US1579628A

US1579628A - Process of weighting fibers and the product thereof

Info

Publication number: US1579628A
Authority: US
Publication date: 1926-04-06
Anticipated expiration: 1943-04-06

Description

April 6 1926. 1,579,628

0. BERG ET AL PROCESS OF WEIGHTING FIBERS AND THE PRODUCT THEREOF Filed Dec. 26, 1922 A B x C @fm ffil Q fl jQfF/Q fi u zmfin 5n (Z4 Wa/er Sod/um Wafer Aluminum W i W fer Wafer Jo/uf/an h P/mp/ml \ju/ v/mfe Glas 17 I 1 mm q wyfl o 0 d lead W512 5m Wa/er Acefaiefoiqfibrz Phw /mte JMutian IN VENTOR 02m) fiery Max fmZwjj A TTORNE Y Patented Apr. 6, 1926.

UNITED STATES PATENT OFFICE.

' OLAV BERG, OF PATERSON, AND MAXIIIHOFF, OF OLIITON, JERSEY.

Application filed December 28, 1922,. Serial Ro. 609,082. v

To all whom it may concern:

Be it known that we, OLAV BERG, a citizen of Norway, and a resident of Paterson, Pas saic County, and State of New Jersey, and MAX IMHoFF, a citizen of the United States,

and a resident of Clifton, Passaic County,

and State of New-Jersey, have invented certain new and useful Improvements in a Process of \Veighting Fibers and the Product Thereof, of which the following is a specification.

This invention relates to the weighting of fibers in general, but more particularly to the weighting of silk; weighting being the term of the art for a process of increasing the size and weight of fiber. ,While the present process is particularly intended for the treatment of natural silk, it is not limited thereto.

Under methods now in vogue and employed in the past, salts of tin, iron, and to a very limited extent, of bismuth and aluminum, have been recognized as the only metal salts which could be used in a practical commercial way for the Weighting of silk.. Of these, only the salts of tin and iron have been employed'generally; and iron only in the case of black or dark colored goods. Heretofore, the extent of weighting has been limited because after a certain amount of weighting material has been taken up, the fiber is injuriously affected. There is a practical limit in the prior art processes to the amount ofmineral matter which the fiber will take up without injuring its physical properties. Usually the result was a compromise between increase in quantity and decrease in qualit While by such known processes it has een possible to add ten percent up to one hundred and thirty percent above pari, above ten percent the efi'ect on the fibers is markedly 1njurious,'tak ing away both elasticity and strength'and mak ing them brittle and tender and subjectto deterioration with age. While the amount of loading permissible in producing commereial Sllk without undue forfeiture of quality varies with the silk and with, the' operator, twenty-five per cent is often considered a practical limlt. 7

The purposes of-the present invention areto improve upon former methods and to provide an inexpensive and: simple method by which it is possible to weight silk or other. fibers to any desired extent 'not only without materially impairing ordestroying, the

essential or desirable qualities thereof, but in fact improving them. Another object is toprovide a new material produced by this process; a material which, in the best embodiment of our invention now known to us, is a fiber possessing all the textile qualities of silk but in which silk substance may be only a minor fraction; the major being composed of tin and lead oxides and P 0 (phosphoric acid) in some form of combination with each other and with the silk substance. The result is a sort of composite fiber which, although silky, flexible and strong, and homogeneous under the microscope, is nevertheless largely mineral matter.

The lead in the-fiber is fixedly'held and is insoluble. The new fiber, although containing in some embodiments as high as two hundred per cent weighting, largely PbO, does not yield lead to boiling vinegar (three per cent acetic acid) or to any of the liquids I l with which, silk is likely to come in in the dye-house or in use.

One phase of the invention relates to the discovery of a method by which there is created in the silk, an aflinity for lead com pounds, making it possible to combine lead compounds with the fibers in such a way as to materially increase its weight and the size of the fiber; that is, so as to give a composite fiber in which a large fraction of the fiber is lead in some form; this composite fibercontact having the desirable properties of ordinary Weighted silk Without its usual disadvantages and having certain new and useful advantages of its own. In this method the silk or other fibrous material is first treated 1 Fi". '1 indicates the preliminary weighting;

an preparational-steps and iin which indicates the subsequent weightingsteps.

A special feature of the 'prelimihary or primary wei hting operations, by which the affinity for e heavier nietallic compounds,

is created, is thatthey may be thesame as "heretofore have been employed in tin-weights ing and like processes, so that the apparatus and the materials now at hand may be eml y ding with'tin may be employed as a first bath,

namely, a solution of tin tetrachloride (stannic chloride) or of pink salt, which .is a combination of tin tetrachloride and ammonium chloride. A solution of sodium stannate has been used in tin weighting. So have potassium or ammonium stannates been used but are not better than Sodium stannate. Any of these'materials used in aqueous sois lution deposit on the silk a certain amount of tin in a. form equivalent to stannic oxide, SnO Y 3 v i I Tlius in Fig. "1 the fibrous material, which in the'case-of silk may be either in' the gum, .de-gummed' or partially de-gummed cond1-- tion and may be in the formof fibers, or woven or knitted fabric, is shown at 5 as passing first into a bath Got a solution of stannic chloride, .(SnCh), then through a wash at 7 of water, then into a fixing bath at i 8, such as of sodium phosphate, (Na HPO 12H O),follo wed by another water wash at 9. -In the first bath, which may be, a cold one, as well known, a certain amount of .weight is added to the fiber andexcess material, stannic chloride and 'HCl, is removed in the first water wash, (which also maybe cold), the latter also apparently having to some'extent a hydrolyzing effect on the tin chloride remaining inthe fiber; breaking it up in a way equivalent to the production oft-iiiv oxide remaining with the fiber and sodium phosphate is the best substance to times. constitute the first stage of our complete hydrochloric acid which goes off with the.

water. I a

In place of sodium phosphate other alkalinesalts or carbonates may be used in what we have termed the fixing bath at 8, the

v temperature of this bath being such asthat heretofore used in the art.- In using a phosphate bath, a large amount of P 0 is taken s far as our present knowledge goes,

process and are designated in the drawings as the A stage.

The next stage in "the process may be either that shown atB or that shown at C in the drawings. The 'stageshown at B is a bath at 10 of aluminum sulphate vfollowed 'bya'water wash at 11. If this is used. it addsfiurther weight to the treated material; the accession in weight being dueto the taking up of A1 0 The stage designated by the drawingsis a bath ofwatemglass The usual solutions used in weight- 1 at 12 followed by a water wash at 13. This stage also adds to'the weight of the treated material; SiO being taken up.

The sta B or the stage C follow after the stage has been repeated as many times as desired. Sometimes both of the stages B and C are utilized after the desired treatment by the stage A, but as far as our process is concerned, the new steps, which we are about to describe as the D stage, may follow directly after the A stage treatment,

after the B stage treatment or after the C stage treatment, (in the latter case whether or not the B stage treatmenthas been used). While our discovery is in the D stage treat.-

for the use of the D stage, and our process therefore comprises some steps preliminary to the D stage. These preliminary steps may. be, as stated, the old and well known operations used in weighting silk. j

lVe have discovered that the A stage treat ments, preparation of the silk is required ment, weighting the fibers with tin salts and fixing them, imparts to the fiber thus treated an affinity. for other metallic compounds. We have found that the fibers can be further weighted to. practically any desired extent by subjecting themto the treatment illustrated diagrammatically in Fig. 2. In the best embodiment of our invention at present known to' us, the further weighting is done suitable soluble lead salt, generally lead acetate.

It is possible to use lead salts for this purpose because of the fact that the preparatory treatments described create in the ma terial the property of taking up lead (PbO) from them. In the embodiment of our in- .vention herein shown and described, we use at 14 a warm solution of lead acetate, which "may be commercial sugar of lead or a more basic acetate. This, followed by a water wash at 15, is the D stage of treatment. This D stage increases the weight of the material usually from 20 per cent to 7 5 'per cent, depending upon the amount of added materials already in the'fiber. The lead acetate furnishes lead which combines or unites with the associated fiber and mineral matters and forms an. insoluble compound. The process may terminate here.

\Ve prefer to follow this treatment by the E stage,- -shown diagrammatically, which is subjecting the fibers toa vwarm bath at 16 containing sodium phosphate, and then giving the fiber a water wash at 17. Sodium phosphate isv the be'st'salt to use at-this stage. A treatment with sodium phosphate much improves the fiber prepared by the present process as so far described.- This E stage not only improves the appearance and the scroop of the fiber. but lmparts to it the property of being able to take up more lead compcunds if it is aga n submerged in. the

.with theaid of lead compounds, using any lead acetate solution at 1%. Thus the D stage may be repeated afterthe 'E stage,- again and again, if desired. The nency. with which the lead is held in the fiberis increased by this phosphate aftertreatment. Y By thus alternately adding weight and creating an afiinity or avidity for further weighting material, it is possible to add to the weight of thefiber at an increasing rate to an extent greatly in excess of what has been possible heretofore.

Whether or not the aluminum sulphate or the sodium silicate treatments (B and C) have been employed up to this point, either or both may be used for 'the purpose of a final weighting and fixing treatment. More over. these B and C treatments impart to the fiber a further aflinity or avidity for the taking up of more lead salts.

As a concrete example, we have found that with a silk treated with three applications of the tin and the phosphate, (the A stage treatment), one hundred pounds of .de-gummed silk fiber which in this stage had added thirty pounds in'weight, with a single treatment by lead acetate and sodium phosphate (the D and E stages) took on an additional sixty-five pounds in weight; a second lead acetate treatment (the D stage) added approximately fifty pounds in weight and with the aflinity or avidity for the lead salts further increasedby the sodium phosphate treatment, (the E stage), an additional sixty pounds in weight was added by a third treatment with the lead acetate (the D stage). Another bath in sodium phosphate after this-put the treated fiber in condition to take up aboutseventy pounds more weight from another bath of lead acetate.

In the present process the weight may be further increased, after'the D and E stages have been repeated as many times as desired, by giving the treated fiber another waterglass bath (the C stage). Such a bath also has the effect of giving'the material a. still further atfinity for more lead compounds.

The process may be carried on so as to 5 .produce practically any desired increase in weight with the'important advantage of effecting increases in weight not only without' injuring the material or causing any substantial deterioration in the mechanical properties or appearance of the fiber either.

immediately,-in subsequent use or from age, but with some actual mprovement in these respects. 1 The: fibers retain their .flexibility gand strength. as'well as their appearance and'their ability to take on dyes or be otherwise .treated.. Dyeing is more even. and better and the elasticityis increased. The

. weighted material, furthermoreQhas" good lasting and wearing qualities, the""desiredv scroop, i-s non-poisonous. and is irggplublem Another important advantage'of the invention is that-this improved lead-weighting process is applicable to such goods as-are already manufactured so that a manufac turer may makeone .quality of goods, for example by spinning or weaving, and by giving such goods different amounts of weight by thisprocess, may make them into any desired number of different grades by weight. Furthermore, a new and useful material is'made by this process. p

The drawing and description which we have made of this invention are for illustrative purposes only as we realize that many variations in the steps and the chemicals employed may be used without departing from the scope of the invention, ,therefore we intend no limitations other than those imposed by the appended claims. In the claims we have not included the water washing steps as it is understood from this disclosure that these follow each bath treatinent.

What we claim is:

' 1. The process of weighting fiber which comprises preliminarily weighting the fiber any known method which in-' with tin 'b eludes the use of a fixing bath, and thereafter treating the fiber with a soluble lead compound.

2. The process of weighting fiber which comprises preliminarily weighting the fiber with tin by any known method which includes the use of a fixing bath, then treat-' mg the fiber with a soluble lead compound,

and thereafter treating the fiber with a fixof a soluble tin compound, treating the same with a soluble phosphate and thereaftertreating the same with a soluble lead compound.

5.- The process of weighting fiber which I comprises treating the fiber witha solution of a soluble tin compound and treating the same with a fixing bath, to render the treated fiber capable of taking up a lead com pound, and thereafter treating thev fiber with asoluble lead compound, then treating the fiber with a soluble phosphate and pound.

6. The process of-weighting'fiber which again-treatingitwith a soluble lead" oomcomprisestreating the fiber with a solution of a tin compound and treating .th'same with a soluble phosphate, to render. -itI capa-..

bleof, taking u'p a lead compound and there after treating it with a soluble lead com pound, then treating it with a soluble phos phate and again treating it w1th a soluble lead compound. r

7. The process of weighting fiber which comprises treating the fiber with soluble tin compounds and soluble lead compounds successively with one or more intercalated treatments with solutions of other weight giving compounds.

8. The process of weighting fiber which comprises mordanting the fiber with a tin compound and thereafter subjecting lt-to the alternate action of baths which contain a soluble lead compound and which contain a soluble phosphate.

9. The process of weightingfiber which comprises 'mordanting the fiber with tin salts, and thereafter subjecting it to repeated successive treatments with [sodium phosphate and lead acetate baths. p

10. The process of weighting fiber whlch comprises treating the fiber with a solution of a soluble tin compound and treating the same with'a fixing bath, to render the treated fiber capable of taking up a lead compound, treating the fiber with a soluble lead compound, then treating the fiber with a soluble'phosphate and then treating the fiber with a water-glass bath.

11 The process of weighting fiber which comprises forming in the fiber compounds containing tin and containing phosphorus to render the same capable of taking up a leadcompound, and thereafter treating it with a'soluble lead compound.

12. The process of weighting "comprises forming in the fiber compounds containing tin and containing phosphorus to render the same capable of taking up a lead compound, treating it with a soluble lead compound and thereafter treating it with a fixing bath.

13. The-process of weighting'fiber which comprises'forming in the fiber compounds containing tin and containing phosphorus to render the same'capable of taking up a lead compound, treating it with a soluble lead compound and thereafter treating it" with a soluble phosphate and then treating it with a water-glass bath.

14:. The process of weighting fiber which comprises forming in the fiber compounds containing tin and containing phosphorus to render the same capable of taking up a lead compound, and thereafter treating it with a soluble lead compound, then treating it with a soluble phosphate, and again treating it with a soluble" lead compound,

followed by another phosphate treatment, gndhthereafter treating it w1th a ,water-glass 15. The process of weighting fiber which fiber which with a fixing bath, to'render the treated fiber capable of taking u a lead compound, treatcompound, thereafter subjecting it to the alternate action of baths which contain a soluble lead compound and which contain a soluble phosphate, and thereafter treating it with a water-glass bath.

17. The process of weighting fiber which comprises treating a fiber which contains tin in fixed and insoluble form with a soluble lead compound.

18. A- textile fiber containing tin an lead y 19. A textile fiber of which at least fifty per cent is tin and lead compounds in fixed compounds in fixed'and insoluble form;

and insoluble form. 20. A textile'fiber containing compounds of tin, lead and phosphorus;

21. A textile fiber containing tin, lead and phosphorus in fixed and insoluble" form.

22. A textile'fiber of which at least fifty per cent s tm', lead and-phosphorus in fixed 23. A textile fiber containing substantial amounts of lead in o'xidized. colorless form, said fiber possessing -'fle'xibility,'- resilience and textile strength ;and said lead being irremo'vablefby the action of warm acetic acid in strength up to live per cent.- 7

24. A textile fiber containing?substantial amounts of tin and of lead in oxidized color less form, said fiber possessing flexibility, resilience and textile strength, and said lead being irremovable by the action of warm acetic acid in strength up to five per cent.

25. A textile fiber containing substantial amounts of tin and of lead and ofphosphorus in oxidized colorless forms, said fiber possessing textile properties and said phosphorus and said lead being irremovable by the actionof warm acetic acid in strength up to five per cent.

26. A textile fiber comprising natural silk containing substantial amounts of tin and of lead in oxidized colorless form, said fiber possessing flexibility, resilience and textile strength, and said lead being irremovable by the action of warm acetic acidin strength up to five per cent.

In witness whereof, I have hereunto set,

December, 1922.

q OLAV BERG. In witness whereof, I have hereunto set my hand this 21" day of December, 1922 MAX IMHoFF.

my hand this 21" day of