CN106996039A - A kind of preparation method of durable flame-retardant silk fabric - Google Patents

A kind of preparation method of durable flame-retardant silk fabric Download PDF

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Publication number
CN106996039A
CN106996039A CN201710207596.6A CN201710207596A CN106996039A CN 106996039 A CN106996039 A CN 106996039A CN 201710207596 A CN201710207596 A CN 201710207596A CN 106996039 A CN106996039 A CN 106996039A
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China
Prior art keywords
retardant
flame
preparation
silk
silk fabric
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CN201710207596.6A
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CN106996039B (en
Inventor
程献伟
杨旭红
关晋平
唐人成
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Suzhou University
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Suzhou University
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244Treating 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
    • D06M13/282Treating 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
    • D06M13/292Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/32Treating 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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating 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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/46Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating 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 oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/192Polycarboxylic acids; Anhydrides, halides or salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/10Animal fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30Flame or heat resistance, fire retardancy properties

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)

Abstract

The invention discloses a kind of preparation method of durable flame-retardant silk fabric, with phytic acid, nano titanium oxide and 1,2,3,4 BTCAs are that raw material prepares fire retarding treating liquid, by silk fabric, two leachings two are rolled in fire retarding treating liquid, are then baked under the conditions of 145 155 DEG C, are finally washed, dried.Fire retardant phytic acid derives from natural plants tissue in the present invention, and good biocompatibility is nontoxic, and containing 28% P elements in molecule, can be used as environmentally friendly phosphorus flame retardant.Nano titanium oxide is used as fire retardant and interfibrous crosslinking agent as synergistic flame retardant, 1,2,3,4 BTCA.The flame-retardant silk excellent fireproof performance prepared with the inventive method, and solve the problem of silk fabric flame-proof treatment is not water-fastness.The technology of the present invention technique is simple, easy to operate, meets environmental requirement, is with a wide range of applications.

Description

A kind of preparation method of durable flame-retardant silk fabric
Technical field
The present invention relates to textile finishing field, more particularly to a kind of preparation technology field of flame-retardant silk fabric.
Background technology
At present, fire is continuously increased in countries in the world as caused by textile, and great prestige is caused to human life's property The side of body, the flame-proof treatment of textile is always industrial quarters and a great research topic of academia.Silk is because its gloss is soft, wear The features such as comfortable and soft is referred to as " fiber queen ", is widely used in clothes and high-grade upholstery, such as Furniture decoration articles for use, curtain, bedding, carpet etc., silk belong to inflammable articles, it is necessary to carry out flame-proof treatment to it.
Halogen flame is in the past conventional fire retardant, but part halogen flame is proved easily to accumulate in organism, There is lasting harm to human and animal, increasing halogen flame is used by the limitation of the country such as European Union, or even banned Only use.Phosphorus flame retardant char forming ability is strong in existing commercialization fire retardant, is the preferable substitute of halogen flame, natural production Containing 28% P elements in thing phytate molecule, environmentally friendly phosphorus flame retardant can be used as.Chinese invention patent CN201310284364.2 discloses fire-retardant to silk fabric progress by the method for LBL self-assembly using phytic acid and chitosan, Obtained silk fabric has good flame retardant effect, still, this method need to impregnate repeatedly cationic chitosan solution and Anionic property plant acid solution, so that they produce electrostatical binding, layer upon layer, therefore trivial operations, technique on silk fiber surface Long flow path, and it is unclear to arrange the durability of silk fabric flame retardant effect.
The content of the invention
In order to solve the above technical problems, excellent and good endurance it is an object of the invention to provide a kind of flame retardant effect.
A kind of preparation method of durable flame-retardant silk fabric of the present invention, comprises the following steps:
(1) phytic acid (phytic acid), nano titanium oxide and 1,2,3,4- BTCAs are added into water (preferred pure water Or distilled water) in, mix, blending manner is first to use high-shearing dispersion emulsifying machine high-speed stirred 5-10min, then again with ultrasound Ripple handles 5-10min, obtains fire retarding treating liquid.
(2) silk fabric is impregnated after 0.5-5min in the fire retarding treating liquid obtained by step (1), handled, then After baked, washing, drying, the flame-retardant silk fabric is obtained.
Further, in step (1), the concentration of phytic acid is 90-160g/L, preferably 100- in the fire retarding treating liquid 150g/L。
Further, in step (1), the concentration of nano titanium oxide is 1-10g/L in the fire retarding treating liquid.
Further, in step (1), the concentration of 1,2,3,4- BTCAs is 60-90g/ in the fire retarding treating liquid L, preferably 70-80g/L.
Further, described to be processed as padding in step (2), preferably two leachings two are rolled, and pick-up rate (liquid carrying rate) is 80- 120%, preferably 100%.
Further, in step (2), the silk fabric after processing is first to be dried at 80-95 DEG C before baking, and the time is 3-8min。
Further, in step (2), described bake is carried out at 145-155 DEG C, preferably 150-155 DEG C.
Further, the time baked is 2-5min.
By such scheme, the present invention at least has advantages below:
1st, it is wherein fire-retardant in fire retarding treating liquid the invention discloses a kind of preparation method of durable flame-retardant silk fabric Agent phytic acid derives from natural plants tissue, and good biocompatibility is nontoxic, and containing 28% P elements in molecule, can be used as ring Border friendly phosphorus flame retardant, nano titanium oxide has containing six phosphate groups in synergistic flame retardant effect, phytate molecule, Combination can be produced with nano titanium oxide, the fire resistance of silk fabric can be significantly improved;1,2,3,4- BTCAs can be made For the crosslinking agent between fire retardant and silk fiber, the problem of solving silk fabric flame-proof treatment poor durability;
2nd, the flame-retardant silk fabrics flame resistance excellent performance prepared with preparation method of the present invention, and it is fire-retardant to solve silk fabric The problem of arranging not water-fastness;
3rd, preparation method technique of the present invention is simple, easy to operate, meets environmental requirement, is adapted to industrialized production, with weight The practical value wanted and it is widely applied prospect;
4th, present invention process flow is short, simple to operate, the silk fabric for possessing fire retardant functionality available for production, such as takes The products such as dress, bedding, curtain, wall paper, carpet.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention, And can be practiced according to the content of specification, below with presently preferred embodiments of the present invention and coordinate accompanying drawing describe in detail as after.
Brief description of the drawings
Fig. 1 illustrates the pole of flame-retardant silk fabric under the conditions of different nano titanium oxide consumptions in embodiments of the invention 1 Limited oxygen index;
Fig. 2 illustrates the charcoal of flame-retardant silk fabric under the conditions of different nano titanium oxide consumptions in embodiments of the invention 2 It is long;
The charcoal that Fig. 3 illustrates flame-retardant silk fabric after different number of times washings in embodiments of the invention 3 is long.
Embodiment
With reference to the accompanying drawings and examples, the embodiment to the present invention is described in further detail.Implement below Example is used to illustrate the present invention, but is not limited to the scope of the present invention.
Embodiment 1
The preparation method of durable flame-retardant silk crepe de Chine, comprises the following steps:
(1) preparation of fire retarding treating liquid:Phytic acid, nano titanium oxide, 1,2,3,4- BTCAs are added 5 groups respectively In identical distilled water, wherein, phytic acid concentration is 150g/L, 1, and the concentration of 2,3,4- BTCAs is 80g/L, wherein, nanometer Titanium dioxide concentration is respectively 0g/L, 2g/L, 4g/L, 7g/L, 10g/L, will first be arranged using high-shearing dispersion emulsifying machine respectively Agent high-speed stirred 6min, is then mixed with ultrasonication 8min, obtains 5 groups of fire retarding treating liquids again.
(2) preparation of flame-retardant silk crepe de Chine:5 groups of identical silk crepe de Chines are soaked in 5 groups of fire retarding treating liquids of step (1) After stain 3min, carry out two leachings two and roll processing, then silk crepe de Chine is dried 3min by pick-up rate 100% under the conditions of 95 DEG C respectively, 3min is baked under the conditions of 150 DEG C, is dried after washing, 5 groups of durable flame-retardant silk crepe de Chines are obtained.
The fire resistance for arranging and not arranging silk elephant crepe fabric is tested below:
As shown in figure 1, the limited oxygen index (LOI) of flame-retardant silk crepe de Chine is no under the conditions of different nano titanium oxide consumptions Together, the LOI values in Fig. 1 are according to GB/T 5454-1997《Textile combustion performance test oxygen index method》Determine.Silk is not arranged The LOI of crepe de Chine is 26.3%, as seen from Figure 1, with the increase of nano titanium oxide consumption, the LOI values of silk crepe de Chine by Cumulative big, when nano titanium oxide consumption is 4g/L, finish fabric LOI reaches 37.1%.
Embodiment 2
The preparation method of durable flame-retardant silk habotai, comprises the following steps:
The present embodiment step is substantially the same manner as Example 1, and its difference is:In step (1), 1,2,3,4- BTCA Concentration be 70g/L, nano titanium oxide concentration is respectively 0g/L, 2g/L, 4g/L, 8g/L, 10g/L;Silk is knitted in step (2) Thing is silk habotai, and 10min is impregnated in fire retarding treating liquid, is baked under the conditions of 155 DEG C.
The fire resistance for arranging and not arranging silk habotai is tested below:
As shown in Fig. 2 the charcoal length of flame-retardant silk is different under the conditions of different nano titanium oxide consumptions, the charcoal long-press in Fig. 2 According to GB/T 5455-2014《The measure that textile combustion performance vertical direction char length glows with after flame time》Determine.It is not whole Reason silk habotai fabric burns completely during vertical burn test, a length of 30cm of charcoal, as seen from Figure 2, fire-retardant silkworm The charcoal length of silk habotai is gradually reduced with the increase of nano titanium oxide consumption, and finish fabric charcoal length is respectively less than 10cm, is met China《Flame-retardant decorative fabric》Middle B1Level fire resistance requirement.
Embodiment 3
The preparation method of durable flame-retardant silk crepe de Chine, comprises the following steps:
(1) preparation of fire retarding treating liquid:Phytic acid, nano titanium oxide, 1,2,3,4- BTCAs are added respectively and steamed In distilled water, wherein, phytic acid concentration is that 100g/L, nano titanium oxide concentration are 4g/L, 1, the concentration of 2,3,4- BTCAs For 80g/L, then finishing agent high-speed stirred 6min is first used into ultrasonication 8min again using high-shearing dispersion emulsifying machine, is mixed It is even, obtain fire retarding treating liquid.
(2) preparation of flame-retardant silk crepe de Chine:It will be impregnated in fire retarding treating liquid of the silk crepe de Chine in step (1) after 10min, Carry out two leachings two and roll processing, then silk crepe de Chine is dried 4min by pick-up rate 100% under the conditions of 80 DEG C, then at 155 DEG C of conditions Under bake 3min, dry after washing, obtain durable flame-retardant silk crepe de Chine.
Water-fastness experiment is carried out to the silk elephant crepe fabric of arrangement below:
The wash durability of flame-retardant silk fabric is with reference to GB/T 3921-2008《The resistance to color jail of soaping of textile color stability experiment Degree》Carry out, use detergent for silk and wool 2g/L, bath raio 1:30min is washed under the conditions of 50,40 DEG C for once, repetition is washed to required Washing times.Fire resistance to the flame-retardant silk elephant crepe fabric of different washing times is tested.Fig. 3 is different washing times The charcoal of flame-retardant silk elephant crepe fabric is long, and the charcoal length in Fig. 3 is according to GB/T 5455-2014《Damage in textile combustion performance vertical direction Ruin the measure that length is glowed with after flame time》Determine.As seen from Figure 3, with the increase of washing times, the charcoal of flame-retardant silk Length gradually increases, and shows that fire resistance is gradually reduced, but flame-retardant silk charcoal length after 25 times are washed is still below 15.0cm, meets China《Flame-retardant decorative fabric》Middle B1Level fire resistance requirement.
Above case study on implementation illustrates that the flame-retardant silk fabric prepared with the inventive method has excellent flame retardant effect, and Durability of fire-retardant energy, wash durability are good.
Described above is only the preferred embodiment of the present invention, is not intended to limit the invention, it is noted that for this skill For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is some improvement and Modification, these improvement and modification also should be regarded as protection scope of the present invention.

Claims (8)

1. a kind of preparation method of durable flame-retardant silk fabric, it is characterised in that comprise the following steps:
(1) by phytic acid, nano titanium oxide and 1,2,3,4- BTCAs are added to the water, and mix, obtain fire retarding treating liquid;
(2) silk fabric is impregnated in the fire retarding treating liquid obtained by step (1) and handled, then after baking, obtained The flame-retardant silk fabric.
2. preparation method according to claim 1, it is characterised in that:In step (1), phytic acid in the fire retarding treating liquid Concentration is 90-160g/L.
3. preparation method according to claim 1, it is characterised in that:In step (1), nanometer two in the fire retarding treating liquid The concentration of titanium oxide is 1-10g/L.
4. preparation method according to claim 1, it is characterised in that:In step (1), 1 in the fire retarding treating liquid, 2,3, The concentration of 4- BTCAs is 60-90g/L.
5. preparation method according to claim 1, it is characterised in that:It is described to be processed as padding in step (2).
6. preparation method according to claim 1, it is characterised in that:In step (2), the silk fabric after processing is being baked Before, first dried at 80-95 DEG C.
7. preparation method according to claim 1, it is characterised in that:It is described to bake at 145-155 DEG C in step (2) Carry out.
8. preparation method according to claim 7, it is characterised in that:The time baked is 2-5min.
CN201710207596.6A 2017-03-31 2017-03-31 A kind of preparation method of durable flame-retardant silk fabric Active CN106996039B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109281168A (en) * 2018-10-31 2019-01-29 南通纺织丝绸产业技术研究院 Soluble poly pentalyte and its method to protein fibre flame-proof treatment
CN109355902A (en) * 2018-10-19 2019-02-19 南通纺织丝绸产业技术研究院 A kind of reactive flame retardant and its method to protein fibre durable flame-retardant finishing
CN109487540A (en) * 2018-10-17 2019-03-19 华南理工大学 A kind of antibacterial flame-retardant fabric and preparation method thereof
CN113215859A (en) * 2021-05-11 2021-08-06 安徽工程大学 Simple, convenient, efficient and environment-friendly preparation method of flame-retardant office paper

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CA764924A (en) * 1967-08-08 J. Hirshfeld Julian Flameproofing method
CN103321044A (en) * 2013-07-08 2013-09-25 苏州大学 Flame-retardant pure silk and preparation method thereof
CN104233801A (en) * 2014-09-15 2014-12-24 河南工程学院 Preparation method of flam-retardant and water-repellency dual-function cotton fabric
CN104878595A (en) * 2015-03-26 2015-09-02 鑫源蚕丝绸集团股份有限公司 Mulberry silk flame retardant agent

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CA764924A (en) * 1967-08-08 J. Hirshfeld Julian Flameproofing method
CN103321044A (en) * 2013-07-08 2013-09-25 苏州大学 Flame-retardant pure silk and preparation method thereof
CN104233801A (en) * 2014-09-15 2014-12-24 河南工程学院 Preparation method of flam-retardant and water-repellency dual-function cotton fabric
CN104878595A (en) * 2015-03-26 2015-09-02 鑫源蚕丝绸集团股份有限公司 Mulberry silk flame retardant agent

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109487540A (en) * 2018-10-17 2019-03-19 华南理工大学 A kind of antibacterial flame-retardant fabric and preparation method thereof
CN109355902A (en) * 2018-10-19 2019-02-19 南通纺织丝绸产业技术研究院 A kind of reactive flame retardant and its method to protein fibre durable flame-retardant finishing
WO2020077695A1 (en) * 2018-10-19 2020-04-23 南通纺织丝绸产业技术研究院 Reactive flame retardant and method for durable flame retardant treatment of protein fiber using same
CN109281168A (en) * 2018-10-31 2019-01-29 南通纺织丝绸产业技术研究院 Soluble poly pentalyte and its method to protein fibre flame-proof treatment
CN113215859A (en) * 2021-05-11 2021-08-06 安徽工程大学 Simple, convenient, efficient and environment-friendly preparation method of flame-retardant office paper
CN113215859B (en) * 2021-05-11 2023-11-10 安徽工程大学 Simple, efficient and environment-friendly preparation method of flame-retardant office paper

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