Classifications

• • 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

Definitions

• the present invention relates to a new or improved method for insolubilising artificial filaments, threads, fibres and the like filamentary products spun from protein solutions, and more particularly those obtained by the spinning of solutions of vegetable seed globulins, for instance peanut protein, or phospho-proteins,-for instance casein, in aqueous alkaline or other suitable aqueous solvent media into suitable acidified saline coagulating baths.
• Sodium sulphate solutions slightly acidified with sulphuric acid are in practice most advantageously used as the coagulating baths.
• the filamentary products emerging from the coagulating bath are still easily soluble in dilute saline solutions. They can be rendered insoluble in dilute saline solutions and in cold water by a hardening treatment with formaldehyde, but in order to render the filamentary products capable of ordinary textile application they must be rendered capable of withstanding also the action of boiling water, so that they can be dried off without sticking together, and further the action of hot dilute acid solutions such as are used in the application of acid wool dyes and of hot dilute alkaline solutions such as are used in laundering.
• the method of insolubilising artificial filamentary products obtained by the spinning of solutions of vegetable seed globulins, for instance peanut proteins, or phospho-proteins, for instance casein, in aqueous alkaline or other suitable aqueous solvent media into suitable acidified saline coagulating baths comprises treating the said filamentary products in an aqueous formaldehyde bath saturated to both sodium chloride and sodium sulphate or to both sodium chloride and magnesium sulphate at a pH of 4 to 6 and at a temperature not exceeding 60 C.
• the strongly acidified formaldehyde bath of pH 4 to 6 is saturated to both sodium chloride and sodium sulphate then the strongly acidified formaldehyde bath is saturated with sodium sulphate while if the formaldehyde bath of pH 4 to 6 is saturated to both sodium chloride and magnesium sulphate then the strongly acidified formaldehyde bath is saturated with magnesium sulphate.
• the formaldehyde concentrations in the two baths may be widely varied, but high concentrations are unnecessary.
• the time for which the filamentary products require to remain in contact with the formaldehyde bath at pH 4 to 6 saturated with sodium chloride and sodium or magnesium sulphate depends on the temperature at which this bath is used, and in the region of 50 C. a period of about five minutes is sufficient, or at about 40 C. about eight minutes to fifteen minutes. It is essential that this bath should be saturated both to sodium chloride and sodium sulphate, or sodium chloride and magnesium sulphate otherwise it is impossible to employ the subsequent strongly acidified bath at a temperature suificiently high to effect rapid insolubilisation without at the same time causing the filamentary products to clump together and yield products of inferior physical characteristics.
• the sulphuric acid concentration may advantageously range from about 175 grams sulphuric acid per litre upwards.
• the temperature of this second bath preferably does not exceed 75 C. but it will be understood that the lower the temperature the less rapid is the insolubiisation A t 70 C. the time required is usually about to minutes.
• Example 1 under tension through a saturated sodium chloride bath at approximately C. m which they remained until their. longitudinal contractility had been greatly reduced.
• the filaments were then cut into staple fibre and stored in a saturated sodium chloride solution having a pH value of '7 at room temperature until required.
• the resulting unhardened staple fibre was immersed in a warm solution containing 1 per cent formaldehyde by weight, which solution had been saturated to sodium chloride and sodium sulphate and brought to pH 5.0, the temperature of the resulting bath being'50' C. 'After five minutes immersion the staple fibre was removed from this bath and allowed to drain somewhat.
• Example 2 The unhardened filamentary material treated was the same as in Example 1, and the staple fibre was immersed for five minutes in a warm bath containing 1 per cent by weight of formaldehyde at pH 5 saturated by sodium chloride and sodium sulphate as described in Example 1, It was then transferred to a strongly acidified bath made up as described in Example 1 except that the volume of concentrated sulphuric acid used was only one eighth of that of the formaldehyde solution saturated with sodium sulphate. The fibre was left in this bath for fifteen minutes and was then removed and washed. Its properties were very similar to those of the insolubilisation staple fibre whose preparation is described in Example 1.
• Example 3 The unhardened staple fibre employed was the same as that used according to Example 1. It was immersed in a warm solution containing 1 per cent formaldehyde by weight that had been saturated with sodium chloride and magnesium sulphate and brought to pH 5.0 the temperature of this solution being 50 C. After. five minutes immersion the staple fibre was removed from the bath and allowed to drain somewhat. It was then transferred to a bath consisting of a hot saturated magnesium sulphate solution containing 1 per cent formaldehyde by weight, to which solution had been added one quarter of its volume of concentrated sulphuric acid and sufiicient magnesium sulphate to keep the solution saturated. The temperature of the resulting bath was C. and its sulphuric acid content was 318 grams per litre.
• the bath has a pH value of less than 1 when measured at room temperature.
• the staple fibre was left in this bath for ten minutes and was then removed and washed. It opened well and was found to be unimpaired by boiling water. It also resisted the action of a bath containing 0.1 per cent sulphuric acid and per cent sodium sulphate at 97 C. for minutes without impairment of its form. It closely resembled the fibre produced according to Example 1 in it physical properties, handle and laundering resistance.
• a method of insolubilizing artificial filamentary products obtained by spinning aqueous, alkaline solutions of proteins into acidified saline coagulating baths which comprises treating the coagulated filamentary products, havin a solubility substantially the same as that immediately after coagulation, for up to about fifteen minutes, at a temperature not exceeding 60 C. with an aqueous, formaldehyde solution havin a pH of between about 4 to 6, which is saturated to both sodium chloride and a sulphate from the group consisting of sodium sulphate and mag nesium sulphate at said temperature, and immediately thereafter treating the resulting products at a temperature not exceeding 75 C.
• a method of insolubilizing artificial filamentary products obtained by spinnin aqueous alkaline solutions of proteins into acidified saline coagulating baths which comprises treating the coagulated filamentary products, having a solubility substantially the same as that immediately after coagulation, in untensioned condition at a temperature between about 40 C. to 60 C. for

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

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Citations (5)

• 0
  • NL NL62061D patent/NL62061C/xx active
  • BE BE467120D patent/BE467120A/xx unknown
• 1946
  • 1946-07-02 US US681153A patent/US2533297A/en not_active Expired - Lifetime
  • 1946-07-20 FR FR930905D patent/FR930905A/fr not_active Expired
  • 1946-08-21 CH CH256467D patent/CH256467A/de unknown
• 1949
  • 1949-01-01 DE DEP1221A patent/DE842826C/de not_active Expired

Patent Citations (5)

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