CN109402756A - A kind of preparation method of fire-retardant Lyocell fibers - Google Patents
A kind of preparation method of fire-retardant Lyocell fibers Download PDFInfo
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- CN109402756A CN109402756A CN201811247384.1A CN201811247384A CN109402756A CN 109402756 A CN109402756 A CN 109402756A CN 201811247384 A CN201811247384 A CN 201811247384A CN 109402756 A CN109402756 A CN 109402756A
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- 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
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- 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
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- 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
Abstract
The present invention relates to a kind of preparation methods of fire-retardant Lyocell fibers, it is characterized in that fire retardant tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp, which are dissolved in N-methylmorpholine-N- oxide water solution, is made spinning solution；Spinning solution enters spinning system, the silk thread of ejection perpendicular stretching in air, into coagulating tank, solidificating fiber；Fiber the techniques such as is washed using alcohol, bleaches, washes, oils and is dried and fire-retardant Lyocell fibers are prepared.Lyocell fibers prepared by the present invention do breaking strength between 43~45cN/tex, and dry elongation at break is between 13.5%~15%；Lyocell fibers wet breaking strength is between 31.5~33cN/tex, and for the wet elongation at break of fiber between 15%~17%, the strength property of the Lyocell fibers of main strength property and market purchasing is close.The limit oxygen index of fire-retardant Lyocell fibers prepared by the present invention reaches 33% or more；It is washed by 20 times, flame retardant effect does not still obviously weaken, and shows that fire retardant and cellulose binding force are very strong.
Description
Technical field
The invention belongs to flame retardant textiles technical fields, more particularly to a kind of preparation method of fire-retardant Lyocell fibers.
Background technique
Lyocell fibers are a kind of excellent cellulose fibres, and hygroscopicity and comfort with natural fiber have
The advantages that synthetic fibers intensity is high.The preparation method of Lyocell fibers is using N-methylmorpholine-N- oxide (referred to as: NMMO)
For the direct dissolving spinning pulp of solvent, it is prepared through dry spray-wet spinning spinning technique.The production process of Lyocell fibers is to environment
It is pollution-free, it can natural degradation, referred to as 21 century revolutionary character fiber and textile raw material.But due to the master of Lyocell fibers
Wanting raw material is cellulose, and flame retardant effect is very poor.The research report of literature survey discovery, the flame retardant property of cellulose is more, such as:
Chinese Patent Application No. 201610596273.6 discloses a kind of method for improving organic silazane fire resistance fibre washing resistance performance, in
State's number of patent application 201320427300.9 discloses a kind of fire resistance fibre dipped canvas.However, Lyocell fibers flame retardant property
Research be rarely reported.
Currently, there are many fire retardant type for fabric, wherein organophosphorous fire retardant has lot of advantages, contains phosphorus system
When the high polymer of fire retardant is burned, fire retardant can be catalyzed hydroxy-containing compounds by the oxyacid for thermally decomposing to generate phosphorus, this kind of acid
Be dehydrated into charcoal, reduce the mass loss speed of material and the production quantity of combustible, and phosphorus then largely remains in carbon-coating.Carbon
Layer itself is fire retardant, heat-insulated, oxygen barrier, and burning can be made to suffocate.The thick semisolid of the oxyacid polyphyly of phosphorus, can be in material table
Face forms one layer of liquid film for being covered in coke layer, this can reduce coke layer and be not continued oxidation, is conducive to improve the fire-retardant of material
Property.But the combination of organophosphorous fire retardant and cellulose fibre is relatively difficult, even if organophosphorous fire retardant is attached to cellulose
Fiber surface, fabric may also fall off by repeatedly washing, organophosphorous fire retardant, thus, the flame retardant effect of fabric can seriously be cut
It is weak.
Lyocell fibers have excellent performance, are widely used in many fields, still, the Lai Sai with flame retardant property
You are bound to be used widely in more fields at the hardly seen report of fiber if being assigned fire-retardant performance.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of conventional art, a kind of preparation method of fire-retardant Lyocell fibers is provided.Phosphorus
Sour three (2,3- dibromopropyl) esters are a kind of excellent organic fire-retardants, and the present invention is by tricresyl phosphate (2,3- dibromopropyl) ester and fine
Dimension element is dissolved in organic solvent NMMO simultaneously, is then carried out spinning and is prepared Lyocell fibers, this preparation method overcomes fire-retardant
The weak disadvantage of the binding force of agent and cellulose fibre, realizes the homogeneous blend of fire retardant and cellulose fibre.Present invention preparation
Lyocell fibers have the function of fire-retardant, have a extensive future.
The preparation method of a kind of fire-retardant Lyocell fibers of the present invention, which is characterized in that the method includes as follows
Step:
(1) preparation of spinning solution: the aqueous solution by mass fraction for 50~55% NMMO is evaporated under reduced pressure to 85~90%
NMMO aqueous solution, tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp (Shandong YINYING Chemical Fiber Co., Ltd's production) are dissolved in
NMMO aqueous solution, wherein the mass ratio of tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp is 1 ︰ 25~30, the quality of Cotton Pulp
It (g) is 1 ︰ 15~20 with the bath raio of NMMO aqueous solution volume (mL), 3 are dissolved in 105~125 DEG C of vacuum stirring in a kettle~
4 hours, the uniform spinning solution that mass fraction is 15~18% is made；
(2) spinning of Lyocell fibers: screw extruder is added in step (1) treated spinning solution, at 90~120 DEG C
Lower further dissolution, is then filtered, into spinning system, wherein gas length is 7~9cm, and spinning speed is 45~50m/
Min, the hole diameter of spinneret are 40~115 μm, 400~800 μm of hole long capillary tube；The perpendicular stretching in air of the silk thread of ejection,
Into coagulating tank, solidification forming, the aqueous solution for the NMMO that solidification bath concentration is 15~18%, coagulation bath temperature is 0~8 DEG C；
Lyocell fibers spinning equipment flow chart is as shown in Figure 1；
(3) alcohol of fiber is washed: step (2) treated fiber being immersed the ethanol solution that concentration is 82~88%, is immersed
Time is 3~4 hours, and solution temperature is room temperature, 1 ︰ 15~20 of bath raio；
(4) step (3) treated fiber the bleaching of fiber: is immersed into the bleaching agent solution that concentration is 0.1~0.3g/L
(title: strong chlorine oil, the production of clean water treatment Science and Technology Ltd., Shandong PCI-SLR Technology), immersing the time is 2~4 hours, and solution temperature is
50~55 DEG C, 1 ︰ 15~20 of bath raio；
(5) washing of fiber: step (4) treated fiber being immersed in 85~95 DEG C of hot water, and the time is 2~3 small
When, 1 ︰ 20~25 of bath raio；
(6) fiber oils: by the oil bath solution (model: HY- of step (5) treated fiber immerses 0.5~1g/L
101, the production of Hangzhou Hua Ya Chemical Co., Ltd.), oil bath temperature is 85~90 DEG C, and the time is 2~4 hours, 1 ︰ 20~25 of bath raio；
(7) drying of fiber: by step (6), treated, and fiber obtains Lyocell fibers after drying and processing.
The present invention has following distinguishing feature:
(1) the dry breaking strength of Lyocell fibers prepared by the present invention between 43~45cN/tex, stretch by dry fracture
Long rate is between 13.5%~15%；Its wet breaking strength is between 31.5~33cN/tex, the wet extension at break of fiber
For rate between 15%~17%, the strength property of the Lyocell fibers of main strength property and market purchasing is close.This hair
The cellulose fibre of bright preparation is a qualified Lyocell fibers.
(2) present invention uniformly mixes cellulose and tricresyl phosphate (2,3- dibromopropyl) ester in NMMO aqueous solution, prepares
For Lyocell fibers.Tricresyl phosphate (2,3- dibromopropyl) ester is a kind of excellent fire retardant, and the Lyocell fibers of preparation also have
Excellent flame retardant property.
(3) the initial threshold oxygen index (OI) of Lyocell fibers prepared by the present invention has reached 33% or more, belongs to nonflammable material
Range；After 20 washings, limit oxygen index is not decreased obviously, and has still reached 32% or more；Its flame retardant effect is still
Obviously do not weaken so, shows that fire retardant and cellulose binding force are very strong.The method of the present invention preparation Lyocell fibers have compared with
Strong anti-flammability, whole simple production process are cheap, and production process environmental pollution is small.
Detailed description of the invention
Fig. 1 Lyocell fibers spinning equipment flow chart (1. spin fluids；2. godet；3. coagulating bath；4. godet；5.
Take-up roll；6. spinning head；7. conduit；8. metering pump；9. static mixer；10. filter；11. metering zone；12. gas vent；
13. screw rod；14. hopper；15. paddle；16. suspension)
Specific embodiment
The present invention is described in detail in embodiment described below.
Embodiment 1
A kind of preparation method of fire-retardant Lyocell fibers of the present embodiment, the preparation method comprise the following steps:
(1) preparation of spinning solution: the aqueous solution by mass fraction for 50.4% NMMO is evaporated under reduced pressure to 86.7%
Tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp (Shandong YINYING Chemical Fiber Co., Ltd's production) are dissolved in NMMO by NMMO aqueous solution
Aqueous solution, wherein the mass ratio of tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp be 1 ︰ 25, the quality (g) of Cotton Pulp with
The bath raio of NMMO aqueous solution volume (mL) is 1 ︰ 15, is dissolved 3.5 hours in 105 DEG C of vacuum stirrings in a kettle, and quality is made
The uniform spinning solution that score is 15.8%；
(2) spinning of Lyocell fibers: being added screw extruder for step (1) treated spinning solution, at 90 DEG C into
The dissolution of one step, is then filtered, into spinning system, wherein gas length 7cm, spinning speed 45m/min, spinneret hole
Diameter is 40 μm, 400 μm of hole long capillary tube；The perpendicular stretching in air of the silk thread of ejection, into coagulating tank, solidification forming,
The aqueous solution for the NMMO that bath concentration is 15% is solidified, coagulation bath temperature is 0 DEG C；Lyocell fibers spinning equipment flow chart such as Fig. 1
It is shown；
(3) alcohol of fiber is washed: step (2) treated fiber being immersed the ethanol solution that concentration is 82%, immerses the time
It is 3.5 hours, solution temperature is room temperature, 1 ︰ 16 of bath raio；
(4) bleaching of fiber: by step (3) treated fiber immerse bleaching agent solution that concentration is 0.1g/L (title:
Strong chlorine oil, the production of clean water treatment Science and Technology Ltd., Shandong PCI-SLR Technology), immersing the time is 2 hours, and solution temperature is 50 DEG C, bath raio
1 ︰ 15；
(5) washing of fiber: step (4) treated fiber being immersed in 85 DEG C of hot water, and the time is 2 hours, bath raio
1 ︰ 20；
(6) fiber oils: by the oil bath solution of step (5) treated fiber immerses 0.5g/L (model: HY-101,
The production of Hangzhou Hua Ya Chemical Co., Ltd.), oil bath temperature is 85 DEG C, and the time is 2 hours, 1 ︰ 20 of bath raio；
(7) drying of fiber: by step (6), treated that fiber obtains Lyocell fibers a after drying and processing.
Embodiment 2
A kind of preparation method of fire-retardant Lyocell fibers of the present embodiment, the preparation method comprise the following steps:
(1) preparation of spinning solution: the aqueous solution by mass fraction for 52.6% NMMO is evaporated under reduced pressure to 88.7%
Tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp (Shandong YINYING Chemical Fiber Co., Ltd's production) are dissolved in NMMO by NMMO aqueous solution
Aqueous solution, wherein the mass ratio of tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp be 1 ︰ 30, the quality (g) of Cotton Pulp with
The bath raio of NMMO aqueous solution volume (mL) is 1 ︰ 20, is dissolved 4 hours in 125 DEG C of vacuum stirrings in a kettle, and quality point is made
The uniform spinning solution that number is 17.6%；
(2) spinning of Lyocell fibers: being added screw extruder for step (1) treated spinning solution, at 100 DEG C into
The dissolution of one step, is then filtered, into spinning system, wherein gas length 8cm, spinning speed 48m/min, spinneret hole
Diameter is 65 μm, 500 μm of hole long capillary tube；The perpendicular stretching in air of the silk thread of ejection, into coagulating tank, solidification forming,
The aqueous solution for the NMMO that bath concentration is 17.3% is solidified, coagulation bath temperature is 6 DEG C；Lyocell fibers spinning equipment flow chart is as schemed
Shown in 1；
(3) alcohol of fiber is washed: step (2) treated fiber being immersed the ethanol solution that concentration is 84%, immerses the time
It is 3.5 hours, solution temperature is room temperature, 1 ︰ 18 of bath raio；
(4) bleaching of fiber: by step (3) treated fiber immerse bleaching agent solution that concentration is 0.2g/L (title:
Strong chlorine oil, the production of clean water treatment Science and Technology Ltd., Shandong PCI-SLR Technology), immersing the time is 4 hours, and solution temperature is 55 DEG C, bath raio
1 ︰ 19；
(5) washing of fiber: step (4) treated fiber being immersed in 90 DEG C of hot water, and the time is 2.5 hours, bath
Than 1 ︰ 23；
(6) fiber oils: by the oil bath solution of step (5) treated fiber immerses 0.8g/L (model: HY-101,
The production of Hangzhou Hua Ya Chemical Co., Ltd.), oil bath temperature is 88 DEG C, and the time is 2.5 hours, 1 ︰ 23 of bath raio；
(7) drying of fiber: by step (6), treated that fiber obtains Lyocell fibers b after drying and processing.
Embodiment 3
A kind of preparation method of fire-retardant Lyocell fibers of the present embodiment, the preparation method comprise the following steps:
(1) preparation of spinning solution: the aqueous solution by mass fraction for 54.9% NMMO is evaporated under reduced pressure to 87.6%
Tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp (Shandong YINYING Chemical Fiber Co., Ltd's production) are dissolved in NMMO by NMMO aqueous solution
Aqueous solution, wherein the mass ratio of tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp be 1 ︰ 26, the quality (g) of Cotton Pulp with
The bath raio of NMMO aqueous solution volume (mL) is 1 ︰ 20, is dissolved 3 hours in 105 DEG C of vacuum stirrings in a kettle, and quality point is made
The uniform spinning solution that number is 16.6%；
(2) spinning of Lyocell fibers: being added screw extruder for step (1) treated spinning solution, at 100 DEG C into
The dissolution of one step, is then filtered, into spinning system, wherein gas length 9cm, spinning speed 50m/min, spinneret hole
Diameter is 115 μm, 800 μm of hole long capillary tube；The perpendicular stretching in air of the silk thread of ejection, into coagulating tank, solidification forming,
The aqueous solution for the NMMO that bath concentration is 17.9% is solidified, coagulation bath temperature is 8 DEG C；Lyocell fibers spinning equipment flow chart is as schemed
Shown in 1；
(3) alcohol of fiber is washed: step (2) treated fiber being immersed the ethanol solution that concentration is 83.7%, when immersion
Between be 3 hours, solution temperature is room temperature, 1 ︰ 20 of bath raio；
(4) bleaching of fiber: by step (3) treated fiber immerse bleaching agent solution that concentration is 0.3g/L (title:
Strong chlorine oil, the production of clean water treatment Science and Technology Ltd., Shandong PCI-SLR Technology), immersing the time is 4 hours, and solution temperature is 52 DEG C, bath raio
1 ︰ 19；
(5) washing of fiber: step (4) treated fiber being immersed in 89 DEG C of hot water, and the time is 3 hours, bath raio
1 ︰ 25；
(6) fiber oils: by the oil bath solution of step (5) treated fiber immerses 0.8g/L (model: HY-101,
The production of Hangzhou Hua Ya Chemical Co., Ltd.), oil bath temperature is 87 DEG C, and the time is 3 hours, 1 ︰ 24 of bath raio；
(7) drying of fiber: by step (6), treated that fiber obtains Lyocell fibers c after drying and processing.
Embodiment 4
A kind of preparation method of fire-retardant Lyocell fibers of the present embodiment, the preparation method comprise the following steps:
(1) preparation of spinning solution: the aqueous solution by mass fraction for 52.8% NMMO is evaporated under reduced pressure to 88.9%
Tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp (Shandong YINYING Chemical Fiber Co., Ltd's production) are dissolved in NMMO by NMMO aqueous solution
Aqueous solution, wherein the mass ratio of tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp be 1 ︰ 27, the quality (g) of Cotton Pulp with
The bath raio of NMMO aqueous solution volume (mL) is 1 ︰ 17, is dissolved 39 hours in 109 DEG C of vacuum stirrings in a kettle, and quality point is made
The uniform spinning solution that number is 17%；
(2) spinning of Lyocell fibers: being added screw extruder for step (1) treated spinning solution, at 110 DEG C into
The dissolution of one step, is then filtered, into spinning system, wherein gas length 8cm, spinning speed 48m/min, spinneret hole
Diameter is 65 μm, 600 μm of hole long capillary tube；The perpendicular stretching in air of the silk thread of ejection, into coagulating tank, solidification forming,
The aqueous solution for the NMMO that bath concentration is 17% is solidified, coagulation bath temperature is 3 DEG C；Lyocell fibers spinning equipment flow chart such as Fig. 1
It is shown；
(3) alcohol of fiber is washed: step (2) treated fiber being immersed the ethanol solution that concentration is 85%, immerses the time
It is 3 hours, solution temperature is room temperature, 1 ︰ 19 of bath raio；
(4) bleaching of fiber: by step (3) treated fiber immerse bleaching agent solution that concentration is 0.2g/L (title:
Strong chlorine oil, the production of clean water treatment Science and Technology Ltd., Shandong PCI-SLR Technology), immersing the time is 3 hours, and solution temperature is 55 DEG C, bath raio
1 ︰ 18；
(5) washing of fiber: step (4) treated fiber being immersed in 92 DEG C of hot water, and the time is 2 hours, bath raio
1 ︰ 24；
(6) fiber oils: by the oil bath solution of step (5) treated fiber immerses 0.6g/L (model: HY-101,
The production of Hangzhou Hua Ya Chemical Co., Ltd.), oil bath temperature is 89 DEG C, and the time is 3 hours, 1 ︰ 24 of bath raio；
(7) drying of fiber: by step (6), treated that fiber obtains Lyocell fibers d after drying and processing.
Embodiment 5
A kind of preparation method of fire-retardant Lyocell fibers of the present embodiment, the preparation method comprise the following steps:
(1) preparation of spinning solution: the aqueous solution by mass fraction for 54.8% NMMO is evaporated under reduced pressure to 89% NMMO
It is water-soluble with Cotton Pulp (Shandong YINYING Chemical Fiber Co., Ltd's production) to be dissolved in NMMO by aqueous solution for tricresyl phosphate (2,3- dibromopropyl) ester
Liquid, wherein the mass ratio of tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp is 1 ︰ 29, the quality (g) and NMMO water of Cotton Pulp
The bath raio of liquor capacity (mL) is 1 ︰ 19, is dissolved 4 hours in 109 DEG C of vacuum stirrings in a kettle, and obtained mass fraction is
18% uniform spinning solution；
(2) spinning of Lyocell fibers: being added screw extruder for step (1) treated spinning solution, at 100 DEG C into
The dissolution of one step, is then filtered, into spinning system, wherein gas length 8cm, spinning speed 47m/min, spinneret hole
Diameter is 80 μm, 700 μm of hole long capillary tube；The perpendicular stretching in air of the silk thread of ejection, into coagulating tank, solidification forming,
The aqueous solution for the NMMO that bath concentration is 16.4% is solidified, coagulation bath temperature is 7 DEG C；Lyocell fibers spinning equipment flow chart is as schemed
Shown in 1；
(3) alcohol of fiber is washed: step (2) treated fiber being immersed the ethanol solution that concentration is 86%, immerses the time
It is 4 hours, solution temperature is room temperature, 1 ︰ 18 of bath raio；
(4) bleaching of fiber: by step (3) treated fiber immerse bleaching agent solution that concentration is 0.2g/L (title:
Strong chlorine oil, the production of clean water treatment Science and Technology Ltd., Shandong PCI-SLR Technology), immersing the time is 3 hours, and solution temperature is 55 DEG C, bath raio
1 ︰ 20；
(5) washing of fiber: step (4) treated fiber being immersed in 90 DEG C of hot water, and the time is 2 hours, bath raio
1 ︰ 25；
(6) fiber oils: by the oil bath solution (model: HY-101, Hangzhoupro of step (5) treated fiber immerses 1g/L
The production of Zhou Huaya Chemical Co., Ltd.), oil bath temperature is 90 DEG C, and the time is 4 hours, 1 ︰ 25 of bath raio；
(7) drying of fiber: by step (6), treated that fiber obtains Lyocell fibers e after drying and processing.
Performance evaluation example:
Strength property is carried out to Lyocell fibers a, b, c, d, e that specific embodiment 1~5 above-mentioned in the present invention is prepared
Test, test method with reference to GB/T-24218.3-2010 " textile, non-woven cloth test method third portion: ultimate strength and
The measurement of elongation at break ", the strength property of sample is measured using the full-automatic single fiber universl tester of FAVIMAT-BOBOT2,
Test sample is no less than 30, takes testing mean.Test result is as shown in table 1, wherein Lyocell fibers a, b, c, d, e letter
Claim fiber a, b, c, d, e, the Lyocell fibers of buying are from Shaoxing Dan Ao Fabritex S.r.l.
The mechanical property of table 1 Lyocell fibers a, b, c, d, e and the Lyocell fibers of buying
| Project | Fiber a | Fiber b | Fiber c | Fiber d | Fiber e | The Lyocell fibers of buying |
| Dry breaking strength (cN/tex) | 44.3 | 44.8 | 44.9 | 43.7 | 43.6 | 47.3 |
| Dry elongation at break (%) | 14.6 | 14.8 | 14.7 | 14.9 | 13.8 | 12.9 |
| Wet breaking strength (cN/tex) | 31.7 | 32.8 | 32.1 | 32.9 | 32.3 | 35.2 |
| Wet elongation at break (%) | 15.4 | 16.3 | 16.8 | 15.9 | 16.7 | 14.1 |
As seen from Table 1, Lyocell fibers do breaking strength between 43~45cN/tex, slightly below the Lai Sai of buying
That fiber, the dry elongation at break of Lyocell fibers are slightly above the Lyocell fibers of buying between 13.5%~15%；Lay
Sai Er fiber wet breaking strength is between 31.5~33cN/tex, and lower than the Lyocell fibers of buying, Lyocell fibers are wet
Elongation at break is slightly above the Lyocell fibers of buying between 15%~17%.Come from the test result of mechanical property
It sees, the main mechanical properties of Lyocell fibers prepared by the present invention and the Lyocell fibers ratio of Shaoxing Dan Ao Fabritex S.r.l
It is closer to, it can be seen that, cellulose fibre prepared by the present invention is a kind of Lyocell fibers of qualification.
In order to preferably detect the anti-flammability of the Lyocell fibers prepared in the present invention, by specific implementation above-mentioned in the present invention
The flame retardant property of the Lyocell fibers of Lyocell fibers a, b, c, d, e and buying that example 1~5 is prepared is tested, test
Method uses oxygen index (OI) test method, i.e., according to GB/T 5454-1997 " textile combustion performance test oxygen index method ", reference
GB/T 20944.1-2007 color fastness to washing testing machine washing methods carries out standard wash to fiber.Test result such as 2 institute of table
Show.
The flame retardant test result of table 2 Lyocell fibers a, b, c, d, e and the Lyocell fibers of buying in different washing times
Limit oxygen index LOI is one of fire proofing important indicator, and the oxygen index (OI) of common viscose fiber is less than 20%, very
It is easy burning, material of the general limit oxygen index greater than 28% belongs to nonflammable material.As can be seen from Table 2, Lay match prepared by the present invention
You have reached 33% or more by the initial threshold oxygen index (OI) of fiber, belong to nonflammable material range；After 20 washings, limit oxygen
Index is not decreased obviously, and has still reached 32% or more；And the limit oxygen index for the Lyocell fibers purchased is lower, only
13.4%.Flame retardant property experiment test shows: Lyocell fibers prepared by the present invention have good flame retardant effect, are a kind of conjunctions
The fire resistance fibre of lattice.
Claims (10)
1. a kind of preparation method of fire-retardant Lyocell fibers, which is characterized in that the method comprises the following steps:
(1) preparation of spinning solution: the aqueous solution by mass fraction for 50~55% NMMO is evaporated under reduced pressure to suitable concentration
Tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp are dissolved in NMMO aqueous solution by NMMO aqueous solution, the quality (g) of Cotton Pulp with
The bath raio of NMMO aqueous solution volume (mL) is 1 ︰ 15~20, small in 105~125 DEG C of vacuum stirring dissolutions 3~4 in a kettle
When, the uniform spinning solution of appropriate mass score is made；
(2) spinning of Lyocell fibers: being added screw extruder for step (1) treated spinning solution, at 90~120 DEG C into
The dissolution of one step, is then filtered, into spinning system, wherein gas length, spinning speed, the hole diameter of spinneret, hole long capillary tube are set
It is set to desired value；The perpendicular stretching in air of the silk thread of ejection, into coagulating tank, solidification forming, coagulating bath NMMO is water-soluble
Liquid is adjusted to suitable temperature and concentration；
(3) alcohol of fiber is washed: step (2) treated fiber being immersed to the ethanol solution of suitable concentration, immersing the time is 3~4
Hour, solution temperature is room temperature, 1 ︰ 15~20 of bath raio；
(4) bleaching of fiber: immersing the bleaching agent solution that concentration is suitable concentration for step (3) treated fiber, when immersion
Between be 2~4 hours, solution temperature be 50~55 DEG C, 1 ︰ 15~20 of bath raio；
(5) washing of fiber: step (4) treated fiber being immersed in 85~95 DEG C of hot water, and the time is 2~3 hours, bath
Than 1 ︰ 20~25；
(6) fiber oils: by step (5) treated fiber immerses certain density oil bath solution, oil bath temperature is 85~
90 DEG C, the time is 2~4 hours, 1 ︰ 20~25 of bath raio；
(7) drying of fiber: by step (6), treated, and fiber obtains Lyocell fibers after drying and processing.
2. a kind of preparation method of fire-retardant Lyocell fibers according to claim 1, it is characterised in that: the step
(1) mass ratio of tricresyl phosphate (2,3- dibromopropyl) ester and Cotton Pulp is 1 ︰ 25~30 in.
3. a kind of preparation method of fire-retardant Lyocell fibers according to claim 1, it is characterised in that: the step
(1) concentration in after the vacuum distillation of NMMO aqueous solution is 85~90%.
4. a kind of preparation method of fire-retardant Lyocell fibers according to claim 1, it is characterised in that: the step
(1) mass fraction of spinning solution is 15~18% in.
5. a kind of preparation method of fire-retardant Lyocell fibers according to claim 1, it is characterised in that: the step
(2) gas length is 7~9cm in, and spinning speed is 45~50m/min, and the hole diameter of spinneret is 40~115 μm, hole long capillary tube
400~800 μm.
6. a kind of preparation method of fire-retardant Lyocell fibers according to claim 1, it is characterised in that: the step
(2) coagulation bath temperature is 0~8 DEG C in.
7. a kind of preparation method of fire-retardant Lyocell fibers according to claim 1, it is characterised in that: the step
(2) concentration of coagulating bath NMMO aqueous solution is 15~18% in.
8. a kind of preparation method of fire-retardant Lyocell fibers according to claim 1, it is characterised in that: the step
(3) concentration of ethanol solution is 82~88% in.
9. a kind of preparation method of fire-retardant Lyocell fibers according to claim 1, it is characterised in that: the step
(4) concentration of bleaching agent solution is 0.1~0.3g/L in.
10. a kind of preparation method of fire-retardant Lyocell fibers according to claim 1, it is characterised in that: the step
(6) concentration of oil bath solution is 0.5~1g/L in.
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| CN110184745A (en) * | 2019-05-24 | 2019-08-30 | 武汉纺织大学 | A kind of method that dry spinning prepares uvioresistant Lyocell fibers non-woven fabrics at network method |
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| CN112538663A (en) * | 2020-12-04 | 2021-03-23 | 上海即索实业有限公司 | Lyocell fiber, Lyocell fiber mask cloth and manufacturing method thereof |
| CN113322530A (en) * | 2021-05-06 | 2021-08-31 | 湖北金环绿色纤维有限公司 | Preparation method of flame-retardant cellulose fiber |
| CN113957557A (en) * | 2021-11-08 | 2022-01-21 | 当阳市鸿阳新材料科技有限公司 | Efficient flame-retardant lyocell fiber and preparation method thereof |
| CN115537956A (en) * | 2022-09-28 | 2022-12-30 | 百事基材料（青岛）股份有限公司 | Lyocell macrobiological fiber containing bioactive components and preparation method thereof |
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| CN113957557A (en) * | 2021-11-08 | 2022-01-21 | 当阳市鸿阳新材料科技有限公司 | Efficient flame-retardant lyocell fiber and preparation method thereof |
| CN113957557B (en) * | 2021-11-08 | 2023-10-03 | 当阳市鸿阳新材料科技有限公司 | Efficient flame-retardant lyocell fiber and preparation method thereof |
| CN115537956A (en) * | 2022-09-28 | 2022-12-30 | 百事基材料（青岛）股份有限公司 | Lyocell macrobiological fiber containing bioactive components and preparation method thereof |
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