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

• This invention relates to the production of artificial protein threads, fibres, filaments and the like, hereinafter generally referred to as threads, and is particularly concerned with the production of spinning solutions of keratin and regenerated keratin threads made from such solutions.
• peracetic acid as an oxidising agent on a commercial scale, however, is undesirable; the acid itself is corrosive and unpleasant to operatives and in addition the manufacture of the acid from acetic anhydride and hydrogen peroxide is dangerous in that the reaction mixture may explode.
• the bb-ject of the present invention is to provide an improved oxidative pretreatment of keratin particularly for the manufacture of regenerated keratin fibres.
• a process for the oxidative pretreatment of keratin comprises subjecting the keratin to the action of hydrogen peroxide in the presence of ferrous sulphate and an acid.
• the preferred acid is sulphuric acid but other acids such as phosphoric acid and acetic acid may also be used.
• the amounts of hydrated ferrous sulphate and of sulphuric acid used may be from 2 to 20 per cent by weight of the weight of keratin. It is preferred to use from 8 to 10 per cent of ferrous sulphate based on the weight of keratin.
• the amount of acid used should be sufficient to keep the ferrous sulphate in solution; 1 gram per litre of ferrous sulphate usually requires approximately 1 gram per litre of sulphuric acid.
• the keratin pretreated according to the invention is readily soluble in dilute alkali and the present invention therefore also includes a process for the production of keratin solutions comprising subjecting the keratin to the action of hydrogen peroxide in the presence of ferrous sulphate and an acid and dissolving the oxidised keratin in an aqueous alkaline solution.
• the solutions obtained according to the invention may be used directly as spinning solutions in the manufacture of artificial threads; they may also be used as sizes and dispersing agents.
• the invention also includes a process for the production of regenerated keratin threads comprising subjecting the keratin to the action of hydrogen peroxide in the presence of ferrous sulphate and an acid, dissolving the oxidised keratin in an aqueous alkaline solution, such as aqueous ammonia or aqueous caustic soda solution, and extruding the solution so obtained into an aqueous coagulant bath containing one or more metal salts known to coagulate proteins; suitable salts are sodium sulphate, magnesium sulphate and aluminium sulphate; mixtures of such salts may also be used.
• the bath preferably has a pH'value between 5.0 and 9.0.
• the threads obtained according to the invention may be treated in the manner usual for artificial protein threads, including stretching, hardening, and insolubilising treatments.
• the stretching of the threads may be effected by passing the thread between godets, rollers or reels the peripheral speeds of which are adjusted to give the desired amount of stretching; alternatively a pair of tapered rollers may be used.
• the stretching should usually be at least per cent but is preferably higher, for example from to 300 per cent. Stretching may be efiectedin air or in the presence of a coagulant bath free or substantially free from hardening agents.
• the hardening baths may be any of the usual baths proposed for this purpose with casein threads, for example aqueous formaldehyde either alone or preferably in conjunction with one tract as described in United States iPatentspecification No. 2,290,789.
• the regenerated keratin fibres obtained according to the invention are generally of thealpha configuration as shown by 'X-Yray analysis, and possess a wool-like elasticity.
• Example 1 The mixture was stirred for 3 hours with external cooling to keep the temperature about 20 centigrade. The mixture was then diluted with an equal volume of water and, after stirring, allowed to stand for 3 days. The solid material was separated, dissolved and extruded as described in Example 1.
• g A prpgess for, the oxidative pretreatment of keratin preparatory to its solution in an aqueous alkaline solverm which comprises subjecting the keratin .to .the action of hydrogen peroxide in the presence o'fferrous sulphate and an acid chosen f rom tthegroup-cgnsisting of sulphuric acid, phosphoric acid and acetieacid.
• the viscous solution obtained was then centrifuged free from air and other particles and was then extruded into an aqueous solution containing in-each litre 450 grams of crystalline magnesium sulphate (MgSO4.7I-Iz0) and 150'grams of anhydrous sodium sulphate, the pH value "of the solution being 7.0.
• the freshly extruded thread- was stretched 200 per centon tapered rollers with inclined axes with the lower rollers rotating in a solution having the same'composi tionas the coagulant bath.
• the threads were then collected on a godet andthardened for 2 hours at 50 centrigra-de in a bath containing-in each litre 10 grams of formaldehyde, 450-grams of crystalline magnesium sulphateiand 150 grams of anhydrous-sodium sulphate and then insolubilised by further treatmentfor 2 hours in abath at 45.centrigrade containing in each litre l0 gramsof formaldehyde, 300 grams-of sodium sulphate and 100 grams of sulphuric acid. The threads were then washed in water and dried.
• Example 2 alkaline solvent which comprises subjecting the keratin to the action of hydrogen peroxide in the presence of ferrous sulphate and sulphuric acid.
• a process for the oxidative pretreatment of keratin preparatory :to its solution in an aqueous alkaline solvent which comprises subjecting the keratin to the action of hydrogen peroxide in the presence of from 2 to 20 per cent by weight of ferrous sulphate and from 2 to 20 per cent by weight of sulphuric acid, both percentages being based on the weight of the keratin.
• a process for the production of keratinsolutions which comprises subjecting the keratin to the action of hydro-gen :peroxide in the presence of ferrous sulphate and-an acid chosen from the group consisting of sulphuric acid, phosphoric acid and acetic acid and dissolving theoxidised keratin inan aqueous alkaline solution.
• a process .for the production of keratin solutions which comprisessubjecting the keratin to the action of hydrogen peroxide-in the presence of ferrous sulphate and sulphuric acidand dis- 7 solving the-oxidised keratinin a aqueous alkaline solution.
• a process for the production of keratin solutions which comprises stirring together keratin and vhydrogenhperoxide in the presence of from 2 to 20 per cent by .Weightof ferrous sulphate and from 2 to 20 per cent by-weightof sulphuric acid, both percentagesbeing based on the weightof the keratin thereby oxidising the keratin, and dissolving the oxidised keratin .in an aqueous al.- kaline solution.
• Aprocess for the-production of regenerated keratin-threads which comprises stirring together keratin and hydrogen peroxide in the presence of ferrous sulphate and an acid chosen from the group consisting of sulphuric acid, phosphoric acid and acetic acid, thereby oxidising the keratin, dissolving the oxidisedikeratin in anaqueous ,alkaline solution and extrudingrthe solutionso obtained into anaqueous salt bath having a pH value between 5.0 and 9.0.
• a process for the-production of regenerated keratin 'threads which comprises stirring together keratin and hydrogen peroxide in the presence of ferrous sulphate and sulphuric acid, thereby oxidising the keratin, dissolving the oxidised keratin'in an aqueous alkalinesol-ution and-extruding the solution soobt-ai-ned yintozan aqueous l thsh vineiapHwalueibetween 5.0;and 9.0..
• i l-process for: the-production of;r.egenerated k ratinathreads which .eQmprises-stirring together keratin and hydrogen peroxide in the presence of from 2 to 20 per cent by weight of ferrous sulphate and from 2 to 20 per cent by weight of sulphuric acid, both percentages being based on the weight of the keratin, thereby oxidising the keratin, dissolving the oxidised keratin in an aqueous alkaline solution and. extruding the solution so obtained into an aqueous salt bath having a pH value between 5.0 and 9.0.

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

Applications Claiming Priority (1)

Publications (1)

Family

ID=10219474

Family Applications (1)

Country Status (4)

Cited By (3)

Citations (1)

• 1950
  • 1950-10-12 GB GB24927/50A patent/GB692876A/en not_active Expired
• 1951
  • 1951-09-18 US US247194A patent/US2649357A/en not_active Expired - Lifetime
  • 1951-10-09 DE DEC4797A patent/DE906007C/de not_active Expired
  • 1951-10-12 FR FR1043794D patent/FR1043794A/fr not_active Expired

Patent Citations (1)

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