US1779494A - Dyeing of cellulose derivatives - Google Patents

Description

Patented Oct. 28, 1930 UNITED STATES PATENT, OFFICE GEORGE RIVAT,

SEY, CAMILLE DREYFU S, POBATION OF AMERICA, A

0F PATEBSON, ERNEST GADGENE, OF ENGLEWOOD GLHFS, NEW JER- OF NEW YORK, N. Y., ASSIGNORS TO CELANESE GOR- GORZPORATION OF DELAWARE DYEING OF GELLULOSE DERIVATIVES Io Drawing.

The object of this invention is to provide a process of fixing iron salts on or in materials containing organic derivatives of cellulose. Another object of this invention is to provide a process for fixing iron salts on or in materials containing organic esters of cellulose, more particularly cellulose acetate. Still another object of the invention is to provide a process for treating organic derivatives of cellulose so that they may be dyed more easily and with more satis fabctory results than has heretofore been possi le.

It is customary when it is desired to mordant silk, etc., with iron salts, that'an iron salt solution of 1 to 5% strength he used. This process when applied to materials containing organic esters of cellulose, results in no appreciable fixation of iron in the material. The applicants have now discovered that if material containing organic esters of cellulose is treated with a highly concentrated solution of iron salts, appreciable amounts of the iron are easily fixed in or on the cellulose derivative treated. The strength of the iron salt solution should be between 40 to by weight in order to obtain good results.

As an example of the operation of the process the following is given:

A fabric made from cellulose acetate was treated in a 50% bath of ferric chloride for one hour. The bath was first heated to 40 degrees centigrade which was gradually increased to degrees centigrade. The material was then squeezed or whizzed to remove the excess of the iron solution, after which it was washed in water for twenty minutes. After this washing the material was again washed, this time in cold water containg 1 c. c. of ammonia per litre of water.

The fabric after the above treatment was orange colored but was unchanged in other respects. It still retained its lustre and its softness. The iron was per anently fixed in the cellulose acetate and co (1 not be removed even when the material was treated with hydrochloric acid. The fabric treated as above when washed was found to contain 1.8-2% of 113011.

The applicants have discovered that a fab- Application filed June 30,

materials containing 1926. Serial No. 119,742.

ric which has been subjected to the above treatment can be dyed with the so-called natural or vegetable dyes. When such fab- -rics are dyed with this class of dyes unexpected results are obtained. The colors are very fast and deep whereas similar fabrics when untreated do not this class of dyes.

Thus when a cellulose acetate fabric which Was first treated with ferric chloride, washed, etc., as set out above, was immersed in a regular log-wood black bath in soap, say at a temperature of .C., for one hour it was found to have been dyed a beautiful black, much superior in appearance to that previously ob tainable with this dye.

Where a mixed fabric of cellulose acetate and silk, of cellulose acetate and wool or of dye at all well withcellulose acetate, silk and wool, was treated since the mixed fabric does not have to be" passed thru two or three different dye baths, as is the practice today. What has been said above with respect to the logwood dyeing of the organic derivatives of cellulose is also true of other natural or vegetable dyes or dye extracts such as, for example, young fustic, fustic, quercitron, Persian berries, weld extract, turmeric, sandalwood, cutch, etc. or any other dyes or mi tures of dyes which are suitable for dyeing a material mordanted with iron. The choices of dyes will depend upon the color which it is desired to dye the material. In all cases after the dyeing the goods must be washed as is customary in similar ordinary dyeing processes.

In the event it is desired to tint the black obtained by the logwood dyeing-either bluer or greener, this can be accomplished by adding the proper dyestuffs to the logwood bath. For the cellulose acetate fabric an SRA dyestulf (that is a water insoluble dyestuif having an affinity for cellulose acetate material and. generally applied in the form of an lose,

. terials such aqueous dispersion obtained for instance with the aid of a. dispersing agent) may be used whereas a basic dyestuif may be employed to tint real silk if it is present and an acid dyestuff for W001. The above examples are mere- 1 illustrative and merely set out a few of the numerous possible methods of carrying out the applicants invention. Thus the ferric chlorlde can be replaced by any other soluble ferric salt such as, for instance, ferric sulphate, ferric nitrate, etc. Also the cellulose acetate can be replaced by cellulose propionate, cellulose butyrate, ethyl celluetc. and, as stated above, logwood may be replaced by, fustic or other dyes as stated above.

This process is applicablenot only to materials made wholly of organic derivatives of cellulose but can also be utilized to treat mixtures of such derivatives and other maas, for example, mixtures of cellulose acetate and wool, cellulose acetate and silk, and cellulose acetate and wool and silk with very desirable results. The treatment of such mixtures, however, is to be considered within the scope of this invention.

Having described our invention what we desire to claim by "Letters Patent is:

1. A process of treating organic derivatives of cellulose which comprises subjecting the same to the action of a concentrated solution of a ferric salt.

2. A process of treating organic derivatives of cellulose which comprises subjecting the same to the action of a 40 to 55% solution of ferric chloride. 1

3.' A process of treating organic esters of cellulose .which comprises subjecting the same to the action of a concentrated solution of a ferric salt.

4. A process of treating organic esters of cellulose which comprises subjecting the same to the action of a 4:0 to 55% solution of ferric chloride.

5. A process of treating organic esters of cellulose which comprises subjecting the same to the action of a 50% solution of ferric chloride.

6. A process of treating organic esters of cellulose which comprises subjecting the same to the action of a concentrated sol ion of ferric chloride at temperatures above atmospheric and below C.

7. A process of treating organic esters of cellulose which comprises subjecting the same to the action of a 50% solutionof ferric chloride for approximately one hour at 40 to 60 C.

8. A process of treating organic esters of cellulose which comprises subjecting the same' to the action of a 50% solution of ferric chloride for approximately one hour at 40 to 60 C. removing the excess iron chlothen washing the material with which action warm water and finally washing it with cold water containing ammonia.

9. A process of treating cellulose acetate which comprises subjecting the same to the acltion of a concentrated solution of a ferric sa t.

10. A process'of treating cellulose acetate which comprises subjecting the same to the action of a concentrated solution of ferric chloride.

11. A process of treating cellulose acetate comprises subjecting the same to the of a 50% solution of ferric chloride. A process of treating cellulose acetate comprises subjecting the same to the of a 50% solution of ferric chloride. for approximately one hour at 40 to 60 C.

13. A process of treating cellulose acetate which comprises subjecting the same to the action of a 50% solution of ferric chloride for. approximately one hour at 40 to 60 C. removin the'excess iron chloride solution, then washing the cellulose acetate with water and finally washing it with cold water containing ammonia.

14. A process of treating organic esters of cellulose which comprises subjecting the same to the action of a concentrated solution of a ferric salt, removing the excess ferric salt solution, then washing the material with warm water, again washing with cold water containing ammonia, and then treating the thus Washed material with a dye extract and then finally washing the dyed material as action 12. which usual. I

15. A process of treating organic esters of cellulose which comprises subjecting the same to the action of a 50% solution of ferric chloride removing the excess ferric chloride solution, then washing the material with water, again washing with cold water containing ammonia, and then treating the thus washed material with a natural dye extract and then finally washing the dyed material as usual.

16. A process of treating cellulose acetate which comprises subjectin the same to the action of a 50% solution of erric chloride for approximately one hour at 40 to 60 0., removing the excess ferric chloride solution, then washing the acetate with warm water, again washing, with cold Watef containing ammonia, then'treating the thus washed material with a natural dye'extract and finally subjecting the dyed material to the usual washing operations.

7. A process of treating cellulose acetate washing wi subjecting the dyed material to the usual washing operations.

18. A process of treating cellulose acetate which comprises subjecting the same to-the action of a 50% solution of ferric chloride for approximately one hour at 40 to 60 C., re-

moving the excess ferric chloride solution, then washin the acetate with water, again t h cold water containing ammonia, then treatin the thus washed material with the regu ar logwood black bath in soap for one hour at approximately 70 C.

19. A process of treating a mixed fabric containing wool and cellulose acetate which comprises subjecting said fabric to the action of a 50% solution of ferric chloride for approximately 1 hour at 4.0 to 60 C.

20. A process of treating a mixed fabric of wool and cellulose acetate which comprises subjecting said fabric to the action of a 50% solution of ferric chloride for approximately 1 hour at 40 to 60 (3., removing the excess ferric chloride solution, then washing the fabric with water, again washing with cold water containing ammonia, then treating the thus washed fabric with 10 wood extract and thereafter subjecting the yed fabric to the usual washing operations.

21. Cellulose acetate having 1.82% of iron fixed therein by treating the cellulose acetate with a 50% solution of ferric chloride.

22. Cellulose acetate havin 1.82% of iron fixed therein and dyed with ogwood extract thereon.

23. A mixed fabric containing wool and cellulose acetate having 1.82% iron fixed therein.

In testimony whereof, they have hereunto subscribedtheir names.

GEORGE RIVAT. ERNEST CADGENE. I CAMILLE DREYFUS.