WO2015101312A1 - Flame retardant working solution and flame retardant finishing method for pure cotton fabrics and/or cotton-polyester blend fabrics - Google Patents

Flame retardant working solution and flame retardant finishing method for pure cotton fabrics and/or cotton-polyester blend fabrics Download PDF

Info

Publication number
WO2015101312A1
WO2015101312A1 PCT/CN2014/095774 CN2014095774W WO2015101312A1 WO 2015101312 A1 WO2015101312 A1 WO 2015101312A1 CN 2014095774 W CN2014095774 W CN 2014095774W WO 2015101312 A1 WO2015101312 A1 WO 2015101312A1
Authority
WO
WIPO (PCT)
Prior art keywords
flame retardant
flame
retardant
cotton
polyester
Prior art date
Application number
PCT/CN2014/095774
Other languages
French (fr)
Chinese (zh)
Inventor
黄尚东
郭玉良
卢霜
李世琪
朱泉
Original Assignee
广东德美精细化工股份有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 广东德美精细化工股份有限公司 filed Critical 广东德美精细化工股份有限公司
Publication of WO2015101312A1 publication Critical patent/WO2015101312A1/en

Links

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
    • 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
    • D06M15/667—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing phosphorus in the main chain
    • 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/282—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
    • D06M13/292—Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
    • 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/44—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen containing nitrogen and phosphorus
    • D06M13/447—Phosphonates or phosphinates containing nitrogen atoms
    • 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
    • D06M15/432—Amino-aldehyde resins modified by phosphorus compounds by phosphonic acids or derivatives thereof
    • 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 flame-retardant finishing process of a polyester-cotton blended fabric, in particular to a flame-retardant working fluid for a pure cotton fabric and/or a polyester-cotton blended fabric and a flame-retardant finishing method using the flame-retardant working fluid.
  • polyester-cotton blended fabrics The flammability of polyester-cotton blended fabrics is larger than that of pure cotton and pure polyester fabrics, and the flame retardant finishing technology is particularly difficult. This is because the burning properties of both polyester and cotton fibers are different, and the combustion process becomes more complicated after blending.
  • the polyester burns, it becomes molten, and after the cotton fiber burns, it becomes a support body, so that the melt spreads on the support, which increases the contact area with the air, and causes the combustion of the fabric to be more intense, so-called "wicking effect".
  • the polyester melt fails to break away from the fabric, so that the self-extinguishing property of the polyester fiber is prolonged until the cracked product can not be burned, so that the after-burning time is greatly lengthened.
  • polyester-cotton blended fabrics are difficult to achieve flame retardancy is the mutual heat induction of the two polymers of polyester and cotton or their cracking products, which accelerates the overflow of cracked products, so the speed of burning of polyester-cotton fabrics is higher than that of pure polyester and pure cotton. It is much faster; at the same time, in the combustion process, the flame retardant will migrate between the two components of polyester and cotton, and the mutual influence will be different with the difference of the blending ratio, resulting in more complicated and varied combustion process.
  • the main method is to flame-retard each component of the fabric, but the polyester part of the flame retardant finishing still uses pure polyester fabric flame retardant, which is used for polyester/cotton fabrics.
  • Most of the flame retardant finishing is adsorbed by cotton fibers, and such flame retardants are difficult to transfer from cotton fibers to polyester fibers like disperse dyes. Therefore, it is difficult to use polyester when using the baking and baking method or the dyeing and bathing method.
  • the flame retardant is fixed to the polyester fiber of the blended fabric, so that it does not give good flame retardancy.
  • the present invention provides a flame-retardant working fluid and a finishing method using the same, which is formed by a reaction between a phosphorus-based polyester-cotton flame retardant and a nitrogen-containing crosslinking agent.
  • Polyester fiber surface for excellent flame retardancy
  • the flame-retardant working fluid of the invention can also react with cotton fibers to reduce the burning performance of the cotton fibers. Since the flame-retardant working fluid of the invention acts as a flame retardant for both fibers, mutual interference between different flame retardants is avoided, and a very good flame retarding effect is achieved.
  • the fabric finished by the finishing method of the present invention has a long-lasting flame retarding effect due to film formation on the surface of the fiber or covalent bond crosslinking reaction with the fiber.
  • the present invention provides a flame retardant working fluid comprising the following components: a flame retardant and a crosslinking agent, the balance being water; and the concentration of the flame retardant in the flame retardant working fluid is in the range of 200 ⁇ 600g / L, the concentration of the cross-linking agent is in the range of 30 ⁇ 100g / L; wherein the flame retardant is selected from the flame retardant Pyrovatex CP (N-hydroxymethyl-3-(dimethoxyphosphonyl) Propionamide), flame retardant Pyrovatex HP, flame retardant RDP (resorcinol tetraphenyl diphosphate, CAS accession number 57583-54-), flame retardant BDP (bisphenol A bis(diphenyl phosphate) Ester), CAS accession number 5945-33-5), one or more of reactive halogen-free flame retardant DOPO, cyclic phosphate flame retardant, cotton flame retardant DM-3070;
  • the agent is selected from one or more of
  • the concentration of the crosslinking agent ranges from 80 g/L.
  • the flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant.
  • the crosslinking agent is dimethylol dihydroxyethylene urea resin (abbreviated as 2D resin).
  • a mass ratio of the flame retardant Pyrovatex HP and a cyclic phosphate flame retardant is (1 to 10): 1; preferably, the flame retardant
  • the mass ratio of the Pyrovatex HP to the cyclic phosphate flame retardant was 2:1.
  • a flame retardant working fluid comprising the following components: a flame retardant and a crosslinking agent, and the balance being water; wherein the concentration of the flame retardant ranges from 200 to 600 g/ L, preferably 300 to 600 g/L, particularly preferably 600 g/L; the concentration of the crosslinking agent is in the range of 30 to 100 g/L, preferably 80 g/L; and the flame retardant is a flame retardant Pyrovatex HP and a ring
  • the phosphate ester flame retardant is mixed at a mass ratio of (1 to 4):1; the crosslinking agent is dimethylol dihydroxyethylene urea resin (abbreviated as 2D resin).
  • the mass ratio of the flame retardant Pyrovatex HP to the cyclic phosphate flame retardant is preferably 2:1.
  • a flame retardant working fluid comprising the following components: a flame retardant and a crosslinking agent, the balance being water, and the concentration of the flame retardant is 600g / L, the cross-linking agent concentration is 80g / L; wherein the flame retardant is a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant mixed in a mass ratio of 2:1
  • the crosslinking agent is a 2D resin.
  • the invention also provides the application of the above flame retardant working fluid in the flame retardant finishing of pure cotton fabric and/or polyester-cotton blended fabric.
  • the invention also provides a flame-retardant finishing method for a polyester-cotton blended fabric, wherein the flame-retardant finishing method is to dip and dip the polyester-cotton blended fabric in the above flame-retardant working fluid, with a liquid ratio (50-120%), Dry at 100-120 ° C, bake at 140-180 ° C for 0.5 to 5 minutes, then wash with water and then dry.
  • the flame-retardant finishing method is to dip and dip the polyester-cotton blend fabric in the above flame-retardant working fluid, with a liquid ratio (50-120%), drying at 100 ° C, and baking at 150 ° C for 3-4 minutes. After that, wash and then dry.
  • the method before the step of "washing and drying" of the flame-retardant finishing method, the method further comprises the steps of: dip and distilling the polyester-cotton blended fabric in the flame retardant working fluid of the cotton fabric with a liquid ratio of 50 % ⁇ 120%, 80 ⁇ 120 ° C drying, 140 ⁇ 180 ° C baking 0.5 ⁇ 5 minutes.
  • the cotton fabric flame-retardant working fluid comprises the following components: cotton flame retardant DM-3070, magnesium chloride catalyst and cross-linking agent, and the rest is water; the concentration of the cotton flame retardant DM-3070 is 300 g/L, The concentration of the magnesium chloride catalyst was 40 g/L, and the concentration of the crosslinking agent was 80 g/L.
  • the polyester-cotton blended fabric needs to be subjected to two flame-retardant finishings, once by the flame-retardant working solution of the present invention, and once by the above-mentioned cotton fabric flame-retardant working solution. .
  • the drying step in the flame-retardant finishing method of the above-mentioned polyester-cotton blended fabric may be replaced by a stacking step, that is, the flame-retardant finishing method is to mix the polyester-cotton blend fabric
  • the flame-retardant working fluid is immersed in two times, with a liquid ratio (50-120%), stacked for 8-24 hours, baked at 140-180 ° C for 0.5-5 minutes, washed with water and then dried.
  • the stacking step has a stacking time of 16 hours.
  • the invention also provides a flame-retardant finishing method for pure cotton fabric, which is to dip two-rolled pure cotton textile in a flame-retardant working fluid, the liquid ratio is 50%-120%, drying at 80-120 °C, 140 After baking at -180 ° C for 0.5 to 5 minutes, washing with water and drying; wherein the flame-retardant working solution comprises the following components: a flame retardant and a crosslinking agent, and the balance is water;
  • the concentration of the flame retardant ranges from 200 to 600 g/L, particularly preferably 330 g/L; the concentration of the crosslinking agent ranges from 30 to 100 g/L, particularly preferably 80 g/L; and the flame retardant is flame retardant
  • the reagent Pyrovatex HP and the cyclic phosphate flame retardant are mixed at a mass ratio of 10:1; the crosslinking agent is a dimethylol dihydroxyethylene urea resin.
  • the flame-retardant working fluid of the invention and the finishing method using the same adopting the phosphorus-based polyester cotton flame retardant and a
  • the nitrogen cross-linking agent reacts to form a film, and combines the padding method to make the flame retardant in the flame-retardant working solution adsorb and wrap on the surface of the polyester fiber, and forms on the surface of the polyester fiber under the cross-linking agent and a certain temperature condition.
  • a layer of flame-retardant film that not only reduces the flammability of polyester fibers, but also prevents the formation of melts when polyester fibers are burned, thus completely solving the "wicking effect" of polyester-cotton blended fabrics.
  • the flame-retardant working fluid to which the present invention is applied can simultaneously react with cotton fibers to achieve durable flame retardancy of the cotton fibers.
  • both polyester-cotton fibers use the same flame retardant, even if burned, it can overcome the migration between the flame retardants of the flame retardant fixed on the polyester and cotton fibers under high temperature conditions.
  • the technical problem of reducing the flame retardant performance, therefore, the flame retardant working fluid of the invention is a perfect solution for achieving durable flame retardant of different blending ratio polyester/cotton fabrics.
  • the polyester-cotton fabric obtained by applying the flame-retardant working fluid and the finishing method of the invention has good flame retardant effect and washing durability, and the polyester-cotton fabric is tested by GB/T 5455-1997, and the after-burning after 30 washings and The smoldering time is less than 5 seconds, the damage length is less than 15 cm, and it reaches B1 according to GB/T 17591-2006 "flame retardant fabric" standard. It can be widely used for flame retardant finishing of clothing, tents, decorative fabrics and vehicle fabrics.
  • the applicant tested and evaluated the burning performance of the finished polyester-cotton blended fabric obtained in the different examples.
  • the following are the standards for measurement methods and evaluation methods.
  • the flame retardant performance of the fabric is evaluated according to GB/T 17591-2006 "flame retardant fabric" standard, wherein the B1 flame retardant standard is: continuous burning time ⁇ 5s, smoldering time ⁇ 5s, damage length ⁇ 150mm.
  • the Applicant tested different amounts of flame retardant in the flame retardant working fluid of the present invention.
  • the flame-retardant working fluid comprises the following components: a flame retardant and a crosslinking agent, and the balance is water, the concentration of the flame retardant is 300-600 g/L, and the concentration of the crosslinking agent is 80g/L.
  • the flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant in a ratio of (1 to 4):1 by mass;
  • the crosslinking agent is a 2D resin.
  • the swatches are made of polyester cotton yarn cards (116 x 46, 20 s x 16 s , blend ratio 50: 50).
  • the flame retardant finishing is as follows: the swatches are immersed in the flame retardant working solution twice, dried at 100 ° C, and baked at 150 ° C for 3 minutes; then washed with hot water, washed with cold water and dried to obtain polyester wool after flame retardant finishing. Blended fabric.
  • the flame-retardant working liquid of the present embodiment is used for the flame-retardant finishing of the polyester-cotton blended fabric, and the initial flame retardant performance is excellent, and the flame retardant performance is not significantly decreased after 10 washings. It is indicated that the polyester-cotton blended fabric after the flame retardant finishing of the flame retardant working fluid of the embodiment has obtained a very good long-lasting flame retardant effect.
  • Example 2 Stacking method flame retardant finishing method
  • the applicant has tested the stacking method flame-retardant finishing method of the present invention.
  • the flame retardant working fluid comprises the following components: a flame retardant and a crosslinking agent, the balance being water, a concentration of the flame retardant of 600 g/L, and a concentration of the crosslinking agent of 80 g/L.
  • the flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant in a ratio of 2:1 by mass;
  • the crosslinking agent is a 2D resin.
  • the swatches are made of polyester cotton yarn cards (116 x 46, 20 s x 16 s , blend ratio 50: 50).
  • the flame retardant finishing is as follows: the cloth sample is immersed and immersed in the flame retardant working solution for two hours, stacked for 16 hours, and baked at 150 ° C for 4 minutes; then washed with hot water, washed with cold water and dried to obtain a polyester cotton after flame retardant finishing. Blended fabric.
  • the polyester-cotton blended fabric after flame retardant finishing by the stacking method flame retardant finishing method of the present embodiment has excellent excellent flame retardant performance in the initial state, and has no flame retardant property after 10 washings. Significant decline. It is indicated that the polyester-cotton blended fabric after flame-retardant finishing by the stacking method flame-retardant finishing method of the present embodiment has obtained a very good long-term flame retardant effect.
  • the applicant has flame retardant effect on the polyester-cotton blended fabric after flame retardant finishing of the flame retardant working fluid of the present invention. Fruit and its durability were tested.
  • the flame retardant working fluid comprises the following components: a flame retardant and a crosslinking agent, and the balance is water, the concentration of the flame retardant is 600 g/L, and the concentration of the crosslinking agent is 80 g/ L.
  • the flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant in a ratio of 2:1 by mass; the crosslinking agent is a 2D resin.
  • the swatches are made of polyester cotton yarn cards (116 x 46, 20 s x 16 s , blend ratio 50: 50).
  • the flame retardant finishing is as follows: the swatches are immersed in the flame retardant working solution twice, dried at 100 ° C, and baked at 150 ° C for 3 minutes; then, the swatches are woven in the cotton fabric flame retardant working fluid (cotton flame retardant DM- 3070300g / L, magnesium chloride catalyst 40g / L, 2D resin 80g / L) two dip two rolling, 100 ° C drying, baking at 160 ° C for 3 minutes; then hot water wash, cold water wash and air dry, after the flame retardant finishing Polyester-cotton blend fabric.
  • the swatches are immersed in the flame retardant working solution twice, dried at 100 ° C, and baked at 150 ° C for 3 minutes; then, the swatches are woven in the cotton fabric flame retardant working fluid (cotton flame retardant DM- 3070300g / L, magnesium chloride catalyst 40g / L, 2D resin 80g / L) two dip two rolling, 100 ° C drying, baking at
  • the flame-retardant working liquid of the present embodiment is used for the flame-retardant finishing of the polyester-cotton blended fabric, and the initial flame retardant performance is excellent, and the flame retardant performance is not significantly decreased after 10 times and 30 times of washing. It is indicated that the polyester-cotton blended fabric after the flame retardant finishing of the flame retardant working fluid of the embodiment has obtained a very good long-lasting flame retardant effect.
  • the applicant tested the flame retardant effect and durability of the polyester/cotton fabric of different blending ratios after the flame retardant finishing of the flame retardant working fluid of the present invention.
  • the flame retardant working fluid comprises the following components: a flame retardant and a crosslinking agent, and the balance is water, the concentration of the flame retardant is 600 g/L, and the concentration of the crosslinking agent is 80 g/ L.
  • the flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant in a ratio of 2:1 by mass; the crosslinking agent is a 2D resin.
  • the swatches were made of polyester-cotton knitted double-sided cloth (35 ⁇ cylinder, yarn roving 32 s , blending ratio 65: 35).
  • the flame retardant finishing is as follows: the swatches are immersed in the flame retardant working solution twice, dried at 100 ° C, and baked at 150 ° C for 3 minutes; then, the swatches are woven in the cotton fabric flame retardant working fluid (cotton flame retardant DM- 3070300g / L, magnesium chloride catalyst 40g / L, 2D resin 80g / L) two dip two rolling, 100 ° C drying, baking at 160 ° C for 3 minutes; then hot water wash, cold water wash and dry, obtained A polyester-cotton blended fabric that has been flame-retarded.
  • the swatches are immersed in the flame retardant working solution twice, dried at 100 ° C, and baked at 150 ° C for 3 minutes; then, the swatches are woven in the cotton fabric flame retardant working fluid (cotton flame retardant DM- 3070300g / L, magnesium chloride catalyst 40g / L, 2D resin 80g / L) two dip two rolling, 100 ° C
  • the flame-retardant working fluid and the flame-retardant finishing process of the present embodiment have obvious effects on the polyester-cotton knitted fabrics of different blending ratios.
  • the polyester/cotton knitted fabric after flame retardant finishing has excellent initial flame retardant performance, and the flame retardant performance does not decrease significantly after 10 washings. It is indicated that the polyester-cotton knitted fabric after the flame-retardant working liquid of the flame-retardant working liquid of the embodiment has obtained a very good long-term flame retardant effect.
  • the Applicant also tested the flame retardancy and durability of the cotton fabric finished with the flame retardant working fluid of the present invention.
  • the flame-retardant working fluid comprises the following components: a flame retardant and a crosslinking agent, the balance being water, the concentration of the flame retardant is 330 g/L, and the concentration of the crosslinking agent is 80 g/L.
  • the flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant at a mass ratio of 10:1; the crosslinking agent is a 2D resin.
  • the swatches are made of pure cotton yarn cards (128 x 60, 20 s x 16 s ).
  • the flame retardant finishing is as follows: the swatches are immersed in the flame retardant working solution twice, dried at 100 ° C, and baked at 150 ° C for 3 minutes; then washed with hot water, washed with cold water and dried to obtain polyester wool after flame retardant finishing. Blended fabric.
  • the flame retardant working fluid of the present invention can also be applied to a cotton fabric.
  • the cotton fabric finished by the flame-retardant working fluid of the present invention also has excellent flame retardant properties, and is flame-retarded after 10 and 30 washings. There is no significant drop in performance. It is indicated that the pure cotton fabric after the flame-retardant finishing of the flame-retardant working fluid of the invention has a very good long-term flame retardant effect.
  • the flame-retardant working fluid of the invention and the finishing method using the flame-retardant working fluid, the film is formed by reacting a phosphorus-based polyester-cotton flame retardant with a nitrogen-containing crosslinking agent, and the finishing process of the padding method is used to make the flame-retardant work
  • the flame retardant in the liquid adsorbs and wraps on the surface of the polyester fiber, and forms a flame-retardant flame-retardant film on the surface of the polyester fiber under the cross-linking agent and a certain temperature condition, the film not only reduces the burning property of the polyester fiber At the same time, it can prevent the melted material from being generated when the polyester fiber is burned, thereby completely solving the "wicking effect" of the polyester-cotton blended fabric.
  • the flame-retardant working fluid to which the present invention is applied can simultaneously react with cotton fibers to achieve durable flame retardancy of the cotton fibers.
  • both polyester-cotton fibers use the same flame retardant, even if burned, it can overcome the migration between the flame retardants of the flame retardant fixed on the polyester and cotton fibers under high temperature conditions.
  • the technical problem of reducing the flame retardant performance, therefore, the flame retardant working fluid of the invention is a perfect solution for achieving durable flame retardant of different blending ratio polyester/cotton fabrics.
  • the polyester-cotton fabric obtained by applying the flame-retardant working fluid and the finishing method of the invention has good flame retardant effect and washing durability, and the polyester-cotton fabric is tested by GB/T 5455-1997, and the after-burning after 30 washings and The smoldering time is less than 5 seconds, the damage length is less than 15 cm, and it reaches B1 according to GB/T 17591-2006 "flame retardant fabric" standard. It can be widely used for flame retardant finishing of clothing, tents, decorative fabrics and vehicle fabrics.

Abstract

Provided are a flame retardant working solution and flame retardant finishing method for pure cotton fabrics and/or cotton-polyester blend fabrics employing the flame retardant working solution. The flame retardant working solution comprises the following components: a flame retardant, a crosslinking agent, and the balance being water; the flame retardant in the flame retardant working solution has the concentration of 200-600 g/L, and the crosslinking agent has the concentration of 30-100 g/L. Cotton-polyester fabrics or pure cotton fabrics obtained by employing the flame retardant working solution and finishing method has good flame retardant effect and good washing resistance; the cotton-polyester fabrics pass through the GB/T 5455-1997 test, with the afterflaming time and smoldering time of less than 5 seconds after being washed thirty times, and a damaged length of less than 15 centimeters, reaching level B1 according to the GB/T 17591-2006 "flame retarded fabrics" standards, and can be widely used in flame retardant finishing of clothing, tents, upholstery fabrics and fabrics for transportation vehicles.

Description

一种阻燃工作液及纯棉织物和/或涤棉混纺织物的阻燃整理方法Flame-retardant working liquid and flame-retardant finishing method of pure cotton fabric and/or polyester-cotton blended fabric 技术领域Technical field
本发明涉及一种涤棉混纺织物的阻燃整理工艺，具体涉及一种针对纯棉织物和/或涤棉混纺织物的阻燃工作液及应用该阻燃工作液的阻燃整理方法。The invention relates to a flame-retardant finishing process of a polyester-cotton blended fabric, in particular to a flame-retardant working fluid for a pure cotton fabric and/or a polyester-cotton blended fabric and a flame-retardant finishing method using the flame-retardant working fluid.
背景技术Background technique
涤棉混纺织物的可燃性比纯棉和纯涤纶织物都大，其阻燃整理技术的难度特别高。这是因为涤纶和棉两种纤维的燃烧性能各异，混纺后使燃烧过程变得更为复杂。涤纶燃烧时成为熔融状态，而棉纤维燃烧后炭化成为了支撑体，使熔融物在支撑体上铺展，增大了与空气的接触面积，造成织物的燃烧更加剧烈，即所谓“烛芯效应”。另外，涤纶熔融物未能脱离织物，使涤纶纤维的自熄性延长，直到裂解产物不能燃烧为止才能自灭，从而使续燃时间大大加长。The flammability of polyester-cotton blended fabrics is larger than that of pure cotton and pure polyester fabrics, and the flame retardant finishing technology is particularly difficult. This is because the burning properties of both polyester and cotton fibers are different, and the combustion process becomes more complicated after blending. When the polyester burns, it becomes molten, and after the cotton fiber burns, it becomes a support body, so that the melt spreads on the support, which increases the contact area with the air, and causes the combustion of the fabric to be more intense, so-called "wicking effect". . In addition, the polyester melt fails to break away from the fabric, so that the self-extinguishing property of the polyester fiber is prolonged until the cracked product can not be burned, so that the after-burning time is greatly lengthened.
涤棉混纺织物难以实现阻燃化的另一个原因涤纶和棉两种聚合物或它们的裂解产物的相互热诱导，加速了裂解产物的溢出，因此涤棉织物的着火速度比纯涤和纯棉都快得多；同时在燃烧过程中，阻燃剂会在涤和棉两种组分间迁移，而且随着混纺比例的不同导致相互影响也不一样，导致燃烧过程更加复杂多变。Another reason why polyester-cotton blended fabrics are difficult to achieve flame retardancy is the mutual heat induction of the two polymers of polyester and cotton or their cracking products, which accelerates the overflow of cracked products, so the speed of burning of polyester-cotton fabrics is higher than that of pure polyester and pure cotton. It is much faster; at the same time, in the combustion process, the flame retardant will migrate between the two components of polyester and cotton, and the mutual influence will be different with the difference of the blending ratio, resulting in more complicated and varied combustion process.
目前降低涤棉混纺织物的可燃性，主要采用的方法是将织物中的每一组分都进行阻燃整理，但涤纶部分阻燃整理仍然使用纯涤纶织物阻燃剂，它用于涤棉织物阻燃整理时大部分被棉纤维吸附，而这类阻燃剂难以类似分散染料一样从棉纤维转移到涤纶纤维上，因此无论是使用轧焙烘法还是染色同浴法整理，都难以将涤纶阻燃剂固着在混纺织物的涤纶纤维上，从而无法使其获得很好的阻燃性。如果使用阻燃涤纶纤维，由于织物需要经过一系列的加工才能到成品，在加工过程中已造成大部分阻燃剂脱落，阻燃性能也会明显下降。当前对涤棉混纺织物阻燃整理的研究很多，但很少见到有工业化生产，都是基于以上原因不能彻底解决。要实现涤棉织物具有永久性的阻燃性能，首要任务是解决混纺织物中的涤纶纤维具有很好的阻燃效果，并且不产生熔滴物。At present, the flammability of polyester-cotton blended fabrics is reduced. The main method is to flame-retard each component of the fabric, but the polyester part of the flame retardant finishing still uses pure polyester fabric flame retardant, which is used for polyester/cotton fabrics. Most of the flame retardant finishing is adsorbed by cotton fibers, and such flame retardants are difficult to transfer from cotton fibers to polyester fibers like disperse dyes. Therefore, it is difficult to use polyester when using the baking and baking method or the dyeing and bathing method. The flame retardant is fixed to the polyester fiber of the blended fabric, so that it does not give good flame retardancy. If flame-retardant polyester fiber is used, since the fabric needs to undergo a series of processing to obtain the finished product, most of the flame retardant has been peeled off during the processing, and the flame retardant performance is also significantly reduced. At present, there are many researches on the flame retardant finishing of polyester-cotton blended fabrics, but it is rare to see industrialized production, which cannot be completely solved based on the above reasons. In order to achieve permanent flame retardant properties of polyester-cotton fabrics, the primary task is to solve the polyester fiber in the blended fabric with good flame retardant effect and no droplets.
因此，有需要提供一种新的、专门针对涤棉混纺织物的阻燃工作液及应用该阻燃工作液的阻燃整理方法，可以解决涤棉混纺织物阻燃整理困难的技术问题，获得一种阻燃效果好的涤棉混纺织物。Therefore, there is a need to provide a new flame retardant working fluid specifically for polyester-cotton blended fabrics and a flame retardant finishing method using the flame retardant working fluid, which can solve the technical problem of difficult flame retardant finishing of polyester-cotton blended fabrics, and obtain a A kind of polyester-cotton blended fabric with good flame retardant effect.
发明内容Summary of the invention
为解决现有技术的不足，本发明提出一种阻燃工作液及应用该阻燃工作液的整理方法，通过磷系涤棉阻燃剂与一种含氮交联剂反应成膜并包裹在涤纶纤维表面，产生优异的阻燃 效果和耐洗性，可防止涤纶纤维燃烧时产生熔融物，大大降低混纺织物燃烧的剧烈性。同时本发明的阻燃工作液也可以与棉纤维反应，降低棉纤维的燃烧性能。由于本发明的阻燃工作液对两种纤维都起到阻燃作用，因此避免了不同阻燃剂间的相互干扰，起到非常好的阻燃效果。同时，由于在纤维的表面成膜或与纤维发生共价键交联反应，使得应用本发明的整理方法整理的织物具有长久的阻燃效果。In order to solve the deficiencies of the prior art, the present invention provides a flame-retardant working fluid and a finishing method using the same, which is formed by a reaction between a phosphorus-based polyester-cotton flame retardant and a nitrogen-containing crosslinking agent. Polyester fiber surface for excellent flame retardancy The effect and the washing resistance can prevent the melt from being generated when the polyester fiber is burned, and the burning of the blended fabric is greatly reduced. At the same time, the flame-retardant working fluid of the invention can also react with cotton fibers to reduce the burning performance of the cotton fibers. Since the flame-retardant working fluid of the invention acts as a flame retardant for both fibers, mutual interference between different flame retardants is avoided, and a very good flame retarding effect is achieved. At the same time, the fabric finished by the finishing method of the present invention has a long-lasting flame retarding effect due to film formation on the surface of the fiber or covalent bond crosslinking reaction with the fiber.
为了达到上述目的，本发明提供一种阻燃工作液，包含以下组份：阻燃剂和交联剂，其余为水；所述阻燃工作液中所述阻燃剂的浓度范围为200～600g/L，所述交联剂的浓度范围为30～100g/L；其中，所述阻燃剂选自阻燃剂Pyrovatex CP(N-羟甲基-3-(二甲氧基膦酰基)丙酰胺)、阻燃剂Pyrovatex HP、阻燃剂RDP(间苯二酚四苯基二磷酸酯，CAS登录号为57583-54-)、阻燃剂BDP(双酚A双(二苯基磷酸酯)，CAS登录号为5945-33-5)、反应型无卤阻燃剂DOPO、环状磷酸酯阻燃剂、棉阻燃剂DM-3070中的一种或几种；所述交联剂选自二羟甲基二羟基乙烯脲树脂(简称2D树脂)、三羟甲基三聚氰胺树脂、六羟甲基三聚氰胺树脂及其醚化物中的一种或几种。In order to achieve the above object, the present invention provides a flame retardant working fluid comprising the following components: a flame retardant and a crosslinking agent, the balance being water; and the concentration of the flame retardant in the flame retardant working fluid is in the range of 200 ～ 600g / L, the concentration of the cross-linking agent is in the range of 30 ~ 100g / L; wherein the flame retardant is selected from the flame retardant Pyrovatex CP (N-hydroxymethyl-3-(dimethoxyphosphonyl) Propionamide), flame retardant Pyrovatex HP, flame retardant RDP (resorcinol tetraphenyl diphosphate, CAS accession number 57583-54-), flame retardant BDP (bisphenol A bis(diphenyl phosphate) Ester), CAS accession number 5945-33-5), one or more of reactive halogen-free flame retardant DOPO, cyclic phosphate flame retardant, cotton flame retardant DM-3070; The agent is selected from one or more of a dimethylol dihydroxyethylene urea resin (abbreviated as 2D resin), a trimethylol melamine resin, a hexamethylol melamine resin, and an ether compound thereof.
在本发明一实施例中，所述交联剂的浓度范围为80g/L。In an embodiment of the invention, the concentration of the crosslinking agent ranges from 80 g/L.
在本发明一实施例中，所述阻燃剂为阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂的混合物。In an embodiment of the invention, the flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant.
在本发明一实施例中，所述交联剂为二羟甲基二羟基乙烯脲树脂(简称2D树脂)。In an embodiment of the invention, the crosslinking agent is dimethylol dihydroxyethylene urea resin (abbreviated as 2D resin).
在本发明一实施例中，在所述阻燃剂中，所述阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂的质量比为(1～10):1；优选地，所述阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂的质量比为2:1。In an embodiment of the present invention, in the flame retardant, a mass ratio of the flame retardant Pyrovatex HP and a cyclic phosphate flame retardant is (1 to 10): 1; preferably, the flame retardant The mass ratio of the Pyrovatex HP to the cyclic phosphate flame retardant was 2:1.
在本发明一较佳实施例中，提供一种阻燃工作液，包含以下组份：阻燃剂和交联剂，其余为水；其中，所述阻燃剂的浓度范围为200～600g/L，优选300～600g/L，特别优选600g/L；所述交联剂的浓度范围为30～100g/L，优选80g/L；并且，所述阻燃剂为阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂以质量比为(1～4):1的比例混合而成；所述交联剂为二羟甲基二羟基乙烯脲树脂(简称2D树脂)。In a preferred embodiment of the present invention, a flame retardant working fluid is provided, comprising the following components: a flame retardant and a crosslinking agent, and the balance being water; wherein the concentration of the flame retardant ranges from 200 to 600 g/ L, preferably 300 to 600 g/L, particularly preferably 600 g/L; the concentration of the crosslinking agent is in the range of 30 to 100 g/L, preferably 80 g/L; and the flame retardant is a flame retardant Pyrovatex HP and a ring The phosphate ester flame retardant is mixed at a mass ratio of (1 to 4):1; the crosslinking agent is dimethylol dihydroxyethylene urea resin (abbreviated as 2D resin).
在上述较佳实施例中，所述阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂的质量比优选为2:1。In the above preferred embodiment, the mass ratio of the flame retardant Pyrovatex HP to the cyclic phosphate flame retardant is preferably 2:1.
在本发明一极其优选的实施例中，提供一种阻燃工作液，所述阻燃工作液包含以下组份：阻燃剂和交联剂，其余为水，所述阻燃剂的浓度为600g/L，所述交联剂浓度为80g/L；其中，所述阻燃剂是阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂以质量比为2:1的比例混合 而成；所述交联剂为2D树脂。In a highly preferred embodiment of the present invention, a flame retardant working fluid is provided, the flame retardant working fluid comprising the following components: a flame retardant and a crosslinking agent, the balance being water, and the concentration of the flame retardant is 600g / L, the cross-linking agent concentration is 80g / L; wherein the flame retardant is a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant mixed in a mass ratio of 2:1 The crosslinking agent is a 2D resin.
本发明还提供上述阻燃剂工作液在纯棉织物和/或涤棉混纺织物的阻燃整理中的应用。The invention also provides the application of the above flame retardant working fluid in the flame retardant finishing of pure cotton fabric and/or polyester-cotton blended fabric.
本发明还提供一种涤棉混纺织物的阻燃整理方法，所述阻燃整理方法是将涤棉混纺织物在上述阻燃工作液中二浸二轧，带液率(50～120％)，100～120℃烘干，140～180℃焙烘0.5～5分钟后，水洗再烘干。优选地，所述阻燃整理方法是将涤棉混纺织物在上述阻燃工作液中二浸二轧，带液率(50～120％)，100℃烘干，150℃焙烘3～4分钟后，水洗再烘干。The invention also provides a flame-retardant finishing method for a polyester-cotton blended fabric, wherein the flame-retardant finishing method is to dip and dip the polyester-cotton blended fabric in the above flame-retardant working fluid, with a liquid ratio (50-120%), Dry at 100-120 ° C, bake at 140-180 ° C for 0.5 to 5 minutes, then wash with water and then dry. Preferably, the flame-retardant finishing method is to dip and dip the polyester-cotton blend fabric in the above flame-retardant working fluid, with a liquid ratio (50-120%), drying at 100 ° C, and baking at 150 ° C for 3-4 minutes. After that, wash and then dry.
本发明一实施例中，在上述阻燃整理方法的“水洗再烘干”步骤之前还包含以下步骤：将涤棉混纺织物在棉织物阻燃工作液中二浸二轧，带液率为50％～120％，80～120℃烘干，140～180℃焙烘0.5～5分钟。其中，所述棉织物阻燃工作液包含以下组份：棉阻燃剂DM-3070、氯化镁催化剂和交联剂，其余为水；所述棉阻燃剂DM-3070的浓度为300g/L，所述氯化镁催化剂的浓度为40g/L，所述交联剂的浓度为80g/L。In an embodiment of the present invention, before the step of "washing and drying" of the flame-retardant finishing method, the method further comprises the steps of: dip and distilling the polyester-cotton blended fabric in the flame retardant working fluid of the cotton fabric with a liquid ratio of 50 % ~ 120%, 80 ~ 120 ° C drying, 140 ~ 180 ° C baking 0.5 ~ 5 minutes. Wherein, the cotton fabric flame-retardant working fluid comprises the following components: cotton flame retardant DM-3070, magnesium chloride catalyst and cross-linking agent, and the rest is water; the concentration of the cotton flame retardant DM-3070 is 300 g/L, The concentration of the magnesium chloride catalyst was 40 g/L, and the concentration of the crosslinking agent was 80 g/L.
也就是说，在本发明一实施例中，涤棉混纺织物需要经过两次阻燃整理，一次是以本发明的阻燃工作液进行整理，另一次是以上述棉织物阻燃工作液进行整理。That is to say, in an embodiment of the present invention, the polyester-cotton blended fabric needs to be subjected to two flame-retardant finishings, once by the flame-retardant working solution of the present invention, and once by the above-mentioned cotton fabric flame-retardant working solution. .
在本发明一可选的实施例中，可以将上述涤棉混纺织物的阻燃整理方法中烘干步骤替换为堆置步骤，也就是说，所述阻燃整理方法是将涤棉混纺织物在上述阻燃工作液中二浸二轧，带液率(50～120％)，堆置8-24小时，140～180℃焙烘0.5～5分钟后，水洗再烘干。优选地，所述堆置步骤的堆置时间为16小时。In an optional embodiment of the present invention, the drying step in the flame-retardant finishing method of the above-mentioned polyester-cotton blended fabric may be replaced by a stacking step, that is, the flame-retardant finishing method is to mix the polyester-cotton blend fabric The above-mentioned flame-retardant working fluid is immersed in two times, with a liquid ratio (50-120%), stacked for 8-24 hours, baked at 140-180 ° C for 0.5-5 minutes, washed with water and then dried. Preferably, the stacking step has a stacking time of 16 hours.
本发明还提供一种纯棉织物的阻燃整理方法，是将纯棉纺织物在阻燃工作液中二浸二轧，带液率为50％～120％，80～120℃烘干，140～180℃焙烘0.5～5分钟后，水洗再烘干；其中，所述阻燃工作液包含以下组份：阻燃剂和交联剂，其余为水；所述阻燃工作液中所述阻燃剂的浓度范围为200～600g/L，特别优选330g/L；所述交联剂的浓度范围为30～100g/L，特别优选80g/L；并且，所述阻燃剂是阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂以质量比为10:1的比例混合而成；所述交联剂为二羟甲基二羟基乙烯脲树脂。The invention also provides a flame-retardant finishing method for pure cotton fabric, which is to dip two-rolled pure cotton textile in a flame-retardant working fluid, the liquid ratio is 50%-120%, drying at 80-120 °C, 140 After baking at -180 ° C for 0.5 to 5 minutes, washing with water and drying; wherein the flame-retardant working solution comprises the following components: a flame retardant and a crosslinking agent, and the balance is water; The concentration of the flame retardant ranges from 200 to 600 g/L, particularly preferably 330 g/L; the concentration of the crosslinking agent ranges from 30 to 100 g/L, particularly preferably 80 g/L; and the flame retardant is flame retardant The reagent Pyrovatex HP and the cyclic phosphate flame retardant are mixed at a mass ratio of 10:1; the crosslinking agent is a dimethylol dihydroxyethylene urea resin.
需要说明的是，本发明中所述的试剂均是有市售的产品，其中所述棉阻燃剂DM-3070是广东德美精细化工股份有限公司对外市售的产品。所述阻燃剂Pyrovatex HP的分子式为
Figure PCTCN2014095774-appb-000001
名称为羟乙基磷酸酯缩聚物，是阿克苏诺贝尔公司(Akzonobel)生产的一款阻燃剂。It should be noted that all the reagents described in the present invention are commercially available products, wherein the cotton flame retardant DM-3070 is a commercially available product of Guangdong Demei Fine Chemical Co., Ltd. The molecular formula of the flame retardant Pyrovatex HP is
Figure PCTCN2014095774-appb-000001
The name is hydroxyethyl phosphate polycondensate, a flame retardant produced by Akzonobel.
本发明的阻燃工作液及应用该阻燃工作液的整理方法，通过磷系涤棉阻燃剂与一种含 氮交联剂反应成膜，结合浸轧法的整理工艺，使阻燃工作液中的阻燃剂吸附并包裹在涤纶纤维表面，并在交联剂和一定温度条件下，在涤纶纤维表面形成一层具有耐洗性的阻燃膜，该膜不仅降低涤纶纤维的燃烧性，同时可防止涤纶纤维燃烧时产生熔融物，从而彻底解决了涤棉混纺织物的“烛芯效应”。另外，应用本发明的阻燃工作液可以同时与棉纤维反应，实现棉纤维的耐久阻燃性。在本发明中，由于涤棉两种纤维都使用了同一种阻燃剂，即使燃烧起来，也能够克服阻燃剂在高温条件下固着在涤和棉纤维上的阻燃剂发生组分间迁移而使阻燃性能下降的技术问题，因此本发明的阻燃工作液是一种不同混纺比例涤棉织物实现耐久阻燃的完美解决方案。The flame-retardant working fluid of the invention and the finishing method using the same, adopting the phosphorus-based polyester cotton flame retardant and a The nitrogen cross-linking agent reacts to form a film, and combines the padding method to make the flame retardant in the flame-retardant working solution adsorb and wrap on the surface of the polyester fiber, and forms on the surface of the polyester fiber under the cross-linking agent and a certain temperature condition. A layer of flame-retardant film that not only reduces the flammability of polyester fibers, but also prevents the formation of melts when polyester fibers are burned, thus completely solving the "wicking effect" of polyester-cotton blended fabrics. In addition, the flame-retardant working fluid to which the present invention is applied can simultaneously react with cotton fibers to achieve durable flame retardancy of the cotton fibers. In the present invention, since both polyester-cotton fibers use the same flame retardant, even if burned, it can overcome the migration between the flame retardants of the flame retardant fixed on the polyester and cotton fibers under high temperature conditions. The technical problem of reducing the flame retardant performance, therefore, the flame retardant working fluid of the invention is a perfect solution for achieving durable flame retardant of different blending ratio polyester/cotton fabrics.
应用本发明的阻燃工作液及整理方法获得的涤棉织物具有很好的阻燃效果和耐洗性，该涤棉织物通过GB/T 5455-1997测试，三十次洗涤后的续燃和阴燃时间小于5秒，损毁长度小于15厘米，按照GB/T 17591-2006《阻燃织物》标准达到B1级，可广泛用于服装、帐篷、装饰织物和交通工具用织物的阻燃整理。The polyester-cotton fabric obtained by applying the flame-retardant working fluid and the finishing method of the invention has good flame retardant effect and washing durability, and the polyester-cotton fabric is tested by GB/T 5455-1997, and the after-burning after 30 washings and The smoldering time is less than 5 seconds, the damage length is less than 15 cm, and it reaches B1 according to GB/T 17591-2006 "flame retardant fabric" standard. It can be widely used for flame retardant finishing of clothing, tents, decorative fabrics and vehicle fabrics.
具体实施方式detailed description
以下结合实施例对本发明做详细的说明，实施例旨在解释而非限定本发明的技术方案。The invention is described in detail below with reference to the embodiments, which are intended to be illustrative and not restrictive.
为了检验本发明的阻燃工作液及应用该阻燃工作液的阻燃整理方法的效果，申请人对不同实施例中获得的整理后的涤棉混纺织物进行了燃烧性能的测试及评价。以下为测量方法和评价方法的标准。In order to test the effect of the flame-retardant working fluid of the present invention and the flame-retardant finishing method using the flame-retardant working fluid, the applicant tested and evaluated the burning performance of the finished polyester-cotton blended fabric obtained in the different examples. The following are the standards for measurement methods and evaluation methods.
①织物的燃烧性能按照GB/T 5455-1997《纺织品燃烧性能试验-垂直法》标准测定。1 The burning performance of the fabric is determined in accordance with GB/T 5455-1997 "Textile Combustion Performance Test - Vertical Method".
②织物的阻燃性能评价按照GB/T 17591-2006《阻燃织物》标准评定，其中，B1级阻燃标准为：续燃时间≤5s，阴燃时间≤5s，损毁长度≤150mm。2 The flame retardant performance of the fabric is evaluated according to GB/T 17591-2006 "flame retardant fabric" standard, wherein the B1 flame retardant standard is: continuous burning time ≤ 5s, smoldering time ≤ 5s, damage length ≤ 150mm.
③织物的洗涤方法按照GB/T 17595-1998《织物燃烧试验前的洗涤程序》标准中B型洗衣机洗涤程序洗涤。3 The washing method of the fabric is washed according to the washing procedure of the type B washing machine in the standard GB/T 17595-1998 "Washing procedure before fabric burning test".
实施例1.阻燃剂不同用量的比较Example 1. Comparison of different amounts of flame retardant
在本实施例中，申请人对本发明的阻燃工作液中阻燃剂的不同用量进行测试。In this example, the Applicant tested different amounts of flame retardant in the flame retardant working fluid of the present invention.
在本实施例中，所述阻燃工作液包含以下组份：阻燃剂和交联剂，其余为水，所述阻燃剂的浓度为300～600g/L，所述交联剂浓度为80g/L。其中，所述阻燃剂是阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂以质量比为(1～4):1的比例混合而成；所述交联剂为2D树脂。In this embodiment, the flame-retardant working fluid comprises the following components: a flame retardant and a crosslinking agent, and the balance is water, the concentration of the flame retardant is 300-600 g/L, and the concentration of the crosslinking agent is 80g/L. Wherein, the flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant in a ratio of (1 to 4):1 by mass; the crosslinking agent is a 2D resin.
在本实施例中，布样采用涤棉纱卡(116×46，20s×16s，混纺比50：50)。In this embodiment, the swatches are made of polyester cotton yarn cards (116 x 46, 20 s x 16 s , blend ratio 50: 50).
阻燃整理如下：将布样在阻燃工作液中二浸二轧，100℃烘干，150℃焙烘3分钟；然后热水洗、冷水洗并晾干，获得经阻燃整理后的涤棉混纺织物。 The flame retardant finishing is as follows: the swatches are immersed in the flame retardant working solution twice, dried at 100 ° C, and baked at 150 ° C for 3 minutes; then washed with hot water, washed with cold water and dried to obtain polyester wool after flame retardant finishing. Blended fabric.
将经阻燃整理后的涤棉混纺织物按照GB/T 17595-1998《织物燃烧试验前的洗涤程序》标准中B型洗衣机洗涤程序洗涤10次后对其阻燃性能进行测试。测试结果如表1所示。The flame-retardant properties of the polyester-cotton blended fabric after the flame-retardant finishing were tested according to the washing procedure of the B-type washing machine in the washing procedure of GB/T 17595-1998 "Washing procedure before fabric burning test" 10 times. The test results are shown in Table 1.
表1.经不同阻燃剂用量的阻燃工作液整理后的涤棉纱卡的阻燃性能对比Table 1. Comparison of flame retardant properties of polyester/cotton yarn cards after finishing with flame retardant working fluids with different flame retardant dosages
Figure PCTCN2014095774-appb-000002
Figure PCTCN2014095774-appb-000002
由表1可以看出，应用本实施例的阻燃工作液进行阻燃整理后的涤棉混纺织物，初始的阻燃性能优秀，经10次洗涤后阻燃性能没有明显下降。说明经本实施例的阻燃工作液阻燃整理后的涤棉混纺织物获得了非常好的长久阻燃效果。It can be seen from Table 1 that the flame-retardant working liquid of the present embodiment is used for the flame-retardant finishing of the polyester-cotton blended fabric, and the initial flame retardant performance is excellent, and the flame retardant performance is not significantly decreased after 10 washings. It is indicated that the polyester-cotton blended fabric after the flame retardant finishing of the flame retardant working fluid of the embodiment has obtained a very good long-lasting flame retardant effect.
实施例2.堆置法阻燃整理方法Example 2. Stacking method flame retardant finishing method
在本实施例中，申请人对本发明的堆置法阻燃整理方法进行了测试。In the present embodiment, the applicant has tested the stacking method flame-retardant finishing method of the present invention.
在本实施例中，阻燃工作液包含以下组份：阻燃剂和交联剂，其余为水，所述阻燃剂的浓度为600g/L，所述交联剂浓度为80g/L。其中，所述阻燃剂是阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂以质量比为2:1的比例混合而成；所述交联剂为2D树脂。In this embodiment, the flame retardant working fluid comprises the following components: a flame retardant and a crosslinking agent, the balance being water, a concentration of the flame retardant of 600 g/L, and a concentration of the crosslinking agent of 80 g/L. Wherein, the flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant in a ratio of 2:1 by mass; the crosslinking agent is a 2D resin.
在本实施例中，布样采用涤棉纱卡(116×46，20s×16s，混纺比50：50)。In this embodiment, the swatches are made of polyester cotton yarn cards (116 x 46, 20 s x 16 s , blend ratio 50: 50).
阻燃整理如下：将布样在阻燃工作液中二浸二轧，堆置16小时，150℃焙烘4分钟；然后热水洗、冷水洗并晾干，获得经阻燃整理后的涤棉混纺织物。The flame retardant finishing is as follows: the cloth sample is immersed and immersed in the flame retardant working solution for two hours, stacked for 16 hours, and baked at 150 ° C for 4 minutes; then washed with hot water, washed with cold water and dried to obtain a polyester cotton after flame retardant finishing. Blended fabric.
将经阻燃整理后的涤棉混纺织物按照GB/T 17595-1998《织物燃烧试验前的洗涤程序》标准中B型洗衣机洗涤程序洗涤10次后对其阻燃性能进行测试。测试结果如表2所示。The flame-retardant properties of the polyester-cotton blended fabric after the flame-retardant finishing were tested according to the washing procedure of the B-type washing machine in the washing procedure of GB/T 17595-1998 "Washing procedure before fabric burning test" 10 times. The test results are shown in Table 2.
表2.经本发明的堆置法阻燃整理后的涤棉纱卡的阻燃性能对比Table 2. Comparison of flame retardant properties of polyester/cotton yarn cards after flame retardant finishing by the stacking method of the present invention
Figure PCTCN2014095774-appb-000003
Figure PCTCN2014095774-appb-000003
由表2可以看出，经本实施例的堆置法阻燃整理方法阻燃整理后的涤棉混纺织物，初始状态下同样具有优异的阻燃性能优秀，经10次洗涤后阻燃性能没有明显下降。说明经本实施例的堆置法阻燃整理方法阻燃整理后的涤棉混纺织物获得了非常好的长久阻燃效果。It can be seen from Table 2 that the polyester-cotton blended fabric after flame retardant finishing by the stacking method flame retardant finishing method of the present embodiment has excellent excellent flame retardant performance in the initial state, and has no flame retardant property after 10 washings. Significant decline. It is indicated that the polyester-cotton blended fabric after flame-retardant finishing by the stacking method flame-retardant finishing method of the present embodiment has obtained a very good long-term flame retardant effect.
实施例3.阻燃效果的耐久性Example 3. Durability of flame retardant effect
在本实施例中，申请人对经本发明的阻燃工作液阻燃整理后的涤棉混纺织物的阻燃效 果及其耐久性进行了测试。In the present embodiment, the applicant has flame retardant effect on the polyester-cotton blended fabric after flame retardant finishing of the flame retardant working fluid of the present invention. Fruit and its durability were tested.
在本实施例中，所述阻燃工作液包含以下组份：阻燃剂和交联剂，其余为水，所述阻燃剂的浓度为600g/L，所述交联剂浓度为80g/L。其中，所述阻燃剂是阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂以质量比为2:1的比例混合而成；所述交联剂为2D树脂。In this embodiment, the flame retardant working fluid comprises the following components: a flame retardant and a crosslinking agent, and the balance is water, the concentration of the flame retardant is 600 g/L, and the concentration of the crosslinking agent is 80 g/ L. Wherein, the flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant in a ratio of 2:1 by mass; the crosslinking agent is a 2D resin.
在本实施例中，布样采用涤棉纱卡(116×46，20s×16s，混纺比50：50)。In this embodiment, the swatches are made of polyester cotton yarn cards (116 x 46, 20 s x 16 s , blend ratio 50: 50).
阻燃整理如下：将布样在阻燃工作液中二浸二轧，100℃烘干，150℃焙烘3分钟；接着，将布样在棉织物阻燃工作液(棉阻燃剂DM-3070300g/L，氯化镁催化剂40g/L、2D树脂80g/L)中二浸二轧，100℃烘干，160℃焙烘3分钟；然后热水洗、冷水洗并晾干，获得经阻燃整理后的涤棉混纺织物。The flame retardant finishing is as follows: the swatches are immersed in the flame retardant working solution twice, dried at 100 ° C, and baked at 150 ° C for 3 minutes; then, the swatches are woven in the cotton fabric flame retardant working fluid (cotton flame retardant DM- 3070300g / L, magnesium chloride catalyst 40g / L, 2D resin 80g / L) two dip two rolling, 100 ° C drying, baking at 160 ° C for 3 minutes; then hot water wash, cold water wash and air dry, after the flame retardant finishing Polyester-cotton blend fabric.
将经阻燃整理后的涤棉混纺织物按照GB/T 17595-1998《织物燃烧试验前的洗涤程序》标准中B型洗衣机洗涤程序洗涤10次和30次后对其阻燃性能进行测试。测试结果如表3所示。The flame-retardant properties of the polyester-cotton blended fabric after the flame-retardant finishing were tested according to the washing procedure of the B-type washing machine in the GB/T 17595-1998 "washing procedure before the fabric burning test" standard for 10 times and 30 times. The test results are shown in Table 3.
表3.经本发明的阻燃工作液阻燃整理后的涤棉纱卡的阻燃耐久性对比Table 3. Comparison of flame retardant durability of polyester/cotton yarn cards after flame retardant finishing of flame retardant working fluid of the present invention
Figure PCTCN2014095774-appb-000004
Figure PCTCN2014095774-appb-000004
由表3可以看出，应用本实施例的阻燃工作液进行阻燃整理后的涤棉混纺织物，初始的阻燃性能优秀，经10次和30次洗涤后阻燃性能没有明显下降。说明经本实施例的阻燃工作液阻燃整理后的涤棉混纺织物获得了非常好的长久阻燃效果。It can be seen from Table 3 that the flame-retardant working liquid of the present embodiment is used for the flame-retardant finishing of the polyester-cotton blended fabric, and the initial flame retardant performance is excellent, and the flame retardant performance is not significantly decreased after 10 times and 30 times of washing. It is indicated that the polyester-cotton blended fabric after the flame retardant finishing of the flame retardant working fluid of the embodiment has obtained a very good long-lasting flame retardant effect.
实施例4.不同混纺比的涤棉织物的阻燃性能Example 4. Flame Retardancy of Polyester/Cotton Fabrics with Different Blending Ratios
在本实施例中，申请人对不同混纺比的涤棉织物在经本发明的阻燃工作液阻燃整理后的阻燃效果及其耐久性进行了测试。In the present embodiment, the applicant tested the flame retardant effect and durability of the polyester/cotton fabric of different blending ratios after the flame retardant finishing of the flame retardant working fluid of the present invention.
在本实施例中，所述阻燃工作液包含以下组份：阻燃剂和交联剂，其余为水，所述阻燃剂的浓度为600g/L，所述交联剂浓度为80g/L。其中，所述阻燃剂是阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂以质量比为2:1的比例混合而成；所述交联剂为2D树脂。In this embodiment, the flame retardant working fluid comprises the following components: a flame retardant and a crosslinking agent, and the balance is water, the concentration of the flame retardant is 600 g/L, and the concentration of the crosslinking agent is 80 g/ L. Wherein, the flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant in a ratio of 2:1 by mass; the crosslinking agent is a 2D resin.
在本实施例中，布样采用涤棉针织双面布(35〃圆筒，纱支32s，混纺比65：35)。In the present embodiment, the swatches were made of polyester-cotton knitted double-sided cloth (35 〃 cylinder, yarn roving 32 s , blending ratio 65: 35).
阻燃整理如下：将布样在阻燃工作液中二浸二轧，100℃烘干，150℃焙烘3分钟；接着，将布样在棉织物阻燃工作液(棉阻燃剂DM-3070300g/L，氯化镁催化剂40g/L、2D树脂80g/L)中二浸二轧，100℃烘干，160℃焙烘3分钟；然后热水洗、冷水洗并晾干，获 得经阻燃整理后的涤棉混纺织物。The flame retardant finishing is as follows: the swatches are immersed in the flame retardant working solution twice, dried at 100 ° C, and baked at 150 ° C for 3 minutes; then, the swatches are woven in the cotton fabric flame retardant working fluid (cotton flame retardant DM- 3070300g / L, magnesium chloride catalyst 40g / L, 2D resin 80g / L) two dip two rolling, 100 ° C drying, baking at 160 ° C for 3 minutes; then hot water wash, cold water wash and dry, obtained A polyester-cotton blended fabric that has been flame-retarded.
经阻燃整理后的涤棉混纺织物按照GB/T 17595-1998《织物燃烧试验前的洗涤程序》标准中B型洗衣机洗涤程序洗涤10次后对其阻燃性能进行测试。测试结果如表4所示。The flame-retardant finishing of the polyester-cotton blended fabric is tested according to GB/T 17595-1998 "Washing procedure before fabric burning test" in the B-type washing machine washing program for 10 times. The test results are shown in Table 4.
表4.经本发明的阻燃工作液阻燃整理后的涤棉针织布的阻燃性能的对比Table 4. Comparison of flame retardant properties of polyester/cotton knitted fabrics after flame retardant finishing of flame retardant working fluid of the present invention
Figure PCTCN2014095774-appb-000005
Figure PCTCN2014095774-appb-000005
由表4可以看出，本实施例的阻燃工作液及阻燃整理工艺对于不同混纺比的涤棉针织布同样具有很明显的效果。经阻燃整理后的涤棉针织布，其初始的阻燃性能优秀，经10次洗涤后阻燃性能没有明显下降。说明经本实施例的阻燃工作液阻燃整理后的涤棉针织布获得了非常好的长久阻燃效果。It can be seen from Table 4 that the flame-retardant working fluid and the flame-retardant finishing process of the present embodiment have obvious effects on the polyester-cotton knitted fabrics of different blending ratios. The polyester/cotton knitted fabric after flame retardant finishing has excellent initial flame retardant performance, and the flame retardant performance does not decrease significantly after 10 washings. It is indicated that the polyester-cotton knitted fabric after the flame-retardant working liquid of the flame-retardant working liquid of the embodiment has obtained a very good long-term flame retardant effect.
实施例5.纯棉织物的阻燃性能Example 5. Flame retardant properties of pure cotton fabric
申请人还对经本发明的阻燃工作液整理后的纯棉织物的阻燃性能及耐久性进行了测试。The Applicant also tested the flame retardancy and durability of the cotton fabric finished with the flame retardant working fluid of the present invention.
本实施例中，所述阻燃工作液包含以下组份：阻燃剂和交联剂，其余为水，所述阻燃剂的浓度为330g/L，所述交联剂浓度为80g/L。其中，所述阻燃剂是阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂以质量比为10:1的比例混合而成；所述交联剂为2D树脂。In this embodiment, the flame-retardant working fluid comprises the following components: a flame retardant and a crosslinking agent, the balance being water, the concentration of the flame retardant is 330 g/L, and the concentration of the crosslinking agent is 80 g/L. . Wherein, the flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant at a mass ratio of 10:1; the crosslinking agent is a 2D resin.
在本实施例中，布样采用纯棉纱卡(128×60，20s×16s)。In this embodiment, the swatches are made of pure cotton yarn cards (128 x 60, 20 s x 16 s ).
阻燃整理如下：将布样在阻燃工作液中二浸二轧，100℃烘干，150℃焙烘3分钟；然后热水洗、冷水洗并晾干，获得经阻燃整理后的涤棉混纺织物。The flame retardant finishing is as follows: the swatches are immersed in the flame retardant working solution twice, dried at 100 ° C, and baked at 150 ° C for 3 minutes; then washed with hot water, washed with cold water and dried to obtain polyester wool after flame retardant finishing. Blended fabric.
将经阻燃整理后的涤棉混纺织物按照GB/T 17595-1998《织物燃烧试验前的洗涤程序》标准中B型洗衣机洗涤程序洗涤10次和30次后对其阻燃性能进行测试。测试结果如表5所示。The flame-retardant properties of the polyester-cotton blended fabric after the flame-retardant finishing were tested according to the washing procedure of the B-type washing machine in the GB/T 17595-1998 "washing procedure before the fabric burning test" standard for 10 times and 30 times. The test results are shown in Table 5.
表5.经本发明的阻燃工作液阻燃整理后的纯棉织物的阻燃性能的对比Table 5. Comparison of flame retardant properties of pure cotton fabrics after flame retardant finishing of the flame retardant working fluid of the present invention
Figure PCTCN2014095774-appb-000006
Figure PCTCN2014095774-appb-000006
由表5可以看出，本发明的阻燃工作液同样可以应用在纯棉织物上。经本发明的阻燃工作液整理后的纯棉织物同样具有优异的阻燃性能，并且，在经10次和30次洗涤后阻燃 性能没有明显下降。说明经本发明的阻燃工作液阻燃整理后的纯棉织物获得了非常好的长久阻燃效果。As can be seen from Table 5, the flame retardant working fluid of the present invention can also be applied to a cotton fabric. The cotton fabric finished by the flame-retardant working fluid of the present invention also has excellent flame retardant properties, and is flame-retarded after 10 and 30 washings. There is no significant drop in performance. It is indicated that the pure cotton fabric after the flame-retardant finishing of the flame-retardant working fluid of the invention has a very good long-term flame retardant effect.
本发明的阻燃工作液及应用该阻燃工作液的整理方法，通过磷系涤棉阻燃剂与一种含氮交联剂反应成膜，结合浸轧法的整理工艺，使阻燃工作液中的阻燃剂吸附并包裹在涤纶纤维表面，并在交联剂和一定温度条件下，在涤纶纤维表面形成一层具有耐洗性的阻燃膜，该膜不仅降低涤纶纤维的燃烧性，同时可防止涤纶纤维燃烧时产生熔融物，从而彻底解决了涤棉混纺织物的“烛芯效应”。另外，应用本发明的阻燃工作液可以同时与棉纤维反应，实现棉纤维的耐久阻燃性。在本发明中，由于涤棉两种纤维都使用了同一种阻燃剂，即使燃烧起来，也能够克服阻燃剂在高温条件下固着在涤和棉纤维上的阻燃剂发生组分间迁移而使阻燃性能下降的技术问题，因此本发明的阻燃工作液是一种不同混纺比例涤棉织物实现耐久阻燃的完美解决方案。The flame-retardant working fluid of the invention and the finishing method using the flame-retardant working fluid, the film is formed by reacting a phosphorus-based polyester-cotton flame retardant with a nitrogen-containing crosslinking agent, and the finishing process of the padding method is used to make the flame-retardant work The flame retardant in the liquid adsorbs and wraps on the surface of the polyester fiber, and forms a flame-retardant flame-retardant film on the surface of the polyester fiber under the cross-linking agent and a certain temperature condition, the film not only reduces the burning property of the polyester fiber At the same time, it can prevent the melted material from being generated when the polyester fiber is burned, thereby completely solving the "wicking effect" of the polyester-cotton blended fabric. In addition, the flame-retardant working fluid to which the present invention is applied can simultaneously react with cotton fibers to achieve durable flame retardancy of the cotton fibers. In the present invention, since both polyester-cotton fibers use the same flame retardant, even if burned, it can overcome the migration between the flame retardants of the flame retardant fixed on the polyester and cotton fibers under high temperature conditions. The technical problem of reducing the flame retardant performance, therefore, the flame retardant working fluid of the invention is a perfect solution for achieving durable flame retardant of different blending ratio polyester/cotton fabrics.
应用本发明的阻燃工作液及整理方法获得的涤棉织物具有很好的阻燃效果和耐洗性，该涤棉织物通过GB/T 5455-1997测试，三十次洗涤后的续燃和阴燃时间小于5秒，损毁长度小于15厘米，按照GB/T 17591-2006《阻燃织物》标准达到B1级，可广泛用于服装、帐篷、装饰织物和交通工具用织物的阻燃整理。The polyester-cotton fabric obtained by applying the flame-retardant working fluid and the finishing method of the invention has good flame retardant effect and washing durability, and the polyester-cotton fabric is tested by GB/T 5455-1997, and the after-burning after 30 washings and The smoldering time is less than 5 seconds, the damage length is less than 15 cm, and it reaches B1 according to GB/T 17591-2006 "flame retardant fabric" standard. It can be widely used for flame retardant finishing of clothing, tents, decorative fabrics and vehicle fabrics.
本发明已由上述相关实施例加以描述，然而上述实施例仅为实施本发明的范例。必需指出的是，已公开的实施例并未限制本发明的范围。相反地，包含于权利要求书的精神及范围的修改及均等设置均包括于本发明的范围内。 The present invention has been described by the above related embodiments, but the above embodiments are merely examples for implementing the present invention. It must be noted that the disclosed embodiments do not limit the scope of the invention. Rather, modifications and equivalent arrangements are intended to be included within the scope of the invention.

Claims (10)

  1. 一种阻燃工作液，其特征在于，可以对涤棉织物进行阻燃整理，织物的棉含量范围为20～100％，所述阻燃工作液包含以下组份：阻燃剂和交联剂，其余为水；所述阻燃工作液中所述阻燃剂的浓度范围为200～600g/L，所述交联剂的浓度范围为30～100g/L；其中，A flame-retardant working fluid characterized in that the polyester-cotton fabric can be subjected to flame-retardant finishing, the cotton content of the fabric is in the range of 20 to 100%, and the flame-retardant working fluid comprises the following components: a flame retardant and a crosslinking agent The remaining portion is water; the concentration of the flame retardant in the flame retardant working fluid ranges from 200 to 600 g/L, and the concentration of the crosslinking agent ranges from 30 to 100 g/L;
    所述阻燃剂选自阻燃剂Pyrovatex CP、阻燃剂Pyrovatex HP、阻燃剂RDP、阻燃剂BDP、反应型无卤阻燃剂DOPO、环状磷酸酯阻燃剂、棉阻燃剂DM-3070中的一种或几种；The flame retardant is selected from the group consisting of a flame retardant Pyrovatex CP, a flame retardant Pyrovatex HP, a flame retardant RDP, a flame retardant BDP, a reactive halogen-free flame retardant DOPO, a cyclic phosphate flame retardant, and a cotton flame retardant. One or several of DM-3070;
    所述交联剂选自二羟甲基二羟基乙烯脲树脂、三羟甲基三聚氰胺树脂、六羟甲基三聚氰胺树脂及其醚化物中的一种或几种。The crosslinking agent is one or more selected from the group consisting of dimethylol dihydroxyethylene urea resin, trimethylol melamine resin, hexamethylol melamine resin, and ether salts thereof.
  2. 如权利要求1所述的阻燃工作液，其特征在于，所述阻燃剂为阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂的混合物。The flame retardant working fluid according to claim 1, wherein the flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant.
  3. 如权利要求1所述的阻燃工作液，其特征在于，所述交联剂为二羟甲基二羟基乙烯脲树脂。The flame retardant working fluid according to claim 1, wherein the crosslinking agent is dimethylol dihydroxyethylene urea resin.
  4. 如权利要求2所述的阻燃工作液，其特征在于，在所述阻燃剂中，所述阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂的质量比为(1～10):1。The flame retardant working fluid according to claim 2, wherein in the flame retardant, the mass ratio of the flame retardant Pyrovatex HP to the cyclic phosphate flame retardant is (1 to 10): 1 .
  5. 如权利要求1所述的阻燃剂工作液在纯棉织物和/或涤棉混纺织物的阻燃整理中的应用。The use of the flame retardant working fluid according to claim 1 in the flame retardant finishing of pure cotton fabrics and/or polyester-cotton blended fabrics.
  6. 一种涤棉混纺织物的阻燃整理方法，其特征在于，所述阻燃整理方法是将涤棉混纺织物在如权利要求1所述的阻燃工作液中二浸二轧，带液率为50％～～120％，80～120℃烘干，140～180℃焙烘0.5～5分钟后，水洗再烘干。A flame-retardant finishing method for a polyester-cotton blended fabric, characterized in that the flame-retardant finishing method is to dip and dip the polyester-cotton blend fabric in the flame-retardant working fluid according to claim 1, the liquid ratio is 50% ~ ~ 120%, 80 ~ 120 ° C drying, 140 ~ 180 ° C baking for 0.5 ~ 5 minutes, washed with water and then dried.
  7. 如权利要求6所述的阻燃整理方法，其特征在于，在水洗再烘干步骤之前还包含以下步骤：将涤棉混纺织物在棉织物阻燃工作液中二浸二轧，带液率为50％～120％，80～120℃烘干，140～180℃焙烘0.5～5分钟。The flame-retardant finishing method according to claim 6, characterized in that before the water washing and re-drying step, the method further comprises the steps of: dip and distilling the polyester-cotton blended fabric in the flame retardant working fluid of the cotton fabric, the liquid ratio is 50% to 120%, dried at 80 to 120 ° C, and baked at 140 to 180 ° C for 0.5 to 5 minutes.
  8. 如权利要求7所述的阻燃整理方法，其特征在于，所述棉织物阻燃工作液包含以下组份：棉阻燃剂DM-3070、氯化镁催化剂和交联剂，其余为水；The flame-retardant finishing method according to claim 7, wherein the cotton fabric flame-retardant working solution comprises the following components: a cotton flame retardant DM-3070, a magnesium chloride catalyst and a crosslinking agent, and the balance is water;
    所述棉阻燃剂DM-3070的浓度为300g/L，所述氯化镁催化剂的浓度为40g/L，所述交联剂的浓度为80g/L。The concentration of the cotton flame retardant DM-3070 was 300 g/L, the concentration of the magnesium chloride catalyst was 40 g/L, and the concentration of the crosslinking agent was 80 g/L.
  9. 一种涤棉混纺织物的阻燃整理方法，其特征在于，所述阻燃整理方法是将涤棉混纺织物在如权利要求1所述的阻燃工作液中二浸二轧，带液率为50％～～120％，堆置8～24小时，140～180℃焙烘0.5～5分钟后，水洗再烘干。A flame-retardant finishing method for a polyester-cotton blended fabric, characterized in that the flame-retardant finishing method is to dip and dip the polyester-cotton blend fabric in the flame-retardant working fluid according to claim 1, the liquid ratio is 50% ~ ~ 120%, stacked for 8 ~ 24 hours, 140 ~ 180 ° C baking for 0.5 ~ 5 minutes, washed with water and then dried.
  10. 一种纯棉织物的阻燃整理方法，其特征在于，所述阻燃整理方法是将纯棉纺织物在如权利要求1所述的阻燃工作液中二浸二轧，带液率为50％～120％，80～120℃烘干，140～180℃ 焙烘0.5～5分钟后，水洗再烘干；其中，A flame-retardant finishing method for a cotton fabric, characterized in that the flame-retardant finishing method is to dip two-rolled pure cotton textile in the flame-retardant working fluid according to claim 1, the liquid ratio is 50 %～120%, 80～120°C drying, 140～180°C After baking for 0.5 to 5 minutes, washing with water and drying;
    所述阻燃剂是阻燃剂Pyrovatex HP和环状磷酸酯阻燃剂以质量比为10:1的比例混合而成；所述交联剂为二羟甲基二羟基乙烯脲树脂。 The flame retardant is a mixture of a flame retardant Pyrovatex HP and a cyclic phosphate flame retardant in a ratio of 10:1 by mass; the crosslinking agent is a dimethylol dihydroxyethylene urea resin.
PCT/CN2014/095774 2013-12-31 2014-12-31 Flame retardant working solution and flame retardant finishing method for pure cotton fabrics and/or cotton-polyester blend fabrics WO2015101312A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201310751796.X 2013-12-31
CN201310751796.XA CN104746338A (en) 2013-12-31 2013-12-31 Inflaming retarding working solution and inflaming retarding finishing method of pure cotton fabric and/or cotton-polyester blended fabric

Publications (1)

Publication Number Publication Date
WO2015101312A1 true WO2015101312A1 (en) 2015-07-09

Family

ID=53493258

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2014/095774 WO2015101312A1 (en) 2013-12-31 2014-12-31 Flame retardant working solution and flame retardant finishing method for pure cotton fabrics and/or cotton-polyester blend fabrics

Country Status (2)

Country Link
CN (1) CN104746338A (en)
WO (1) WO2015101312A1 (en)

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105696318A (en) * 2016-03-14 2016-06-22 湖州新创丝织品有限公司 Method for improving flame-retardant performance of spandex fabric
CN109183409A (en) * 2018-08-16 2019-01-11 重庆消防安全技术研究服务有限责任公司 The method and flame retardant viscose fiber of melamine grafting oxidation viscose rayon preparation flame retardant viscose fiber
CN111877005A (en) * 2020-08-04 2020-11-03 天津兴华织造有限公司 Preparation method of flame-retardant high-temperature-resistant polyphenylene sulfide and nylon interwoven magic tape
CN112609449A (en) * 2020-12-03 2021-04-06 绵阳佳禧印染有限责任公司 Flame-retardant oil-resistant water-repellent multifunctional protective fabric and preparation method thereof
CN113981687A (en) * 2021-10-18 2022-01-28 鲁丰织染有限公司 Production process of short-flow flame-retardant non-ironing fabric
CN114517407A (en) * 2022-02-25 2022-05-20 江苏恒力化纤股份有限公司 Preparation method of cyclic borate flame retardant and flame-retardant polyester fiber product thereof
CN114561793A (en) * 2022-04-21 2022-05-31 河北宁纺集团有限责任公司 Corduroy flame-retardant finishing liquid, flame-retardant finishing method and flame-retardant corduroy
CN114672990A (en) * 2022-04-21 2022-06-28 东北林业大学 Preparation method of flame-retardant cotton fabric
CN114701230A (en) * 2022-03-25 2022-07-05 龙岩东腾再生资源科技有限公司 Needle cotton with good flame-retardant effect and processing method thereof
CN114855468A (en) * 2022-04-14 2022-08-05 浙江彩蝶实业股份有限公司 Flame-retardant antistatic polyester wall cloth and preparation process thereof
CN115029881A (en) * 2022-04-22 2022-09-09 北京嘉诚瑞鑫科技有限公司 Environment-friendly flame-retardant paint-free polyester infiltrated product and manufacturing method thereof
CN115182156A (en) * 2022-06-22 2022-10-14 南通瑞意嘉纺织科技有限公司 Blended flame-retardant fabric containing graphene fibers
CN116623429A (en) * 2023-07-25 2023-08-22 江苏恒力化纤股份有限公司 Preparation method of durable flame-retardant polyester/cotton blended fabric
CN114561793B (en) * 2022-04-21 2024-04-26 河北宁纺集团有限责任公司 Corduroy flame-retardant finishing liquid, flame-retardant finishing method and flame-retardant corduroy

Families Citing this family (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105178003A (en) * 2015-08-10 2015-12-23 东华大学 Phosphorus-containing flame retardant system polyester after-treatment and preparation and application thereof
CN105200768B (en) * 2015-09-01 2017-11-28 广东德美精细化工股份有限公司 The durable fire resistant finish method of cotton/nylon blends and colouring method
CN105113205A (en) * 2015-09-17 2015-12-02 无锡市长安曙光手套厂 Flame retardant tidying method for purified cotton or blended cotton textile fabric
CN105200765A (en) * 2015-09-17 2015-12-30 无锡市长安曙光手套厂 Pure cotton or cotton blended fabric and preparation method thereof
CN105442299A (en) * 2016-01-08 2016-03-30 盐城工学院 Flame-retardant environment-friendly textile and preparation method thereof
CN105586768A (en) * 2016-02-26 2016-05-18 安徽中天纺织科技股份有限公司 Antibacterial wash-and-wear fire-retardant finishing liquid and finishing method thereof
CN105568687A (en) * 2016-03-14 2016-05-11 湖州新创丝织品有限公司 Flame-retardant finishing method for cotton fabric
CN106049049B (en) * 2016-08-02 2018-05-15 丹东优耐特纺织品有限公司 Dacron permanent seal cooling is fire-retardant, water repellent, Waterproof Breathable method for sorting
CN106930106A (en) * 2017-04-05 2017-07-07 苏州联胜化学有限公司 Cotton is with without aldehyde permanent flame-retardant and its preparation method and application method
CN107201654A (en) * 2017-06-30 2017-09-26 四川东方绝缘材料股份有限公司 A kind of washable fire-retardant polyester cotton and preparation method thereof
CN107604496A (en) * 2017-09-28 2018-01-19 四川东方绝缘材料股份有限公司 A kind of permanent fire retardant fiber containing blend polyester and preparation method thereof
CN107829298A (en) * 2017-11-09 2018-03-23 新乡市新科防护科技有限公司 A kind of flame-proof antibiotic polyester cotton blending fabric and preparation method thereof
CN108071014A (en) * 2017-12-08 2018-05-25 天津工业大学 A kind of preparation method of novel flame-retardant finishing agent and fire-retardant regenerated cellulose fabric
CN110804114A (en) * 2019-12-04 2020-02-18 艾蒙特成都新材料科技有限公司 Water-soluble halogen-free flame retardant and preparation method of flame-retardant finished cotton fabric thereof
CN111648132A (en) * 2020-06-11 2020-09-11 周晓珊 Colorless-change environment-friendly composite flame retardant, and preparation method and application thereof
CN112252025A (en) * 2020-10-15 2021-01-22 西安工程大学 Finishing method for improving flame retardant property of polyester-cotton fabric
CN112663338B (en) * 2021-01-27 2022-09-02 广东德美精细化工集团股份有限公司 Novel durable flame-retardant finishing method for cotton and blended fabric thereof
CN113025079B (en) * 2021-02-25 2022-02-08 北华大学 Modified hydrotalcite and preparation method and application thereof
CN113136633B (en) * 2021-04-26 2022-05-17 武汉纺织大学 Long-acting antibacterial flame-retardant double-effect lyocell fiber and preparation method thereof
CN113310809B (en) * 2021-07-29 2021-10-15 南通洁曼纺织品有限公司 Clothing test assistor

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3746572A (en) * 1971-02-23 1973-07-17 Stauffer Chemical Co Process for flame retarding fabrics
JPH0397967A (en) * 1989-09-09 1991-04-23 Kanebo Ltd Flameproofing method of cellulosic fiber cloth
US6491727B1 (en) * 1999-06-09 2002-12-10 Cotton Incorporated Methods for reducing the flammability of cellulosic substrates
CN1668801A (en) * 2002-06-20 2005-09-14 乔治亚大学研究基金会公司 A durable flame retardant finish for cellulosic materials

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3746572A (en) * 1971-02-23 1973-07-17 Stauffer Chemical Co Process for flame retarding fabrics
JPH0397967A (en) * 1989-09-09 1991-04-23 Kanebo Ltd Flameproofing method of cellulosic fiber cloth
US6491727B1 (en) * 1999-06-09 2002-12-10 Cotton Incorporated Methods for reducing the flammability of cellulosic substrates
CN1668801A (en) * 2002-06-20 2005-09-14 乔治亚大学研究基金会公司 A durable flame retardant finish for cellulosic materials

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
"Flame-Retardant For Cotton CP", ADVANCED TEXTILE TECHNOLOGY, vol. 12, no. 1, 29 February 2004 (2004-02-29), pages 27 *
LIU, HONGYU ET AL.: "The Latest Developments in Flame-Retardant Finishing Technology", TEXTILE AUXILIARIES, vol. 27, no. 10, 20 October 2010 (2010-10-20), pages 6 *
SHEN, HUA ET AL.: "Study on Application Performance of Durable Flame Retardant DM-3070 for Cotton Fabric", CHINA TEXTILE LEADER, 8 March 2012 (2012-03-08), pages 44 *
ZHANG, MENGJIE ET AL.: "Experimental Study on the Polyester-Cotton Blended Fabrics' Flame Retardancy", JOURNAL OF ZHEJIANG SCI-TECH UNIVERSITY, vol. 30, no. 1, 10 January 2013 (2013-01-10), pages 36 *

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105696318A (en) * 2016-03-14 2016-06-22 湖州新创丝织品有限公司 Method for improving flame-retardant performance of spandex fabric
CN109183409A (en) * 2018-08-16 2019-01-11 重庆消防安全技术研究服务有限责任公司 The method and flame retardant viscose fiber of melamine grafting oxidation viscose rayon preparation flame retardant viscose fiber
CN109183409B (en) * 2018-08-16 2020-10-13 重庆消防安全技术研究服务有限责任公司 Method for preparing flame-retardant viscose fiber from melamine grafted oxidized viscose fiber and flame-retardant viscose fiber
CN111877005A (en) * 2020-08-04 2020-11-03 天津兴华织造有限公司 Preparation method of flame-retardant high-temperature-resistant polyphenylene sulfide and nylon interwoven magic tape
CN112609449A (en) * 2020-12-03 2021-04-06 绵阳佳禧印染有限责任公司 Flame-retardant oil-resistant water-repellent multifunctional protective fabric and preparation method thereof
CN112609449B (en) * 2020-12-03 2023-12-19 绵阳佳禧印染有限责任公司 Flame-retardant oil-resistant water-repellent multifunctional protective fabric and preparation method thereof
CN113981687B (en) * 2021-10-18 2023-08-04 鲁丰织染有限公司 Production process of short-flow flame-retardant non-ironing fabric
CN113981687A (en) * 2021-10-18 2022-01-28 鲁丰织染有限公司 Production process of short-flow flame-retardant non-ironing fabric
CN114517407A (en) * 2022-02-25 2022-05-20 江苏恒力化纤股份有限公司 Preparation method of cyclic borate flame retardant and flame-retardant polyester fiber product thereof
CN114517407B (en) * 2022-02-25 2023-08-29 江苏恒力化纤股份有限公司 Cyclic borate flame retardant and preparation method of flame-retardant polyester fiber product thereof
CN114701230A (en) * 2022-03-25 2022-07-05 龙岩东腾再生资源科技有限公司 Needle cotton with good flame-retardant effect and processing method thereof
CN114855468A (en) * 2022-04-14 2022-08-05 浙江彩蝶实业股份有限公司 Flame-retardant antistatic polyester wall cloth and preparation process thereof
CN114855468B (en) * 2022-04-14 2024-03-19 浙江彩蝶实业股份有限公司 Flame-retardant and anti-flaming material Electrostatic polyester wall cloth preparation process
CN114672990B (en) * 2022-04-21 2023-03-10 东北林业大学 Preparation method of flame-retardant cotton fabric
CN114672990A (en) * 2022-04-21 2022-06-28 东北林业大学 Preparation method of flame-retardant cotton fabric
CN114561793A (en) * 2022-04-21 2022-05-31 河北宁纺集团有限责任公司 Corduroy flame-retardant finishing liquid, flame-retardant finishing method and flame-retardant corduroy
CN114561793B (en) * 2022-04-21 2024-04-26 河北宁纺集团有限责任公司 Corduroy flame-retardant finishing liquid, flame-retardant finishing method and flame-retardant corduroy
CN115029881A (en) * 2022-04-22 2022-09-09 北京嘉诚瑞鑫科技有限公司 Environment-friendly flame-retardant paint-free polyester infiltrated product and manufacturing method thereof
CN115182156A (en) * 2022-06-22 2022-10-14 南通瑞意嘉纺织科技有限公司 Blended flame-retardant fabric containing graphene fibers
CN115182156B (en) * 2022-06-22 2024-04-16 南通瑞意嘉纺织科技有限公司 Blended flame-retardant fabric containing graphene fibers
CN116623429A (en) * 2023-07-25 2023-08-22 江苏恒力化纤股份有限公司 Preparation method of durable flame-retardant polyester/cotton blended fabric
CN116623429B (en) * 2023-07-25 2023-11-24 江苏恒力化纤股份有限公司 Preparation method of durable flame-retardant polyester/cotton blended fabric

Also Published As

Publication number Publication date
CN104746338A (en) 2015-07-01

Similar Documents

Publication Publication Date Title
WO2015101312A1 (en) Flame retardant working solution and flame retardant finishing method for pure cotton fabrics and/or cotton-polyester blend fabrics
JP6718655B2 (en) Phosphonic acid polymers, copolymers and their respective oligomers as flame retardants for polyester fibers
Jiang et al. Durable flame‐retardant and antidroplet finishing of polyester fabrics with flexible polysiloxane and phytic acid through layer‐by‐layer assembly and sol–gel process
Fang et al. Intumescent flame retardant coatings on cotton fabric of chitosan and ammonium polyphosphate via layer-by-layer assembly
WO2020087503A1 (en) Soluble polyelectrolyte complex and method for flame-retardant finishing of protein fibers using soluble polyelectrolyte complex
CN104387571A (en) Phosphorous-nitrogen-containing polyethylene glycol terephthalate flame retardant copolyester and application of flame retardant copolyester
CN102392356A (en) Manufacturing technique of wash-resistant and flame-retardant blended fabric
CN104611928A (en) Flame-proof treatment method of pure cotton or cotton blended fabric
Forouharshad et al. Flame retardant wool using zirconium oxychloride in various acidic media optimized by RSM
CN107201654A (en) A kind of washable fire-retardant polyester cotton and preparation method thereof
CN105401409A (en) Method for preparing durable flame retardant silk fabrics
CN102534855B (en) Method for preparing halogen-free flame-retarding polyester fibers with durability and droplet resistance
CN114908565B (en) Preparation method of durable flame-retardant polyester fabric
CN107177979A (en) One kind is without molten drop flame retardant polyester fiber/fabric and preparation method thereof
US20140308505A1 (en) Phosphonate polymers, copolymers, and their respective oligomers as flame retardants for polyamide fibers
Meng et al. The fire performance of polyamide66 fabric coated with soybean protein isolation
CN114657779B (en) Durable intumescent flame-retardant protein fiber product and preparation method thereof
CN114645453B (en) Durable flame-retardant protein fiber product and preparation method thereof
EP2635737A1 (en) Flame retarded textile and process for coating textile
CN105780453B (en) One kind is based on antiflaming finishing agent, its preparation method and its application of montmorillonite/DNA hydrosols
KR101651252B1 (en) Manufacturing method of flame retardancy cotton
CN111005214A (en) Flame-retardant anti-dripping finishing agent for polyester fabric and flame-retardant anti-dripping finishing method thereof
TW201114829A (en) Halogen-free flame retarding masterbatch with low phosphorous content, composition and process for preparing the same and flame retarding article containing the same
CN116427173A (en) Washable flame-retardant anti-dripping polyester cotton 65/35 fabric and preparation method thereof
CN113308889B (en) Halogen-free flame-retardant polyester-cotton fabric and preparation method thereof

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 14876641

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

32PN Ep: public notification in the ep bulletin as address of the adressee cannot be established

Free format text: NOTING OF LOSS OF RIGHTS PURSUANT TO RULE 112(1)EPC DATED 03.11.2016(EPO FORM 1205A).

122 Ep: pct application non-entry in european phase

Ref document number: 14876641

Country of ref document: EP

Kind code of ref document: A1