CN104178836A - Flame-retardant viscose staple fiber and preparation method thereof - Google Patents
Flame-retardant viscose staple fiber and preparation method thereof Download PDFInfo
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- CN104178836A CN104178836A CN201410409382.3A CN201410409382A CN104178836A CN 104178836 A CN104178836 A CN 104178836A CN 201410409382 A CN201410409382 A CN 201410409382A CN 104178836 A CN104178836 A CN 104178836A
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- viscose
- fire retardant
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- retardant
- cellulose
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- 229920000297 Rayon Polymers 0.000 title claims abstract description 61
- 239000003063 flame retardant Substances 0.000 title claims abstract description 57
- 239000000835 fiber Substances 0.000 title claims abstract description 40
- 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 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000009987 spinning Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 238000005516 engineering process Methods 0.000 claims abstract description 4
- 229910019142 PO4 Inorganic materials 0.000 claims abstract 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract 2
- 239000010452 phosphate Substances 0.000 claims abstract 2
- 239000003292 glue Substances 0.000 claims description 13
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 229920002678 cellulose Polymers 0.000 claims description 12
- 239000001913 cellulose Substances 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 claims description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 6
- 235000011152 sodium sulphate Nutrition 0.000 claims description 6
- 239000012991 xanthate Substances 0.000 claims description 6
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 6
- 229960001763 zinc sulfate Drugs 0.000 claims description 6
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- 239000011574 phosphorus Substances 0.000 claims description 5
- 239000003398 denaturant Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 150000003014 phosphoric acid esters Chemical class 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 9
- 238000001035 drying Methods 0.000 abstract description 2
- 238000007670 refining Methods 0.000 abstract 1
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000009970 fire resistant effect Effects 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 229920000728 polyester Polymers 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 230000006378 damage Effects 0.000 description 3
- 238000006477 desulfuration reaction Methods 0.000 description 3
- 230000023556 desulfurization Effects 0.000 description 3
- 230000035800 maturation Effects 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 208000014674 injury Diseases 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N Cyclohexylamine Natural products NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- NAGJZTKCGNOGPW-UHFFFAOYSA-N dithiophosphoric acid Chemical compound OP(O)(S)=S NAGJZTKCGNOGPW-UHFFFAOYSA-N 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- -1 ester compound Chemical class 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- WQYSXVGEZYESBR-UHFFFAOYSA-N thiophosphoryl chloride Chemical compound ClP(Cl)(Cl)=S WQYSXVGEZYESBR-UHFFFAOYSA-N 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
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- Artificial Filaments (AREA)
Abstract
The invention discloses a flame-retardant viscose staple fiber and a preparation method of the flame-retardant viscose staple fiber. The flame-retardant viscose staple fiber adopts a special production technology, and is a special phosphorus-series viscose fiber for which organic phosphate as an effective component is added before spinning; the flame-retardant viscose staple fiber is produced by adopting technological processes including spinning, refining, drying and the like.
Description
Technical field
The present invention relates to a kind of viscose technical field, relate in particular to a kind of fire retardant viscose short filament and preparation method thereof.
Background technology
Early stage Fire resistant viscose fiber is that the method arranging after adopting is produced.It is after fiber is made or in process of production, with nitrogenous organophosphorus ester compound, fiber is processed, or antimonous oxide and halogen-containing fire retardant are coated in to the surface of fiber with latex state.Flame-retardant fiber effect prepared by this method is better, but the smog that chance fire produces is large, and fiber wash durability is poor, carries out fire resistance in dyeing and finishing process easily sustain damage at fiber.
Various fire resistance fibres both domestic and external, mostly are polyester fiber now, and their advantage is that the physical and mechanical properties of fiber is obviously better than viscose.But the polyesters fire resistance fibre having while there is burning can produce melting drip phenomenon, ignite low ignition point material or scald people, cause spot fire and injury, and some meetings produce a large amount of poison gas, and people is suffocated.
That expert or people recognize such problem now, fire-retardant product majority is the state of " maintain an army for a thousand days and use military forces for the moment ", it is non-ignitable wearing in most times of fireproof clothes, therefore within most time, intensity, comfortableness are most important, if wear this fireproof clothes, to people, bring strong sense of discomfort, dressing person is reluctant to wear certainly so, and this has just lost the meaning of protection; Even without reaching exhausted uncomfortable degree, also can affect operating efficiency; Moreover, if the insufficient strength of fabric also can affect protection effect.Therefore,, for flame retardant textiles, should take into account intensity, comfortable and fire resistance, from economy and protective, consider, primary index that even should be using intensity as fire retardant protective clothing, comfortableness is placed on second, is then only the fire resistance that may use once in a while.
And can there is not melting drip phenomenon, thereby stop secondary injury in Fire resistant viscose fiber direct charing of when burning or solidify.Meanwhile, Fire resistant viscose fiber has better skin-friendly and dyeability than fire-retardant polyester fibre, and regain is in 13% left and right, and this belongs to the regain category that human body sensory is comfortable.With its intrinsic snugness of fit, just can solve the problem that fire-retardant polyester fibre dissolves drippage completely.
, when blend additive process is produced fire resistance fibre, fire retardant joined in viscose glue stoste before spinning, and this just requires not only alkaline-resisting, acidproof, excellent heat resistance of fire retardant, and water insoluble.
Meanwhile, while producing fire resistance fibre, the anti-flammability of fiber has reached standard, and the mechanical performance of fiber has also reduced really, as dry fracture strength does not reach 2.0cN/dtex, will affect like this serviceability of fiber.
Summary of the invention
The present invention fully and comprehensively considers due to the multiple change that adds fire retardant to bring, select the viscose combustion inhibitor special of our company's independent development production and special cellulose viscose manufacturing technique, guarantee to meet under the prerequisite of fire resistance, between many index, try to achieve best overall balance.
First technical problem to be solved by this invention is: use the phosphorus flame retardant of Halogen, this fire retardant is exclusively used in viscose, the patented technology of Qie Weiwo company.Its structural formula is:
Make by the following method:
1, get solvent cyclohexane in stirred vessel, add neopentyl glycol and fully stir, then adding phosphorus thiochloride, keep 40~55 ℃ of temperature fully to dissolve;
2, the mixed liquor that drips solvent triethylamine or cyclohexane and triethylamine, is warming up to 50~65 ℃ of maintenances l.5~2.5 hours;
3, add solvent triethylamine and water, be warming up to 60~75 ℃, keep 8~12 hours;
4, after filtration, grind, obtain the new penta diester fire retardant suspension of a kind of phosphordithiic acid and be used viscose glue combustion inhibitor special.
Use this fire retardant institute production Fire resistant viscose fiber to have permanent fire retardant, limited oxygen index (LOI value) reaches more than 28, meets simultaneously country and the requirement of relevant environmental protection standard in the world;
Second technical problem to be solved by this invention is: by special spinning technique and add the viscose denaturant that relative fire retardant effective content is 10%--20% in fire retardant, guarantee to produce the fire retardant viscose short filament that physical index reaches common viscose staple fibre country Grade A standard.
For solving first technical problem, technical scheme of the present invention is:
A fire retardant viscose short filament, is characterized in that: described fire-retardant staple fibre is comprised of by following weight ratio cellulose, phosphoric acid ester phosphorus flame retardant, moisture, finish:
Cellulose: 63-75wt%
Organophosphorus ester: 15-20wt%
Moisture: 11-13%
Finish: 0.1-0.3%
In order to solve second technical problem, technical scheme of the present invention is:
A kind of preparation method of fire resistance fibre:
Important technological parameters is as follows:
A) the cellulose xanthate index of preparing is: first kind fiber content 6.0-7.0%, and containing alkali 6.0-7.0%, viscosity 45-75 second, degree of ripeness 15.0~25.0ml (10%NH
4cL meter).
B) before spinning, in cellulose xanthate, adding relative alpha cellulose amount is 10~35% fire retardants, makes anti-flaming viscose.
C) in fire retardant, add the viscose denaturant that relative fire retardant effective content is 10%--20%, to improve every physical index of fire retardant viscose short filament.
D) anti-flaming viscose of preparation is reacted through acid bath, index is: sulfuric acid 90-110g/l, zinc sulfate 50-65g/l, sodium sulphate 160-220g/l, 40~50 ℃ of temperature.
Main production flow process as shown in Figure 1.
Main production stage is:
1, adopt cellulose pulp to make cellulose xanthate after dipping, squeezing, pulverizing, experienced, yellow, dissolving, filtration, deaeration;
2, before spinning, in cellulose xanthate, by spinning front injection, add the phosphorus flame retardant of the viscose glue denaturant that contains certain proportioning, through static mixer, dynamic mixer, fully mix, make anti-flaming viscose.
3, anti-flaming viscose enters spinning machine through pump, in spinning machine, completes reaction and completes spinning and drawing-off through draft apparatus successively through spinning head, acid bath.
4, the fiber of reaction after moulding, through cutting machine, is cut into after the fiber that requires length, on scouring machine through washing, alkali cleaning, on after wet goods process, drying machine is dried, baling press packing makes finished product fire retardant viscose short filament.
Accompanying drawing explanation
Fig. 1 is the production technological process of fire retardant viscose short filament provided by the invention.
The specific embodiment
With concrete example, better set forth the present invention below.Should be appreciated that, these examples only limit to the present invention is described and are not used in and limit the scope of the invention.In addition should be appreciated that, after having read content of the present invention, those skilled in the art can carry out various changes or modification to the present invention, and these equivalent form of values fall within the application's appending claims institute limited range equally.
Embodiment mono-
After filtration, maturation, deaeration make spin front viscose glue, by spinning front injection, to add effective content be that 12% fire retardant joins and spins in front viscose glue, makes anti-flaming viscose, anti-flaming viscose content of alphacellulose is 6.5%, sodium hydrate content is 6.2%, viscosity 48s, degree of ripeness 15ml (10%NH
4cL meter) spinning glue, through acid bath: sulfuric acid content 95g/L, sodium sulphate 220g/l, zinc sulfate 55g/l, temperature 45 C.In acid bath forming process, through drawing-off, produce 1.5D fire retardant viscose short filament, by fiber washing, desulfurization, oil, dry, packing makes the fire-retardant staple fibre of 1.5D.
The fire retardant viscose short filament index making: dry fracture strength 2.24cN/dtex, wet breaking strength 1.15cN/dtex, dry elongation at break 18.4%, line density deviation ratio-1.40%, whiteness 76%, oil content 0.24%, regain 12.l%, limited oxygen index (LOI value) 28.2.
Embodiment bis-
After filtration, maturation, deaeration make spin front viscose glue, by spinning front injection, to add effective content be that 14.0% fire retardant joins and spins in front viscose glue, makes anti-flaming viscose, anti-flaming viscose content of alphacellulose is 7.0%, sodium hydrate content is 7.0%, viscosity 58s, degree of ripeness 24ml (10%NH
4cL meter) spinning glue, through an acid bath: sulfuric acid content 90g/l, sodium sulphate 180g/l, zinc sulfate 65g/l, temperature 50 C.Two acid baths: sulfuric acid content 50g/l, sodium sulphate 65g/l, zinc sulfate 25g/l, 98 ℃ of temperature.In two bath forming processes, through drawing-off, produce 2.0D fire retardant viscose short filament, by fiber washing, desulfurization, oil, dry, packing makes the fire-retardant staple fibre of 2.0D.
The fire retardant viscose short filament index making: dry fracture strength 2.16cN/dtex, wet breaking strength 1.12cN/dtex, dry elongation at break 19.2%, line density deviation ratio-1.50%, whiteness 75%, oil content 0.32%, regain 12.7%, limited oxygen index (LOI value) 28.1.
Embodiment tri-
After filtration, maturation, deaeration make spin front viscose glue, by spinning front injection, to add effective content be that 20% fire retardant joins and spins in front viscose glue, makes anti-flaming viscose, anti-flaming viscose content of alphacellulose is 6.5%, sodium hydrate content is 6.2%, viscosity 45s, degree of ripeness 15ml (10%NH
4cL meter) spinning glue, through acid bath: sulfuric acid content 100g/l, sodium sulphate 220g/l, zinc sulfate 16g/l, temperature 45 C.In acid bath forming process, through drawing-off, produce 1.5D fire retardant viscose short filament, by fiber washing, desulfurization, oil, dry, packing makes the fire-retardant staple fibre of 1.5D.
The fire retardant viscose short filament index making: dry fracture strength 2.16cN/dtex, wet breaking strength 1.05cN/dtex, dry elongation at break 17.4%, line density deviation ratio-1.00%, whiteness 76%, oil content 0.24%, regain 12.l%, limited oxygen index (LOI value) 28.1.
Claims (3)
1. a fire retardant viscose short filament, is characterized in that: described fire-retardant staple fibre is comprised of by following weight ratio cellulose, phosphoric acid ester phosphorus flame retardant, moisture, finish:
Cellulose: 63-75 wt%
Organophosphorus ester: 15-20 wt%
Moisture: 11-13%
Finish: 0.1-0.3%.
2. the preparation method of fire retardant viscose short filament as claimed in claim 1, it is characterized in that: phosphoric acid ester phosphorus flame retardant is joined in viscose solution by injecting systems before spinning before spinning and be mixed into uniform viscose solution, wherein the content of phosphate accounts for 10-35% of alpha cellulose in viscose glue.
3. the preparation method of the fire retardant viscose short filament as described in right 1, is characterized in that: adopt a kind of new viscose production technology to produce, major technique is as follows:
A) the cellulose xanthate index of preparing is: first kind fiber content 6.0-7.0%, and containing alkali 6.0-7.0%, viscosity 45-75 second, degree of ripeness 15.0~25.0ml(10%NH
4cL meter);
B) before spinning, in cellulose xanthate, adding relative alpha cellulose amount is 10~35% fire retardants, makes anti-flaming viscose;
C) in fire retardant, add the viscose denaturant that is 10%--20% with respect to fire retardant effective content, to improve every physical index of fire retardant viscose short filament;
D) anti-flaming viscose of preparation is reacted through acid bath, index is: sulfuric acid 90-110 g/l, zinc sulfate 50-65 g/l, sodium sulphate 160-220 g/l, 40~50 ℃ of temperature.
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Cited By (5)
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---|---|---|---|---|
CN104872872A (en) * | 2015-06-08 | 2015-09-02 | 江苏同康特种活性炭纤维面料有限公司 | Method for production of viscose-based carbonized fireproof fabric with excellent flame retardation performance |
CN104988642A (en) * | 2015-06-08 | 2015-10-21 | 江苏同康特种活性炭纤维面料有限公司 | Viscose glue based carbonization fireproof fabric with excellent flame retardant performance |
CN105220255A (en) * | 2015-10-20 | 2016-01-06 | 恒天海龙股份有限公司 | Fire-retardant regenerated celulose fibre of Bepaint inorganic and preparation method thereof |
CN106521669A (en) * | 2016-08-31 | 2017-03-22 | 浙江益南纤维科技有限公司 | Novel composite viscose fiber special for fireproof flame-retardant fabric |
CN110004554A (en) * | 2019-04-09 | 2019-07-12 | 杭州澳品纺织有限公司 | A kind of highly-flexible inflaming retarding fabric |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104872872A (en) * | 2015-06-08 | 2015-09-02 | 江苏同康特种活性炭纤维面料有限公司 | Method for production of viscose-based carbonized fireproof fabric with excellent flame retardation performance |
CN104988642A (en) * | 2015-06-08 | 2015-10-21 | 江苏同康特种活性炭纤维面料有限公司 | Viscose glue based carbonization fireproof fabric with excellent flame retardant performance |
CN105220255A (en) * | 2015-10-20 | 2016-01-06 | 恒天海龙股份有限公司 | Fire-retardant regenerated celulose fibre of Bepaint inorganic and preparation method thereof |
CN106521669A (en) * | 2016-08-31 | 2017-03-22 | 浙江益南纤维科技有限公司 | Novel composite viscose fiber special for fireproof flame-retardant fabric |
CN110004554A (en) * | 2019-04-09 | 2019-07-12 | 杭州澳品纺织有限公司 | A kind of highly-flexible inflaming retarding fabric |
CN110004554B (en) * | 2019-04-09 | 2020-07-28 | 杭州澳品纺织有限公司 | High-softness flame-retardant fabric |
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