US1816959A - Bene clg - Google Patents

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US1816959A
US1816959A US1816959DA US1816959A US 1816959 A US1816959 A US 1816959A US 1816959D A US1816959D A US 1816959DA US 1816959 A US1816959 A US 1816959A
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silk
weighting
bath
acid
solution
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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 System, e.g. zirconyl chloride
    • 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
    • D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • D06M11/70—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
    • D06M11/71—Salts of phosphoric acids
    • 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
    • Y10S8/916—Natural fiber dyeing
    • Y10S8/917—Wool or silk

Definitions

  • This invention relates to a method of weighting natural silkwith metallic compounds.
  • lhe precipitated stannic acid is then fixed by treating the silk with a solution of di-sodium phosphate of about 6 per cent. strength, at a tempera ture of about 60 G.
  • the tin-salts and phosphate treatments are repeated alternately until the desired weighting has been obtained, and after each bath the silk must undergo a thorough washingor neutralization.
  • the silk may be treated with a solution of sulphate of alumina, and, after subsequent washing, with a solution oi water glass at a temperature of about 50 C.
  • the silk which has been treated in this manner, and weighted with complex compounds of tin, phosphate and water glass,
  • the weighting ofnatural silk is considerably simplified and less expensive, when care is taken that the metal salts come in contact with thesilk only at a certain high acid concentration or in other words that the metal salts are acting upon the silk only in thepresence of acids or acid salts.
  • the acids or acid salts necessary for obtaining the high acid concentration may be added to the metal salt bath for example a tin tetrachloride solution or the silk may be treated with acids or acid salts before taking it into the metal salt bath.
  • the natural silk treated in such a manner with metal salts may then be brought without previous washing-i1 desired after squeezing for removal oi the excess of tin tetrachloride solution into the following phosphate bath.
  • rotective holloids such as glue, gelatine, al umin or the like.
  • protective colloids may be If one uses, however, in accordance brought upon the silk either before bringingit into the acid tin salt solution for example by coating or impregnation if desired together with the, acid substances, for example acids, ormay be added to the tin salt bath.
  • the silk is sulhciently weighted after only a very short treatment.
  • the precipitation reactions which are necessary for perfect weighting and cannot occur in the bath on account or" the high acid concentration, or the presence of the protective colloids, if desired at high acid concentration, occur on the fibre immediately. It is there fore possible to produce weightings, which are-satisfactory and of good quality by a simple application of the solution, such as by remote for example of a solution of ammonium carbonate, can if required also contain dyestuds which contain tanning substances, such as haematein.
  • Example 1 Siliconk fabricswhich have not been boiled oil" are placed on a finishing machine and drawn for example three times through a solution containing the following ingredients: 5 litres of tetrachloride of tin of Baum litre of concentrated orthophosphoric acidan'd 1 litre of a solution of aluminum sulphate of 10 per cent strength.
  • the weighting is completed by a subsequent treatment at a temperature of 60 C. with solution of water glass of 4 Baum.
  • the weighting bath contains the following ingredients 6 litres of solution of tetrachloride of tin of 22 Baum, 1 litre of concentrated formic acid, 1 litre of neutral solution of water glass of 4 Baum, 120 grams of sodium phosphate, together with 100 grams of glue dissolved in 2 litres of water.
  • Boiled ofi' silk after treatment in this weighting bath is pressed, drawn through a solution of ammonium carbonate of 10 per cent strength, and dried.
  • the silk is washed in a soap bath to which haematein hasbeen added, and then dyed.
  • E sample 3.-A crepe de Chine texture consisting of natural silk is drawn in full breadth through a 1% solution of phosphoric acid containing 12 gr. glue per litre. The piece is then drawn through 4 tin chloride baths containing tin tetrachloride solution of Be. The piece then passes a squeezer and enters first a 10% mono-sodium phosphate bath and then a 6% bi-sodium phosphate bath. After the passage ofthe alkaline phosphate bath the silk goes through .a hydro-extractor and is finished in halfan hour in a water glass solution of at least 1 B. at C. which contains 1 gr. soap per litre.
  • Example 4 Si lk skeins are dipped for a short time into a 10% solution of mono-chloroacetic acid. One lets'the skeins drain and brings them then into atin tetrachloride bath of 35 B. The skeins are dipped into this metal salt bath for a shorttime, drawn out again and left in the air for a short time. This process is repeated it necessaryseveral times. The skeins are then carefully hydroextracted and brought for a short time into l1? compounds containing acid compounds, and
  • the skeins are finished by a short treatment in a soap containingcwater glass solution of at least 1 B, at
  • Silk which is weighted in accordance withthis invention does not lose in elasticity or strength and has full brilliancy. Owing to the short treatment in the baths containing several weighting agents the appearance of the silk is considerably improved.
  • the economical advantages of the new process are extraordinarily great, the number of weighting baths is as far as possible reduced to a minimum, the washing and neutralization after each bath is rendered superfluous, and the transport of the silk from one bath to another is avoided.
  • a further advantage ' consists in the fact that owing to the elimination of the washing, acidifying and neutralization, there are not obtained diluted solutions of the weighting substances, or of the transformed products produced by the neutralization, the recovery of which substances or products entails considerable expense and special installations.
  • a further advantage of the invention is that when weighting in the piece on the usual finishing machine, the piece can be drawn through the solutions stretched to their full width, either singly or superimposed on each other, and in this manner the troublesome creases and spots on the silks which often arise in consequence of the washing not having been properly carried out, or other defects, are avoided.
  • a method of weighting natural silk which comprises the steps of treating the silk successively with solutions of acid compounds, aqueous solutions of heavy metal compounds, and aqueous solutions of precipitating agents for the heavy metal compounds 3 taken up by the silk.
  • a method of weighting natural silk which comprises the steps of treating the silk successively with solutions of acid compounds, aqueous solutions of heavy metal aqueous solutions of precipitating agents for the heavy metal compounds taken up by the silk.
  • a method of weighting natural silk which comprises the steps of treating the silk with aqueous solutions of heavy metal compounds in presence of acid compounds and then transferring the silk directly, without washing, neutralizing or acidifying it, into 1 the following weighting bath.
  • a method of weighting natural silk which comprises the steps .of treating the silk with aqueous solutions of heavymetal compounds in presence of acid compounds, squeezing it, and then transferring 1t d1- rectly, without washing, neutralizing or acidifying it, into an aqueous solution of alkali-metal phosphate.
  • a method of weighting natural silk which comprises the steps of treating the silk with solutions of heavy metal compounds in presence of acid compounds and protective colloids, squeezing it andthen transferring it directly, without washing, neutralizing or acidifying it, into an aqueous solution of alkali-metal phosphate.
  • a method of weighting naturall silk which comprises the steps of treating the silk with solutions of tin tetrachloride in presence of acid compounds and protective colloids, squeezing it and transferring it directly, without washing, neutralizing or acidifying it, into an aqueous solution of alkali-metal phosphate.
  • a method of weighting natural silk which comprises the step of treating the silk in a single bath containing in aqueous solution a heavy metal compound, an acid compound,,and a P o -compound.
  • a method of weighting natural silk which comprises the step of treating the silk in a single bath containing tin tetrachloride and phosphoric acid.
  • a method of weighting natural silk which comprises the step of treating the silk in a single bath containing in aqueous solution a. heavy metal compound, an acid compound and protective colloids.
  • a method accordinging to claim 3 in which the precipitation treatment of the silk is followed by a squeezing and a treatment with an aqueous solution of ammonium carbonate.
  • a method of weighting natural silk which comprises the steps of treating the silk with aqueous solutions of heavy metal compounds in presence of organic acids, and precipitating without washing, neutralizing or acidifying the silk, the heavy metal com pounds taken up by the silk as compounds insoluble in water.
  • a method of weighting natural silk which comprises the' steps of successively treating the silk with an aqueous solution of tin tetrachloride in presence of organic acids, and without washing, neutralizing or acidifying the silk with an aqueous solution of primary sodium phosphate.

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

Description

Arne? iris-@1 Patented 4, 1931 re uses RENE GLAVEL, 9F BASEL, SWITZERLAEQ'D WEIGHTING NATURAL SILK fie brewing. Application fil ed May 16, 1927, Serial No. 191,941, and in Germany September 17, 3.928.
This invention relates to a method of weighting natural silkwith metallic compounds.
Hitherto, in processes for weighting silk,
ii a number of substances have been brought m and neutralized.
temperature for rather a long time, say for about an hour or two, and then thoroughly washed with water, in order to hydrolize the tin-salts on the fibre! lhe precipitated stannic acid is then fixed by treating the silk with a solution of di-sodium phosphate of about 6 per cent. strength, at a tempera ture of about 60 G. The tin-salts and phosphate treatments are repeated alternately until the desired weighting has been obtained, and after each bath the silk must undergo a thorough washingor neutralization. fAiter the last phosphate bath the silk may be treated with a solution of sulphate of alumina, and, after subsequent washing, with a solution oi water glass at a temperature of about 50 C. The silk which has been treated in this manner, and weighted with complex compounds of tin, phosphate and water glass,
' is then washed with soap, rinsed and soured.
The method oi weightin which is described above, as well as :ot or methods of wei 'htingwith various substances, wastes rnuc time, on account of the number of baths, and the washing, acidification or neutralization which is necessary between each bath. Such methods are also very expensive, and their disadvantages are not to be overccrueby the use of the modern weighting centrifuges. The greatest of these disadvantages 1s theserious loss of material which is caused by the many washing and neutralization processes, and the troublesome and expensive processes which are necessary for the recovery of the weighting substances from the waste liquors.
According to the invention the weighting ofnatural silk is considerably simplified and less expensive, when care is taken that the metal salts come in contact with thesilk only at a certain high acid concentration or in other words that the metal salts are acting upon the silk only in thepresence of acids or acid salts. The acids or acid salts necessary for obtaining the high acid concentration may be added to the metal salt bath for example a tin tetrachloride solution or the silk may be treated with acids or acid salts before taking it into the metal salt bath. The natural silk treated in such a manner with metal salts may then be brought without previous washing-i1 desired after squeezing for removal oi the excess of tin tetrachloride solution into the following phosphate bath. .Due to the high acid concentration present during the metal salt treatment, the silk undergoes a change and the tin chloride probably forms a compound with the silk, in which it is hydrolized. However, in no .case undesired precipitations take place in the phosphate bath and the tin salt on the fibre combines with the phosphate into a tin-phosphate compound, probably Sn (HPOQQ, adapted and necessary for wei 'hting sil when treating silk with a tin chloride solution without the-presence of acids or acid salts it is not possible to bring the silk treated with the metal salts into the following phosphate bath without previous washing of the silk, to hydrolize the tin chloride; There would occur in the phosphate bath and upon the silk precipitations of tin salts which are not adapted for weighting purposes, make the silk turbid, cloudy and milky and produce spots. with the invention tin salt bathswith increased acid concentration, undesired precipitations do not occur, the silk is abundantly weighed, looks unobjectionable, and shows no s ots.
111 order to prevent the silk from being attacked too much by the increased acid concentration it is advisable to use rotective holloids such as glue, gelatine, al umin or the like. These protective colloids may be If one uses, however, in accordance brought upon the silk either before bringingit into the acid tin salt solution for example by coating or impregnation if desired together with the, acid substances, for example acids, ormay be added to the tin salt bath.
it is also possible to treat the silk before bringing it into the metal salt bath with acid substances such as acids or acid salts and to ke' thispretreatment in presence of protective colloids. The acid concentration may then be kept lower in the metal salt bath or the addition of acids or acid salts may be renounced. Also in these cases a change of the.
silk fibres takes place, which produces a more intensive and more equal taking up of the weighting means. 1 Experiments show the surprising fact, that silks of difi'erent origin took up equal amounts of weighting substances. The weighting of the silk is then carried through by passing the silkthrough one or only a few weighting baths, in which the skeins or textures only had to remain a and unsuitabletin compounds take place, be-
cause theba'th has an increased acid cone-en tration. In this case it is advisable to use instead of phosphates, phosphoric acid, which serves a double purpose namely to produce the tin-phosphate cqmpound and to increase the acid concentration. Here too the addition of protective colloids is advisable, be
cause they do not only protect the silk but also help in-preventing the precipltation of unsuitable tin compounds. It is even possible to addsolutions or" water glass, which is a'substance used in the tin weighting proc ess to the weighting bath containing tin salt 7 and phosphate at increased acid concentration, thus carrying the entire weighting process through with a single bath.
if one treats the silk with weighting baths according to the present invention, using 7 proper concentration of the bath and a suitable temperature, the silk is sulhciently weighted after only a very short treatment. The precipitation reactions which are necessary for perfect weighting and cannot occur in the bath on account or" the high acid concentration, or the presence of the protective colloids, if desired at high acid concentration, occur on the fibre immediately. It is there fore possible to produce weightings, which are-satisfactory and of good quality by a simple application of the solution, such as by remote for example of a solution of ammonium carbonate, can if required also contain dyestuds which contain tanning substances, such as haematein.
The following examples illustrate the invention:
Example 1.Silk fabricswhich have not been boiled oil" are placed on a finishing machine and drawn for example three times through a solution containing the following ingredients: 5 litres of tetrachloride of tin of Baum litre of concentrated orthophosphoric acidan'd 1 litre of a solution of aluminum sulphate of 10 per cent strength.
The weighting is completed by a subsequent treatment at a temperature of 60 C. with solution of water glass of 4 Baum.
Ermmple 2.-The weighting bath contains the following ingredients 6 litres of solution of tetrachloride of tin of 22 Baum, 1 litre of concentrated formic acid, 1 litre of neutral solution of water glass of 4 Baum, 120 grams of sodium phosphate, together with 100 grams of glue dissolved in 2 litres of water. V
Boiled ofi' silk after treatment in this weighting bath is pressed, drawn through a solution of ammonium carbonate of 10 per cent strength, and dried. The silk is washed in a soap bath to which haematein hasbeen added, and then dyed.
E sample 3.-A crepe de Chine texture, consisting of natural silk is drawn in full breadth through a 1% solution of phosphoric acid containing 12 gr. glue per litre. The piece is then drawn through 4 tin chloride baths containing tin tetrachloride solution of Be. The piece then passes a squeezer and enters first a 10% mono-sodium phosphate bath and then a 6% bi-sodium phosphate bath. After the passage ofthe alkaline phosphate bath the silk goes through .a hydro-extractor and is finished in halfan hour in a water glass solution of at least 1 B. at C. which contains 1 gr. soap per litre.
Example 4.Si lk skeins are dipped for a short time into a 10% solution of mono-chloroacetic acid. One lets'the skeins drain and brings them then into atin tetrachloride bath of 35 B. The skeins are dipped into this metal salt bath for a shorttime, drawn out again and left in the air for a short time. This process is repeated it necessaryseveral times. The skeins are then carefully hydroextracted and brought for a short time into l1? compounds containing acid compounds, and
a 1.5% mono-sodium phosphate solution. After squeezing or hydro-extraction of the liquid if desired after washing, the skeins are finished by a short treatment in a soap containingcwater glass solution of at least 1 B, at
Silk which is weighted in accordance withthis invention does not lose in elasticity or strength and has full brilliancy. Owing to the short treatment in the baths containing several weighting agents the appearance of the silk is considerably improved. The economical advantages of the new process are extraordinarily great, the number of weighting baths is as far as possible reduced to a minimum, the washing and neutralization after each bath is rendered superfluous, and the transport of the silk from one bath to another is avoided. A further advantage 'consists in the fact that owing to the elimination of the washing, acidifying and neutralization, there are not obtained diluted solutions of the weighting substances, or of the transformed products produced by the neutralization, the recovery of which substances or products entails considerable expense and special installations.
A further advantage of the invention is that when weighting in the piece on the usual finishing machine, the piece can be drawn through the solutions stretched to their full width, either singly or superimposed on each other, and in this manner the troublesome creases and spots on the silks which often arise in consequence of the washing not having been properly carried out, or other defects, are avoided.
I claim:
1. A method of weighting natural silk which comprises the steps of treating the silk successively with solutions of acid compounds, aqueous solutions of heavy metal compounds, and aqueous solutions of precipitating agents for the heavy metal compounds 3 taken up by the silk.
2. A method of weighting natural silk which comprises the steps of treating the silk successively with solutions of acid compounds, aqueous solutions of heavy metal aqueous solutions of precipitating agents for the heavy metal compounds taken up by the silk.
3. A method of weighting natural silk which comprises the steps of treating the silk with aqueous solutions of heavy metal compounds in presence of acid compounds and then transferring the silk directly, without washing, neutralizing or acidifying it, into 1 the following weighting bath.
4. A method of weighting natural silk which comprises the steps .of treating the silk with aqueous solutions of heavymetal compounds in presence of acid compounds, squeezing it, and then transferring 1t d1- rectly, without washing, neutralizing or acidifying it, into an aqueous solution of alkali-metal phosphate.
5. A method of weighting natural silk which comprises the steps of treating the silk with solutions of heavy metal compounds in presence of acid compounds and protective colloids, squeezing it andthen transferring it directly, without washing, neutralizing or acidifying it, into an aqueous solution of alkali-metal phosphate.
6. A method of weighting naturall silk which comprises the steps of treating the silk with solutions of tin tetrachloride in presence of acid compounds and protective colloids, squeezing it and transferring it directly, without washing, neutralizing or acidifying it, into an aqueous solution of alkali-metal phosphate.
7. A method of weighting natural silk which comprises the step of treating the silk in a single bath containing in aqueous solution a heavy metal compound, an acid compound,,and a P o -compound.
8. A method of weighting natural silk which comprises the step of treating the silk in a single bath containing tin tetrachloride and phosphoric acid.
9. A method of weighting natural silk which comprises the step of treating the silk in a single bath containing in aqueous solution a. heavy metal compound, an acid compound and protective colloids.
10. A method according to claim 3 in which the precipitation treatment of the silk is followed by a treatment with an aqueous solution of alkaline reacting substances.
11. A method according to claim 3 in which the precipitation treatment of the silk is followed by a squeezing and a treatment with an aqueous solution of alkaline reacting substances.
12. A method ;.according to claim 3 in which the precipitation treatment of the silk is followed by a squeezing and a treatment with an aqueous solution of ammonium carbonate.
13. A method of weighting natural silk which comprises the steps of treating the silk with aqueous solutions of heavy metal compounds in presence of organic acids, and precipitating without washing, neutralizing or acidifying the silk, the heavy metal com pounds taken up by the silk as compounds insoluble in water. 1
14. A method of weighting natural silk which comprises the' steps of successively treating the silk with an aqueous solution of tin tetrachloride in presence of organic acids, and without washing, neutralizing or acidifying the silk with an aqueous solution of primary sodium phosphate.
In testimony whereof I affix my signature.
RENE OLAVEL.
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