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
  • D01F6/02—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
• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
  • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
  • A01N37/10—Aromatic or araliphatic carboxylic acids, or thio analogues thereof; Derivatives thereof
• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
  • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
  • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
  • A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
  • A01N47/22—O-Aryl or S-Aryl esters thereof
• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
  • A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
• • 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
  • D01F1/00—General methods for the manufacture of artificial filaments or the like
  • D01F1/02—Addition of substances to the spinning solution or to the melt
  • D01F1/10—Other agents for modifying properties
  • D01F1/103—Agents inhibiting growth of microorganisms

Definitions

• the invention relates to acaricidal polymer fibers, their manufacturing process and their applications.
• Dust mites are well known today for causing a number of direct or indirect pathologies in humans and animals.
• One of the essential scourges that we seek to overcome is that of allergies, in particular allergies to dust mites. It is well known that mites feed mainly on human and animal dander as well as various molds.
• One of their favorite places for development is made up of textile wall and floor coverings, but also and above all bedding.
• fibers will denote both the fibers themselves and all the textile products such as filaments, threads, fibers, hairs, cables, obtained by spinning both dry and wet. polymer solutions.
• spinning products for example carded, combed or drawn ribbons, fiber yarns, etc.
• polymeric fibers means both fibers consisting of a single polymer or copolymer and fibers consisting of a mixture of polymers and / or copolymers.
• polymeric material constituting the polymeric fiber one also understands mixtures of polymer (s) and / or copolymer (s), when the fibers consist of such a mixture.
• the inventors of the present invention have now developed new fibers with acaricidal activity which have the advantage of a high persistence of their acaricidal properties as well as a particularly flexible method of preparation.
• the inventors of the present invention have developed new polymeric fibers containing, distributed homogeneously within them, well-defined proportions of particular acaricide agents allowing obtaining a residual acaricide activity while allowing a particularly advantageous process for obtaining since these fibers can be obtained by spinning a collodion incorporating within it well-defined proportions of said acaricide agent.
• the invention relates to textile products obtained by spinning a solution based on polymers as well as products obtained after spinning of said products, consisting of a polymeric material containing in its mass a effective amount of at least one miticide agent chosen from benzyl benzoate, carbamates, pyrethroids and pyrethrins.
• the acaricide agent is present in the fiber in proportions of between 1 and 30 phr (per cent of resin), expressed by weight relative to the total weight of the polymeric material. Concentrations of acaricide agent of between 5 and 30 pcr will preferably be chosen, more preferably concentrations of between 10 and 20 pcr.
• the acaricide agent used will be chosen from benzyl benzoate, carbamates, pyrethroids and pyrethrins, compounds which are particularly appreciated for their effectiveness with regard to mites and their harmlessness.
• Benzyl benzoate will advantageously be chosen for economic reasons.
• other products from the families mentioned above can also be used. Mention will be made, more particularly, of carbaryl and permethrin.
• the polymers constituting said polymeric materials may be synthetic, natural polymers or derivatives of natural polymers.
• synthetic polymeric materials constituting the fibers it is preferable to choose polymers or copolymers chosen from the family consisting of polyvinyl chloride, chlorinated polyvinyl chloride, polyvinylidene chloride, acrylic polymers, cellulose acetate, cellulose and mixtures thereof.
• the polymeric material will advantageously consist of polyvinyl chloride or a mixture of polyvinyl chloride and chlorinated polyvinyl chloride. Chlorofibres denote fibers based on this type of polymeric material.
• An example of a natural polymer which can be used according to the invention is cellulose.
• viscose As an example of a polymer derived from a natural polymer, mention will be made of viscose.
• the invention relates not only to fibers incorporating therein an acaricidal agent giving them acaricidal properties. It also relates to a process for the preparation of these fibers.
• Such a process advantageously comprises a first step of solubilization of the polymer in an appropriate solvent, in which at least one acaricide agent is also dissolved, and a second step of obtaining the fiber with dry or wet extraction of said solvent.
• a first step of solubilization of the polymer in an appropriate solvent in which at least one acaricide agent is also dissolved
• a second step of obtaining the fiber with dry or wet extraction of said solvent are understood to mean: - dry extraction, a process in which the solvent is extracted by evaporation,
• the method generally also comprises a step of regenerating said natural polymer.
• the invention also relates to the process intended for the preparation of the fibers described above.
• fibers are advantageously obtained by a process comprising a wet or dry spinning step of a gel in which the acaricide agent defined above is found.
• This process will also include, where appropriate, a step of spinning the preceding product.
• Those skilled in the art will choose the type of spinning method, dry or wet, depending on the nature of the polymer used.
• the dry route is preferred for the transformation of
• PVC acetone / carbon sulfide solvent or acetone / benzene
• cellulose acetate acetone solvent
• the wet process is preferred for obtaining acrylic fibers (solvent: dimethylformamide) or cellulose fibers (solvent: N - methyl morpholine oxide or viscose process).
• the polymers from the polyvinyl chloride (PVC) family will be chosen, as well as mixtures of polyvinyl chloride and chlorinated polyvinyl chloride.
• PVC a PVC of molecular weight in number of between 50,000 and 120,000 and the fiber will advantageously be produced according to the method described in European patent EP 0091384, the acaricide agent preferably being dissolved beforehand in the solvent or mixture of solvents before introduction PVC in said solvent or mixture of solvents.
• the acaricide agent may be introduced into any fiber based on a mixture of PVC and PVCC, capable of being obtained by wet or dry spinning of a gel containing such a mixture and in which this acaricide agent is dissolved beforehand.
• the fibers For the production of fibers based on mixtures of PVC and PVCC, it is advantageous to choose mixtures containing from 5 to 80% by weight of a polymer or of a mixture of chlorinated vinyl chloride polymers, having a transition temperature of the second order greater than or equal to 100 ° C.
• the fibers can then be obtained by any known method of dry or wet spinning of a gel containing this mixture.
• the acaricide agent is then advantageously dissolved in the solvent used for the preparation of the gel before dissolution of the polymer mixture.
• the acaricide agent is then advantageously dissolved in the solvent used for the preparation of the gel before dissolution of the polymer mixture.
• PVCC is present in an amount of 17 to 20% by weight relative to the mixture in said mixture and the fibers are obtained under the conditions described in the European patent application EP-A-0530119.
• the polymer fibers can of course contain, in addition to the polymer and the acaricide agent, all the additives conventionally added, in particular in the case of textile fibers.
• additives for example, mention will be made of whitening and mattifying agents intended to thermally stabilize polymers, anti UV agents and pigments.
• the fibers of the invention may also incorporate products with antibacterial or bactericidal activity intended to confer on said fibers properties complementary to acaricide properties. These products with antibacterial or bactericidal properties will advantageously be chosen from products soluble in the gel used for the preparation of the fibers of the invention.
• the fibers of the invention can be used, alone or in admixture with other fibers, for the preparation of different materials, in particular knitted, woven or nonwoven textile products.
• the invention also relates to fibrous materials incorporating fibers as described above.
• fibrous materials means any material incorporating the fibers of the invention, in particular knitted fabrics, woven or nonwoven textiles.
• Fibers can be used, alone or in admixture with other types of fibers, to prepare different fibrous materials, for the production in particular of wall fabrics, floor coverings (carpets, rugs), bedding items such as sheets, duvet and upholstery covers, in particular for filling mattresses, pillows, duvets.
• Miticide fibers can be used for the manufacture of knitted, woven or non-woven articles.
• the fibers and materials of the invention find a particularly advantageous application for the production of various products for filling household objects, such as in particular pillows, cushions, mattresses, duvets.
• Example 1 Preparation of Different Chlorofibers Based on PVC / PVCC Mixtures a) A PVC / PVCC fiber is prepared from PVC with a viscosity index of between 113 and 115 (measured according to standard NFT 51013) and from PVCC to 69 % of chlorine and viscosity index of the order of 100 measured according to standard NFT 51013.
• the two polymers are mixed in proportions of 80 parts by weight of PVC for 20 parts by weight of PVCC.
• a gel containing approximately 30% by weight of polymer is prepared by dissolving in a mixer at room temperature, the corresponding amount of mixture of the two polymers in a solvent consisting of an acetone / carbon sulphide mixture in a 50/50 by volume ratio. , in which a quantity of benzyl benzoate representing 5 pcr, expressed by weight relative to the resin, has previously been dissolved, in the proportions given below. This test is noted A in Table 1 given in Example 5 below.
• a chlorofiber is prepared from a PVC with a viscosity index of between 113 and 115 (measured according to standard NFT 51013).
• a mixture of solvents consisting of acetone and CS2 in proportions 50-50 by volume is introduced into a mixer fitted with a marine propeller, and 5 parts by weight are then added relative to the benzoate resin (pcr). benzyl.
• the above mixture is homogenized for 24 h.
• PVC is introduced into this mixture at a rate of 30% by weight.
• the PVC / solvent mixture is stored in a buffer mixer and the procedure is then carried out according to European patent EP-034 548 introduced here by reference.
• the gel is then heated to 120 ° C, filtered, cooled to 80 ° C, then extruded through a die of 1,200 holes.
• the solvent is extracted by evaporation in hot air.
• the cable is then stretched at 100 ° C in water, vapor stabilized under
• EXAMPLE 3 Cellulose Acetate Fiber A cellulose acetate gel 2.5 to 30% by weight is produced in acetone, into which 10 phr of benzyl benzoate are introduced. This gel is extruded through a die of 80 holes with a diameter of 60 ⁇ m. Drying is ensured by air circulation at 80 ° C under the die. The recovered yarn is dried. The test is noted H in Table 4 of Example 5.
• An acrylic fiber is prepared containing 10 phr of benzyl benzoate relative to the acrylic polymer, by operating as follows.
• a commercial acrylic polymer based on acrylonitrile, methyl methacrylate and sodium sulfonate is suspended in DMF, in which the acaricide has previously been dissolved. This suspension is carried out at a temperature of 3 ° C to allow degassing, then dissolution is brought about by increasing the temperature up to 20 ° C.
• the gel formed contains 25% of acrylic polymer. It is extruded through a die of 150 holes 55 ⁇ m in diameter. The wire then undergoes the following treatment:
• the species used for the tests is Dermatophagoid farinae.
• the mites used come from laboratory strains raised under the following conditions: 25 ° C - 75% relative humidity (RH).
• Four test tubes (repetitions) per product are infested.
• a series of untreated surfaces (filter paper) is produced for each of the supports.
• Mites are removed from breeding environments and sorted using a heat gradient in order to recover the most active individuals, then are deposited on the surfaces (approximately 100 to 200).
• Reinfestations take place 30, 60 and 90 days (noted time T30, T60, T90 in the tables below) after the first infestation with healthy mites and mortality is monitored 24 hours a day after 24 hours after these contacts.
• the controls are carried out by counting under a binocular magnifier; this count is not an estimate because all the mites are counted.
• the mortality percentages obtained will be considered validated if the mortality of the control lots is less than 15%.
• Tables 1, 2 and 3 below respectively give the results obtained with knits produced with the fibers of Example 1 (A and B), of Example 2a, 2b and 2c (C, D and E) and of Example 2d and 2e (F and G) in comparison with a control product and with a knitted fabric of control fibers denoted respectively T1 and T2 obtained respectively with the same collodions and under the same conditions as in Examples 1 and 2 but do not containing no miticide agent.
• Table 3 gives the results obtained with knits produced with the fibers of Examples 3 and 4 (tests H and I) in comparison with a control product.

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• Life Sciences & Earth Sciences (AREA)
• Engineering & Computer Science (AREA)
• General Health & Medical Sciences (AREA)
• Dentistry (AREA)
• Environmental Sciences (AREA)
• Zoology (AREA)
• Wood Science & Technology (AREA)
• Agronomy & Crop Science (AREA)
• Pest Control & Pesticides (AREA)
• Plant Pathology (AREA)
• Health & Medical Sciences (AREA)
• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Textile Engineering (AREA)
• General Chemical & Material Sciences (AREA)
• Manufacturing & Machinery (AREA)
• Artificial Filaments (AREA)
• Agricultural Chemicals And Associated Chemicals (AREA)

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• 1998
  • 1998-01-20 FR FR9800548A patent/FR2773823B1/fr not_active Expired - Fee Related
• 1999
  • 1999-01-20 AU AU20603/99A patent/AU2060399A/en not_active Abandoned
  • 1999-01-20 EP EP99900961A patent/EP1049825A1/de not_active Withdrawn
  • 1999-01-20 JP JP2000540300A patent/JP2002509201A/ja active Pending
  • 1999-01-20 WO PCT/FR1999/000102 patent/WO1999036601A1/fr not_active Ceased

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