US2665966A - Method for insolubilizing spun protein filamentary products - Google Patents

Method for insolubilizing spun protein filamentary products Download PDF

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Publication number
US2665966A
US2665966A US235718A US23571851A US2665966A US 2665966 A US2665966 A US 2665966A US 235718 A US235718 A US 235718A US 23571851 A US23571851 A US 23571851A US 2665966 A US2665966 A US 2665966A
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Prior art keywords
tow
solution
filaments
trough
sodium
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Expired - Lifetime
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US235718A
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English (en)
Inventor
Robin H K Thomson
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Imperial Chemical Industries Ltd
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Imperial Chemical Industries Ltd
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F4/00—Monocomponent artificial filaments or the like of proteins; Manufacture thereof
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/04—Supporting filaments or the like during their treatment
    • D01D10/0436—Supporting filaments or the like during their treatment while in continuous movement

Definitions

  • the present invention relates to a new or improved method for insolubilising artificial filaments, threads, fibres and the like filamentary products obtained by the spinning of solutions of proteins, for instance, peanut protein or. casein, in aqueous alkaline or other suitable aqueous solvent media into suitable acidified. saline coagulating baths.
  • the coagulated filaments can first be passed through a saturatedsodium chloride bath at approximately C. in which they remain until their longitudinal contractility has been greatly reduced. It is filamentary productswhichhave been thus relaxed which are subsequently treated in the twoaforesaid baths.
  • the treating liquid in whichthe filamentary products are thus relaxed will. hereinafter he referred to as relaxing solutions or relaxing treating liquids.
  • British patent specification No. 623,460 describes and claims inter alia a method of treating a continuously advancin tow o1 filaments by immersion in a treating liquid for a relatively long period of time by providing a horizontal ring-trough rotatable about a vertical axis, passing treaung liquid in acontinuous manner through said, ring-trough and rotating the ring-trough with substantially the same directional speed as the mean circular velocity attained by the said treating liquid in said ringtrough, inducing a vibratory motion substantially radial to the centre of the rotating ring-trough in the advancing tow at a position vertically above the treat-mg liquid, permitting the thus treated swaying advancing tow to fall into the treating liquid and to form itself therein into folds on thefioor of the rotating trough immediately below the region where it enters the liquid and also regulating the speed of rotation of the ring-trough so that on withdrawing the tow from out of the treating liquid at any desired
  • the object of the present invention is to provide a process which is adapted to insolubilise under non-tensioning conditions a continuously travelling tow of protein filaments and in which the filaments of the travelling tow remain open and distinct by employing a series of solutions wherein the total quantity of sodium chloride included and distributed in the series formed by a relaxing solution having sodium sulphate as its stipulated saline constituent, a formaldehyde solution having a pH preferably between 4 and 7 and having sodium sulphate as its stipulated saline constituent and a formaldehyde solution strongly acidified with sulphuric acid and having sodium sulphate as its main stipulated saline constituent and sodium chloride as an additional stipulated constituent at least approaches the minimum quantity required for insolubilisation to occur in a stipulated time lying between a period of time of 1 and 30 minutes.
  • a further object of the present invention is to employ solutions having a lower concentration of reagents than was heretofore considered possible, and particularly with respect to the ooncentration of the reagents in the formaldehyde solution strongly acidified with sulphuric acid thereby effecting economies in the amount of reagents lost due to the taking up of the solutions by the filaments undergoing insolubilisation with the subsequent removal by washing of the reagents thus present in the finally insolubilised filaments.
  • the method of insolubilising under non-tensioning conditions in a period of time lying for instance between 1 and30 minutes a continuous travelling tow of coagulated filaments obtained by the spinning of aqueous alkaline solutions of protein into sulphuric acid/sodium sulphate coagulating baths and under such conditions that the travelling tow remains open and the filaments distinct comprises treating the travelling tow of coagulated filaments in a relaxing solution containing not less than 220 g. of sodium sulphate per litre of solution, treating the thus relaxed filaments at a temperature not exceeding 80 and preferably above 40 C. in an aqueous formaldehyde solution containing not less than 210 g.
  • sodium sulphate per litre of solution and having a pl-I value preferably between 4 and 7 and thereafter treating the travelling tow at a raised temperature in a strongly acidified aqueous formaldehyde solution containing per litre of solution not less than 340 g. sodium sulphate, not less than 15 g. sodium chloride, or a quantity of a reagent producing a chlorine ion and equivalent to an amount at least not less than 15 g. sodium chloride, and not less than 200 g. sulphuric acid.
  • the second formaldehyde bath i. e. the said strongly acidified formaldehyde solution can be used at temperatures higher than 90 though preferably the temperature is between 70 and 98 C.
  • the treating solutions preceding the said strongly acidified formaldehyde solution prefferably be free of sodium chloride unless it is required to shorten the time of treatment. Again the higher the quantity of sodium chloride present in the said strongly acidified formaldehyde solution the shorter is the time necessary to obtain insoluoilised protein filaments, i. e. protein filaments which do notdissolve in a solution of r 0.1% sulphuric acid and 0.25% sodium sulphate when immersed therein for minutes at 97 C.
  • a higher sulphuric acid concentration may be compensated for by a higher sodium sulphate or a lower sodium chloride concentration and a higher sodium chloride concentration may be compensated for a lower sulphuric acid or higher sodium sulphate concentration it being understood that the concentrations of sodium sulphate, sulphuric acid and sodium chloride must not be allowed to fall below the minimum concentration stipulated for each of these ingredients.
  • the temperature should be above 40 C.
  • a spinneretj into a coagulating bath 2 containing 240 1 g./l. sodium sulphate and 20 g./l. sulphuric acid.
  • the coagulated tow 3 is stretched between godets, 5 and then treated for 4 minutes with a solution containing 230 g./l. sodium sulphate, at a pH 8.5 at 23 to 30 C. contained in the trough of a ringtrough 7 according to the method described and claimed in patent specification No. 623,460.
  • This treatment is effected by leading the tow 3 under tension to a godet 6 situated vertically above the centre line of the trough of the ring-trough 7 through a reciprocating device 8 at least 3 feet above the surface of the liquor in the trough and so into the trough in which the fibre is deposited in a zig-zag manner.
  • This ring-trough consists of a solid centre section 2 feet in diameter with a trough 0.5 feet wide and 4 inches deep but integrally joined to it and is made of mild steel.
  • the ring-trough contains a base of wire gauze 9 and revolves in a circular trough l3 3 feet 4 inches external diameter, 1 foot 7 inches internal diameter and 6 inches deep, also of mild steel fitted with an adjustable weir so that the height of liquor in the trough may be varied at will.
  • the tow 3 sinks on to the base 9 of the trough i and is carried around with the trough l which revolves once in 3 minutes.
  • the tow 3 is taken up not less than 3 inches from the fibre met and is then mangled between squeeze rolls i i after which it is stretched between two godets l2 and [3.
  • the tow is now treated for 4 minutes in a solution containing 220 g./l. sodium sulphate, and 10 to g./l. formaldehyde at pH 5 and at 55 C. contained in the trough of a ring-trough 16 similar to the ring-trough 1 and again according to the method described and claimed in patent specification No. 623,460.
  • This operation is effected by passing the tow 3 from a godet l3 situated vertically above the centre line of the trough of the said ring-trough I6 through a reciprocating spacing device I5.
  • the tow 3 after leaving the trough of the ring-trough I6 is mangled between squeeze rolls l1 and passed from a godet l8 vertically downwards according to the method described and claimed in patent specification No. 642,359 into the constant feed cone l9 where it is picked up by the insolubilising liquid which enters the feed cone through a pipe 20 and is then carried through the tube 2
  • is of inch diameter and the glass cone 22 is 4 inches in diameter at the open end.
  • the composition of the insolubilising liquid is 340 g./l. sodium sulphate, 40 g./l. sodium chloride, 270 g./l.
  • sulphuric acid and 10 to 15 g./1. formaldehyde enters the tube 23 at 90 C., and overflows at 85 C.
  • is controlled by the difference in levels of the liquid at the inlet cone I9 and the overflow at the exit end of the tube 23 which in this case is 4 inches.
  • the tube 23 is of glass 6 inches in diameter and 8 feet long inclined so that the exit end is raised 14 inches above the inlet end.
  • a perforated lip 24 made of lead Which raises the level of the liquid in the tube 12,3 and allows aitrto -flow away:without giving rise toilocal. regions iof high speed fiow.
  • n process -of insolubilizing'at least un'tlrthe filaments do not dissolve in a bath containing 0.1% sulfuric acid and 0.25% sodium sulfate when immersed therein for 90 minutes at 97 C., under conditions substantially free from tension, a continuous travelling tow of protein filaments obtained by spinning aqueous alkaline solutions of proteins selected from the group consisting of vegetable seed globulins and phospho-proteins into a sulfuric acid-sodium sulfate coagulating bath, said process comprising the steps of relaxing said tow of coagulated filaments by impregnating the same with an aqueous solution which contains at least 220 grams of sodium sulfate per liter of solution, and is substantially free of sodium chloride, thereafter impregnating the thus relaxed tow at a temperature up to C.
  • aqueous formaldehyde solution having a pH of between 4 and 7 which contains at least 210 grams of sodium sulfate per liter of solution and is substantially free of sodium chloride and thereafter impregnating the tow at a temperature between 70 and 98 C. in a strongly acidified.
  • aqueous formaldehyde solution containing, per liter of solution, at least 340 grams of sodium sulfate, at least 15 grams of sodium chloride and at least 200 grams of sulfuric acid said process taking from one to thirty minutes.
  • aqueous formaldehyde solution having a pH of between 4 and 7 which contains 210 grams of sodium sulfate per liter of solution and is substantially free of sodium chloride and thereafter impregnating the tow at a temperature between 70 and 98 C. in a strongly acidified aqueous formaldehyde solution containing, per liter of solution, 340 grams of sodium sulfate, 15 grams of sodium chloride and 200 grams of sulfuric acid said process taking from one to. thirty minutes.

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Artificial Filaments (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
US235718A 1950-08-28 1951-07-09 Method for insolubilizing spun protein filamentary products Expired - Lifetime US2665966A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB303631X 1950-08-28

Publications (1)

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US2665966A true US2665966A (en) 1954-01-12

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US235718A Expired - Lifetime US2665966A (en) 1950-08-28 1951-07-09 Method for insolubilizing spun protein filamentary products

Country Status (7)

Country Link
US (1) US2665966A (de)
BE (1) BE505443A (de)
CH (1) CH303631A (de)
DE (1) DE915491C (de)
FR (1) FR1048386A (de)
GB (1) GB708057A (de)
NL (1) NL79057C (de)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB512640A (en) * 1937-04-27 1939-09-21 Ig Farbenindustrie Ag Improved process for hardening casein fibres
GB597497A (en) * 1945-08-22 1948-01-27 Robin Hamilton Kendall Thomson Improvements in or relating to the production of insolubilised protein-artificial filamentary products
GB623460A (en) * 1947-03-10 1949-05-18 Robin Hamilton Kendall Thomson Improvements in or relating to a method of treating a tow of filaments or threads
US2533297A (en) * 1945-08-22 1950-12-12 Ici Ltd Production of insolubilized protein artificial filamentary products
US2565935A (en) * 1941-03-20 1951-08-28 Ici Ltd Method for insolubilizing vegetable seed globulin and phospho-protein artificial filamentary products
US2565908A (en) * 1947-10-06 1951-08-28 Ici Ltd Method of insolubilizing artificial filaments of vegetable protein

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB512640A (en) * 1937-04-27 1939-09-21 Ig Farbenindustrie Ag Improved process for hardening casein fibres
US2565935A (en) * 1941-03-20 1951-08-28 Ici Ltd Method for insolubilizing vegetable seed globulin and phospho-protein artificial filamentary products
GB597497A (en) * 1945-08-22 1948-01-27 Robin Hamilton Kendall Thomson Improvements in or relating to the production of insolubilised protein-artificial filamentary products
US2533297A (en) * 1945-08-22 1950-12-12 Ici Ltd Production of insolubilized protein artificial filamentary products
GB623460A (en) * 1947-03-10 1949-05-18 Robin Hamilton Kendall Thomson Improvements in or relating to a method of treating a tow of filaments or threads
US2565908A (en) * 1947-10-06 1951-08-28 Ici Ltd Method of insolubilizing artificial filaments of vegetable protein

Also Published As

Publication number Publication date
FR1048386A (fr) 1953-12-22
DE915491C (de) 1954-07-22
GB708057A (en) 1954-04-28
CH303631A (de) 1954-12-15
BE505443A (de)
NL79057C (de)

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