CN107254720A - A kind of far-infrared anti-biotic organic silazane fire resistance fibre and its production method - Google Patents
A kind of far-infrared anti-biotic organic silazane fire resistance fibre and its production method Download PDFInfo
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- CN107254720A CN107254720A CN201710536062.8A CN201710536062A CN107254720A CN 107254720 A CN107254720 A CN 107254720A CN 201710536062 A CN201710536062 A CN 201710536062A CN 107254720 A CN107254720 A CN 107254720A
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- fire resistance
- organic silazane
- resistance fibre
- far
- spinning
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
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- 238000009987 spinning Methods 0.000 claims abstract description 38
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000001354 calcination Methods 0.000 description 4
- 238000004079 fireproofing Methods 0.000 description 4
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- 238000012545 processing Methods 0.000 description 4
- 229920002994 synthetic fiber Polymers 0.000 description 4
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- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
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- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 description 1
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- 230000007096 poisonous effect Effects 0.000 description 1
- 229920000548 poly(silane) polymer Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- 230000002829 reductive effect Effects 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
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- 230000001954 sterilising effect Effects 0.000 description 1
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- 235000002906 tartaric acid Nutrition 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical group Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
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Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
- D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/02—Chemical after-treatment of artificial filaments or the like during manufacture of cellulose, cellulose derivatives, or proteins
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
A kind of far-infrared anti-biotic organic silazane fire resistance fibre and its production method, the production method are comprised the technical steps that：(1) cellulose solution is prepared；(2) injected before spinning：Cellulose solution is mixed with organic silazane composite flame-retardant agent, spinning glue is made；Wherein organic silazane composite flame-retardant agent hydrolyzes dispersion liquid using organosilan and poly- borate is mixed；(3) spinning：Spinning glue sprays spinning by spinning head, is molded through acid bath, washes and obtain fire resistance fibre head product；(4) refine：The process fixation of obtained fire resistance fibre head product is crosslinked, washed, is oiled and baking operation obtains fire resistance fibre finished product.The organic silazane fire resistance fibre of the present invention has fire-retardant far-infrared anti-biotic performance stable, good endurance, wash resistant, the features such as wearing safe, with higher technology content and huge market prospects.
Description
Technical field
The present invention relates to a kind of organic silazane fire resistance fibre, category textile product field.
Background technology
The inside fire in the whole world more than 60% is that as caused by textile, more than 80% fire fatality is due to inhale at present
Entering toxic smoke or asphyxia causes.With the development and the formulation of every country fire safety regulation of human civilization, fire proofing is carried
Higher and higher requirement is gone out.From initially only consider material fire resistance, to fire proofing environmental protection, health care, outward appearance, comfortably
Requirement in terms of property.Flame retardant synthetic fibers (flame-resistant terylene, flame-retardant acrylic fibre etc.) and inherent fire-retardant fiber (aramid fiber, polyimides
Deng) although with good anti-flammability, because the comfortableness of fabric is poor, and meet fire shrink, melting, drippage etc. it is scarce
Fall into, can not meet requirement of the people to dress ornament comfortableness and security.
Current fire-retardant regenerated cellulose fiber (such as FRC) on the market, although fire-retardant dress ornament can be met
Processing and people's comfortableness basic to dressing (moisture absorption, ventilative) are required, but there is different degrees of defect.For example, phosphorus system hinders
Fire to produce in largely harmful flue gas, fiber and fabric when viscose rayon has burning and contain P elements, what is produced during burning has
Evil flue gas easily makes one asphyxia, and its discarded object makes the ill effects such as water resource eutrophication in degradation process；Silicon systems are fire-retardant viscous
There is strength defect low, intolerant to alkali cleaning in glue fiber, can only be used as nonwoven or inserts, it is impossible to as fabric.
Compared to above-mentioned fire-retardant regenerated cellulose fiber, silicon nitrogen system fire-retardant regenerated cellulose fiber is as a result of silicon nitrogen system
Fire retardant, overcome the phosphorous flame-retardant viscose rayon burning a large amount of harmful smokes of release and silicon systems anti-flaming viscose strength it is low and intolerant to
The defect of alkali cleaning, results in high fire-retardance, the product of high textile performance, is that the fire-retardant regenerated cellulose of great development prospect is fine
Dimension.Silicon nitrogen FRC for example disclosed in Publication No. CN103789858 and CN104032401 patent.
Nowadays the increase in demand with market to flame-retardant textile material, Prospect for Flame Retardant Fiber Materials be not applied only to army, fire-fighting,
The individual protection fields such as industrial protection clothes, the application of the commercial market such as vehicles interior trim, home textile, specific group's clothes is equally not
It can estimate.Therefore multi-functional to the fire resistance of fire resistance fibre and fabric, the requirement of the feature of environmental protection and durability is also increasingly carried
It is high.
The content of the invention
It is an object of the invention to provide a kind of organic silazane fire resistance fibre with long-acting far infrared transmission and antibacterial functions
And its production method.
According to the production method of the far-infrared anti-biotic organic silazane fire resistance fibre of the present invention, comprise the technical steps that：
(1) cellulose solution is prepared；
(2) injected before spinning：Cellulose solution is mixed with organic silazane composite flame-retardant agent, spinning glue is made；It is wherein organic
Silicon nitrogen composite combustion inhibitor hydrolyzes dispersion liquid using organosilan and poly- borate is mixed；
(3) spinning：Spinning glue sprays spinning by spinning head, is molded through acid bath, washes and obtain fire resistance fibre head product；
(4) refine：The process fixation of obtained fire resistance fibre head product is crosslinked, washed, is oiled and baking operation is obtained
Fire resistance fibre finished product.
Under preferable case, wherein the addition of organic silazane composite flame-retardant agent is 20 of content of cellulose in cellulose solution
~30% (w/w).
Under concrete condition, wherein organosilan hydrolysis dispersion liquid chemical formula is：
[MexOy·nSiO2]+[--CONH]
Wherein：Me represents metal ion；The metal ion is Ti4+And Ca2+；
Under preferable case, silicon, titanium, calcium, the mol ratio of boron ion are 1 wherein in organic silazane composite flame-retardant agent:0.5~1:
1~2:0.5~1.
Under preferable case, wherein the structural formula of poly- borate is as follows：
Molecular weight is 800-1200.
Boron ion not only has excellent flame retardant effect, also with excellent sterilization, fungistatic effect.But if using inorganic
Boron salt class, because steric hindrance effect is poor, is very easily hydrolyzed and dissolution, it is impossible to retain in the fibre.The present invention, which is used, to be had
The poly- borate of specific structure formula and molecular weight, steric hindrance is big, can be permanently kept in fiber, be hindered all the life with fiber lifetime
Combustion.Product addition can play fire-retardant, antibacterial double effectses 5~8%.
In one embodiment, injecting step is specially before spinning：The compound resistance of organic silazane is injected into cellulose solution
Agent is fired, dynamic mixing is first passed through, then by static mixing, finally enter tempering tank and be mixed to get spinning glue again.Preferable case
Under, the temperature of hybrid reaction is 20~30 DEG C in tempering tank, and the time is 30-120 minutes.Under the selection process, cellulose with
Organic silazane composite flame-retardant agent can be fully combined together.
In another specific embodiment, the fixation cross-linking process step wherein in refinement step is specially：By water, fixed crosslinking
Agent, NaHSO3Fixed crosslinking 10-30min in the fixation bath prepared according to a certain ratio.Under preferable case, the pH value of fixation bath is kept
In 6.0~8.0,75-90 DEG C of the temperature of fixation bath；At the process conditions, inventors be surprised to learn that, fixed friendship can be greatly improved
Join reactivity, that is, improve organic silazane fire resistance fibre washing resistance performance；It is 20-25wt%'s that the concentration of crosslinking agent, which need to only be fixed,
Fixation bath ensures that the resistance to alkali cleaning performance of organic silazane fire resistance fibre, Loss Rate≤2% of fire retardant during alkali cleaning.
Under concrete condition, the composition of the fixed crosslinking agent includes multi-hydroxy carboxy acid, polyhydroxy-alcohol, sugar and metal component.
Under preferable case, the multi-hydroxy carboxy acid is one or more of mixing in lactic acid, tartaric acid, citric acid or beta-hydroxy-butanoic acid
Thing；The polyhydroxy-alcohol is one or more of mixtures in propane diols, glycerine, ethylene glycol or polyhydroxy sterol；It is described
Sugar is one or more of mixtures in sucrose, fructose or glucose；The metal component is titanium tetrachloride, calcium chloride, sulphur
One or more of mixtures in sour aluminium or titanium tetraisopropylate acid esters.
In a preferred embodiment, the fixed cross-linking process step is to react fiber head product by cross-linked graft twice,
Processing is pressed dry by pressure roller progress in the middle of cross-linked graft reaction twice.The fiber of preceding working procedure is carried out pressing dry place by pressure roller
Reason, beneficial to follow-up graft crosslinking agent and the abundant reaction of fiber, abundant reacted its enduring quality of resistance to alkali cleaning of fire resistance fibre shows
Write and improve.
The organic silazane fire resistance fibre of the present invention, can contain other adding ingredients, such as mill base, antistatic additive were being produced
In journey colored regenerated cellulose fiber, antistatic regenerated celulose fibre are produced by adding above heterogeneity.
The present invention organic silazane fire resistance fibre, both can pure spun yarn, fabric and fabric, again can be with other fibers or original
Blend fibre is made in material, such as with phosphorous flame-retardant regenerated celulose fibre, silicon systems fire-retardant regenerated cellulose fiber, pure cotton, fire-retardant
Cotton, various regenerated celulose fibres (such as common viscose fiber, Modal fibre, tencel), wool, cashmere, aramid fiber, fragrant sulfone
Synthetic fibre, polyimides, alginate fibre, various synthetic fibers, various flame retardant synthetic fibers, pre-oxidized fibers, glass fibre etc. are a variety of
Fiber blending in all proportions, makes the different yarn of function, fabric and fabric.
The organic silazane fire resistance fibre or blend fibre of the present invention, can also exist in glassine paper form, can be as high-end
Ornament materials and packaging material.
The organic silazane fire resistance fibre or blend fibre of the present invention, can also exist in foamed cotton form, can be used as various
Flame retardant filler, such as fire blocked mattress, flame-retardant sofa pad.
The fabric being made according to the organic silazane fire resistance fibre of the present invention can be used for protective garment, noneffectives' clothes, old age
People's clothes, infant clothing, land, sea and air transport interior trim, the cover for seat of public place, sofa, mattress curtain, underskirt, socks
Son, wrap for joints (knee-pad, elbow support, wrister), bedding, intelligent garments worn etc..
The organic silazane fire resistance fibre of the present invention has fire-retardant far-infrared anti-biotic performance stable, and good endurance, wash resistant is worn
The features such as safe.The discovery of a variety of functions has also widened application for the fire resistance fibre product：Not only fire resistance is good
It may be used as special protective garment, home textile, vehicles interior trim etc..Simultaneously because its traffic safety and riding comfort, excellent far-infrared anti-biotic
Also it is very suitable for making such as antibacterial underwear Deng healthcare function, antibacterial socks, health care textile etc., with higher technology content
With huge market prospects.
Brief description of the drawings
Fig. 1 is the scanning electron microscope image of the organic silazane fire resistance fibre of the present invention；
Fig. 2 is Fig. 1 partial enlargement image；
Fig. 3 is the cross-sectional image of fiber in Fig. 1；
Fig. 4 is the scanning electron microscope image after 700 DEG C of calcinations of organic silazane fire resistance fibre of the present invention.
Embodiment
First, primary raw material and equipment
Organic silazane series composite flame retardant：The blue fire resistance fibre Co., Ltd of Beijing Sail.
Fixed crosslinking agent：The blue fire resistance fibre Co., Ltd of Beijing Sail.
Injection device before cellulose solution and spinning:Shandong YINYING Chemical Fiber Co., Ltd.
Spinning and equipment for after-treatment:Shandong YINYING Chemical Fiber Co., Ltd.
Detecting instrument and unit：National textile fabrics Quality Supervision and Inspection Center, Donghua University, Beijing Institute of Technology are fire-retardant
Material tests center, the blue fire resistance fibre Co., Ltd of Beijing Sail.
2nd, production process
Embodiment 1
Using first fibre 7.5%, containing alkali 5.5%, viscosity 53 seconds, degree of ripeness 16.2ml cellulose solution, inject to fiber
Element amount 20wt% organic silazane composite flame-retardant agent, silicon, titanium, calcium, mole of boron ion wherein in organic silazane composite flame-retardant agent
Than for 1:0.5:1:0.5.Dynamic mixing is first passed through, then by static mixing, finally enters tempering tank and is mixed to get spinning again
Glue.Incorporation time is 50min to tempering tank again, and temperature is 25 DEG C.Mix adhesiveness 70 seconds, degree of ripeness (10% ammonium chloride)
10ml.Regenerated by spinning head spinning in coagulating bath, coagulation bath composition is sulfuric acid 75g/l, sodium sulphate 160g/l, zinc sulfate
40 DEG C of 20g/l, temperature.Fibre bundle progress drawing-off, cut-out, washing, fixation after regeneration are crosslinked, bleached, oiling, drying, beating
Bag.The condition of wherein fixed crosslinking bath is：The concentration of fixed crosslinking agent is 15%, and pH value is maintained at 7.5 or so, 80 DEG C of temperature；
Fixed cross-linking process step is to react fiber head product by cross-linked graft twice, is entered in the middle of cross-linked graft reaction twice by pressure roller
Row press dry processing, and the total time of cross-linked graft reaction twice is 30min.
Embodiment 2
Using first fibre 7.5%, containing alkali 5.5%, viscosity 53 seconds, degree of ripeness 16.2ml cellulose solution, inject to fiber
Element amount 28wt% organic silazane composite flame-retardant agent, silicon, titanium, calcium, mole of boron ion wherein in organic silazane composite flame-retardant agent
Than for 1:1:1:1.Dynamic mixing is first passed through, then by static mixing, finally enters tempering tank and is mixed to get spinning glue again.It is mixed
Closing bucket, incorporation time is 60min again, and temperature is 30 DEG C.Mix adhesiveness 70 seconds, degree of ripeness (10% ammonium chloride) 10ml.Pass through
Spinning head spinning regenerates in coagulating bath, and coagulation bath composition is sulfuric acid 75g/l, sodium sulphate 160g/l, zinc sulfate 20g/l, temperature
40℃.Fibre bundle progress drawing-off, cut-out, washing, fixation after regeneration are crosslinked, bleached, oiling, drying, packing.Wherein fix
Being crosslinked the condition bathed is：The concentration of fixed crosslinking agent is 25%, and pH value is maintained at 8.0 or so, 85 DEG C of temperature；Fixed cross-linking process step
It is to react fiber head product by cross-linked graft twice, processing is pressed dry by pressure roller progress in the middle of cross-linked graft reaction twice,
The total time of cross-linked graft reaction twice is 20min.
3rd, characterize and test
Fiber surface morphology and cross-sectional structure are characterized using ESEM (SEM).ESEM：Japanese JEOL
Company produces, JSM-5600LV.
Limiting oxygen index determination：Organic silazane fire-retardant regenerated cellulose chopped fiber is made into 200g/m2Non-woven fabrics, respectively with organic
Silicon nitrogen fire-retardant regenerated cellulose chopped fiber and non-woven fabrics determine oxygen index (OI).Oxygen index (OI) method of testing is according to GB/T 5454-1997
《Textile combustion performance test oxygen index method》Fire proofing inspection center of commission Beijing Institute of Technology is detected.Main test
Equipment：FTA II oxygen index instruments.
Resistance to alkali cleaning performance test：By standard HX/T 51011-2015《Organic silazane fire retardant viscose short filament》Tested.
Alkali cleaning specific method is that fiber sample is placed in into bath raio 1：50 concentration is 3g/L Na2CO395 DEG C of heating 1h in solution.Then
Respectively by before alkali cleaning, 700 DEG C of calcinations of fiber sample after alkali cleaning are eliminated after organic matter, determine the quality of ignition residue (fire retardant)
Percentage.Fire retardant mass percent difference is the numerical value of resistance to alkali cleaning before and after alkali cleaning.
Far infrared performance test：The short fibre of fire resistance fibre is woven into density for 200g/m2Pure spinning fabric, washing 50 times after
Tested and (change water 2 in wash conditions washing 12.5h, rinsing 1.5h, rinse cycle in washing methods reference GB/T 17596
It is secondary, 4min is dehydrated, whole process is washing 50 times).Reference standard FZ/T 64010-2000 are measured, CAS 115-2005
《Healthcare function textile》Evaluated.Consignment unit is national textile fabrics Quality Supervision and Inspection Center.
Antibacterial functions are tested：The short fibre of fire resistance fibre is woven into density for 200g/m2Pure spinning fabric, washing 50 times is (same
On) tested afterwards.According to standard GB/T/T 20944.3-2009《Antibacterial textile performance evaluation Part III succusion》
Carry out evaluation measure.Consignment unit is national textile fabrics Quality Supervision and Inspection Center.
The architectural feature of 3.1 organic silazane fire resistance fibres
It will be seen from figure 1 that there is a big longitudinal groove in the organic silazane fire resistance fibre surface of the present invention, favorably
It is ventilative in fiber hydrofuge.Fig. 2 shows that fiber surface is relatively smooth, the solid particle without fire retardant, because fire retardant is
Added in precursor solution form, the polysilane that coagulating bath generation solgel reaction generation solid is met in spinning process is equal
It is even to be dispersed in fibrous inside, so surface observation is less than fire-retardant particles.Fiber surface only has some vertically small thin
Line, this may illustrate that cellulosic molecule axially has preferable orientation along fiber in forming process, and flame retardant constituent is not parcel
It is, with " T-shaped " structure and line style regenerated cellulose formation crossover network, to be tightly combined with fiber bodies in fiber surface.Fig. 3 is
Fiber cross sections figure, because flame retardant constituent is difficult to quench disconnected in liquid nitrogen, small protrusion or depression can be caused in section, so can
To observe that section is more coarse, degree of roughness is more uniform, and display fire retardant is distributed also more uniformly on cross section, and
There is no obvious interfacial separation situation, illustrate that fire retardant and cellulose matrix bonding state are preferable.Fig. 4 is 700 DEG C of calcinations of fiber
Fall to retain after organic matter the distribution situation of fire retardant, picture show, after calcination fire retardant into graininess in the fibre in continuously
Net distribution, particle diameter is small, average in below 100nm, and is evenly distributed, without substantially reunion.
The fire resistance and washing resistance performance of 3.2 organic silazane system fire resistance fibres
Limited oxygen index LOI is one of fire proofing important indicator.The oxygen index (OI) of common viscose fiber is less than 20%, very
Easily burning.The general material for being more than 28% in limited oxygen index belongs to nonflammable material.
The fire resistance test result of the organic silazane fire resistance fibre of table 1.
Through overtesting and test, when the total effective content of fire retardant is more than 28% in fiber, the fire-retardant regeneration of organic silazane is fine
The limited oxygen index of the plain chopped fiber of dimension is more than 36%.The oxygen index (OI) of its non-woven fabrics fabric is also greater than 33%.In oxygen index (OI), this refers to
Put on, be sufficiently close to aramid fiber 1313, be better than phosphorus system, silicon systems FRC.And smog is small when burning, without poisonous and harmful
Gas is produced, the phenomenon such as no melting drippage contraction.
The washing resistance performance of the organic silazane fire-retardant regenerated cellulose fiber of table 2.
A is noted：Washing process is to wash 12.5h by wash conditions in GB/T 17596, rinses in 1.5h, rinse cycle and changes water
2 times, 4min is dehydrated, whole process is washing 50 times.Detect unit：Beijing Sail blue fire resistance fibre Co., Ltd research center is real
Test room.
From result of the test, its resistance to alkali cleaning performance of organic silazane fire resistance fibre and wash durability are preferable, fire retardant
Amount lost is few, because fire retardant T-shaped network structure distribution in the fibre, close with Hydrogenbond with cellulosic molecule.
And by after crosslinking curing, fire retardant is changed into alkalescence from faintly acid, resistance to alkali cleaning performance is further improved.
The far-infrared functional research of 3.3 organic silazane fire resistance fibres
Ultrared wavelength is 0.76~1000 μm of electromagnetic wave, and its medium wavelength is more than 5 μm of commonly referred to as far infrareds.Far
Infrared fibre and its fabric can absorb the energy that human body and surrounding environment are distributed in infra-red radiation form, it is possible to radiate 4~14 μ
M, which goes out this human body, needs the electromagnetic wave of wave band.Under the wave band, human body surface molecule absorption radiation, temperature rise, human body is produced
Warmth sensation, internal Marjoram Extract accelerates blood circulation and metabolism.
Remove outside coating Final finishing, ceramic powder is added when general far IR fibre is spinning or contains ceramic powder
Prepared by master batch, but this method has higher limitation to the content and granularity of ceramic powder.Content is low, and far-infrared functional is not
Significantly.Too high levels or granularity, which cross conference, causes difficulty in spinning, and fibrous mechanical property is greatly reduced.And with far-infrared functional
Organic silazane composite flame-retardant agent is that organic solution form adds spinning, has a certain degree of carry to the upper limit of additive level
After height, spinning moulding, fire retardant is uniformly dispersed in fibre substrate, and particle diameter is small, reaches sub-micron rank, then hand over by solidification
Silicon, titanium, calcium, boron element and organosilan in connection, fire retardant are further incorporated on regenerated cellulose main chain, form silicon titanium calcium
Boron system ceramic network, constitutes far infrared transmission group, so as to possess stronger far-infrared transmitting function.
The pure textile fabric far infrared test result of the organic silazane fire resistance fibre of table 3.
Through overtesting and test, when the total effective content of fire retardant is more than 20% in fiber, organic silazane fire resistance fibre is pure
The normal emittance of textile fabric is more than 89%, higher than the requirement of far infrared product normal emittance 80%, illustrates that the fiber has
There is preferable far-infrared transmitting function.
The fungistatic effect research of 3.4 organic silazane fire resistance fibres
The organic silazane fire resistance fibre uni-material fabric fungistatic effect of table 4.
According to experiment and testing result, when the total effective content of fire retardant is more than 20% in fiber, by the organic of washing
The pure cloth that spins of silicon nitrogen fire resistance fibre has exceeded 96% to the 24h bacteriostasis rates of three kinds of bacteriums or fungi, can assert the fire-retardant fibre of silicon nitrogen
Effect of the dimension with preferable antibacterial.Especially for staphylococcus aureus, antibacterial effect is notable.And this result is fabric
Antibacterial effect after washing 50 times, illustrates that additive component is firmly combined with cellulosic matrix, and antibacterial effect will not be because anti-
After backwashing is washed and eliminated, good endurance.
The antibacterial flame-retardant agent composition of organic silazane fire resistance fibre is mainly submicron-scale nonmetal oxide and metal oxygen
The silicon titanium calcium boron system ceramic network that compound is constituted, its antifungal mechanism makes to divide in microbial body for the far infrared radiation ability of the fiber
Son vibration aggravation, cell metabolism is abnormal, causes the death of microorganism.Cellulose surface is grafted with a large amount of poly- borates simultaneously
Molecule, most of bacterium and fungi are in the case where pH is neutrality, and cell membrane or cell body are negatively charged, due to Electrostatic Absorption effect
Should, the presence of a large amount of poly- boric acid ester molecules has fettered the free degree of bacterium, that is, sloughing the free amino cation of acyl group can neutralize
The negative electrical charge of bacterium surface, changes its surface charge number and causes " bacterolysis ", or enters inside bacterium, is sent out with bacterial cytoplasm
Raw reaction, the metabolism for suppressing bacterium causes it dead.
In the present invention, due to organic silazane far-infrared anti-biotic fire retardant be before spinning in add precursor solution to spinning
In liquid, first it is grafted in spinning process and cellulose blending, then crosslinks curing reaction with fiber again, so as to uniform jail
Solid be distributed in fiber, it is difficult for drop-off, belong to long-acting far-infrared anti-biotic fire resistance fibre.Therefore added relative to Final finishing fire-retardant
The fiber or textile of agent/antiseptic, organic silazane fire-retardant regenerated cellulose fiber of the invention have fire-retardant far-infrared anti-biotic
Performance is stable, good endurance, wash resistant, the features such as wearing safe.The discovery of a variety of functions is also widened for the fire resistance fibre product
Application：Not only fire resistance well may be used as special protective garment, home textile, vehicles interior trim etc..Simultaneously because its
Traffic safety and riding comfort, the healthcare function such as excellent far-infrared anti-biotic is also very suitable for making such as antibacterial underwear, antibacterial socks, health care
Textile etc..In summary, organic silazane fire-retardant regenerated cellulose fiber meets all of novel flame-retardant far-infrared anti-biotic fiber
It is required that, with higher technology content and huge market prospects.
Claims (10)
1. a kind of production method of far-infrared anti-biotic organic silazane fire resistance fibre, is comprised the technical steps that：
(1) cellulose solution is prepared；
(2) injected before spinning：Cellulose solution is mixed with organic silazane composite flame-retardant agent, spinning glue is made；Wherein organic silazane
Composite flame-retardant agent hydrolyzes dispersion liquid using organosilan and poly- borate is mixed；
(3) spinning：Spinning glue sprays spinning by spinning head, is molded through acid bath, washes and obtain fire resistance fibre head product；
(4) refine：The process fixation of obtained fire resistance fibre head product is crosslinked, washed, is oiled and baking operation obtains fire-retardant
Fiber finished product.
2. the production method of far-infrared anti-biotic organic silazane fire resistance fibre according to claim 1, wherein organic silazane are answered
The addition for closing fire retardant is 20~30% (w/w) of content of cellulose in cellulose solution.
3. the production method of far-infrared anti-biotic organic silazane fire resistance fibre according to claim 1, wherein organosilan water
Solving dispersion liquid chemical formula is：
[MexOy·n SiO2]+[--CONH]
Wherein：Me represents metal ion；The metal ion is Ti4+And Ca2+。
4. the production method of far-infrared anti-biotic organic silazane fire resistance fibre according to claim 3, wherein organic silazane are answered
It is 1 to close silicon in fire retardant, titanium, calcium, the mol ratio of boron ion:0.5~1:1~2:0.5~1.
5. the production method of far-infrared anti-biotic organic silazane fire resistance fibre according to claim 1, wherein poly- borate
Structural formula is as follows：
Molecular weight is 800-1200.
6. the production method of far-infrared anti-biotic organic silazane fire resistance fibre according to claim 1, injecting step tool before spinning
Body is：Organosilicon nitrogen composite combustion inhibitor is injected into cellulose solution, dynamic mixing is first passed through, then by static mixing, finally
It is mixed to get spinning glue again into tempering tank.
7. mixed in the production method of far-infrared anti-biotic organic silazane fire resistance fibre according to claim 6, tempering tank anti-
The temperature answered is 20~30 DEG C, and the time is 30-120 minutes.
8. the production method of far-infrared anti-biotic organic silazane fire resistance fibre according to claim 1, wherein in refinement step
Fixation cross-linking process step be specially：By water, fixed crosslinking agent, NaHSO3Fixed crosslinking 10-30min in the fixation bath of preparation.
9. the production method of far-infrared anti-biotic organic silazane fire resistance fibre according to claim 8, the fixed crosslinking agent
Composition include multi-hydroxy carboxy acid, polyhydroxy-alcohol, sugar and metal component.
10. the far-infrared anti-biotic organic silazane fire resistance fibre produced according to any described production methods of claim 1-9.
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| CN111020737B (en) * | 2019-12-19 | 2022-06-14 | 陕西元丰纺织技术研究有限公司 | Antibacterial flame-retardant fiber and preparation method of fabric thereof |
| CN110982107A (en) * | 2019-12-27 | 2020-04-10 | 北京赛欧兰阻燃纤维有限公司 | Flame-retardant, antibacterial and anti-mite regenerated cellulose foam cotton and preparation method thereof |
| CN113046892A (en) * | 2019-12-27 | 2021-06-29 | 北京赛欧兰阻燃纤维有限公司 | Novel three-proofing fabric |
| CN112575409A (en) * | 2020-12-01 | 2021-03-30 | 江苏合源纺织科技有限公司 | Flame-retardant cotton-like polyester-nylon composite superfine fiber and production method thereof |
| CN115387113A (en) * | 2022-07-28 | 2022-11-25 | 郑喜才 | Far infrared deodorization fabric and preparation method thereof |
| CN117468110A (en) * | 2023-11-01 | 2024-01-30 | 广东秋盛资源股份有限公司 | Far infrared antibacterial organic silicon nitrogen flame-retardant fiber and production method thereof |
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