DE1213373B - Water repellent for all kinds of textiles - Google Patents

Description

FEDERAL REPUBLIC OF GERMANY GERMAN -007WW PATENT OFFICE

EDITORIAL

Int. α .:

Number:
File number:
Registration date:
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D 06m

German class: 8 k-3

1213 373
C23947IVc / 8k
April 22, 1961
March 31, 1966

It is Z. B. from the German patent specification 700 767 or the Austrian patent specification 208 078 known, Methylol compounds of nitrogen derivatives which are at least two by alkylene groups with 2 to Urea residues linked to 4 carbon atoms and at least one linked to 1 nitrogen atom of a urea residue Contains alkyl group of more than 10 carbon atoms, to be used for textile treatment, besides water-repellent effects can be achieved with a soft grip. These products represent more or less viscous emulsions.

They can be made up primarily through the implementation of heating products of diethyientriamine and the like Polyalkylenepolyamines and urea with higher alkyl isocyanates and subsequent methylolation to win.

The stability of the liquors produced therefrom is not uniform, or that of different ones Products originating from manufacturing cannot always be converted into the desired uniform liquors but sometimes show signs of agglomeration. This deterioration in the products often occurs even after prolonged storage.

It has now been found that these disadvantages can be eliminated if the products described above are mixed with small amounts of water-insoluble, basic substances soluble in dilute acids are added, which are caused by monohydric alcohols with 1 to 4 C-atoms etherified methylol compounds represent aminoplast-forming substances in which additionally still lower alkanolamines and alkyl radicals with at least 10 carbon atoms, optionally via one Ether, amido or carboxyl groups are incorporated, the water-insoluble, basic substances with Water-insoluble, liquid, organic solvents are mixed.

Such water-insoluble, basic compounds can be produced in various ways. Man can, for example, according to US Pat. No. 2 210 831, melamines acylated by fatty acids with formaldehyde and converting diethanolamine or triethanolamine into the water-insoluble, acid-soluble base by heating. or according to German patent specification 956 990, fatty acid amides can be obtained with etherified methylolmelamines and tertiary alkanolamines ^ ζ. Β. Triethanolamine, react by heating until it is acid-soluble. Furthermore, one can be etherified by lower alcohols Methylolurea or an equally etherified methylolmelamine partially encapsulated with a fatty alcohol or transesterified with a fatty acid and this reaction product with formaldehyde and alkanolamine with further heating in the acid-soluble base

Waterproofing agent for textiles of all ax

Applicant:

Chemical factory Pfersee G. mb H.,
Augsburg, Färberstr. 4th

Named as inventor:

Heinz Enders, Stadtbergen near Augsburg;

Hans yours,

Eugen Kurz, Augsburg

to be changed. Also the joint heating of urea, thiourea, aminotriazines and others aminoplast-forming compounds with para-shaped

ao aldehyde, a monohydric alcohol with 1 to 4 carbon atoms, an alkanolamine and a fatty acid anhydride leads, according to Belgian patent specification 547 294, to products which are insoluble in water and soluble in acid.

as All of these compounds which act hydrophobicizing on fabrics ,, net of the organic solvent in amounts of preferably 1 to 5 ° / ₀ of the weight of the above-described methylol of nitrogen derivatives that at least two joined by alkylene groups having 2 to 4 carbon atoms Urea residues and at least one alkyl group bonded to 1 nitrogen atom of a urea residue and having more than 10 carbon atoms is added.

As water-insoluble, liquid, organic solvents, those with the basic compounds mentioned are mixed, preferably chlorinated hydrocarbons, such as carbon tetrachloride or Trichlorethylene, but also non-chlorinated hydrocarbons, such as gasoline, benzene or tetrahydro-

'naphthalene, into consideration. Axxch mixtures are suitable those solvents whose specific gravity is approximately 1. The amount of to use Solvent is about the same weight as that of the acid-soluble, basic compounds mentioned.

By adding these mixtures of the basic acid-soluble compounds and organic solvents, the shelf life of the methylol compounds described above is improved. Mixtures of the invention can be even with a sub-cooling for 3 days at -15 ⁰ C to pre-

609 540/393

Claims (2)

3 4 Thawing again to perfect liquors of stearic anhydride and 300 g of methanol with dilution, distill and stir until it is soluble in The durability of the fleets of dilute acetic described, cooling to 80 ⁰ C and diluting The addition of methylol compounds becomes noticeable with 380 g of trichlorethylene. loaned improved, from about 3 to 4 days to 5 ... over 3 weeks. The addition also enables: An example2 reversibility of the liquors at a higher temperature, 50 g of one in an analogous manner by heating The liquors must be prepared with the addition of dilute 1 mole of triethylenetetramine and 2 moles of urea inorganic acids, such as acetic acid. preserved product are described in aqueous solution, such as in the are added to the inventive mixture of the io Example 1, 160 g of hexadecyl two products about 30 to 40% acetic acid (60 ° / ₀ ig) strength, and then with 150 g of a 30% Formaldehyde-related to the solids content, and about the 3-to-hyd solution converted. 6 times the amount of water from 60 to 70 ⁰ C and diluted The resulting emulsion is then with 5 g with cold water to the application concentration. of a water-insoluble, acid- It is surprising that these liquors are intimately mixed according to the soluble product. Invention a much longer shelf life with 100 parts by weight of dipalmitylmelamine because they react acidic on the one hand and 50 parts by weight of paraformaldehyde, 130 parts by weight on the other hand, acid-curable methylol compounds split ethanol and 13 parts by weight of triisopropanol keep. amine heated to solubility in dilute acids You can also use other thermosetting 20 and with the same weight of a mixture Precondensates, such as unetherified or etherified ones of perchlorethylene and benzene (volume ratio Methylol compounds of urea or melamine 1; 3) stirred, as well as water repellants, such as. B. zirconia example 3
saline paraffin wax emulsions or silicone Also use emulsions if special effects are desired in example 1 or 2 are. Additions of these compounds alone produce an emulsion of the methylol compound but increase the stability of the emulsions of the 60 parts by weight of the emulsion of an N-alkyl-N'N'-aleingang mentioned connections not. kylenurea ,. their production is described below It is also possible to use the mixtures of the inscribed, and 15 parts by weight of one of the included described methylol compounds and the 30 game 1 or 2 described solvent-based, Solvent-based, water-insoluble, acid-soluble, water-insoluble, acid-soluble condensation products, basic condensation products are also emulsified. This mix is done as well aqueous emulsions of N-alkyl, N'N'-alkylene urine- addition of 60% acetic acid and hot water to add substances in which the alkyl radical is at least dissolved for the application and is used in particular in the 12 carbon atoms and the alkylene radical 2 to 3 carbon atoms in combination with oil-repellent compounds, the sits, such connections are z. B. from the German perfluorinated aliphatic hydrocarbon patent 946 132 as a textile waterproofing agent. known. This combination is particularly interesting. The emulsion of the N-alkyl-N'N'-alkylene urea, if it is both water and oil repellent, can be produced as follows; Hermachende the equipment is, the position 40 under Mitver- is not the subject of the invention: 28,5 turn from compounds containing perfluorinated chain be ethyleneimine with 125 g distilled water like groups on the one hand and unsaturated poly- diluted at 2O ⁰ C with a solution of 45 g of rizimerizable groups on the other hand, nolsäuretriglycerid, which is etherified with 30 mol of ethylene oxide, in 126.5 g of distilled water, the 15 g of Example _{1 4g w} ^ ß _r jg _e ammonia solution (density 0 , 90) admitted 50 g of one according to the German patent specification 700 767 was mixed. This solution is now under by heating 1 mole of diethylenetriamine and stirring and cooling well, 200 g of octadecyl isocyanate 2 mol of urea obtained nitrogen compound with slowly added dropwise. After the implementation Urea residues are finished in the tenfold amount of water, 450 g of distilled water and of 4O ⁰ C solved. With vigorous stirring, 50 10 g of aqueous ammonia solution are added, and that 135 g of octadecyl isocyanate are added, stirring is continued for 15 minutes. Mixture is now mechanically, e.g. B. with a at this temperature and then for 1 hour at 70 ⁰ C. high-speed stirrer homogenized .. With a In the resulting emulsion are in the same solution of 66 g of octadecyl-oxymethylene-oxyäthyl- Temperature 160 g of formaldehyde solution (40%) monomorpholimum chloride in 134 g of distilled water stirred undnachl5 minutes is cooled to 45 ⁰ C. 55 is then made up to 1000 g. Stir into this emulsion of the methylol compound 8 g of the acid-soluble patent claims described below:
Product and homogenizes the whole thing in a 1st water repellent for textiles of all kinds colloid mill. The pasty, white mixture, based on aqueous emulsions of Methylolwelches is close to neutral, is used for text lien application 60 compounds of nitrogen derivatives that mindung with the 4- to 5-fold amount of water from 6O ⁰ C, least two of alkylene groups having 2 to 10 % acetic acid (60 ° / _o ig), based on the weight 4 carbon atoms linked urea residues and Minim mixture of the invention contains dissolved least diluted and a to 1 nitrogen atom of the Harnstoffanschließend with cold water to the desired residue bonded alkyl group of more than use concentration . 65 having 10 carbon atoms, additionally containing The acid-soluble, basic condensation product minor amounts of a water-repellent is z. B. obtained by heating 150 g of paraforming agent known per se, approximately equal parts aldehyde, 50 g melamine, 55 g triethanolamine, 180 g mixture of water-insoluble, acid-soluble Substances containing methylol compounds etherified by monohydric alcohols with 1 to 4 carbon atoms Represent aminoplast-forming substances and in which also lower alkanolamines and alkyl radicals with at least 10 carbon atoms, optionally via an ether, amido or carboxyl group are built in, furthermore water-insoluble, liquid, organic solvents stabilizing the emulsion Amounts. 2. Water repellent according to claim 1, characterized in that it is used as a further stabilizing additive minor amounts of N'-alkyl-N'N'-alkylene ureas known per se as water repellants, in which the alkyl radical has at least 12 carbon atoms and the alkylene radical Has 2 to 3 carbon atoms contains. IO Publications considered:
German patents No. 700 767, 946 132,
990; Austrian Patent Specification No. 208 078,209 309; Belgian patents nos. 569 962, 571 306. 609 540/393 3.66 © Bundesdruckerei Berlin