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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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)
| 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 |
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| CN1289869A (en) * | 1999-09-29 | 2001-04-04 | 吉林化纤股份有限公司 | Shaped viscose staple and its preparing process and spinneret |
| CN1904156A (en) * | 2006-07-31 | 2007-01-31 | 唐山三友集团化纤有限公司 | Fire retardant viscose short filament and its production technology |
| CN101948487A (en) * | 2010-09-09 | 2011-01-19 | 吉林市吉溧化工有限责任公司 | Method for synthesizing dithio dineopentyl phosphate fire retardant |
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| CN1289869A (en) * | 1999-09-29 | 2001-04-04 | 吉林化纤股份有限公司 | Shaped viscose staple and its preparing process and spinneret |
| CN1904156A (en) * | 2006-07-31 | 2007-01-31 | 唐山三友集团化纤有限公司 | Fire retardant viscose short filament and its production technology |
| CN101948487A (en) * | 2010-09-09 | 2011-01-19 | 吉林市吉溧化工有限责任公司 | Method for synthesizing dithio dineopentyl phosphate fire retardant |
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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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