Classifications

• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
  • D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
  • D06M11/59—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with ammonia; with complexes of organic amines with inorganic substances
  • D06M11/60—Ammonia as a gas or in solution
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
  • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
  • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
  • D06M15/41—Phenol-aldehyde or phenol-ketone resins
  • D06M15/415—Phenol-aldehyde or phenol-ketone resins modified by compounds containing phosphorus
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
  • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
  • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
  • D06M15/423—Amino-aldehyde resins
  • D06M15/43—Amino-aldehyde resins modified by phosphorus compounds
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
  • D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
  • D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
  • D06M15/423—Amino-aldehyde resins
  • D06M15/43—Amino-aldehyde resins modified by phosphorus compounds
  • D06M15/431—Amino-aldehyde resins modified by phosphorus compounds by phosphines or phosphine oxides; by oxides or salts of the phosphonium radical
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
  • D06M2101/02—Natural fibres, other than mineral fibres
  • D06M2101/04—Vegetal fibres
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
  • D06M2101/02—Natural fibres, other than mineral fibres
  • D06M2101/04—Vegetal fibres
  • D06M2101/06—Vegetal fibres cellulosic
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
  • D06M2101/16—Synthetic fibres, other than mineral fibres
  • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • D06M2101/32—Polyesters
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
  • D06M2101/16—Synthetic fibres, other than mineral fibres
  • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • D06M2101/34—Polyamides
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
  • D06M2200/30—Flame or heat resistance, fire retardancy properties

Definitions

• the invention relates to a process for the flame-retardant finishing of fiber materials.
• the object of the present invention was to develop a process with which fiber materials, in particular textile fabrics, are effectively flame-retarded using of tetrakis-hydroxymethyl-phosphonium compounds or their condensation products can be equipped with organic nitrogen compounds, without that after the implementation of the process, a high content of formaldehyde is present on the fiber materials or forms later.
• the inventive method makes it possible to provide textile fabrics of fiber material very effective flame retardant and still keep the use of suitable amounts of solution A on the fiber material, the content of formaldehyde, which is present after carrying out the process, low, ie to a maximum value of 150 ppm or even at most 100 ppm, based on the total weight of the fiber material.
• the flame-retardant properties of the fiber materials which can be achieved by the process according to the invention have good permanence over washing processes.
• step e the application of the aqueous solution A is carried out later than step e). It is advantageous if, after carrying out the flame-retardant finishing of textile fabrics, the phosphorus content on the fabric is only slightly lower than the value obtained directly after the application of the phosphorus compound and the subsequent drying. The reason is that a higher phosphorus content leads to a more effective flame retardant effect. With the method according to the invention it is possible to achieve not only effective flame retardant properties but also a pleasantly soft feel of the fiber materials.
• the method steps a) to e) are carried out continuously in succession.
• the fiber materials which are treated by the process according to the invention are preferably textile fabrics, in particular in the form of woven or nonwovens. They can consist of synthetic fibers such as polyester or polyamide or of natural fibers such as cotton. There are also mixtures of different fibers into consideration.
• the fiber materials are from 50 to 100% by weight of cellulosic fibers such as e.g. Cotton or regenerated cellulose. The remaining 0 to 50% by weight may be synthetic fibers, e.g. Polyester fibers or polyamide fibers.
• a particular advantage of the method according to the invention is that the method makes it possible, after the treatment of the fiber materials, to achieve a low formaldehyde content on the fiber materials, namely a content of 150 ppm or less, based on the total weight of the fiber material.
• the first step (step a) of the process according to the invention is to apply an aqueous mixture to the fiber material, preferably to a textile fabric in the form of a nonwovens or nonwovens.
• the application of the aqueous mixture to the fiber material can be carried out by methods generally known in textile finishing or finishing.
• An application via a padding process is well suited.
• the liquor used for padding can contain the tetrakis-hydroxymethyl-phosphonium compound described in greater detail below in a concentration which is customary for flameproofing equipment. The concentration in this case will depend, among other things, on the level of the desired flame-retardant effect.
• the aqueous mixture applied to the fiber material in step a) contains, in addition to water, a tetrakis-hydroxymethyl-phosphonium compound, which is referred to below as "THP", or a product which is formed by reacting THP with an organic nitrogen compound. It can also contain both types of these products, ie a mixture of THP and said THP reaction product. Further, the aqueous mixture may contain other products known for textile finishing. Examples of these are oil and / or water repellents, such as fluorine-containing polymers and / or polysiloxanes, or known softeners, or known cellulosic crosslinkers, such as are used for crease-resistant finishing of cellulosic materials.
• THP tetrakis-hydroxymethyl-phosphonium compound
• X ⁇ is an anion and t is the valence of this anion.
• Suitable anions X are, for example, sulfate, hydrogen sulfate, phosphate, mono- or dihydrogen phosphate or acetate.
• anion X ⁇ is the chloride anion.
• the aqueous mixture used in process step a) may also contain a product which is formed by reacting THP with an organic nitrogen compound. It can also be a mixture of THP and such a THP reaction product.
• Suitable THP reaction products are, for example, those which are formed by reacting THP with melamine, dicyandiamide, urea or thiourea or by reacting THP with a mixture containing two or more products of the type mentioned.
• a product which is formed by condensation reaction of THP with urea with tetrakis-hydroxymethyl-phosphonium chloride being preferred as THP P ⁇ (CH 2 OH) 4 Cl ⁇ is used.
• THP compounds in particular the chloride, are available on the market and can be prepared by generally known processes.
• Step a) of the process according to the invention is followed by process step b), in which the fiber material is dried.
• This drying is preferably carried out under conditions such that the fiber material after carrying out step b) has a water content of at least 3% by weight.
• the upper limit for the water content after drying is preferably 25% by weight.
• the value for the water content here is based on the total weight of the fiber material after carrying out step b).
• Step b) is followed by step c). It consists in a treatment of the fiber material with ammonia.
• Ammonia can be used for this purpose as a gas or as a solution in a solvent.
• water is well suited. It is also possible to treat the fiber material both with gaseous and with dissolved ammonia, these two treatment steps can be carried out sequentially.
• the fiber material is treated in step c) with an aqueous ammonia solution, it is then preferably dried, suitably so that it has a water content of 5 to 25 wt.%, Based on the total weight of the fiber material after drying.
• Step c) can be carried out under conditions which are known from the prior art, for example from US-A 2,983,623 and the US-A 2,772,188 ,
• step d) of the process according to the invention is not absolutely necessary, but is preferably carried out and consists in the treatment of the fiber material with an oxidizing agent. Suitable for this purpose are metal peroxides, perborates, air or oxygen. It is particularly preferred to carry out step d) of the process according to the invention with an aqueous solution of hydrogen peroxide. This solution suitably contains 0.1 to 20% by weight of H 2 O 2 , and the fiber material is preferably immersed in this solution for a time between 20 and 90 seconds. Suitable process conditions for this oxidation step go from "Example 1" of US-A 2,983,623 from column 3, lines 20 to 27 of US Pat. No.
• step d) is advantageous because it makes it possible to increase the permanence of the flame-retardant effects and to adjust the free formaldehyde content on the fiber material to lower values after the end of the process.
• step e The fiber material obtained after step d) of the process according to the invention is washed in the next step, process step e).
• This washing is carried out with an aqueous solution having a pH of at least 7.5, preferably in the range of 7.5 to 12.0, at 20 ° C.
• inorganic salts may be used, for example sodium carbonate.
• the washing process can be carried out, for example, by dipping the fiber material in the aqueous solution for a period of 1 to 90 minutes, and preferably during the immersion phase brings about a mechanical movement of the aqueous solution.
• additional washing processes may also be carried out in the course of the process according to the invention, for example between step c) and step d) and / or between step d) and step e).
• the aqueous solution A has a pH at 20 ° C in the acidic range, namely in the range of 0.5 to 6.5, preferably from 1.5 to 5.5, either from the beginning or after the heating process described. This is caused by ingredients in the solution A.
• phosphoric acid e.g. also be used sulfuric acid.
• sulfuric acid e.g. also be used sulfuric acid.
• monoammonium phosphate or a mixture of dicyandiamide and phosphoric acid are also suitable as ingredients of the aqueous solution A. Of course, several of the compounds mentioned in the solution A may be present.
• the treatment of the fiber material with the solution A can for example be such that directly after step e) the fiber material is rinsed with water and spun and that it is then treated with an acidic bath containing solution A, which in turn is a step e ) and drying, eg at 110 ° C, followed.
• Another suitable process variant is to first dry the fiber material after step e) and then treat it with solution A by padding. It is then advisable to store the material at room temperature for about 20-25 hours or to briefly heat it to a temperature of 140 ° C - 170 ° C. This is preferably followed again by a step e).
• the aqueous solution A contains a product which binds formaldehyde.
• products which can chemically bind formaldehyde nitrogen compounds such as amines or acid amides are suitable. These are converted by reaction with formaldehyde into the corresponding N-methylol compounds.
• An example of a suitable product is dicyandiamide (cyanoguanidine)
• Particularly suitable as a formaldehyde-binding product is urea.
• a preferred embodiment of the method according to the invention is therefore characterized in that the aqueous solution A contains urea.
• a fabric of 100% cotton (dyed blue) was treated in step a) with an aqueous solution of a THPC adduct.
• the THPC adduct was an adduct of tetrakis-hydroxymethyl-phosphonium chloride and urea used as an about 75 wt% solution in water.
• the treatment of the fabric was done by padding, wherein 500 g of said adduct per liter of liquor were used.
• the padder liquor contained 4 g / l triethanolamine and 5 g / l of a wetting agent.
• the liquor pickup at padding was about 78% by weight, based on untreated fabric.
• the tissue samples were dried and treated via padding with solutions A, as described in Example 2. Following the padding, a portion of the samples were stored at room temperature for 20 hours, another portion heated to 160 ° C. for a few minutes. Then, a step e) (afterwashing with soda solution as described in Example 2) was repeated, followed by drying (10 minutes / 110 ° C). The determination of the formaldehyde content showed values of about 40 ppm for the samples stored for 20 hours and about 45 ppm for the samples heated to 160 ° C.

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• 2007
  • 2007-05-11 EP EP07009463A patent/EP1990468A1/fr not_active Withdrawn
• 2008
  • 2008-05-07 BR BRPI0807106-3A patent/BRPI0807106A2/pt not_active IP Right Cessation
  • 2008-05-07 EP EP08749364A patent/EP2145044B1/fr not_active Not-in-force
  • 2008-05-07 WO PCT/EP2008/003644 patent/WO2008138523A2/fr active Application Filing
  • 2008-05-07 AT AT08749364T patent/ATE538240T1/de active
  • 2008-05-07 CN CN200880004968A patent/CN101627158A/zh active Pending
  • 2008-05-07 MX MX2009010326A patent/MX2009010326A/es active IP Right Grant
  • 2008-05-07 KR KR1020097017049A patent/KR20100014793A/ko not_active Application Discontinuation
  • 2008-05-07 US US12/599,712 patent/US20100304030A1/en not_active Abandoned

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