DE2731318A1 - Spray granulate of perfume and hard paraffin wax - contg. disperse dye for simultaneous printing and perfuming of polyester, etc. - Google Patents

Abstract

Spray granulate of particle size 10-600 mu m contains perfumes (I) and hard paraffin wax (II) plus opt. dyes (III), plasticisers, surfactants and/or other auxiliaries. Dye compsns. are prepd. by spraying dispersion or solns. of (I) and opt. the other components, in molten (II). The granules are pref. 5-40 mu m or 70-400 mu m and opt. after prepn. their surfaces are treated with surfactant. Pref. (III) are disperse dyes sublimable at 140-220 degrees C and the (II) has softening point >50 degrees C. Granules contg. (III) are useful for dyeing or printing (esp. transfer printing with a mottled effect) polyester, cellulose ester, polyamides, polyester-cotton etc. (I) is incorporated at the same time as (III) so that prints, of flowers, etc. can be produced having the corresp. perfume. Granulates with no dye are useful in finishing baths, as additives for washing or rinsing compsns. and esp. as room fresheners.

Description

Spray granules

The invention relates to spray granules with particle sizes of 10 to 600 / u, containing paraffin waxes and fragrances and optionally Colorants, plasticizers, surfactants and / or other auxiliaries.

Suitable wax components of these granulates are hydrocarbons with melting points above 500C, as e.g. in the paint raw material tables of Erich Karsten (Verlag R. Vincentz, Hanover, page 403) and in Ullamnn's encyclopedia the tech. Chemie, Volume 18, pages 270-280 are listed.

Suitable fragrances are those with boiling points above 1200C lie.

Examples are: coumarin, vanillin, ethyl vanillin, musk bodies, Xylene musk, ambret musk, pentadecanolide-1,15, 4-tertiary -butylcyclohexanol, 2-phenylethanol, phenylacetic acid, benzaldehyde dimethylacetal, 1,7,7-trimethylbicycloZ2.21gheptan-2-olacetate, 2,2,2-trichloro-1-phenylethyl acetate, phenoxyethyl isobutyrate, thymol, Tonalid, Benzyl cinnamate. ß-methylnaphthyl ketone, citral and autantiol.

In general, the preparations contain 1-35 percent by weight these fragrances.

Phosphoric acid and phthalic acid esters, such as Trioctyl phosphate, dibutyl phthalate, dioctyphthalate in question.

Nonionic, anionic or cationic surfactants, in particular ethylene oxide or propylene oxide batteries from alkylphenols, alkyl alcohols or long-chain carboxylic acids and condensation products from naphthalene, foemaldehyde and H2SO4, amines and ammonium salts, especially long-chain or acyclic amines or their salts are used.

The granules according to the invention can contain 0.1 to 50 8 plasticizers and / or contain surfactants.

Pigments and, above all, commercially available dyes, for example, are used as dyes Dispersion dyes in question, in particular azo and anthraquinone dyes, such as they e.g. in the Color Index, 3rd edition (1971), Volume 2, Pages 2479 - 2742 or in Ullmann's encyclopedia of teflon. Chemie, Volume 4, pages 128 ff., And Volume 3, pages 726 ff. Are described, as well as commercially available dispersion whiteners.

The proportion of dye in the preparations according to the invention can be 1 to 80, preferably 5 to 40 wt .-%.

Preferred preparations are made up as follows: 85 - 5 (; possibly wax 0-30% by weight fragrance 0-35% by weight dye 0-30% by weight plasticizer 0-10% by weight surfactants 0-10% by weight other auxiliaries (fillers, buffer substances etc.) The particle sizes of the preparations can - as mentioned at the beginning - within a wide range Ranges vary and are generally 5 to 600 µ as well as i.e. depending on the intended use a) 10 to 40 µm and b) 40 to 600 µm, preferably 70 up to 100 / µm.

The granules claimed can be produced according to known methods Methods are carried out, e.g. by spraying solutions of the fragrances and, if necessary Plasticizers, surfactants and other auxiliaries in paraffin wax melts.

It is expedient to proceed in such a way that the fragrances and optionally dyes, surfactants, plasticizers and the like. initially discontinuous in a stirred tank or continuously in a screw with the wax intensively mixed and heated, taking the temperature is chosen so that the resulting solutions or dispersion of fragrances, surfactants, dyes etc. can nat atomize in the wax melt. The continuous business world is used as an advantage for temperature-sensitive fragrances, as the Cert the thermal stress can be kept very small. The smear is solann in a übli chen manner with a single-fluid nozzle or two-fluid nozzles or an atomizer sheabe in kaites gas or a katte plüsengkeit atomized. By The preparation particles reimburse the contact with the gas or the plusiness to @@ gel-shaped granules. When atomizing into a gas (@lutt emplindtechen daft and Color stumps are chosen from nitrogen or argen) one obtains the end product; at Atomization into a liquid is required to be exhaustive from walls you do not win an end product in the form of a suspension. The atomization can through if a suitable atomizing device is chosen, it is carried out in such a way that the particle diameter of the resulting spherical granules practically completely in the preferred Lying areas.

The preferred range of 10 to 40 µm is obtained by using of single-fluid nozzles with high pre-pressures up to 200 bar, preferably up to 100 bar, or by using two-fluid nozzles. The preferred range is 40 to 600 µm obtained by spraying with single-fluid nozzles at pressures of up to 100 bar. The viscosity the melt can be up to 500 cP in the case of the single-fluid nozzles, in the case of the two-fluid nozzles up to 2000 cP.

The preparations obtainable according to the invention are free from stagnation and free-flowing if the particle size is greater than approx. 40 μm; they have a high Dense, are not hyqroscopic, do not bake and dissolve at room temperature easily in organic media.

For application in aqueous media, it is advisable to use it add surfactants to spraying melts. But it is particularly advantageous that the Cover the surfaces of the granules with surfactants subsequently by adding the granules stirred into an aqueous surfactant solution, then filtered off and dried.

The new spray granules with a scent note can be used in a variety of ways.

The colored preparations are suitable e.g. for coloring cosmetics, such as lipsticks, creams and the like. Another area of use for these preparations represents the classic wet textile print (acramin (R) print), wol> <i under Use of a suitable binder and dye granules with particle sizes from 40-400 / µm, preferably 70-100 / µm, speckled prints on synthetic fibers or virgin fibers, preferably polyester, cellulose ester, polyamide and polyester / cotton fibers possible are. But it is also possible with suitable preparations, which are listed under 2200C sublimable disperse dyes contain, initially an intermediate carrier (Paper) to print and after the transfer process speckle effects on goods preferably to transfer synthetic fiber materials. ei use of dye preparations more appropriate Particle size (less than 40 µm) can also be obtained in two-dimensional prints.

To transfer the fragrances and dyes from the auxiliary carriers to the substrates, both are brought into close contact and during 20-60 Heat treatment (1400-2400C, preferably 180-2200C) for seconds.

With these auxiliary carriers can be simple and environmentally friendly (no sewage!) white fragrances, in combination with colored patterns on textile materials transfer. Surprisingly, the transfers are distinguished by a comparative satisfactory wash fastness.

In a particularly interesting embodiment of the new subcarrier are on these colored motifs of flowers or fruits with the associated fragrances upset. In this application, the form of fragrances is expediently chosen air and heat resistant bodies with a high boiling point or sublimation point.

Furthermore, the colored preparations according to the invention can be used for Preparation of printing pastes for the creation of speckle effects on preferably synthetic fiber materials are used. The printing pastes used for this are primarily of an aqueous nature and contain, in addition to the fragrance / dye granules according to the invention with particle sizes of 40 to 400 μm, preferably 70 to 400 μm (0.4-4% by weight) usual Print thickener (40-50 wt.). The rest is water.

For example, when making speckle effects, one goes like follows: The powdery fragrance / dye preparation is in an aqueous print thickener, E.g. in a 5 - 10% solution of a locust bean gum ether. Thereafter the desired white or pre-colored substrates are printed with this preparation, impregnated or coated (with a doctor blade), then dried and thoroughly Hot air or an inert gas between 170 and 200 ° C fixed for 3 to 1 minutes. In addition, the fixation can also be carried out with steam under atmospheric pressure, preferably but take place under overpressure. The fixing times in this case are between 15 and 60 minutes. After washing out the thickening, a colored speckle effect is obtained on an undyed or pre-colored ground with a scented note. But you can also have several Preparations with different colored dyes and different scents below Print the same conditions, so that you can get sprinkles with different hues and receives scent notes.

Suitable substrates are woven, knitted fabrics, foils, fleeces and the like from aromatic polyesters, synthetic superpolyamides, cellulose esters, etc.

The colorless fragrance granules according to the invention are suitable for production of finishing liquors, as an additive to detergents and dishwashing detergents and, above all, to improve indoor air quality.

For this purpose, the fragrance globules, which are preferably relative Contain low-boiling fragrances, filled into air-permeable containers and attached at suitable points in the room.

The process for the production of the dye preparations as well as their Usage are explained in more detail below. Examples A) Production of the spray granules Example 1 A 150 g of the dye Disperse Red 60 (C.J. 60756) and 600 g of vanillin were mixed with 2400 g of paraffin wax EH 100, which has a melting point of 90-94 ° C, melted in a stirred vessel at 190 ° C. After that, the Melt atomized into air through a single-fluid nozzle. The resulting granules possessed a particle size distribution of 70-400 μm.

Example 2 A The procedure is as in Example 1, but none are used Color and replaces the vanillin with 600 g of musk body. A corresponding one is obtained colorless granules.

Example 3 A As in Example 1 A, a dye-paraffin wax melt was used produced and atomized in air through a two-substance nozzle. The resulting granules had a particle size distribution of less than 40 μm.

Example 4 A 12 kg per hour of a mixture consisting of 20% by weight phenylethanol and 80% by weight paraffin wax EH 100 (Melting point 90 - 94 0C), melted in a screw and brought to a temperature of 1900C. The melt was atomized and solidified in air by means of a two-fluid nozzle. That The resulting granules had a particle size distribution of less than 40 μm.

Example 5 A As in Example 4 A, a melt was produced, atomized in air with a single-fluid nozzle and solidified. The resulting granules had a particle size distribution of 70-400 μm.

Example 6 A As in Example 1 A, fragrant dye granules were produced produced with the following dyes: Disperse Yellow 60 (C. J. 12712), Disperse Violet 1 (C.J. 61100) and Disperse Blue 14 (C.J. 61500).

B) Use of dye preparations Example 1 B Production of Sprinkle effects 20 g of the preparation described in Example 1 A are used in 500 g Indalca PAi 1 (carob gum derivative) 4% in water and mixed with 480 ml of water added to 1000 g. This printing paste is printed on a polyester fabric, dried, fixed by hot air at 1700C for one minute and washed.

A clearly separated red speckle effect with a scented note is obtained.

Example 2 B Production of a pigment print 30 g of that in example 3 A described dye preparation are converted into a binding combination of a) 600 g of a binder based on hydroxyethyl cellulose (1% solution), 15 g of one Crosslinker based on a condensation product of epichlorohydrin and N-methyldipropylamine, 25 g of a printing auxiliary based on N-alkylphthalimides and b) 150 g a binder based on a copolymer of dichloroethane and acrylic acid, 100 g of a binding agent based on a polyurea (10% acetic acid solution) 20 g of a crosslinker (see a)) 5 g of a defoamer (isooctyl alcohol) are stirred in.

This printing paste is used to print cotton t-shirts.

All that is required for fixation is air drying.

Prints with a scented effect are obtained on the textiles mentioned.

Example 3 B Production of a sprinkle print In an emulsion binder, made from copolymers of butyl acrylate, styrene, vinyl isobutyl ether and the methyl ether of methacrylic acid methylolamide and an aqueous solution of one Formaldehyde condensate, an emulsifier (stearyl alcohol + 10 mol ethylene oxide) and an ammonium polyacrylate solution (10%) is stirred in 30-40% gasoline (Boiling point 160-220 ° C).

Then 30 g of the dye preparation described in Example 1A are added Stirred into one kilo of the above binding emulgates and prints on polyester fabric with this paste manufactured. After fixing for 1 min. At 160 ° -1700 ° C., clear red speckles are obtained with scented effect.

Example 4 B Production of a pigment print 25 g of a fragrance preparation According to Example 4 A, 935 g of a binding combination as in Example 2 B described, registered. Then 40 g becomes one 30% Dispersion of Pigment Blue 15 (C.J. 74160) stirred in. With this printing paste will be Textiles made of polyester / cotton blended fabrics printed and dried at 400C.

A blue print with an intense fragrance is obtained.

Example 5 B Production of a transfer print The procedure is as in Example 3 B, however, the dye preparation described in Example 3 A is used and a paper (80 g / m2) is printed. The printed, dried paper is in a Thermal printing system heated to 1700C for 30 seconds in contact with a polyester fabric. A two-dimensionally colored print with an intense fragrance is obtained. If you use on the other hand, preparations according to Example 6 A, this gives transfer prints with a speckle and scented effect.

Example 6 B Production of a finish Consisting of a finish liquor from 28 g of a finishing agent based on a polyvinyl ether, 15 g of a fragrance preparation according to Example 4 A 2 g of nonionic emulsifier 25 g of a cotton whitening agent of the styryl type and 930 g of water are applied to a cotton fabric on a padder.

After drying at 70-850C the fabric shows a plump softness Handle and at the same time an intense fragrance.

Claims (11)

Claims 1. Spray granules with particle sizes from 10 to 600 μm, Containing fragrances and hard paraffin waxes and optionally dyes, plasticizers, Surfactants and / or other auxiliaries. 2. Process for the production of dye preparations, characterized in that that dispersions or solutions of fragrances and optionally dyes, Plasticizers, surfactants and other auxiliaries in hard paraffin wax melts sprayed. 3. The method according to claim 1, characterized in that the Melt of wax and fragrances into granules with particle sizes of 5 to 40 μm respectively. 70 - 400 / um sprayed and, if necessary, then the surface coated with surfactants. 4. The method according to claim 1, characterized in that as Dyes in the range from 140 to 2200C sublimable disperse dyes are used. 5. The method according to claim 1, characterized in that as Waxes Paraffin waxes with softening points above 500 are used. 6. Dye preparations in granulate form obtained by the process of claims 2 - 5. 7. Process for dyeing and / or printing organic materials, characterized in that colored granules according to Claim 1 are used. 8. Process for dyeing synthetic fiber materials in speckle effects, characterized in that color pastes are used which colored granules according to Claim 1 with particle sizes of 40 to 600 μm, preferably 70 to 400 μm, is used. 9. Process for the production of auxiliary carriers for transfer printing, characterized in that printing pastes are used prepared with colored granules according to claim 1. 10. Process for printing preferably synthetic fiber materials according to the transfer printing principle, characterized in that one auxiliary carrier according to Claim 9 used. 11. A method for improving indoor air, characterized in that granules according to claim 1 are used.