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
  • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
  • D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
  • D01F6/48—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of halogenated hydrocarbons
• • 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
  • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
  • D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
  • D01F6/08—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of halogenated hydrocarbons
  • D01F6/10—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of halogenated hydrocarbons from polyvinyl chloride or polyvinylidene chloride

Definitions

• the present invention relates to filaments, yarns, monofilament fibers and other similar articles of synthetic material consisting of polyvinyl chloride and superchlorinated polyvinyl chloride. It relates more particularly to yarns and fibers of better mechanical qualities and yarns of fibers of better toughness obtained from these fibers.
• the fibers thus obtained can withstand heat treatment temperatures that are higher the higher the percentage of superchlorinated polyvinyl chloride in the mixture, which results in a reduction in the residual thermal shrinkage.
• high percentages of superchlorinated polyvinyl chloride significantly increase the cost price of the son and fibers obtained, all the more so since their production process is discontinuous, in particular the heat treatment for fixing.
• French Patent No. 85,126 / 1,359,178 also recommends the use of mixtures of atactic polyvinyl chloride and superchlorinated polyvinyl chloride in proportion to 5 to 50% of the mixture and specifies that the fibers obtained can, after spinning and drawing, at instead of being stabilized under tension under the conditions indicated in the main patent, be directly shrunk by heating in an appropriate medium, for example boiling water.
• an appropriate medium for example boiling water.
• the aforementioned processing conditions only allow fibers with good properties to be obtained when the proportion of superchlorinated polyvinyl chloride is relatively large.
• the toughness and elongation of the threads obtained are good thanks to the relatively large proportion of superchlorinated polyvinyl chloride: 20% by weight.
• the difficulty with this type of atactic polyvinyl chloride and superchlorinated polyvinyl chloride mixture therefore consists, in fact, of finding a compromise making it possible to obtain fibers having the highest possible mechanical qualities for the lowest possible cost price.
• the present invention relates to fibers based on a PVC / superchlorinated PVC mixture containing 17 to 20% of superchlorinated PVC, with strand strength ⁇ 2.3 dtex, a residual shrinkage after treatment in oil at 115 ° C. for 30 min (ASTM Standard D 210 262 T) ⁇ 6%.
• the present invention also relates to a process for obtaining fibers based on a mixture of atactic polyvinyl chloride and superchlorinated polyvinyl chloride, in a proportion of 17 to 20% by weight of superchlorinated PVC, by spinning a solution of the mixture of polymer in a solvent mixture carbon sulfide / acetone 60/40 in a manner known per se, drawing of the filaments in boiling water at a rate between 3 and 6 X, continuous stabilization of the filaments under tension at a temperature between 125 and 140 ° C, preferably 130-135 ° C in the presence of steam at a pressure of 2.7 to 2.8 bar for 1 to 3 seconds, then mechanical or pneumatic crimping of the cable thus obtained in known manner and fixing treatment at temperature> 100 ° C. in the presence of pressurized steam, continuously, then shrinking in a known manner in boiling water or by any suitable means, then drying in a known manner continuously and cutting under form of fibers.
• the present invention also relates to yarns of fibers obtained from the fibers described above, having good toughness, finer strands than those obtained hitherto and better workability of textiles, in particular in weaving.
• the fibers according to the invention it is possible with the fibers according to the invention to obtain yarns of fibers of metric number (NM) 50 (20 tex) which was not possible until then because the titles of the PVC / superchlorinated PVC fibers were too high to obtain yarns of sufficiently fine fibers.
• NM 20 50 tex
• the yarns of fibers have a toughness of at least 10 or 13 CN / tex which allows them to be woven at high speed.
• the term “atactic polyvinyl chloride” is understood to mean essentially the vinyl chloride homopolymer having a second order transition temperature generally between 65 and 85 ° C.
• Polyvinyl chloride is predominantly constituted by the atactic isomer form, that is to say that it is a polymer whose chlorine and hydrogen atoms are predominantly located randomly on both sides of the chain constituting the skeleton of the molecule. Therefore, such a poymer is normally of a non-crystallizable nature.
• Such a polymer is most commonly obtained in the least costly manner by known techniques of bulk polymerization, suspension or emulsion at temperatures generally above 0 ° C, more generally between 20 and 60 ° C or even more.
• the superchlorinated polyvinyl chloride usable according to the present invention can be obtained for example, by chlorination of a suspension of polyvinyl chloride in the presence of actinic light, or by chlorination at high temperature, or in the presence of active chemical radiation; it generally has a second order transition temperature of at least 100 ° C.
• the staple fibers according to the present invention have mechanical properties and thermal resistance never obtained until now, thanks to a selection of different elements.
• This state of crystallinity is further improved by subsequent heat treatments, namely drawing in boiling water at temperatures between 85 and 100 ° C, at a rate between 3 and 6 X, preferably 3.5 - 5 X.
• the drawing of the filaments according to the present invention is generally preceded by preheating, for example in water, at temperatures between 60 and 100 ° C, more generally between 75 and 85 ° C.
• preheating for example in water
• the actual stretching can be carried out in 1 or 2 stages, but it is preferred to gradually raise the temperature of the filaments by preheating, pre-stretching for example in a bath, the water of which can be maintained between 70 and 95 ° C. then continuous stretching at a temperature slightly higher than that of the pre-stretching, preferably between 85 and 100 ° C or overall stretching indicated above.
• preheating pre-stretching for example in a bath, the water of which can be maintained between 70 and 95 ° C.
• continuous stretching at a temperature slightly higher than that of the pre-stretching, preferably between 85 and 100 ° C or overall stretching indicated above.
• an overall drawing rate of 6 it is easier to limit the drawing of the filaments just after the die, by adjusting the speed of the take-up roller
• the filaments thus stabilized are crimped by any known mechanical or pneumatic means, for example by means of a nozzle such as that described in French patent No. 83329 addition to FR No. 1,289,491.
• a nozzle such as that described in French patent No. 83329 addition to FR No. 1,289,491.
• the filaments are treated by saturated steam at a temperature between 110 and 130 ° C and are simultaneously shrunk and crimped which allows better textile workability later.
• the crimping thus produced must be set at high temperature, generally between 110 and 120 ° C, in the presence of steam under pressure for at least 20 seconds, preferably at least 30 seconds, and preferably continuously.
• the permanently crimped filaments are then dried in the usual way, generally at a temperature in the region of 100 ° C.
• the process according to the present invention can be carried out completely continuously from the drawing or even from the dissolution of the polymers until the final yarns or fibers are obtained. Therefore, it is easy to carry out industrially economically.
• the polymers or solutions spun according to the present application can contain usual fillers such as stabilizers with regard to light, heat, brighteners, pigments, dyes capable of improving some of their properties such as their color, dye affinity, thermal and light stability, electrical resistivity ...
• the fracture toughness values and the elongation at break are improved, which makes it possible to obtain much more efficient yarns of fibers, of improved wearability. They can also be used for the production of knits, non-woven articles, alone or in mixtures with other fibers and can in particular undergo all the usual washing and dry cleaning treatments under appropriate conditions.
• Said yarns and fibers according to the invention are also particularly appreciated in the textile field because of certain properties inherent in the composition of the mixtures: non-flammability, resistance to light, chemical inertness and power of thermal, electrical and acoustic insulation.
• a polymer solution of concentration 28% by weight is prepared in a solvent mixture of carbon disulphide / acetone at 60/40 by volume.
• the solution thus obtained is filtered and, while being maintained at approximately 70 ° C., is spun through a die having 908 orifices of 0.06 mm in diameter in a dry spinning cell allowing the continuous recovery of the solvent mixture such as described in French patent n ° 913 927.
• the filaments are then preheated in a water bath maintained at 80 ° C and then drawn a first time in a water bath maintained at 85 ° C at a rate of 3.15 X , then stretched a second time in a second water bath maintained at 100 ° C at a rate of 1.2 X (total rate 3.78 X).
• the filaments are then stabilized continuously under tension in a tube containing saturated steam at 125 ° C under a pressure of 2.32 bar, the inlet and outlet speeds of the filaments being strictly identical, and the residence time in the tube being 2 seconds.
• the filaments are then subjected to mechanical crimping and free shrinking in a nozzle as described in French Patent No. 83,329 addition to FR No. 1,289,491 at 120 ° C in the presence of water vapor.
• the filament cable is then vaporized in a device known commercially under the brand name Tow Fix from the lich Anonyme Serracant, continuously, at a temperature of 110 ° C. for 30 seconds, the cable being treated in a densified form at the rate of 450 kg / m3. It is then dried in the usual way in an oven at 105 ° C and will be cut to obtain staple fibers in the usual way.
• Example 1 is reproduced with the exception of the fixing treatment which is carried out under tension in the presence of steam at 130 ° C., under a pressure of 2.7 bars.
• the characteristics of the fibers obtained are shown in Table 1.
• Example 1 is reproduced with the exception of the fixing treatment which is carried out under tension in the presence of steam at 135 ° C., under a pressure of 3 bars.
• the characteristics of the fibers are listed in the table below; the tests corresponding to examples 1 to 3 were carried out compared to control fibers obtained according to French patent n ° 2 495 642 from a PVC / PVC mixture superchlorinated at 17.5% or PVC superchlorinated in a sulfur mixture of carbon / acetone 50/50, spun and drawn in the same way, the filaments being subjected to a thermal fixing treatment in the presence of water vapor carried out at 113 ° C, under a pressure of 1.7 bars, then crimped in a nozzle as shown in Example 1 and dried at 105 ° C.
• Example 2 Example 3
• Example 3 Witness title to the strand 2.3 2.26 2.22 2.7 residual shrinkage 115 ° C in oil% 6 5.1 4.2 12 tenacity CN / tex 21.8 22.3 22.9 18 elongation% 36 34 31 65
• the shrinkage constraint which expresses the degree of orientation of the yarns is measured by means of a retractometer: the samples of filaments of length 4 cm, assembled in the form of test pieces of 400 dtex on average (each test being carried out on two test pieces) are subjected, after each of the different stages of drawing, stabilization and finally of shrinking, to a temperature rise of 1 ° C per minute, from 30 ° C to 170 ° C.
• the retraction force expressed in 10 ⁇ 2 g / dtex is measured on each test piece as a function of the temperature.
• This withdrawal constraint or withdrawal force in each case passes through a maximum at a certain temperature. It is this maximum withdrawal force which represents the molecular orientation characteristic of the products, which is designated by withdrawal constraint.
• a fiber whose titer has been determined is subjected to a tensile test until it reaches a fully relaxed state (detection on the force / elongation curve).
• yarns of fibers are prepared, the characteristics of which are as follows: the invention NM 20 witness the invention NM 50 witness Title (tex) 51.81 52.1 19.65 impossible to achieve NM 19.30 19.19 50.88 CV Uster% 9.57 12.19 15.10 - Imperfections over 1000m: - fine points 0 0 27 - - big dots 2 10 43 - - buttons 3 6 68 - breaking force (cN) 696 416.8 208.4 - CV breaking force 6.14 18.8 10.36 - Elongation at break % 26.7 29.3 21.25 - Fracture toughness cN / tex 13.4 8 11.43 -

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Artificial Filaments (AREA)
• Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
• Woven Fabrics (AREA)

Applications Claiming Priority (2)

Publications (2)

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Family Applications (1)

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• 1991
  • 1991-08-23 FR FR9110704A patent/FR2680525B1/fr not_active Expired - Fee Related
• 1992
  • 1992-08-20 JP JP4221732A patent/JP2535124B2/ja not_active Expired - Lifetime
  • 1992-08-21 CA CA002076586A patent/CA2076586A1/fr not_active Abandoned
  • 1992-08-21 ES ES92420282T patent/ES2117657T3/es not_active Expired - Lifetime
  • 1992-08-21 EP EP92420282A patent/EP0530119B1/de not_active Expired - Lifetime
  • 1992-08-21 AT AT92420282T patent/ATE165124T1/de not_active IP Right Cessation
  • 1992-08-21 DE DE69225099T patent/DE69225099T2/de not_active Expired - Fee Related

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