Classifications

• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
  • C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
  • C08B15/005—Crosslinking of cellulose derivatives
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
• • 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
  • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
  • D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
• • 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
  • D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
  • D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
  • D01F2/08—Composition of the spinning solution or the bath
  • D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either

Definitions

• U. S. Patent No. 2,495,232 dated January 24, 1950 describes a method of obtaining new cellulose derivatives by associating with the cellulose substances which contain free hydroxyl groups, monomeric polymethylol' phenols, and more particularly trimethylol phenols, and then subjecting the materials to heat treatment in the presence of an acid catalyst, which gives rise to the formation of bridge linkages of resinous groups between the cellulose chains.
• the essential basis of the aforesaid processes is the formation of a substance resulting from the association of cellulose with a resinous substance. This association is obtained with the aid of groups of the resinous substance which are capable of reacting with the cellulose during, the subsequent condensing operation. It is therefore necessary to use a combination capable of increasing its molecular size by internal condensation while reacting with the cellulose. that it is possible to arrive at the same result by combining the cellulose, not with substances of low molecular weight which are capable of subsequent condensation, but with high polymers which are already condensed. In the latter case, the high polymers have. not sufficient reactivity to become associated with the active groups of the cellulose. .
• an agent able to combine simultaneously with the hydroxyl groups of the cellulose and with the residual reactive groups of the high polymer employed.
• the object of the present invention is toprovide complexes of this type by intimately incorporating in the cellulose, linear polyesters of the polyacid-polyalcohol type, in such a state of condensation that their molecular weight is -al-
• linear polyesters of the polyacid-polyalcohol type in such a state of condensation that their molecular weight is -al-
• suflicient free hydroxyl groups in the cellulosic material to enable them to react with the linking agent which will subsequently be employed.
• various linking reagents may be employed. However, the most convenient is formaldehyde, which reacts with the free hydroxyls of the cellulose and the linear polymer ester and forms stable methylene bridges.
• linear superpolyesters or superpolyamides to the cellulosic solutions to be spun, in order to obtain certain special delustering or tinting effects, but the said linear super-polyesters or superpolyamides cannot undergo any further condensation on the fiber without damaging the fiber. Moreover, they are not capable of reacting readily with the free hydroxyl groups of the cellulose and their solubility in dilute alcohol is generally very reduced, except in the case of certain interpolymers.
• a further feature of the invention is the supplementary treatment of yarns containing soluble linear polyesters of aliphatic diacids and dialcohols or other polyalcohols, with formaldehyde by heating in the presence of an acid catalyst, for the purpose of polymerizing the said polyesters on the fiber.
• This treatment affords a verv substantial increase in the stability of the effects obtained especially with regard to the reduction of the swelling in aqueous media.
• the supplementary treatment renders the effect much more stable to washing.
• the swelling referred to is the quantity of water retained by the dry cellulosic substance after steeping in water, followed by centrifuging for ten minutes in a laboratory hydro-extractor rotating at 3000 revolutions per minute and having a diameter of, for example, 25 cm.
• the viscose solution is incorporated in the viscose solution in the form of a concentrated solution in dilute caustic soda containing 40% to 50% of the product.
• aqueous dispersions containing wetting agents or of organic solutions, for example alcohol solutions.
• the invention will be more readil understood with reference to the following examples, which are not intended to constitute any limitations.
• the invention is concerned more especially with the manufacture of artificial yarns such as rayon, artificial staple fiber, or bristles, it is also applicable to the manufacture of films.
• the invention is in no way limited to viscose filaments, but includes all artificial fila ments of cellulose or of cellulose derivatives still containing free hydroxyl groups. It covers in general all filaments containing chain molecules comprisinug active hydroxyl groups, such for example as yarns of polyvinyl alcohol or of partially saponified polyvinyl acetals.
• the appearance of the filaments may be modified, for example by suitable de-lustering agents, b any known method.
• Coloring agents may also be incorporated in the filaments by adding to the solutions to be spun coloring agents suitable for dyeing in the mass. The white color of the filainents facilitates the production of bright pure ones.
• Example I To l0 liters of a viscose containing 6% of caustic soda and 9% of cellulose are added 20 cc. of a 50% solution, in 6% caustic soda, of the product of condensation of adipic acid and glycerm prepared in the manner hereinbefore described. This viscose is then cured to a salt point of 6.0 and is spun through a spinneret having 2500 holes of a diameter of 0.08 mm. in a bath containing 120 g. of sulphuric acid, 250 g. of sodium sulphate and 15 g. of zinc sulphate per liter, at a temperature of 48 C'. After travelling a distance of 50 cm.
• the yarn is passed into a second bath of acidified water at 90 C. and stretched by 75%.
• the output of the spinning pump is adjusted to produce, after stretching, filaments of 1.5 denier.
• the stretched bundle of filaments is washed, wound on a large perforated roller, and dried. It is then formed into skeins, which are desulphurized with a hot sodium sulphate solution and rinsed again, thereafter they are impregnated with an aqueous solution containing 7 g. of formaldehyde and 3.5 g. of ammonium chloride per liter.
• the skeins are then washed at 80 C. to 85 C.,
• the filaments thus obtained have a swelling value of 55.
• the tenacity is 2.2 g. per denier in the dry state and 1.2 g. per denier in the wet state, and the elongation at rupture is 14% when dry and 12% when wet.
• Example II To liters of a viscose containing 6% of caustic soda and 8% of cellulose are added 120 cc. of a 50% solution of the product of condensation of adipic acid and glycerin in 6% caustic soda. The mixture is cured to a salt point of 3.0 and spun through a spinneret having 100 holes 0.75 in diameter, into a bath containing 100 to 110 g. of sulphuric acid, 200 to 220 g. of ammonium sulphate and 120 to 130 g. of sodium sulphate per liter, at 45 C. The bristles thus obtained are collected in hydro-extractors and are washed and then formed into skeins.
• skeins are subjected to bleaching with a hypochlorite solution containing from 2.0 to 2.5 g. of active chlorine per liter, and having a pH of from 8 to 10, and then to treatment with a bath containing from 1.5 to 2.0 g. of sulphuric acid per liter, thereafter they are thoroughly washed.
• the skeins are then immersed in a bath containing 8 g. of formaldehyde and 3.5 g. of ammonium chloride, centrifuged and dried at 80 C. to 85 C.
• the bristles thus obtained have a swelling value of from to and are of very pale creamy white color. They are suitable for the production of brushes and like articles.
• the process for producing colorless artificial regenerated cellulose filaments with reduced swelling characteristics which comprises incorporating in a viscose spinning solution, a partly condensed linear polyester of an aliphatic diacid and a polyalcohol which is soluble in dilute soda, spinning said solution into a filament and reacting the spun filament by treatment at C. to C. with not over 10 g. per liter of formaldehyde and an acid catalyst.
• the process for producing colorless artificial regenerated cellulose filaments with reduced swelling characteristics which comprises incorporating in a viscose spinning solution, a partly condensed linear polyester of an aliphatic diacid and a polyalcohol which is soluble in dilute soda, spinning said solution into a filament and reacting the spun filament by treatment at 80 C. to 90 C, at a temperature of not over 90 C. with formaldehyde in a concentration of not over 10 g. per liter and an acid catalyst.
• the process for producing colorless artificial regenerated cellulose filaments with reduced swelling characteristics which comprises incorporating in a viscose spinning solution, a partly condensed linear polyester of adipic acid and glycerin, spinning said solution into a filament and reacting the spun filament by treatment at 80 C. to 90 C. with not over 10 g. per liter of formaldehyde and an acid catalyst.
• the process for producing colorless artificial regenerated cellulose filaments with reduced swelling characteristics which comprises incorporating in a viscose spinning solution, a partly condensed linear polyester of adipic acid and glycol, spinning said solution into a filament and reacting the spun filament by treatment at 80 C. to 90 C. with not over 10 g. per liter of formaldehyde and an acid catalyst.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Medicinal Chemistry (AREA)
• Textile Engineering (AREA)
• Health & Medical Sciences (AREA)
• General Chemical & Material Sciences (AREA)
• Polymers & Plastics (AREA)
• Organic Chemistry (AREA)
• Life Sciences & Earth Sciences (AREA)
• Biochemistry (AREA)
• Materials Engineering (AREA)
• Artificial Filaments (AREA)

Applications Claiming Priority (1)

Publications (1)

Family

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Family Applications (1)

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Cited By (6)

Citations (3)

• 0
  • BE BE494801D patent/BE494801A/xx unknown
• 1949
  • 1949-04-05 FR FR987569D patent/FR987569A/fr not_active Expired
• 1950
  • 1950-03-20 US US150798A patent/US2597624A/en not_active Expired - Lifetime

Patent Citations (3)

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