CN101016694A - Flame-proof treatment method for light and thin natural fiber material - Google Patents
Flame-proof treatment method for light and thin natural fiber material Download PDFInfo
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- CN101016694A CN101016694A CNA2007100203735A CN200710020373A CN101016694A CN 101016694 A CN101016694 A CN 101016694A CN A2007100203735 A CNA2007100203735 A CN A2007100203735A CN 200710020373 A CN200710020373 A CN 200710020373A CN 101016694 A CN101016694 A CN 101016694A
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- 239000002657 fibrous material Substances 0.000 title claims abstract description 78
- 238000000034 method Methods 0.000 title claims abstract description 45
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001868 water Inorganic materials 0.000 claims abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 14
- 238000004043 dyeing Methods 0.000 claims abstract description 7
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 6
- 229920001410 Microfiber Polymers 0.000 claims abstract description 4
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 4
- 239000003063 flame retardant Substances 0.000 claims description 91
- 239000000463 material Substances 0.000 claims description 56
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- 239000007788 liquid Substances 0.000 claims description 18
- 239000002114 nanocomposite Substances 0.000 claims description 18
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 17
- 239000006185 dispersion Substances 0.000 claims description 16
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 15
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
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- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 3
- 239000004814 polyurethane Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 2
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- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
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- 238000010306 acid treatment Methods 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
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- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- IABIVYBXAHDOTD-UHFFFAOYSA-N hydroxymethylphosphanium urea chloride Chemical compound NC(=O)N.[Cl-].OC[PH3+] IABIVYBXAHDOTD-UHFFFAOYSA-N 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229920006277 melamine fiber Polymers 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
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- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 1
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- 229910052698 phosphorus Inorganic materials 0.000 description 1
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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
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/08—Processes in which the treating agent is applied in powder or granular form
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with 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
- D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with 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
- D06M11/46—Oxides or hydroxides of elements of Groups 4 or 14 of the Periodic Table; Titanates; Zirconates; Stannates; Plumbates
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
A flameproof treatment method of thin natural fiber material comprises that ultra-fine fiber fabric, poaching treatment or dyeing, low-temperature expansion flameproof treatment, baking crosslink, oxidization, neutralization, washing with water, checking final product, wherein the low-temperature immersion condition comprises 15-30Deg. C and 10-30s, the expansion treatment temperature is 35-60Deg. C for 20-40min, the baking crosslink temperature is 145-185Deg. C for 2-8min. Then the invention uses cleaning agent to process the ultra-fine flameproof fiber, while the cleaning agent is nanometer TiO2 or/and ZnO whose mass ratio is 1-12.0wt%, while the disperser is 0.2-1.5wt% as nanometer composite disperser to be treated in water solution.
Description
Technical field
The present invention relates to the post-processing approach of light and thin natural fiber material, especially fire-retardant and clean processing method.
Technical background
The ecological performance of fibrous material has been World Focusing, and American-European and China has all formulated strict ecological criteria.The satisfactory fibrous material of ecological performance can be guaranteed user's hygiene and health, development promotes social harmony.
In industrial production, communications and transportation and resident living, the use amount of fibrous material increases year by year.By fibrous material, particularly the fire damage that inflammability caused and the casualties of the ultra-fine super-soft fiber material of ultra-thin and ultra-light-ultra micro fibrous material are startling, and have been paid attention to by national governments.More than 700,000,000 dollar of the U.S.'s annual fire injures and deaths nearly 10000 people, economic loss.In the period of the 1989-1999, more than 100 hundred million yuan of altogether 67.9 ten thousand of breaking out of fires of China, dead 22469 people, direct economic loss.50% of these fire are caused by fibrous material.Railway, traffic, naval vessel, ocean, aerospace vehicle, tourist hotel, extraordinary hospital, apartment for elderly people, prison, school, kindergarten even each family, often lighted because of ultra micro fibrous material (bedding, nightwear, children's garment, drapery etc.), personnel are difficult to escape in indoor, the cabin, and the pernicious major accident that causes the dead group of group to hinder.Invent and use ecological fire-retardant natural fiber material, can prevent fire disaster fire incident and the loss that is caused thereof take place, reduce, to assuring the safety for life and property of the people, promote social stability, strengthen national defense construction and quickening economic construction, all be that crucial meaning is arranged.
The seventies, the domestic fire retardants such as THPC-APO, the fine resin of phosphorus, ammonium dihydrogen phosphate (ADP) of once using instead were put all-cotton fabrics in order, and effect is still undesirable.The beginning of the eighties is because the demand of domestic market, two fire-retardant all-cotton fabric production lines of Proban have successively been introduced from Britain Albrightant-wilso company in Beijing, two places, Liaoning, and then ground such as Beijing, Shanghai, Tianjin, Shaanxi have started the synthetic of fire retardant and used upsurge.To the domestic Pykovetex CP (Switzerland) that can the produce nineties.Fxorl 76 (U.S.), Proban fire retardants such as (Britain), finishing technique also reaches its maturity, but after country in 1998 issues " fire retardant protective clothing " standard, just begins small lot batch manufacture and application.
There is Shi Duojia in the at present domestic enterprise that produces fire-retardant all-cotton fabric with the CP route, there is 5-6 house in the enterprise that produces fire-retardant all-cotton fabric with the Proban route, but its product mostly is medium weight fabric (more than the 160g/m2), and wiriness, peculiar smell is arranged, mainly use at home.System's report is not seen in the invention of light and thin natural fiber fire proofing (90-150g/m2).Because frivolous fine and soft, fire-retardant processing is very difficult.
The production of external fire-retardant all-cotton fabric is also based on the technology of Pykovetex CP New and Proban, and mostly is medium weight fabric, and the invention report of light and thin natural fiber fire proofing is few, and specific performance is not quite clear.The external comparative maturity of fire-retardant process technology of Fire resistant viscose fiber.In recent years, country all hankers after the invention and the exploitation of special high temperature-resistant fire resistance fibre and material Europe, the United States, day etc.The invention of fire-retardant natural fiber material and the trend of producing big oriented external transfer.In a word, the domestic and international invention of fire-retardant light and thin natural fiber material is less, and difficulty is bigger.
Though disclosing of some patented methods arranged at present, the method that also comprises the present application people, as CN200510112307.1 thermal resistant fire resistant fibric and preparation method thereof, thermal resistant fire resistant fibric is formed by two kinds of fire resistance fibre blending, a kind of fire resistance fibre is the aramid fiber 1313 fiber, another kind of fire resistance fibre is a Fire resistant viscose fiber, and the fire-retardant percentage composition of various fibers is in the flame-retardant textile: aramid fiber: 20%～80%, and Fire resistant viscose fiber: 20%～80%.
The fabric of CN01813559.5 flame-resistant thread and manufacturing thereof comprises: a) 5-90wt.% melamine fiber, b) 5-90wt.% natural fabric, c) polyamide fiber made by polyamide 66, polyamide 6 or its mixture of 0.1-30wt.%.
The high fire prevention of CN03811280.9 BLENDED FABRIC, it passes through co-braided: the strand of 30%～70% weight (A), prepare with the cellulose fibre yarn (B) of 70%～30% weight, this strand (A) obtains by compound halogen-containing Flame Retardant Fibers (a-1) and another kind of fiber (a-2), halogen-containing Flame Retardant Fibers (a-1) comprises 25～50 parts antimonial in the 100 parts by weight of acrylic base co-polymers, this AP-52 obtains by polymeric monomer intermixture, this monomer mixture comprises the acrylonitrile of 30%～70% weight, the halogen-containing vinyl monomer of 30%～70% weight, 0%～10% weight can with the vinyl monomer of their copolymerization, be 300mg/ metric count No.17 at load, temperature range is that strand (A) has the percentage elongation less than 5% under 100 ℃～500 ℃ the condition.
The preparation of the anti-near-infrared dacron tarpaulin of CN200610085269.X ventilating, antiflame, oilproof, waterproof, acidproof acid-proof, earlier to the polyester canvas durable flame-retardant finishing, durable flame-retardant arrangement comprise pad, bake, baking temperature and time, 170 ℃-200 ℃, 1-10 minute, and on fabric, comprise be coated with scrape, stoving process carries out fire-retardant PU coating adhesive coating and carries out the anti-acid treatment of waterproof, is applied directly on the fabric, drying and high temperature 170-230 ℃ bakes 1-10min; Base cloth is carried out durable flame-retardant arrangement, dyeing: the front is coated with fire-retardant PU coating adhesive or adds mill base simultaneously carries out grease proofing, waterproof, acid-proof arrangement.
200410065744.8 permeable acid-alkali-oil-water-proof fabric finishing method adopts the method for putting in order after the first coating to improve the acid-proof permeance property of fabric; The macromolecular material that is used for fabric coating mainly contains polyacrylic water-based or solvent type resin or polyurethanes water-based or solvent type resin; Fluoro-containing macromolecule material is adopted in the acid-proof arrangement.
The manufacture method of the dirty natural fabric of CN200310112733.6 anti-static inflaming-retarding waterproof and oilproof, the test weaving of antistatic grey cloth, pad fire resistant fluid, bake, soap, go flavor, the dirty arrangement of waterproof and oilproof, tentering, finished product inspection; The anti-static method of antistatic grey cloth test weaving natural fabric is with electrically conductive organic fibre or metallic conduction fiber.
Though report on September 25th, 2006 " China Textile News ", units such as Xi'an Polytechnic University have succeeded in developing " the soft fire-resistant antistatic fabric of novel high-strength ", and claim this achievement to fill domestic blank.This achievement is with different textile fabrics of three class functions such as high-performance fiber, fire resistance fibre and conductive fibers, form novel fabric with blending and the mode that interweaves, emphasis has solved fiber species and has chosen, used with key technical problems such as determination of ratio, blended union processing and dyeing.Can see from above report: though this achievement also has soft fire-retardant characteristics (not having ecological clean processing), raw materials used, technology path and key technology, properties of product also are different from the present invention.The normal employing of the fire-retardant processing of the composite material of natural fiber material and natural fabric and other fiber (containing textiles) rolled the roasting method and padded two kinds of ammonia cure methods, these methods are effectively to the fire-retardant processing of medium weight fabric, but can not obtain good effect for the ultra-fine super gentle fibrous material of ultra-thin and ultra-light.
Summary of the invention
The present invention seeks to: propose a kind of flame-proof treatment method of light and thin natural fiber material, further propose clean treatment method fabric; Thereby make the ultra-fine super gentle natural fiber material of ultra-thin and ultra-light obtain good flame-retardant effect; The ultra-fine super gentle fibrous material of ultra-thin and ultra-light is had from clean performance (sterilization degerming).
Technical solution of the present invention is: the flame-proof treatment method of light and thin natural fiber material, handle with following technology: ultra micro fiber material fabric (light and thin type cotton grey cloth) that---bleaching is handled or dyeing, and---low temperature soaks into expanded (fire-retardant)---bakes---oxidation, neutralization, washing---finished product inspection crosslinked; Wherein low temperature infiltration condition is: 15-30 ℃, 10-30 second; 35-60 ℃ and 20-40 minute of expanding treatment temperature; Bake crosslinking temperature: 145-185 ℃, time: 2-8 minute.
The infiltration of fabric low temperature is expanded, high temperature bakes crosslinked; Fire retardant adopts Pyrovatex CPNew or fire retardant JSJ-111: crosslinked resin mostly is the modification alkyl melamine derivative with active group, and crosslinked resin especially is JSJ-302.Consumption 5-20%, the working concentration of fire retardant is with 25%-38%; Ultra micro fibrous material low temperature (15-30 ℃) soaks into materials such as fire retardant, crosslinked resin, bleeding agents down, time 20-30 second; And parked 20-40 minute at 20-80 ℃; Bake process using and bake crosslinking temperature: 135-185 ℃, time: 2-8 minute.Infiltration temperature 20-30 ℃, time 20-30 second; And it is expanded with 20-40 minute at 40-60 ℃.
Then ultra micro fire resistance fibre material is handled with purificant, purificant is nano level titanium dioxide (TiO2) or/and zinc oxide ZnO, and weight proportion is 1-12.0wt%, dispersant 0.2-1.5wt%; And add the nano composite material dispersant and in the aqueous solution, handle.Dispersant also adds water, and under agitation also high speed shear was mixed 20-60 minute; Or the NaOH that adds 0.1-0.5wt% again stirred 10-30 minute.The nano composite material dispersion liquid adopts conventional dipping to the ecological clean processing of ultra micro fire resistance fibre material---dry or bake technology; Bake process using and bake crosslinking temperature: 135-185 ℃, time: 2-8 minute, or behind the crosslinked resin dipping, bake crosslinked resin consumption 2-10% again.Nano combined purificant consumption 3-7wt%, titanium dioxide and zinc oxide ZnO ratio be that 20-80wt% compares 80-20wt%.
Flame-retardant formulations: fire retardant JSJ-111 25-38, crosslinked resin JSJ-302 5-10, auxiliary crosslinked resin JSJ-303 0.5-2.0, formaldehyde eliminating agent JSJ-504 0.3-1.5; Softener JSJ-151 2-3; Catalyst JSJ-523 1-2; Bleeding agent JSJ-3121-2; The cold water surplus more than is percent by weight %, adds up to 100%.
Purificant nano composite material dispersion liquid prescription: nano material titanium dioxide 0.2-2.0, absorbent-type material oxidation zinc 0.9-12.0, dispersant adopts surface-activity, cosolvent JSJ-701 0.8-7.0; 30% NaOH aqueous solution 1.0-10.0; Softener JSJ-312 E; Bleeding agent JSJ-151 F; E, F is 1-10; Water is surplus, more than is percent by weight %, adds up to 100%.
Characteristics of the present invention are: this is a kind of cleaning and flame-proof treatment method to light and thin natural fiber material; Thereby make the ultra-fine super gentle natural fiber material of ultra-thin and ultra-light obtain good flame-retardant effect.The ultra-fine super gentle fibrous material of ultra-thin and ultra-light is had from clean performance (sterilization degerming).The present invention adopts low temperature to soak into expanded and high temperature bakes crosslinking technological and anti-flammability, durability, the gentle may just as well harmonious configuring technical of feel, and the fibrous material processing of weight 90-150g/m2 has all been reached expected result.Adopt the ecological clean new technology of nano composite material, the material that will have the nano material of photocatalysis performance, peculiar smell and formaldehyde are had absorption property and chemical reaction performance, make stable composite dispersion liquid with special method, again with this dispersion liquid with particular process process, the durable fibrous material surface that is attached to.This processing had both kept original sex character of fiber, gave fibrous material safe and reliable ecological index again.
Description of drawings
Fig. 1 is the influence of fire retardant concentration to the fabric weightening finish
The relation of weightening finish of Fig. 2 fabric and char length
Among Fig. 1 and Fig. 2: 1-cotton plain cloth 128.4g/m
2(133 * 100), 2-cotton drillipg 119.1g/m
2(128 * 68)
Fig. 3. crosslinked resin is to the influence of fabric washability and weightening finish
The eluting rate (40 of 1-crosslinked resin consumption and fabric
s* 40
s128 * 68 washings 5 times)
The weightening finish (40 of 2-crosslinked resin consumption and fabric
s* 40
s128 * 68)
The specific embodiment
1, the fire retardant consumption is to the anti-flammability of fibrous material, gentle influence may just as well
Because frivolous, bulk, the softness of ultra micro fibrous material and the bigger characteristics of specific area, the air capacity that fibrous material comprised of unit mass is bigger, oxygen-supplying amount abundance during burning, thereby the burning that is easier to catch fire of ultra micro fibrous material ratio, the fire-retardant consumption of selecting the ecological efficient fire retardant man-hour for use and suitably improving fire retardant that adds.
The permanent seal cooling fire retardant that can be used at present natural and composite material both at home and abroad mainly contains two kinds of the condensation bodies (Proban class) of N-methylol-3-dimethyl phosphorus propionamide (PyrovatexCP class) and Tetrakis hydroxymethyl phosphonium chloride-urea, because the Proban based flame retardant adds man-hour to natural fiber material, it is the ammonia cure set, crosslinking degree is difficult to control, and running product is stiffening, ultra micro fibrous material fire-retardant adding can't use man-hour.Pyrovatex CP based flame retardant is produced house both at home and abroad, brand performance more, that quality also has a certain distance, table 1 to provide six kinds of fire retardants compares.
Table 1 flame retardant performance both at home and abroad compares
Annotate: fabric is the cotton drillipg of 119.1g/m2.
Use these two kinds of fire retardants in soft smooth, the research of higher, the fabric feeling of the flame retarding efficiency of import fire retardant Pyrovatex CP New and homemade fire retardant JSJ-111 as can be seen from Table 1.
Fig. 1. fire retardant concentration is to the influence of fabric weightening finish, Fig. 2. the relation of fabric weightening finish and char length
The use amount of fire retardant directly has influence on anti-flammability, feel and the production cost of fibrous material.With material ,-high temperature expanded such as fire retardant JSJ-111 to soak into bake crosslinked be technology, two kinds of natural fiber materials are processed, have been provided the influence of fire retardant working concentration to the fabric weightening finish according to orthogonal experiments, Fig. 1; Fig. 2 has provided the relation of fabric weightening finish with char length; Table 2 has provided the influence of fire retardant to fabric property.Increase, fabric along with the fire retardant working concentration increases weight as seen from Figure 1
Table 2 fire retardant is to the influence of fabric property
Annotate: crosslinked resin is JSJ-302, and consumption is identical.
Increase sharply, but concentration reaches 35% when above, the fabric speed of weight increment slows down; Then can see from Fig. 2: along with the increase of fabric weightening finish, char length reduces (anti-flammability increase), but after weightening finish reached certain value, the speed that char length reduces slowed down, simultaneously because the difference of fabric construction, the weightening finish also different (12.5%, 14.5%) that reaches fire-retardant requirement; Can see also that by the data of table 2 the fire retardant working concentration also has certain influence to brute force, the change color of fabric.Comprehensive above the analysis, the working concentration of fire retardant is an optimum value with 25%-38%.
2, crosslinked resin and durability of fire-retardant
The ultra micro fibrous material is fire-retardant to add man-hour, crosslinked resin commonly used mostly is the modification alkyl melamine derivative with active group, but because chemical constitution, molecular weight and activity group content is different, its performance also has than big difference, and the performance that table 3 has been listed five kinds of crosslinked resins compares.
The performance of five kinds of crosslinked resins of table 3 relatively
Annotate: fabric is 119.1g/m
2The cotton drillipg; Fire retardant is homemade JSJ-111.
As can be seen from Table 3: the cross-linking coefficient of CHN and JSJ-302 crosslinked resin fabrics feel soft higher, arrangement is smooth, and these two kinds of crosslinked resins are used in this research.
Crosslinked resin can not only form firm chemical bond with the active group of fire retardant, fibrous material under given conditions, and can also be attached to the superfine structure surface of fibrous material by infiltration, by intermolecular secondary bond power strong bonded.The ultra micro fibrous material is fire-retardant to add man-hour, and the use amount of crosslinked resin can directly have influence on indexs such as the fastness to washing, weightening finish, feel of finish fabric.Fig. 3 has provided the crosslinked resin consumption to influences such as fabric washability and weightening finishes, and table 4 has been listed the relation of indexs such as crosslinked resin and fabric feeling, brute force, change color.
As seen from Figure 3: under the constant situation of fire retardant consumption, along with the increase of dosage of crosslinking agent, the weightening finish increase of fabric, eluting rate obviously reduce; Can also see from table 4, along with increase, fabric feeling hardening, its colour changed into yellow of dosage of crosslinking agent, comprehensively various
The performance of table 4 crosslinked resin and fabric
Annotate: fabric is cotton twill (119.1g/m
2); Fire retardant is that JSJ-111, use amount are identical; Crosslinked resin is JSJ-302.The coordination of index, the working concentration 5.0%-10% of crosslinked resin is the most suitable.
3, low temperature soaks into expanded, high temperature and bakes crosslinked
Ultra micro fibrous material low temperature (15-30 ℃) descends with the infiltration of materials such as fire retardant, crosslinked resin, bleeding agent, also (20-80 ℃) parks certain hour at a lower temperature, at this moment expanded loose, the low molecule auxiliary agent of fibrous material very easily is penetrated in the fine structure of fibrous material, carry out drying again and when crosslinked, can not improve indexs such as the feel of fire resistance fibre material and brute force greatly thereby can not form surface resin.Table 5 has provided the influence to fabric property of swelling temperature and time.
Table 5 swelling temperature and time are to the influence of fabric property
Annotate: 1. flame-retardant formulations is a factory formula;
2. 20 ℃ of infiltration temperatures, time 20-30 second;
3. fibrous material is: cotton drillipg (40
s* 40
s119.1g/m
2).
As can be seen from Table 5: when 20 ℃ of (1) swelling temperatures, expanded time 20-40 minute, though the smooth fabric weightening finish of fabrics feel soft low (12.2%, 13%), eluting rate higher (48.8%, 48.1%), char length also higher (126mm, 123mm); (2) when 80 ℃ of swelling temperatures, expanded time 20-40 minute, though the anti-flammability of fabric fine (char length is respectively 90.5mm and 90mm), eluting rate low (28.2%, 28.0%) fabric weightening finish too high (15.6%, 16.0%) and fabric feeling are soft inadequately smooth.(3) when 50 ℃ of swelling temperatures, expanded time 20-40 minute, not only anti-flammability meets the project indicator and requires (char length is respectively 110mm and 112mm) but also eluting rate lower (25.9%, 28.0%), fabric weightening finish moderate (14.5%, 13.9%), fabric strength higher.So 50 ℃ and 20-40 minute is optimal swelling temperature and expanded time.
It is very crucial operation in the fire-retardant processing of fibrous material that high temperature bakes crosslinked, and it has determined feel, washability, strength loss and the change in color of finished product to a great extent.It is a very complex physicochemical process that high temperature bakes crosslinked; Crosslinked between crosslinked, the fibrous material of existing fire retardant and fibrous material, fire retardant and the crosslinked resin, also have simultaneously fire retardant, crosslinked resin to the internal penetration of fibrous material, adhere to, form very firm physical absorption by intermolecular secondary bond power.It is baking temperature and baking the time that high temperature bakes crosslinked key parameter: temperature height, time are long, though chemical reaction is thorough, crosslinking degree is high, the fabric washability is good, but can make feel hardening, strength loss bigger, the compound that side reaction simultaneously strengthens, generates and free formaldehyde reaction, formation have the fatty amine substance of fishlike smell; Baking temperature is low excessively, the time is too short, then crosslinked insufficient, thereby influence the fastness to washing and the anti-flammability of fibrous material, a large amount of evidences: baking temperature 145-185 ℃, to bake time 2-8 minute be that rational high temperature bakes crosslinked condition.
4, the ecological clean technology research of nano composite material
The ecological clean theory analysis of 4-1, ultra micro fire resistance fibre material
The ultra micro fibrous material can produce the free formaldehyde of trace and have the fatty amine of fishy smell flavor in fire-retardant process, and the fatty amine that has a fishy smell flavor in the storage of product and in transit, also can produce as running into suitable temperature and humidity on a small quantity.In the ecological index of fibrous material, content of beary metal, limit fire retardant and pH value and all more easily solve, and peculiar smell has become the emphasis index with free formaldehyde, these two indexs are mutually related again to a great extent.Be currently available for the major technique approach of removing peculiar smell and formaldehyde and have three kinds:
(1). the photocatalysis clean technology of nano material
Ultra micro fire resistance fibre material is being introduced nano level zinc oxide (ZnO) or titanium dioxide (TiO
2) after, they can produce free electron and hole under the irradiation of sunshine or light, through the reaction of airborne oxygen and hydrone, just can produce the hydroxyl free radical and the active oxygen of extremely strong oxidability, thereby have extremely strong photooxidation restoring function.Harmful organic matter (formaldehyde, fatty amine etc.), peculiar smell, bacterium etc. can be reduced into harmless carbon dioxide, water and oxygen after being adsorbed by active oxygen at once.But the weak point of this technology is: the fire resistance fibre material is at the packing warehouse-in or in transit, no visible light or light are faint, and this will influence the photocatalysis effect of nano material.
(2). the absorption-desorption technology
With having micropore, hole or the very big material of specific area, the peculiar smell on the ultra micro fire proofing or formaldehyde are adsorbed and is stored in its internal structure.The problem of this method is this saturation history that is adsorbed with, simultaneously when washing, can desorb take place, portion gas discharges again.
(3). chemical taste removal technology
Select a kind of can putting in the material of fatty amine and formaldehyde chemically reactive in the ultra micro fire resistance fibre material for use, removing peculiar smell and formaldehyde that can be very convenient, but this material is an intractable problem to the adhesive ability and the use amount of fibrous material.
This research select for use three kinds have photo-catalysis function, adsorption function, chemical reaction materials with function compound, ultra micro fiber fire proofing is carried out cleaning processing, has obtained good result.
4.2 five kinds of purificants are to the influence of fibrous material
Utilize three kinds of ecological clean theories, select five kinds of purificants that ultra micro fire resistance fibre material is handled, it the results are shown in table 6.
The performance of table 6. purificant and fibrous material
Annotate: 1. fibrous material is: fire-retardant cotton plain cloth (40
s* 40
s128.4g/m
2);
2. wet heat condition: 45 ℃ of temperature, humidity 80%, time 24-48 hour;
3. the purificant use amount is identical.
As can be seen from Table 6: the taste removal of three kinds of nano materials (JSJ-602, JSJ-603, JSJ-606) is effective, there are slight dust sense and color yellowing in fabrics feel soft but surface, it will have influence on the use of product; Absorbent-type purificant (JSJ-605) is though taste removal is effective, fabric color does not change but feel is hard slightly; Chemical reaction type purificant (JSJ-601) taste removal effect, feel, change color are all smaller, but relatively poor with the affinity of fiber.In a word, three types purificant, respectively have pluses and minuses, their Application of composite to be only best selection.
The preparation of the stable dispersion liquid of 4-3, nano composite material and application
Owing to the ultrafine dust of nano material has bigger surface energy and the active tendency that presents reunion, so the stable dispersion liquid preparation of nano material is very difficult, this has also become the bottleneck that it uses on fibrous material.This project system studied the consumption and the ratio of the kind of the kind of dispersant and consumption, cosolvent and consumption, nano composite material purificant, the factors such as technological parameter of dispersion liquid preparation, having prepared can be steady in a long-term (not stratified more than three months, do not precipitate) nano composite material dispersion liquid, and the ecological clean processing that is used for ultra micro fire resistance fibre material of success.Through 73 groups of tests with to the analysis of 2284 data, drawn the prescription and the preparation technology of nano composite material dispersion liquid the best.
Nano composite material dispersion liquid prescription:
Purificant JSJ-606 (nano material) 0.2-2.0
Purificant JSJ-605 (absorbent-type material) 0.9-12.0
Purificant JSJ-601 (reactive materials) 0.5-5.2
Dispersant JSJ-504 0.2-1.5
Cosolvent JSJ-701 0.8-7.0
The NaOH aqueous solution (30%) 1.0-10.0
Softener JSJ-312 E
Bleeding agent JSJ-151 F
Water (deionization) G
Add up to 100 parts
Nano composite material dispersion liquid configuration technology:
------------JSJ-504, JSJ-601, JSJ-606 (high speed shear mix, 40 minutes)------JSJ-151, JSJ-312, NaOH (stir, 30 minutes) add cold water simultaneously or only to add one or both the effect difference of SJ-606, JSJ-605 little for JSJ-701, JSJ-605 (stir down).
The nano composite material dispersion liquid adopts conventional dipping---oven dry---to bake technology, the results are shown in table 7 to the ecological clean processing of ultra micro fire resistance fibre material.
The performance of nano combined purificant of table 7 and ultra micro fire proofing
Annotate: 1. fibrous material: fire-retardant cotton plain cloth (40
s* 40
s128.4g/m
2).
2. nano combined cleaning liquid is not stratified in using, breakdown of emulsion, nothing do not precipitate.
3. after washing 6 times (180 minutes), anti-flammability and ecological index are constant.
As can be seen from Table 7: not only anti-flammability is unaffected with the ultra micro fire resistance fibre material of nano combined cleaning liquid processing, and main ecological index and other physical property meet project indicator requirement.This has proved the science and the reliability of the ecological clean technology of nano composite material.
5, industrial production was carried out on the production equipment of the company of the Changjiang river printing and dyeing newly in September, 2006 in batches, symbiosis produces three kinds of attitude fire resistance fibre material, more than 14000 meter (about 2800kg), yield rate reach more than 90%, and product colour is bleaching, rice ash and bottle green.In whole batch commercial process, because the preparation of laboratory research and each operation is more abundant, produce as a trial more smooth, process stabilizing, equipment move normal, and properties of product not only meet the project technical requirement, and reach the regulation of country and international relevant criterion, product has more than 12000 meter to sell to Britain and Australia respectively, also have more than 1000 meter to be bought as sample by the foreign trade client, clients such as English, Australia are satisfied with to product quality, and the purpose that continues cooperation is arranged.
6, batch industrialized producing technology and prescription
(1). technological process:
---bleaching is handled or dyeing, and---low temperature soaks into expanded (fire-retardant)---bakes---oxidation, neutralization, washing---nano ecological cleaning---finished product inspection crosslinked to ultra micro fibrous material (light and thin type cotton grey cloth)
(2) key process parameter:
Low temperature soaks into expanded infiltration: 15-30 ℃, 10-30 second
Expanded: 50 ℃ 20-40 minute
Bake crosslinking temperature: 145-185 ℃
Time: 2-8 minute
(3) flame-retardant formulations:
Fire retardant JSJ-111 25-38
Crosslinked resin JSJ-302 5-10
Auxiliary crosslinked resin JSJ-303 0.5-2.0
Formaldehyde eliminating agent JSJ-504 0.3-1.5
Softener JSJ-151 A
Catalyst JSJ-523 B
Bleeding agent JSJ-312 C
Cold water (deionization) D
Add up to 100 (%)
(4) nano combined cleaning liquid prescription
Purificant JSJ-606 (nano material) 0.2-2.0
Purificant JSJ-605 (absorbent-type material) 0.9-12.0
Purificant JSJ-601 (reactive materials) 0.5-5.2
Dispersant JSJ-504 0.2-1.5
Cosolvent JSJ-701 0.8-7.0
The NaOH aqueous solution (30%) 1.0-10.0
Softener JSJ-312 2 bleeding agent JSJ-151 2 add water to 100 (%)
The main performance index of ecological fire resistance fibre material is listed in table 9 and table 10.
Fire-retardant and the ecological performance of the ecological ultra micro fire resistance fibre of table 9 material
Annotate: fibrous material is: ecological fire-retardant cotton plain cloth (40
s* 40
s, 133 * 100).
The physical property of the ecological ultra micro fire resistance fibre of table 10 material
Annotate: fibrous material is: ecological fire-retardant cotton plain cloth (40
s* 40
s, 133 * 100).
Can see from table 9 and table 10:
(1) anti-flammability of ecological ultra micro fire resistance fibre material and washability meet project indicator requirement, and are better than fire retardant protective clothing and fire-retardant bedding standard both at home and abroad such as GB8965, GB50222 and BSEN533.
(2) ecological criteria of ecological ultra micro fire proofing not only meets project indicator requirement, and is better than ecological textile specification requirement both at home and abroad such as GB/T18885, Oeko-Texstandard100.
(3) ultimate strength of ecological ultra micro fire resistance fibre material, washing size changing rate, COLOR FASTNESS, bending rigidity indexs such as (fabric feelings) all are better than the project indicator and national sector standard.
Selection by technology path, the research of anti-flammability, durability, gentle may just as well harmonious configuration and the ecological clean technology of nano composite material, engineer testing, batch suitability for industrialized production, product quality overall merit, trial sale client's feedback opinion proves that the research of ecological ultra micro fire resistance fibre material and manufacture method has reached the requirement of original project technical indicator.
The numerical value of the numerical value project specifies that technical indicator reaches
Anti-flammability (before washing and after washing)
After flame time, s 0≤2
Time, s 0≤2 glow
Char length, mm 115 (washing back 135)≤150
The fusion drippage does not have
Burn till the hole nothing
Free formaldehyde, mg/kg 55≤75
Technical indicator reaches the numerical value project specifies
The peculiar smell nothing
But extracting heavy metal, mg/kg cadmium, no cadmium≤0.1
Plumbous, unleaded≤0.1
PH value 6.0 4.5-7.5
Limit unlimited three kinds of fire retardant
Ultimate strength, N T=578 〉=250
W＝450
Color fastness to washing, level 3.5 3-4
Colour fastness to rubbing, level are done 3.5 wet 3.0 and are done the wet 3-4 of 3-4
Bending rigidity, mN.cm 4.0≤5.5
11, the preparation of the stable dispersion liquid of nano composite material and application
The use amount of nano material dispersion liquid-nano combined purificant directly have influence on fibrous material ecological performance, feel gentle may just as well, index such as production cost, table 11 has provided nano combined purificant to the fibrous material Effect on Performance.
The nano combined clean dose of consumption of table 11 is to the fibrous material Effect on Performance
Annotate: (1) fibrous material is: cotton plain cloth (40s * 40s, 128.4g/m
2)
(2) can obtain close effect to different fibrous material compositions and structure.
Can see from table 7.2: (1) along with the increase of nano combined purificant consumption, the fabric weightening finish increases, manufacturing cost is higher.(2) along with the increase of nano combined purificant consumption, fabric feeling runs down.(3) after nano combined purificant consumption reached certain value, the ecological index of fibrous material changed little.Consider the composite factor of production cost and fibrous material performance indications, nano combined purificant consumption 3-7% is comparatively reasonable.
Claims (10)
1, the flame-proof treatment method of light and thin natural fiber material is characterized in that handling with following technology: the ultra micro fiber material fabric, and---bleaching is handled or dyeing, and---low temperature soaks into expanded flame treatment---bakes---oxidation, neutralization, washing---finished product inspection crosslinked; Wherein low temperature infiltration condition is: 15-30 ℃, 10-30 second; 35-60 ℃ and 20-40 minute of expanding treatment temperature; Bake crosslinking temperature: 145-185 ℃, time: 2-8 minute.
2, the flame-proof treatment method of light and thin natural fiber material according to claim 1, it is characterized in that then ultra micro fire resistance fibre material being handled with purificant, purificant is nano level titanium dioxide or/and zinc oxide ZnO, and weight proportion is 1-12.0wt%, dispersant 0.2-1.5wt%; And add the nano composite material dispersant and in the aqueous solution, handle.
3, the flame-proof treatment method of light and thin natural fiber material according to claim 1 and 2, its feature is expanded to the infiltration of fabric low temperature, high temperature bakes crosslinked; Fire retardant adopts Pyrovatex CP New or fire retardant JSJ-111: crosslinked resin mostly is the modification alkyl melamine derivative with active group, consumption 5-20%, and the working concentration of fire retardant is with 25%-38%; 15-30 ℃ of ultra micro fibrous material low temperature soaks into materials such as fire retardant, crosslinked resin, bleeding agents down, time 20-30 second; And parked 20-40 minute at 20-80 ℃; Bake process using and bake crosslinking temperature: 135-185 ℃, time: 2-8 minute.
4,, it is characterized in that crosslinked resin especially is JSJ-302 by the flame-proof treatment method of the described light and thin natural fiber material of claim 3.
5,, it is characterized in that 20-30 ℃ of low temperature infiltration temperature, time 20-30 second by the flame-proof treatment method of the described light and thin natural fiber material of claim 3; And 40-60 ℃ carry out 20-40 minute expanded.
6, the clean treatment method of light and thin natural fiber material according to claim 2 is characterized in that dispersant and adds water, and under agitation also high speed shear was mixed 20-60 minute; Or the NaOH that adds 0.1-0.5wt% again stirred 10-30 minute.
7, the clean treatment method of light and thin natural fiber material according to claim 2 is characterized in that the nano composite material dispersion liquid adopts conventional dipping to the ecological clean processing of ultra micro fire resistance fibre material---dry or bake technology; Bake process using and bake crosslinking temperature: 135-185 ℃, time: 2-8 minute, or behind the crosslinked resin dipping, bake crosslinked resin consumption 2-10% again.
8, according to the clean treatment method of claim 2 or 6 described light and thin natural fiber materials, it is characterized in that nano combined purificant consumption 3-7wt%, titanium dioxide and zinc oxide ZnO ratio be that 20-80wt% compares 80-20wt%.
9, according to the clean treatment method of claim 2 or 6 described light and thin natural fiber materials, it is characterized in that purificant nano composite material dispersion liquid prescription: nano material titanium dioxide 0.2-2.0, absorbent-type material oxidation zinc 0.9-12.0, dispersant adopts surface-activity, cosolvent JSJ-701 0.8-7.0; 30% NaOH aqueous solution 1.0-10.0; Softener JSJ-312 E; Bleeding agent JSJ-151 F; E, F is 1-10; Water is surplus, more than is percent by weight %, adds up to 100%.
10, according to the clean treatment method of claim 2 or 6 described light and thin natural fiber materials, it is characterized in that flame-retardant formulations: fire retardant JSJ-11125-38, crosslinked resin JSJ-302 5-10, auxiliary crosslinked resin JSJ-303 0.5-2.0, formaldehyde eliminating agent JSJ-504 0.3-1.5; Softener JSJ-151 2-3; Catalyst JSJ-523 1-2; Bleeding agent JSJ-312 1-2; The cold water surplus more than is percent by weight %, adds up to 100%.
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| PCT/CN2008/070297 WO2008098518A1 (en) | 2007-02-15 | 2008-02-13 | The flame retardant treatment method for light natural fiber material |
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Also Published As
| Publication number | Publication date |
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| WO2008098518A1 (en) | 2008-08-21 |
| CN100545343C (en) | 2009-09-30 |
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