desorption during storage # 30 The drawbacks mentioned are alleviated according to the invention by the process for preparing n detergents, in particular powder detergents and cleaning agents, discarded; in this process, the individual components of the agent are mixed in the required ratio, the perfume is added and the mixture is homogenized. The principle of the invention lies in that the perfume is adsorbed on a porous support before addition to the other components of the mixture, preferably on the basis of the hydrated silica, titanium dioxide, polyethylene acrylate, polyvinyl chloride, polymethyl acrylate, poly-ifo methyl methacrylate, acetyl cellulose, polyphenylene oxide, polyethylene-8007006, 3. - * Lent terephthalate, polyamide, urea-formaldehyde resin, melamine-formaldehyde resin, the copolymer of acrylonitrile with butadiene. and styrene, polyacrylonitrile, the copolymer of vinyl chloride with vinyl acetate, polyethylene, polypropylene, polystyrene and mixtures 5 of these substances · The perfume absorbed in the carrier is added to the powder detergent in an amount of 0.05 to 10 wt. preferably 0.2 to 1.0 wt.% added and complete! ; homogenized · The perfume content in this sorbent is 10 to 65% by weight. The detergent preparation process of the invention utilizes the excellent properties of the perfumed; ; Sorbent based on the stability of the perfume preparation absorbed in the porous support. This stability is due to the definable, controllable and considerably reduced desorption of the perfume preparation and to its physical and physico-chemical properties; properties given; these allow direct mixing with the powdery detergent, which is after the homogenization of the powder. 1! mixture until the recovery of a product, wherein the perfume composition "1! ; Nons on the porous support evenly throughout the volume of the.

If the powdered detergent is distributed, the preferred method of preparing detergents according to the invention over the known methods is also that the perfumed sorbent having the required particle size can be treated in this way with the aid of the perfume preparation content. that its physical properties, in particular the bulk density, correspond to the bulk density of the powdered detergent; this permits a simple mixing thereof with the detergent to obtain a homogeneous product, which can be stored under long-term storage. Furthermore, the properties of the sorbent allow to stabilize the perfume composition absorbed thereon, which considerably reduces the volatility. Its nature and its elimination of chemical changes in its composition during storage of the powdered detergent results, which manifests itself as a change in odor character. A further favorable property of the porous perfume-containing sorbents is that they underline the intensity and character of the fragrance of the original perfume composition.

The operation of the method for preparing detergents ifO according to the invention is also contained therein, 8007006 *. . ^. That by adding the perfume preparation, which was sorted on a porous support before mixing with the other detergent components, a high odor intensity of the articles is achieved even after a long storage, which leads to a substantial increase in the efficacy of the beneficial use of the perfume and the maintenance of the original useful properties. The operation of the detergent preparation process according to the invention furthermore consists in that by reducing the perfuming of the powdered detergent by 50 to 60% by weight when producing after a rather long storage time, the same or even a greater odor intensity of the product as compared to the hitherto known methods of perfuming detergents can be achieved.

The process for the preparation of powdered detergents according to the invention is further elucidated hereinbelow by means of a few examples.

Example I

A powdered detergent, prepared by mixing 39.5 wt.% Mixture, which was obtained in a tower by spray drying in heat, and which contained 25 wt.% Surfactants based on sodium dodecyl benzene sulfonate and 2 wt.% Carboxymethyl cellulose , K0 wt. # Sodium Tripolyphosphate, 6 wt. # Sodium Silicate, 1.5 wt. # Optical Bleach and 25 * 5 wt. # Sodium Sulphate, with 60.2 wt. # mixture, containing 30 wt. # soap based on the sodium salts of higher fatty acids, 60 wt% sodium carbonate and 10 wt% sodium sulfate, are mixed with 0.3 wt% perfumed sorbent containing 50 wt porous hydrated silica and 50 wt% perfume composition base of eucalyptus oil * of the benzoe entoluyl acid derivatives, the terpinyl and dehydrolinalyl acetate, of the aldehydes and ketones and their derivatives · A homogeneous detergent with an intensive characteristic odor is obtained both in the solid state and after dissolving in water · After 12 months of storage, stick with it Detergent prepared in this manner practically retains the original intensity and nature of the fragrance of the perfume composition.

Example II

95 * 0 wt.% Powder detergent, prepared in a similar manner as in Example 1, was mixed with 5 wt.% Perfumed sorbent containing 97 wt.% Porous hydrated silica and ifO 3 wt.% Perfume composition as in Example I. , mixed. From the standpoint of the stability of the perfume composition after 12 months of storage, the properties of the detergent thus prepared remained the same as in Example I 8007006.

Example III

(5 * 99 wt.% Powder detergent, prepared in a similar manner as in Example 1, were mixed with 0.3 wt. Perfumed sorbent, which is 67 wt.% Porous polyethylene terephthalate sorbent and 33 wt. # perfume preparation based on the limonene, dipentene and veratrene contained * A homogeneous detergent with an intensive and characteristic odor was obtained · After 12 months of storage, the detergent prepared in this way had the same properties as the product of Example I.

Example IV

A detergent composition having the following composition was prepared by a conventional method of preparing powder detergents: 8 wt.% Sodium dodecylbenzene sulfonate, 3 wt.% Soap based on the sodium salts of higher fatty acids, 27 wt.% Sodium tripolyphosphate, 5 wt. , 5 wt # nitrilotriacetic acid sodium salt, 22 wt sodium sulfate, 1.5 wt carboxymethyl cellulose, 20 wt sodium carbonate, 0.3 wt * optical brightener, 3 wt nonyl polyglycol ether, 0.5 # of an alkaline protease with an activity of 300 * 000 Delf-i-present. This agent is mixed with 0.3% by weight of a perfume carrier containing porous hydrated silica and a perfume preparation in a weight ratio of 1: 1. preparation used was formulated from geraniol, geranyl acetate, terpinol, diphenyloxide and other aromatic components. * The powdered detergent thus prepared had the original intensity and nature of the fragrance of the use even after 12 months of storage. extracted perfume preparation in the solid state as well as after dissolving in water.

". Example V

In a similar manner as in Example IV, a powdered detergent composition of the following composition was prepared: 8 wt% sodium dodecylbenzene sulfonate, 5 wt% soap based on the sodium salts of higher fatty acids, 10 wt% sodium carbonate, 30 wt% after tri tripolyphosphate, 18 wt% sodium sulfate, 19 wt% sodium perborate, 1.5 wt% carboxymethyl cellulose, k wt sodium sulfate, 2.5 wt% of an epoxyethane-epoxypropane copolymer, 0, 3 wt. # Optical brightener; this agent was mixed with 0.5 wt. #. of perfume perfume, which was porous hydrated silica and 8007005.

a perfume composition in a weight ratio of 3: 1 contained * The composition of the perfume composition was the same as in Example IV * The properties of the detergent composition prepared in this way were true from the standpoint of the quality and stability of the perfume after 12 months of storage the same as in example IV. Example VLV

According to a conventional heat spray drying technique in φβη tower, a homogeneous powdered soaking and prewashing detergent of the following composition was prepared: 50 wt.% Na-10 triumcarbonate, 2 wt.% Sodium dodecylbenzene sulfonate, 2 wt.% Sodium lauryl sulfonate, 10 wt. Sodium tripolyphosphate, 10 wt. Sodium silicate and if wt. Sodium pyrophosphate. * The resulting detergent was homogenized with 0 * 3 wt. * Perfume sorbent * containing porous hydrated silica and a perfume composition based on eucalyptus oil in a weight ratio of 5. 1 contained * The soaking and prewashing detergent prepared in this way had the same intensity and the same character of the perfume used both after solid storage and when used in an aqueous solution after 12 months of storage.

Example VII

Using a homogenizing drum mixing method, a powdered detergent of the following composition was prepared: 4 wt.% Sodium dodecylbenzene sulfonate, 2 wt.% Sodium tripolyphosphate * 17 wt.% Sodium pyrophosphate, 32 wt.% Sodium sulfate * 25 4 * 5 wt.% Sodium silicate and 0 * 3 wt.% Perfume carrier containing porous hydrated silica and a perfume composition in a 4: 3 weight ratio. The perfume preparation used consisted of limonene, dipentene and veratrene.

After a storage period of 12 months, the properties of the powdered cleansing detergent prepared in this way remained at the same level from the standpoint of just after preparation, from the point of view of the quality and intensity of the perfume.

Example VIII

97% by weight powder detergent, prepared in a similar manner as in Example 1 *, was mixed with 0.3% by weight of a perfumed sorbent, which is 67% by weight porous sorbent based on an alkaline polyamide-6 and 33% by weight. # Perfume preparation based on limonene, dipentene and veratrene. A homogeneous detergent with an intensive and characteristic odor was obtained.

4 & After 12 months storage of the detergent prepared in this way 8007006 7 - - * the quality and intensity of the perfume was the same as just after preparation *

Example IX

97 wt% powdered detergent * prepared in the same manner as in Example 1 * were mixed with 0.3 wt% perfumed sorbent containing 67 wt% porous polyphenylene oxide sorbent and 33 wtm perfume composition based on limonene * dipentene and veratrene, a homogeneous wax mixture with an intensive and characteristic odor was obtained, which was retained at the same intensity after storage for 10 months.

Example X.

97% by weight powder detergent, prepared in the same manner as in Example 1, was mixed with 0.3% by weight perfumed sorbent, which is 67% by weight porous sorbent based on acrylonitrile-butadiene-styrene copolymer (ABS polymer ) and 33 wt% perfume composition based on limonene * dipentene and veratrene.

A homogeneous wax mixture with an intensive and characteristic odor was obtained, which had not changed from the point of view of intensity even after 12 months of storage.

Example XI

50 wt.% Porous hydrated silica having a specific surface area of 110 m / g were mixed with 50 wt.% Perfume preparation based on eucalyptus oil, benzoic acid and tolyl acid derivatives, terpenyl and dehydrolinalyl acetate and aldehydes * ketones and deri-25 vessels, mixed thereof », the maximum sorption of the composition on this sorbent being 2.2 parts by weight of perfume per part by weight of sorbent. * After homogenization, a powdered immobilized perfume was obtained with the characteristic odor of the original perfume, the intensity of which after storage of 12 Has remained unchanged for 30 months *

Example XII

67 wt% porous sorbent based on polyethylene terephthalate having a surface area of 70 m / g were mixed with 33 wt% perfume composition based on limonene, dipentene and veratrene, their maximum sorption on the present sorbent 1.6 wt. * parts perfume per weight part of sorbent was * After homogenization, a powdered immobilized perfume with the same properties and with the same shelf life after long-term storage as in Example 1 was obtained.

1 * 0 The method of preparing detergents according to the invention 8 Q 0 7 0 0 6 o ·.

This is particularly suitable for the preparation of powdered detergents with the stabilized perfume component. The process is used in the manufacture of powdered prewash, soaking and detergent compositions and in the manufacture of perfumed cosmetics and powder deodorants.

8007006

Claims (2)

9 r. 1. A process for the preparation of perfumed detergents, powdered detergents and cleaning agents, wherein the individual components of the agent are mixed in the required ratio, the perfume is added and the mixture is homogenized, characterized in that it is perfume prior to addition to the other components of the mixture adsorbs in a porous support and the perfume immobilized in this way in an amount of 0.05 to 10% by weight, preferably 0.2 10 to 1% by weight, based on the amount of detergent. 2. Process according to claim 1, characterized in that a porous carrier is used with a sorbent with a high active surface area based on polyacrylates, polyvinyl chloride, polyalkyl methacrylate, acetyl cellulose, polyphenylene oxide, polyethylene terephthalate, polyamides, urea-formaldehyde and melamine. formaldehyde resins, acrylonitrile-butadiene-styrene-vinyl chloride copolymers, polyacrylonitrile, vinyl acetate copolymer, polyethylene, polypropylene, polystyrene, hydrated silicon and titanium oxide. alumina or mixtures, the perfume content of 20 in this sorbent being from 10 to 65% by weight. - 8 0 0 7 0 0 6 1 1 1 1 1