US2010324A - Treatment of fiber and the product - Google Patents

Treatment of fiber and the product Download PDF

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Publication number
US2010324A
US2010324A US620735A US62073532A US2010324A US 2010324 A US2010324 A US 2010324A US 620735 A US620735 A US 620735A US 62073532 A US62073532 A US 62073532A US 2010324 A US2010324 A US 2010324A
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lead
fiber
solution
basic
silk
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US620735A
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Bruno E Roetheli
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    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D06M11/20—Halides of elements of Groups 4 or 14 of the Periodic Table, e.g. zirconyl chloride
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S8/00—Bleaching and dyeing; fluid treatment and chemical modification of textiles and fibers
    • Y10S8/92—Synthetic fiber dyeing
    • Y10S8/921—Cellulose ester or ether

Definitions

  • the invention provides on the fiber or fabric insoluble compounds of lead in commercially useful amounts, whereby the weight thereof is increased and a variable delustering effect is attained to the extent desired by the operator.
  • Preliminary treatment with tin has, however, a highly deteriorating effect on silk and rayon, decreasing both the tensile strength and the elasticity of fibers processed in this manner.
  • the present invention provides an improved and practical method for the Weighting and delustering of natural and artificial silks directly with a lead compound. The necessity for any preliminary treatment of the fibers is dispensedwith, and the deteriorating effect on the fiber of such preliminary treatment is avoided. The process results in a much improved weighting operation and in 'a decidedly superior product.
  • the solvent employed for the lead compound must be one, such as water, which does not affect the fiber deleteriously.
  • suitable lead compounds may be mentioned the water-soluble acetate and the nitrate, the acetate being preferable because of its greater solubility in water.
  • the desired basic lead solution may be obtained by the action of -alkalis such as ammonia, sodium hydroxide or potassium hydroxide on a solution of neutral or slightly acidic acetate of lead. or by dissolving oxides of lead in a solution of neutral or slightly acidic acetate of lead, the latter method being preferable.
  • -alkalis such as ammonia, sodium hydroxide or potassium hydroxide
  • dissolving oxides of lead in a solution of neutral or slightly acidic acetate of lead the latter method being preferable.
  • strong bases such as sodium hydroxide. or potassium hydroxide
  • concentrations of alkali which, with the lead compound, will furnish the maximum amount of lead in basic solution.
  • the most favorable degree of basicity for the practice of my invention varies somewhat according to the nature of the fiber to be treated. This applies especially to artificial silk fibers, depending upon the process by which they have been manufactured. Thus artificial silk produced by the viscose process, the nitrocellulose process, the cupro-ammoniu'm process or ester types such as cellulose acetate, require each a somewhat different degree of basicity for best results.
  • the preferred basicity in any particular case is readily determined in practice.
  • the fibers or fabrics to be weighted, or weighted and delustered, are immersed in a basic solution of a lead salt, preferably a basic solution of lead acetate, the basicity of which varies according to the type of fiber treated. I have obtained excellent results with a pH of eight or slightly higher.
  • the solution may be either cold or warm, and the time of immersion for best results is about 30 minutes.
  • the excess of solution is then removed in the .usual manner, by centrifugal machines or otherwise, and the fibers or fabrics are rinsed thoroughly in cold water.
  • the wash waters may be collected for the purpose of recovering the lead lost in the washing operations.
  • the fibers or fabrics are treated in a so-called fixing bath, the purpose of which is to transform all lead compounds retained by the fibers or fabrics which may still contain acid and be partly soluble, into non-irritating compounds of lead which are insoluble in water and the secretions of the human body.
  • fixing baths solutions of various chemicals which are capable of producing insoluble lead compounds may be used. Mild alkalis may be used, such as carbonates, phosphates, or silicates of alkali metals, the phosphates having been found in general to be the best.
  • the material is usually rinsed again, but this is not indispensable.
  • the fixing bath restores to the partially-weighted fibers or fabrics the ability to take up additional quantities of lead from the basic lead solution.
  • the additional lead taken up is rendered insoluble by another fixing treatment, and the complete cycle of operations, i. e., basic lead solution, rinse and fixing, may be repeated, until the desired amount of weighting is accomplished.
  • a final bath of silicate of soda may be'used, but this is not essential.
  • the dyeing of fibers or fabrics weighted by my process may be carried out in the usual manner.
  • Fibers and fabrics weighted by my process vary in appearance, especially in lustre, according to the degree of basicity used in the lead solution, higher basicity resulting in general in greater reduction of the natural lustre of the fiber. This is particularly true of artificial silk. I am thus able to control the delustering effect by control of the basicity of the lead solution.
  • My product possesses greater tensile strength, elasticity and durability than materials weighted by the usual tin weighting process, or by processes requiring substantial previous applications of tin or other metal salts.
  • My preferred product is a silk weighted to the desired extent with a lead compound only.
  • Neutral or acid solutions of lead are capable in normal operation of weighting silk fibers only to a very minor extent.
  • U. S. Patent No. 1,845,037 to Clavel for example, it has been suggested to pass silk through a phosphate bath and then to pass it without previous washing into a solution of a metallic salt such as stannic chloride or lead acetate.
  • Such treatment with neutral lead solutions is capable in normal operation of weighting silk fibers only up to about 30%.
  • my process I am able to produce fibers weighted with lead, in the absence of other metal, to any desired extent up to more than two hundred per cent of the weight of the fiber.
  • silk unless specifically limited to natural or artificial. silk, is intended to include both natural silk and/or artificial silk, and the term fiber" includes both the fiber and the fabric manufactured therefrom.
  • a process of weighting silk fiber with lead which comprises treating a fiber which is free from other weighting metals with a solution containing a basic substance and a lead compound, said solution having a basic reaction, and subsequently treating the fiber to fix a water-insoluble lead compound thereon.
  • a process of weighting fiber with lead which comprises treating a fiber which is free from other metal with a solution of a lead compound, said solution containing a substance imparting a basic reaction thereto, and subsequently treating the fiber to fix thereon a water-insoluble lead compound.
  • a process of weighting silk fiber with lead which comprises treating a fiber which is free from other metal with an aqueous solution containing a weak alkali and a water-soluble lead compound, said solution having a basic reaction, whereby a soluble basic lead compound is deposited upon the fiber, and then treating the fiber to convert the said soluble basic lead compound into a water-insoluble lead compound.
  • a process of weighting silk fiber with lead which comprises treating a silk fiber which is free from other weighting metals with a solution of a water-soluble lead compound, said solution having a pH of approximately 8, whereby a water-soluble basic lead compound is deposited upon the fiber, and then treating the fiber to convert the said water-soluble lead compound into a water-insoluble lead compound.
  • a process of weighting silk fiber with lead which comprises treating a silk fiber which is free from other weighting metals with a solution of a water-soluble lead compound, said solution containing a weak alkali and having a basic reaction, whereby a water-soluble basic lead compound is absorbed by the fiber, and washing the fiber with water to convert the said water-soluble lead compound into a water-insoluble lead compound, and converting the said insoluble compound at least in part to lead phosphate.
  • a process of weighting silk fiber with lead which comprises preparing an aqueous solution of lead acetate and adding thereto a substance imparting a basic reaction, thereby providing a basic solution of lead acetate, and immersing silk fiber which is free from tin in the resulting solution, whereby a water-soluble basic lead acetate adheres to the silk fiber, then washing the fiber with water and thereby precipitating a waterins'oluble basic lead acetate on the fiber.
  • a process of weighting silk fiber with lead which comprises immersing a fiber which is free from other metal in an aqueous solution containing lead acetate and ammonium hydroxide, said solution having a basic reaction, removing the silk and treating the same with a phosphate solution to precipitate on the fiber a water-insoluble phosphate.
  • a processor weighting silk fiber with lead which comprises immersing a fiber which is free from other weighting metal in an aqueous solution containing lead acetate and lead oxide, said solution having the basic reaction, removing the silk and treating the same with an alkaline solution to precipitate on the fiber a water-insoluble lead compound.
  • a textile fiber weighted with lead and tree from other weighting metal said lead being deposited on the fiber by immersion of the fiber in a basic solution of a lead compound and being fixed thereon by subsequent treatment to convert the lead absorbed by the fiber into a water-insolubie lead compound.
  • a process of weighting fiber with lead which comprises preparing a solution of a lead compound and adding to the said solution a basicity-imparting substance, thereby providing in solution lead ions and sufilcient hydroxyl ions to impart a basic reaction to the solution, immersing in the solution a fiber the natural afiinity mersing silk fiber which is free from other weighting metal in the resulting solution, whereby a water-soluble basic lead compound is absorbed by the silk fiber, and then treating the, fiber to fix a water-insoluble lead compound thereon.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Description

Patented Aug. 6, 1935 PATENT OFFICE TREATMENT OF FIBER AND THE PRODUCT Bruno E. Roetheli, Boston, Mass.
No Drawing. Application July 2, 1932, Serial No. 620,735
11 Claims.
products of this nature, and to produce an improved natural and/or artificial silk product.
The invention provides on the fiber or fabric insoluble compounds of lead in commercially useful amounts, whereby the weight thereof is increased and a variable delustering effect is attained to the extent desired by the operator.
Various proposals have been made for the weighting of silk fibers, principally by the use of tin compounds. It has heretofore been believed to be impossible to accomplish any considerable weighting with lead compounds without a preliminary treatment of the materials by the application of tin or other metal salts, or other preliminary treatment to create in the fibers a special affinity for lead. In U. S. Patent No. 1,579,628 to Berg, et al., for example, it has been suggested to subject silk fibers to substantial weighting with tin to create in the fiber an affinity for lead, and then to treat the fiber with a soluble lead compound. Preliminary treatment with tin, has, however, a highly deteriorating effect on silk and rayon, decreasing both the tensile strength and the elasticity of fibers processed in this manner. The present invention provides an improved and practical method for the Weighting and delustering of natural and artificial silks directly with a lead compound. The necessity for any preliminary treatment of the fibers is dispensedwith, and the deteriorating effect on the fiber of such preliminary treatment is avoided. The process results in a much improved weighting operation and in 'a decidedly superior product.
I have discovered that lead in substantial amounts is readily accepted by .natural and/or artificial silk fibers, without the necessity for any preparatory treatment to create in the fiber a special affinity for lead, if the'lead is applied in the form of a basic solution of a lead compound. I have found the basicity of the lead solution with which the fiber is treated to be the only agency necessary to cause the fiber to take up substantial amounts of lead and to create the desired affinitybetween thefiber and the lead. Ihave further found that by varying the basicity the degree of delustering of artificial silk may be controlled. The basic lead compound itself may be dissolved in a suitable solvent, or neutral or slightly acid lead compounds may be dissolved and the solution then made basic to the extent desired in accordance with principles hereinafter set forth. The solvent employed for the lead compound must be one, such as water, which does not affect the fiber deleteriously. As examples of suitable lead compounds may be mentioned the water-soluble acetate and the nitrate, the acetate being preferable because of its greater solubility in water.
The desired basic lead solution may be obtained by the action of -alkalis such as ammonia, sodium hydroxide or potassium hydroxide on a solution of neutral or slightly acidic acetate of lead. or by dissolving oxides of lead in a solution of neutral or slightly acidic acetate of lead, the latter method being preferable. In the use of strong bases such as sodium hydroxide. or potassium hydroxide, care should obviously be taken to use concentrations of alkali which, with the lead compound, will furnish the maximum amount of lead in basic solution. As the principle of operation of my invention requires the presence in solution of lead ions and a sufficient quantity of hydroxyl ions to impart a basic reaction to the solution, it is obvious that only those bases and/or concentrations thereof which provide those ions in solution should be used and bases and/or concentrations thereof which cause precipitation of 'either or both of those ions are undesirable to the extent that such precipitation occurs.
The most favorable degree of basicity for the practice of my invention varies somewhat according to the nature of the fiber to be treated. This applies especially to artificial silk fibers, depending upon the process by which they have been manufactured. Thus artificial silk produced by the viscose process, the nitrocellulose process, the cupro-ammoniu'm process or ester types such as cellulose acetate, require each a somewhat different degree of basicity for best results. The preferred basicity in any particular case is readily determined in practice.
Generally speaking, the higher the basicity used,
the more the natural lustre of the fiber or fabric is reduced. The delustering effect of the more basic solutions is especially useful in the processing of artificial silk goods, in which case the undesirable glossy appearance of the fiber or fabrics is eliminated, either in part or entirely,
according to the basicity of the lead solution used. As an example of the practice of my process, I may proceed as follows:
The fibers or fabrics to be weighted, or weighted and delustered, are immersed in a basic solution of a lead salt, preferably a basic solution of lead acetate, the basicity of which varies according to the type of fiber treated. I have obtained excellent results with a pH of eight or slightly higher. The solution may be either cold or warm, and the time of immersion for best results is about 30 minutes. The excess of solution is then removed in the .usual manner, by centrifugal machines or otherwise, and the fibers or fabrics are rinsed thoroughly in cold water. The wash waters may be collected for the purpose of recovering the lead lost in the washing operations.
After washing, the fibers or fabrics are treated in a so-called fixing bath, the purpose of which is to transform all lead compounds retained by the fibers or fabrics which may still contain acid and be partly soluble, into non-irritating compounds of lead which are insoluble in water and the secretions of the human body. For such fixing baths solutions of various chemicals which are capable of producing insoluble lead compounds may be used. Mild alkalis may be used, such as carbonates, phosphates, or silicates of alkali metals, the phosphates having been found in general to be the best.
After the fixing bath the material is usually rinsed again, but this is not indispensable. Besides producing the required insolubility of the lead compound, the fixing bath restores to the partially-weighted fibers or fabrics the ability to take up additional quantities of lead from the basic lead solution. After further immersion in the basic lead solution, the additional lead taken up is rendered insoluble by another fixing treatment, and the complete cycle of operations, i. e., basic lead solution, rinse and fixing, may be repeated, until the desired amount of weighting is accomplished. A final bath of silicate of soda may be'used, but this is not essential.
The dyeing of fibers or fabrics weighted by my process may be carried out in the usual manner.
Fibers and fabrics weighted by my process vary in appearance, especially in lustre, according to the degree of basicity used in the lead solution, higher basicity resulting in general in greater reduction of the natural lustre of the fiber. This is particularly true of artificial silk. I am thus able to control the delustering effect by control of the basicity of the lead solution.
My product possesses greater tensile strength, elasticity and durability than materials weighted by the usual tin weighting process, or by processes requiring substantial previous applications of tin or other metal salts.
My preferred product is a silk weighted to the desired extent with a lead compound only. Neutral or acid solutions of lead are capable in normal operation of weighting silk fibers only to a very minor extent. In U. S. Patent No. 1,845,037 to Clavel, for example, it has been suggested to pass silk through a phosphate bath and then to pass it without previous washing into a solution of a metallic salt such as stannic chloride or lead acetate. Such treatment with neutral lead solutions, however, in the 'absence of preliminary treatment of the fiber with tin, is capable in normal operation of weighting silk fibers only up to about 30%. By my process I am able to produce fibers weighted with lead, in the absence of other metal, to any desired extent up to more than two hundred per cent of the weight of the fiber.
As stated above, no treatment with tin or other compounds preliminary to the treatment with basic lead salt solution is necessary in the practice of my invention. Such tin or other treatment may, however, be given to the fibers without interfering with the treatmentwith basic lead solutions in accordance with my invention. I therefore claim a process in which the basicity of the lead solution with which the fiber is treated is utilized as the substantial and material factor for causing the fiber to take up lead, whether or not the fiber is subjected to a minor or superficial treatment with tin or other compounds which does not materially affect the afiinity of the fiber for basic lead salts and leaves such fiber substantially free from weighting metal prior to the basic lead treatment. I also claim a product which is weighted principally by treatment with basic lead compounds, although it may contain minor amounts of tin.
In the appended claims the term silk, unless specifically limited to natural or artificial. silk, is intended to include both natural silk and/or artificial silk, and the term fiber" includes both the fiber and the fabric manufactured therefrom.
What I claim is:
1. A process of weighting silk fiber with lead which comprises treating a fiber which is free from other weighting metals with a solution containing a basic substance and a lead compound, said solution having a basic reaction, and subsequently treating the fiber to fix a water-insoluble lead compound thereon.
2. A process of weighting fiber with lead which comprises treating a fiber which is free from other metal with a solution of a lead compound, said solution containing a substance imparting a basic reaction thereto, and subsequently treating the fiber to fix thereon a water-insoluble lead compound.
3. A process of weighting silk fiber with lead which comprises treating a fiber which is free from other metal with an aqueous solution containing a weak alkali and a water-soluble lead compound, said solution having a basic reaction, whereby a soluble basic lead compound is deposited upon the fiber, and then treating the fiber to convert the said soluble basic lead compound into a water-insoluble lead compound.
4. A process of weighting silk fiber with lead which comprises treating a silk fiber which is free from other weighting metals with a solution of a water-soluble lead compound, said solution having a pH of approximately 8, whereby a water-soluble basic lead compound is deposited upon the fiber, and then treating the fiber to convert the said water-soluble lead compound into a water-insoluble lead compound.
5. A process of weighting silk fiber with lead which comprises treating a silk fiber which is free from other weighting metals with a solution of a water-soluble lead compound, said solution containing a weak alkali and having a basic reaction, whereby a water-soluble basic lead compound is absorbed by the fiber, and washing the fiber with water to convert the said water-soluble lead compound into a water-insoluble lead compound, and converting the said insoluble compound at least in part to lead phosphate.
6. A process of weighting silk fiber with lead which comprises preparing an aqueous solution of lead acetate and adding thereto a substance imparting a basic reaction, thereby providing a basic solution of lead acetate, and immersing silk fiber which is free from tin in the resulting solution, whereby a water-soluble basic lead acetate adheres to the silk fiber, then washing the fiber with water and thereby precipitating a waterins'oluble basic lead acetate on the fiber.
7. A process of weighting silk fiber with lead which comprises immersing a fiber which is free from other metal in an aqueous solution containing lead acetate and ammonium hydroxide, said solution having a basic reaction, removing the silk and treating the same with a phosphate solution to precipitate on the fiber a water-insoluble phosphate.
8. A processor weighting silk fiber with lead which comprises immersing a fiber which is free from other weighting metal in an aqueous solution containing lead acetate and lead oxide, said solution having the basic reaction, removing the silk and treating the same with an alkaline solution to precipitate on the fiber a water-insoluble lead compound.
9. A textile fiber weighted with lead and tree from other weighting metal, said lead being deposited on the fiber by immersion of the fiber in a basic solution of a lead compound and being fixed thereon by subsequent treatment to convert the lead absorbed by the fiber into a water-insolubie lead compound.
10. A process of weighting fiber with lead which comprises preparing a solution of a lead compound and adding to the said solution a basicity-imparting substance, thereby providing in solution lead ions and sufilcient hydroxyl ions to impart a basic reaction to the solution, immersing in the solution a fiber the natural afiinity mersing silk fiber which is free from other weighting metal in the resulting solution, whereby a water-soluble basic lead compound is absorbed by the silk fiber, and then treating the, fiber to fix a water-insoluble lead compound thereon.
BRUNO E. ROE'I'HELI.
US620735A 1932-07-02 1932-07-02 Treatment of fiber and the product Expired - Lifetime US2010324A (en)

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