US2416890A - Manufacture of fibers and foils - Google Patents

Description

. polyamides.

Patented Mar. 4, 1947 2,416,890 MANUFACTURE OF FIBERS AND FOILS Joachim Amende and Willibald hafen-on-the-Rhein,

Attorney General of No Drawing.

12 Claims.

This invention relates to the manufacture of fibers and foils.

It is an object of this invention to .produce fibers and foils of special properties.

A further object is to produce these fibers and foils from viscose solutions treated with superpolyamides.

A still further object is the provision of fibers and foils from ammoniacal copper oxyde solutions treated with superpolyamides.

These and other objects will appear from the detailed specification following hereinafter. It ha been found that fibers and foils of excellent properties are obtained, if solutions of viscose and cellulose in ammoniacal copper oxyde treated with alkali-soluble .superpolyamides containing sulfamide groups, are spun or worked up into foils. Alkali-soluble superpolyamides are obtained according to the German patent application I. 64,124 IVd/lZo, filed March 20, 1939, by condensing diamines containing sulfamide groups and/or dicarboxylic acids or their functional derivatives or salts of these acids with the diamines or amino carboxylic acids containing sulfamide groups or their functional derivatives, especially lactams.

According to the description in said German application, the starting materials containing sulfamide groups can be employed inthe quantities necessary for the condensation. However, a part of these starting materials may be substituted by corresponding starting materials free of sulfamide groups. It is necessary, however, that the final product have a certain content of sulfamide groups, to obtain a ready alkali-solubility. The quantity of the starting material containing sulfamide groups required for this process varies depending upon the chemical property of the starting material-and can be easily determined by test.

The 'manufacture of the condensation products is carried out in the manner conventional for uperpolyamides, especially by heating the starting materials to, high temperatures in the presence or in the absence of solvents or diluents.

The superpolyamides obtained are practically colorless, resin-free substances which can be HOOC.

Ender, Ludwigs- Germany; vested in the the United States Application April 6,1940, Serial No.

In Germany March 29, 1939 amide (related to cellulose),

spun into filaments in the molten state in a manner similar to that used for the known super- The superpolyamides obtained are soluble. in aqueous alkalies in contrast to the obtained are better than those of fibers and known superpolyamides which do not contain their color. The fabrics or fib 2- sulfamide groups. Due to this property they are suited especially for the refining of textile fibers, particularly as sizing agents. It is likewise possible to treat fibers or fabrics of textile materials with solutions of these superpolyamides, whereby the fibers or fabric are refined with respect to ers of cellulose filaments thus treated absorb much more easily substantive dyestuffs and can be dyed even with acid dyestuffs, for-example wool dyestuffs, and also with acetate rayon dyestuffs.

In the present invention, solutions of viscose or of cellulose in ammoniacal copper oxyde are preferably mixed with alkaline solutions of these superpolyamides and then spun in a known man: ner or worked up into foils. Hereby the usual coagulation agents like salt solutions or acids may be employed. The quantity of the superpolyamides, to be given to the spinning solution, may vary within wide limits. Preferably there are added not less than 5 per cent superpolyas otherwise the admixture of superpolyamides is of no practical value. On the other hand a multiple of superpolyamide compared with cellulose may be employed.

The fibers obtained are faster to possess a far higher Bauschelastizitat" (bolsterelasticity) and a more elastic grip than viscosefibers. The grip, moreover, on account of the good Bauschelastizitat resembles wool. Also the dyeing properties of the fibers and foils thus foils from .pure viscose or pure ammoniacal copper oxyde cellulose. They absorb dyestuffs for instance much easier and Carl be dyed in darker shades than pure viscose or pure ammoniacal copper oxyde cellulose. Contrary to these they may be dyed with acid dyestuffs, for instance with wool dyestuffs and also with acetate silk dyestufl's. On account of the excellent dyeing properties the fibers are very much adapted for the manufacture of mixed fabrics.

Example I parts by weight of N.N-di-propanecarboxacid-p-sulfo-benzoic-acid-amide Wrinkling and lowish color and is over, possess contrary to page 131) by adding product consisting of soluble in a concentrated aqueous alkali solution. It can be drawn into filaments in the molten state.

A 20 per cent solution of said superpolyamide consisting of 'hexamethylenediamine and N.N- dipropane-carboxylicacid-p-sulfo-benzoic-aciddiamide in a caustic soda solution of about 8 per cent is added to a viscose solution capable of being spun in such a quantity, that after spinning and coagulating filaments containing about: per cent superpolyamide are obtained. The elasticity of these filaments is far greater of pure viscose filaments. The filaments, moregrip and excellent Bauschel tizitat.

The filamentsv may be dyed is boiling one hou with 2 per cent Acid Anthfacene Red 3 BL (Schultz dyestufi tables, year 1932, vol. II, page 187) ratio of the weights of filaments and water 1:50, by adding 10per cent Glauber salt and 4 per cent formic acid. It is then washed with lukewarm water and afterwards dried. The shades obtained are distinctly darker thanon viscose silk without addition of the superpolyamide, whereby the degree of fastness is for both kinds at least the same. If the filaments are dyed in the same way with 2 per cent Palatine Fast Blue GGN (Schultz dyestufi tables, year 1932, vol. II, page 108) by adding 6 per cent formic acid or with 2 per cent Sirius Light Blue BRR. (Schultz dyestufl" tables, year 1934, Vol.1,

also distinctly darker, but more brilliant shades are obtained than on cellulose free from superpolyamides.

' Example If 50 parts by weight of N.N'-di-propanecarboxylic acid-'diphenylether-4A'-disulfonic-aciddiamide than that A the others a wool-like- 20 per cent Glauber salt,.

4 Blue BF (Cellitonechtblau' BF)... concentrated powder, ratio ofthe weights of filaments and water 1:50. The shades-are far darker than,

those one filaments from superpolyamide-efree- 5 viscose solution, whereby the degree vof fastness for both kinds is very much the same.

Example III .An alkaline solution of a s'uperpolyamideconsisting of 1 mol N.N-dipropanecarboxylic-acidp-sulfobenzoic-acid-diamide, 1 mol adipic acid and 2 mols hexamethylenediamine is added to a viscose solution capable of being spun in such a quantity, that the finished filaments contain about 20 per cent superpolyamide. The filaments are dyed by boiling one hour with 2 per cent Sirius Fast Blue (Schultz dyestufi tables, year 1934, supplementary volume I, page 131) ratio of the weights of filaments and water Glauber salt. Far darker shades than on filaments consisting of superpolyamide-free viscose are thus obtained.

What we claim is:

1. A process for the foils from a mixture of an superpolyamide containing sulfamide groups and a cellulosic solution selected from the group'con- 'sisting of viscose and ammoniacal copper oxide cellulose, which comprises adding to the cellulosic solution an alkaline solution of thesuperpolyamide, the amount of superpolyamide added to the cellulosic solution being at least 5%, based on no0o.cHi.0H,.onmnsofiogsomn.among.ontooon and 6 parts by weight of hexamethylenediamine I are condensed as described in Example I. The

superpolyamide obtained is-soluble in an aqueous alkali solution.

An alkaline solution of said condensation N.N' dipropane-carboxylic-acid-diphenylether- 4.4. di-sulfonic-acid-diamide is added to a viscose solution as described in Example I in such a quantity, that the finished filaments spun from the solution contain 15 per cent of the superpolyamide'. They are spun in the way usually adapted for pure viscose. The filaments are very' elastic and show a wool-like grip. If they are boiled one hour with 2 per cent Fast-Mordant- Blue E (Schultz dyestuff tables, year 1934, supplementary volume I, page 90) ratio of the weights of filaments and water 1:50, by adding 10 per cent Glauber salt and 4 per cent formic acid and, if afterwards treated for minutes with 1 per cent potassium chromate, distinctly foils can be obtained and darker shades than 0115 hexamethylenediamine and 5 pane carboxylic acid-p-sulfobenzoic-acid-dilulosic solution is an ammoniacal copper oxide 45 cellulose solution. a

4. A process as' in claim 1 in which the cellulosic solution is a viscose solution and the superpolyamide is the condensation product obtained from hexamethylene diamine and N.N'-diproamide.

5. A process as in claim 1 in which the cellulosic solution is a viscose solution and the superpolyamide is the condensation product from hexamethylene diamine and N.N dipropane-carboxylic-acid-diphenyl ether-4.4'-di-sulfonic-acid-diamide..

g 6. A process as in claim 1 in which the cellulosic solution is a viscose solution and the superc0 polyamide is the condensation product obtained 1 from one mol of N.N'-dipropane-carboxylic-acidp-sulfobenzoic-acid-diamide, one mol of adipic acid and two mols of hexamethylene diamine.

comprising as essential polyamide containing sulfamide'groups, dissolved in a cellulosic solution selected from the'group consisting of viscose and ammoniacal copper 76 oxide cellulose.

BRR (Siriusechtblau BRR) 1:50, by adding 20 per cent manufacture of fibers and alkali-soluble linear obtained '7. A new filament as in claim 11 in which the based on the weight, of the cellulose, of an alkali-soluble linear superviscose solution.

10. A spinning solution as in claim 8 in which the cellulosic solution is viscose and the superpolyamide is the condensation product obtained from hexamethylene diamine and N.N'-dipropane carboxylic acid-p-sulfobenzoic-aciddlamide.

11. A new filament comprising regenerated viscose cellulose containing at least five percent, based on the cellulose, and dissolved in the viscose solution from which the filament is formed, of an alkali-soluble linear superpolyamide containing sulfamide groups, said filament being resistan't to wrinkling, wool-like in character and readily dyed by acid and acetate silk dyes.

12. Filaments and foils comprising essentially a mixture of regenerated cellulose derived from a cellulosic solution selected from the group consisting of viscose and ammoniacal copper oxide cellulose. and at least five percent, based on the weight of the cellulose, of an alkali-soluble linear superpolyamide containing sulfamide groups. the superpolyamide being dissolved in the cellulosic solution, said filaments and foils being resistant to wrinkling, readily dyed by acid and acetate silk dyes and having been obtained by the process of claim 1. I

' JOACHIM AMENDE. WILIBALD ENDER.

REFERENCES CITED UNITED STATES PATENTS Number Name Date 7 1,864,426 Gardner Jan. 21, 1932 2,136,928 Schlack Nov. 15, 1938 2,071,251 Carothers Feb. 16, 1937 2,130,948 Carothers Sept. 20, 1938 950,435 Chavassieu Feb. 22, 1910 2,155,067 Ubbelohde Apr. 18, 1939 2,224,693 Picard et al Dec. 10, 1940 2,149,273 Carothers Mar. '7, 1939 2,191,556 Carothers Feb. 27. 1940 2,265,559 Watkins Dec. 9, 1941 2,223,916

Martin Dec. 3, 1940