US2460372A - Manufacture of artificial protein filaments - Google Patents

Manufacture of artificial protein filaments Download PDF

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Publication number
US2460372A
US2460372A US550487A US55048744A US2460372A US 2460372 A US2460372 A US 2460372A US 550487 A US550487 A US 550487A US 55048744 A US55048744 A US 55048744A US 2460372 A US2460372 A US 2460372A
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United States
Prior art keywords
filaments
filament
solution
formaldehyde
protein
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US550487A
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English (en)
Inventor
Robin H K Thomson
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Imperial Chemical Industries Ltd
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Imperial Chemical Industries Ltd
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Publication date
Application filed by Imperial Chemical Industries Ltd filed Critical Imperial Chemical Industries Ltd
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Publication of US2460372A publication Critical patent/US2460372A/en
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Classifications

    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F4/00Monocomponent artificial filaments or the like of proteins; Manufacture thereof
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/12Stretch-spinning methods
    • D01D5/14Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/22Formation of filaments, threads, or the like with a crimped or curled structure; with a special structure to simulate wool
    • YGENERAL 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
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/29Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913Rod, strand, filament or fiber
    • Y10T428/2922Nonlinear [e.g., crimped, coiled, etc.]
    • YGENERAL 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
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/29Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2913Rod, strand, filament or fiber
    • Y10T428/2933Coated or with bond, impregnation or core
    • Y10T428/2964Artificial fiber or filament

Definitions

  • the present invention relates to the manufacture of filaments of coagulated and insolubilised protein material for textile purposes, and more particularly to a process for the improvement of, filaments obtained by a wet spinning process from solutions of casein or vegetable globulins, which have been subjected in coagulated filamentary form to the action of an acidified aqueous solution of formaldehyde or other aqueous insolubilising bath adapted to render the coagulated protein filament capable of withstanding hot Weakly acid or alkaline solutions such as are used in dyeing and laundering.
  • insolubilised wet spun protein filaments it is usual to apply a stretch to the filament at some part of the process, and to efiect at least a partial stabilisation of the length of the stretched filament by means of the baths through which it passes; so that when the tension is released. it will not shrink excessively in a longitudinal direction.
  • This stretching and length stabilisation may be effected prior to the commencement of the insolubilisation, or in the course of the insolubilisation of the coagulated protein. In either case the insolubilised filaments obtained after the release of any tension upon them are substantially unstrained and exhibit little or no bi-reiringency.
  • textile filaments of various kinds can be improved in strength by steaming them in stretched condition and drying them the said insolubilised filaments, retaining the off while still stretched, but the'improvement so obtained is usually lost when the filaments are subsequently subjected in the untensioned condition to the action of boiling water or steam..
  • the process for the production of improved and crimped filaments from insolubilised filaments obtained by wet-spinning from solutions of casein or vegetable globulins comprises wet-stretching filaments in the stretched condition while subjecting them to raised temperature and treatment with formaldehyde, and thereafter Withdrawing the tension and effecting the shrinkage of the thus treated filaments to the desired degree of crimp.
  • the wet stretched filaments may be dried off under tension at raised temperature before the formaldehyde treatment is commenced. The drying is conducted at'a temperature not less than C., and if desired the filaments may be further heated to a temperature of to C. before commencing the formaldehyde treatment.
  • the Wet stretching is advantageously carried out with hot water or steam, and the extent to which the insolubilised filaments can be stretched without breaking, may depend on the nature of the treatment they have received in their production, but it will usually be possible to apply a stretch of from 50 to 100 per cent.
  • the stretched and if desired dried filaments may then be immersed in commercial formalin solution, i. e. a solution of formaldehyde of a lower acidity than that used in the previous insolubilisation step and left in contact with the solution for several hours if it is used at ordinary temperature.
  • a formaldehyde solution instead of immersing the filaments in a formaldehyde solution they can be subjected to an atmosphere of formaldehyde vapour.
  • the formaldehyde treated filaments may then be washed until their odour is faint and are then dried at a raised temperature not below about 80 C. Preferably the temperature is allowed is to rise somewhat about 100 C.when they havebeen dried. The tension on the filaments may then be released. At this stage they are straight, and silk-like, but on immersion in hot water they shrink, and after drying in untensioned condition have a desirable woolly crimp.
  • Figure 1 shows the three preliminary stages of spinning, insolubilizing and washing of the filaments
  • Figure 2 shows the subsequent steps of' drying and hot drawing of the filaments
  • Figure 3 illustrates the steps of treating the filaments while under tension to insolubilizing, washing and hot drying steps
  • Figure 4 shows the steps of rewinding the tensioned filaments into hank formand subsequently treating the untensioned filaments to boiling and drying.
  • the filament 2 is 'formed by extruding a protein solutionthrough the spinneret l into the 'coagulated :bath 6 and thence to the 'hanking device Where hanks 8 are formed.
  • the hanks are then placed in the insolubilizing bath Ill, where the filaments are insolubilized, after'which they are passed into a washing bath i2. Since the drawing is only diagrammatic in nature, only'one washing tank is illustrated but it will be understood that several such tanks may be employed and that pure water or weak alkaline or other washing solutions may be employed.
  • the filaments are passed to a hot air drier M where the filaments are and subjected to the drying action of hot air. Thence, the dried filaments are passed from winding the roll it to tension rollers I8 and '20 through the steam chamber 24 and are wound upon the winding roller 2-6 at a speed in excess of the speed of the tension rollers 18 and 25, so that the filaments are elongated while within the steam chamber 2 3 and subjected to the action of the steam passed through this chamber.
  • the filaments are retained under the tension produced during the winding operation upon the rollers or bobbins 23. In this condition, they are first immersed in an insolubilizing bath from where they are taken and immersedin the washing bath 32, Finally, while still under tension, the filaments are dried in the drying chamber 34 b hot air.
  • the bobbin of tensioned filament 28 is then rewcund onto a roller 36 so that .the filaments may be formed in hanks for further treatment in an untensioned condition.
  • the filaments In the untensioned state, the filaments are immersedin .the boiling water tank .38. Finally, the filament Ihanks are dried in thehot air drying chamber 40.
  • terial' are prepared by coagulating in .a hot :acidi' fied :sodium --sulphate bath :under tension :a viscous aged solution of peanut protein in :dilute' aqueous sodium hydroxide solution, the protein solution being extruded into the coagulating bath through a multiple hole spinneret, and subsequently insolubilising the coagulated filaments in the untensioned condition in a bath consisti-ngcf a :nearlysaturated solution of sodium chloride containing 1 per cent formaldehyde and 1.75 per cent sulphuric acid for a period of 18 hours at 20 C., and then washin the filaments, treating them first, with an aqueous dispersion of Lissapol C, then with a dilute sodium car-' bonate solution, and then drying them 01?
  • the dried filaments are then thoroughly damped in steam andzthe filaments aredrawn ofi from it through the stearn'itol a roller :01! they are wound helically under such tension that their taut length'is increasedabout '7 5 per cent.
  • the rollers carrying "the filaments in the stretched state are then immersed -.for 16 hours in commercial 'formalin'solution;
  • the filaments v are then washed until substantially free from odourand dried in ai-rat 1110 C. under tension, and are then released from the tension.
  • the resulting filaments have ho crimp and have an artificial silk-like appearance. They are relatively strongly bi refringent. Their tensile strength is approximately 12 kilograms per square .millimetre,ias calculated in the manner already referred to. "The resulting :filaments are now rewound sinto'zhank form and are immersed in boilin water in the 'untensioned condition for '10 minutes.
  • the process for obtaining an" improved, crimped, protein filament which comprises wetstretching an inso'lubilized filament previously formed by wet-spinning-a protein solution of the group consisting "of vegetable globulin solutions andcasein-solutions, contacting thejtaut filament with formaldehyde, dryingthe'taut filament at a temperature or at least C., releasing the tension on the filament and thereafter contacting the filament in relaxed condition with boiling water.
  • the process for obtaining an improved, crimped, protein filament which comprises stretching in steam a washed, formaldehyde-insolubilized filament previously formed by wetspinning a sodium hydroxide peanut protein solution, drying the taut filament at a temperature within the range of from 100 C. to 120 C., immersing the taut filament in a formalin solu tion, washing the taut filament, drying the taut filament at a temperature of at least 100 0., releasing the tension on the filament and thereafter immersing the filament in relaxed condition in boiling water.
  • a process for producing crimped, protein filaments of relatively high tensile strength which comprises Wet-spinning a protein solution into a coagulating medium, insolubilizing the resulting filaments in an acidic saline formaldehyde solution, stretching while wet the insolubilized filaments, contacting the taut filaments with formaldehyde, drying the resultingtaut filament at a temperature between 80 C. and 120 (3;, releasing the tension on the filaments and, thereafter, immersing the filament in a relaxed condition in boiling Water.
  • a process for producing crimped, peanut protein filaments of relatively high tensile strength which comprises wet-spinning a solution of peanut protein dissolved in an aqueous sodium hydroxide solution into a coagulating medium, insolubilizing the resulting filaments in an acidic is j saline formaldehyde solution, stretching while strength which comprises wet-spinning a solution of peanut protein dissolved in an aqueous sodium hydroxide solution into a coagulating medium,

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
US550487A 1943-10-20 1944-08-21 Manufacture of artificial protein filaments Expired - Lifetime US2460372A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB17241/43A GB570631A (en) 1943-10-20 1943-10-20 Improvements in or relating to the manufacture of artificial protein filaments

Publications (1)

Publication Number Publication Date
US2460372A true US2460372A (en) 1949-02-01

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Family Applications (1)

Application Number Title Priority Date Filing Date
US550487A Expired - Lifetime US2460372A (en) 1943-10-20 1944-08-21 Manufacture of artificial protein filaments

Country Status (6)

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US (1) US2460372A (is")
BE (1) BE458874A (is")
DE (1) DE832318C (is")
FR (1) FR910839A (is")
GB (1) GB570631A (is")
NL (1) NL62182C (is")

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2541803A (en) * 1948-12-24 1951-02-13 Courtaulds Ltd Production of artificial protein threads, filaments, and the like
US2685497A (en) * 1948-05-12 1954-08-03 Celanese Corp Treatment of polymeric materials
JPWO2019151436A1 (ja) * 2018-01-31 2021-01-14 Spiber株式会社 タンパク質捲縮ステープルの製造方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US379672A (en) * 1888-03-20 Art of making dry-sand cores
GB502710A (en) * 1937-11-18 1939-03-23 Courtaulds Ltd Improvements in the manufacture and production of artificial filaments, threads and the like
US2211961A (en) * 1937-04-08 1940-08-20 Du Pont Artificial product and method for producing same
US2293989A (en) * 1938-08-08 1942-08-25 American Enka Corp Manufacture of artificial wool
US2338916A (en) * 1937-03-02 1944-01-11 Ferretti Antonio Embodiment in the process for manufacturing artificial textile fibers from animal casein
US2340909A (en) * 1939-01-21 1944-02-08 Ici Ltd Manufacture of artificial fibers from protein material
US2358427A (en) * 1940-08-29 1944-09-19 Ici Ltd Manufacture of filaments from vegetable globulin

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US379672A (en) * 1888-03-20 Art of making dry-sand cores
US2338916A (en) * 1937-03-02 1944-01-11 Ferretti Antonio Embodiment in the process for manufacturing artificial textile fibers from animal casein
US2211961A (en) * 1937-04-08 1940-08-20 Du Pont Artificial product and method for producing same
GB502710A (en) * 1937-11-18 1939-03-23 Courtaulds Ltd Improvements in the manufacture and production of artificial filaments, threads and the like
US2290789A (en) * 1937-11-18 1942-07-21 Courtaulds Ltd Manufacture and production of artificial filaments, threads, and the like
US2293989A (en) * 1938-08-08 1942-08-25 American Enka Corp Manufacture of artificial wool
US2340909A (en) * 1939-01-21 1944-02-08 Ici Ltd Manufacture of artificial fibers from protein material
US2358427A (en) * 1940-08-29 1944-09-19 Ici Ltd Manufacture of filaments from vegetable globulin

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2685497A (en) * 1948-05-12 1954-08-03 Celanese Corp Treatment of polymeric materials
US2541803A (en) * 1948-12-24 1951-02-13 Courtaulds Ltd Production of artificial protein threads, filaments, and the like
JPWO2019151436A1 (ja) * 2018-01-31 2021-01-14 Spiber株式会社 タンパク質捲縮ステープルの製造方法
EP3748066A4 (en) * 2018-01-31 2021-12-15 Spiber Inc. PROCESS FOR MAKING A STAPLE SET WITH PROTEIN

Also Published As

Publication number Publication date
GB570631A (en) 1945-07-16
DE832318C (de) 1952-02-25
BE458874A (is")
FR910839A (fr) 1946-06-19
NL62182C (is")

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