CN1037458C - Flame-retarding fibre of cellulose polysilicate and producing method thereof - Google Patents
Flame-retarding fibre of cellulose polysilicate and producing method thereof Download PDFInfo
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- CN1037458C CN1037458C CN 94110065 CN94110065A CN1037458C CN 1037458 C CN1037458 C CN 1037458C CN 94110065 CN94110065 CN 94110065 CN 94110065 A CN94110065 A CN 94110065A CN 1037458 C CN1037458 C CN 1037458C
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Abstract
The present invention relates to a cellulose and polysilicate compounded flame retardant fiber which is a cellulose fiber formed by the method that cellulose is combined with polysilicate, and is produced by a viscose fiber production process method by the technology of the regeneration and the sealed treatment of composite fibers. The cellulose fiber has the advantages of easy production, no pollution, fire retardance, alkali resistance, soaping resistance and no generation of toxic gas during combustion, and when the cellulose fiber is used for fabric weaving, the technology of weaving, dyeing and finishing is not influenced and varied.
Description
What the present invention relates to is fiber product and production method.Particularly cellulose fire resistance fibre and production method thereof.
Cellulose fibre is with a long history in artificial fibre, of many uses, because its raw material sources are wide, excellent comfortable, good dyeability and the ecological correlation of hygroscopicity, gas permeability, clothing arranged, and occupy stable status in the production of artificial fibre with in using.Yet the general fibre cellulose fiber is being easy to fire burns, and anti-flammability is relatively poor, can not satisfy the social development application requirements, has therefore also limited its application power.
For a long time, lot of domestic and foreign researcher is devoted to the Study of flame retardancy and the product development of cellulose fibre, has obtained certain achievement, and has multiple Fire resistant viscose fiber to put goods on the market.But up to the present Fire resistant viscose fiber still has many deficiencies, and the fire retardant that the Fire resistant viscose fiber of being produced is used all belongs to organic compound, cost an arm and a leg, and Fire resistant viscose fiber product cost height, toxicity and pollution are big, and are difficult to overcome.
Fire resistant viscose fiber is produced comparatively, and the representative products of advanced country has: Pori's nosik (Polynosic) viscose that Austrian human relations green grass or young crops (Lenging) Fire resistant viscose fiber and Japanese Japan are spun, its fire retardant are organic phosphorous or halogen organic compound; Greatly Japanese and spin HFG fiber, its fire retardant is a chlorinated phosphate; The Luo Napu Lang Ke TF-8D fiber of France and the Durvil fire retardant viscose short filament and the PER viscose of the U.S., its fire retardant is an organosilane ester,
In the prior art, " chemical fibre textile industry " magazine (Technische Textilien/Technical Textiles of Germany, Vol.35, July/August 1992) T90-T92 and " textile industry/textile technology " (the lndustrie-Textilien/Technische Textilien Dezember l991) T224-T225 of 92 year the 10th phase disclose a kind of cellulose viscose that uses the inorganic compound fire retardant.Be the Kemira Co.,Ltd (Kemira oy) of Finland propose make fire retardant with waterglass-sodium metasilicate, the mixture of fibers of production of cellulose and poly-silicic acid, its called after Wei Xier (Visil).The chemical composition of Wei Xier fiber is cellulose and poly-silicic acid, See Figure:
Wei Xier fibre manufacturing technique principle is: silicate-→ poly-silicic acid.Poly-silicic acid runs into alkali such as NaOH or sodium carbonate etc., and poly-silicon bronsted lowry acids and bases bronsted lowry just generates sodium metasilicate soluble in water, and poly-silicic acid can be dissolved at an easy rate falls, and loses its fire resistance.So, the Wei Xier fiber can not only be avoided by desulfurization (alkali cleaning) technical process in the cellulose viscose manufacturing technique, does not promptly carry out sulfur removal technology and handles, there is not the caustic wash desulfuration technical process in this process chart given from document, yet provable this point.Therefore this Wei Xier fiber mixture of fibers that is a kind of cellulose and poly-silicic acid contains a large amount of elemental sulfurs on this fiber, and this makes fiber outward appearance look translate yellowing.Because this fiber alkali resistance is poor, when utilizing this fiber to be made into fabric, can bring on weaving, the dyeing and finishing technology because of difficulty, cause fabric color to shade easily, and sulfur-containing aroma arranged, do not meet hygienic requirements, and lose fire resistance.
Though the invention of Wei Xier fiber artificially improves its alkali resistance, mention " available suitable finishing agent; perhaps in spinning process with the cationic compound of polynary divalence or trivalent ", but in the coagulating bath of viscose production, just contain zinc sulfate, spun poly-silicate fiber, by sulfur removal technology the time, poly-silicic acid can all dissolve, and makes fiber have not a particle of fire resistance.This shows that so-called the cationic compound of polynary divalence or trivalent " in the spinning process with " can not play any effect yet.And use " suitable finishing agent " at most once in fiber or fabric surface treatments, be difficult to keep the persistence of fire resistance.
The purpose of this invention is to provide a performance is good, cost is low, production is easy, easy cellulose inorganic salts fire resistance fibre and production method thereof, a kind of cellulose polysilicate fiber and production method thereof particularly are provided.
Flame-retarding fibre of cellulose polysilicate of the present invention is the cellulose fibre that a kind of cellulose and polysilicate mix, and promptly is a kind of cellulose fibre that contains polysilicate, and its structural formula is as follows:
Wherein: n=200～310 m=2～30 Me represent metal
Cellulose polysilicate fiber of the present invention, adopt blended fiber regeneration and sealing treatment technology to produce, for silicate-→ poly-silicic acid-→ the inorganic salts regeneration principle of polysilicate, utilize viscose to produce the existing equipment device, adopt the cellulose viscose manufacturing technique method to produce.Its technological process is as follows:
1. pulp
2. dipping ← NaoH
3. yellow ← CS
2
4. viscose glue ← silicate
5. spinning ← coagulating bath
6. washing
7. sealing is handled
8. desulfurization
9. washing
10. oil
11. it is dry
12. finished product
Cellulose polysilicate fiber production method provided by the present invention is undertaken by the viscose production method, is characterised in that: with modulus (SiO
2: Na
2O) be the waterglass of 2.5-3.5, or potassium silicate, or sodium metasilicate, or, press the 10-50% (weight) of alpha cellulose content in the viscose glue stoste, sneak into that to give the viscose glue that mixes up earlier former, in the liquid, and be mixed, make spinning glue arbitrarily than the potassium silicate and the sodium metasilicate of mixing; It consists of alpha cellulose 7-8% (weight), NaOH 5.5-6.5% (weight), viscosity 40-70 second (falling ball method), degree of ripeness 6-9 (10% sal-ammoniac value); With the spinning of conventional spinning technique method, drawn washing, sealing processing, desulfurization, wash, oil, dry, make finished product.
By improving the quality of the poly-silicate fiber of spun cellulose, as best implementation method, employedly in the spinning technique process doubtfully bathe it admittedly and consist of: sulfuric acid 100-130 grams per liter, zinc sulfate 10-15 grams per liter, sodium sulphate 240-350 grams per liter; Bathing temperature is 45-55 ℃
The crucial part of cellulose polysilicate fiber production method of the present invention is that increasing has sealing to handle in the technological process of production.According to above-mentioned cellulose viscose manufacturing technique production spinning, what obtain earlier is the plain poly-silicate fiber of long or short fiber type, and as handling without closed stablity, wherein poly-silicic acid is extremely unstable under alkali condition, removes totally easily.Therefore, need gather silicic acid-→ the polysilicate chemical treatment, further improve its washing property of alkali resistant, promptly seal processing, will gather the silicic acid strand and be converted into alkali-resisting polysilicate.
It is to carry out after the spinning of the technological process of production, before the desulfurization that sealing is handled.The sealing processing method is: with containing metal (ammonia or ethylenediamine) complex compound 1-10 grams per liter, or contain the sealer that calcium hydroxide 1-1.8 grams per liter solution constitutes, under 1-50 ℃, fiber is carried out shower in 5-120 minute handle.It is a replacement reaction that sealing is handled, and its chemical equation is as follows:
X: bases compound n=2-30 m=2-6 Me represents metal
Said metal (ammonia or ethylenediamine) complex compound comprises silver, copper, zinc, cobalt, nickel complex.Be easy to carry out because sealer is the chemical reaction of metal (ammonia or ethylenediamine) complex compound and poly-silicic acid, temperature influence is little, so when sealer concentration was low, the shower amount just greatly, just can grow by the time; When concentration was high, the shower amount was just little, and the time just can lack.Therefore, the concentration of seal treatment technique, temperature, time parameter can have bigger span.
Through the cellulose polysilicate fiber that above-mentioned closed stablity PROCESS FOR TREATMENT obtains, be 60 ℃ in temperature, contain NaOH greater than handling 60 minutes in the 2 grams per liter solution, polysilicate does not come off, and fiber keeps anti-flammability.And the Wei Xier fiber is 40 ℃ in temperature, contains in the NaOH 2 grams per liter solution to handle 60 minutes, and poly-silicic acid is all dissolved to be fallen, and loses anti-flammability.
Cellulose polysilicate fiber of the present invention is handled and desulfurization by sealing, and its composition of the fiber that makes is cellulose and polysilicate mixture, and this fiber only contains the elemental sulfur of trace, and fiber outward appearance light evenly.Polysilicate has noninflammability, and mixes with cellulose, can fully play anti-combustion fire retardation.Polysilicate and alkali are difficult for producing chemical reaction, be difficult to generate water-soluble sodium metasilicate, so the alkali resistance of this cellulose polysilicate fiber is good, after soaping through dyeing and finishing technology process or its fabric family, this fiber still maintains the same the same fire resistance.And, when utilizing this fiber to be made into fabric, can not influence weaving, dyeing and finishing technology.
Embodiment 1
With modulus (SiO
2: Na
2O) be 2.5 waterglass or potassium silicate or sodium metasilicate or arbitrarily than the potassium silicate and the sodium metasilicate that mix, 20% (weight) of pressing alpha cellulose content in the viscose glue stoste is in the adding viscose glue stoste; Sealer is the calcium hydroxide of concentration 1.6 grams per liters, 10 ℃ of sealing treatment temperatures, 60 minutes processing times; Other is with aforementioned (normal viscose production) technology.
Embodiment 2
With modulus (SiO
2: Na
2O) be 3 waterglass or potassium silicate or sodium metasilicate or arbitrarily than the potassium silicate and the sodium metasilicate that mix, 30% (weight) of press alpha cellulose content in the viscose glue stoste, adding is glued in the handsome stoste; Sealer is that the copper of concentration 8 grams per liters is or/and zinc complex seals 30 ℃ of treatment temperatures, 30 minutes processing times; Other is with aforementioned (normal viscose production) technology.
Embodiment 3
With modulus (SiO
2: Na
2O) be 3.5 waterglass or potassium silicate or sodium metasilicate or arbitrarily than the potassium silicate and the sodium metasilicate that mix, 35% (weight) of press alpha cellulose content in the viscose glue stoste, adding is glued in the handsome stoste; Sealer is nickel or the cobalt or the silver complex of concentration 4 grams per liters, 20 ℃ of sealing treatment temperatures, 10 minutes processing times; Other is with aforementioned (normal viscose production) technology.
Fibre quality index:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Fine Xi Er | |
| Fiber number dt | ?1.67-6.8 | ?1.67-6，8 | ?1.67-6.8 | 5.0 and 8.0 |
| Dry strength CN/dt | ?1.2-1.5 | ?1.2-1.5 | ?1.2-1.5 | ?1.2-1.5 |
| Wet strength CN/dt | ?0.6-0.7 | ?0.6-0.7 | ?0.6-0.7 | |
| Stem elongation % | ?18-23 | ?18-23 | ?18-23 | ?20-30 |
| Residual sulfur content mg/100g | ?＜30 | ?＜30 | ?＜30 | |
| Oil content % | ?0.2-0.3 | ?0.2-0.3 | ?0.2-0.3 | |
| Regain % | ?11-13 | ?11-13 | ?11-13 | ?9-11 |
| SiO 2 | ?25-35 | ?25-35 | ?25-35 | ?33 |
| The LOI value | ?25-27 | ?25-27 | ?25-27 | ?23-25 |
| Cross sectional shape | Random zigzag | Lenticular shaped | ||
The used fire retardant of the present invention---silicate inorganic raw material, resource is wide, and price is low, can realize that suitability for industrialized production has the cellulose polysilicate fiber of lingering performance, the pollution-free factor of fire retardant, fiber meets hygienic requirements.This cellulose polysilicate fiber not only has anti-flammability, alkali resistance and soaps, and does not produce toxic gas when burning, and is free from environmental pollution.When utilizing this fiber to be made into fabric, do not influence and change and weave and dyeing and finishing technology.
Claims (5)
1, flame-retarding fibre of cellulose polysilicate is the cellulose fibre that a cellulose and polysilicate mix, and its structural formula is as follows:
Wherein: n=200-310 m=2-30 Me represents metal
2, cellulose polysilicate fiber according to claim 1, it is characterized in that being: Me is silver, copper, cobalt, zinc, nickel, calcium.
3, a kind of method of producing cellulose polysilicate fiber as claimed in claim 1 includes pulp-dipping-yellow-viscose glue-spinning-washing-desulfurization-wash-oil-drying process, it is characterized in that:
A, with modulus (SiO
2: Na
2O) be the waterglass of 2.5-3.5, or potassium silicate, or sodium metasilicate, or, press the 10-50% (weight) of alpha cellulose content in the viscose glue stoste arbitrarily than the potassium silicate and the sodium metasilicate that mix, and sneak into and give in the viscose glue stoste that mixes up earlier, make spinning glue;
B, after spinning, there is closed stablity to handle, poly-silicic acid → polysilicate chemical treatment is promptly arranged fiber.
4, cellulose polysilicate fiber production method according to claim 3, it is characterized in that: it is with containing metal (ammonia or ethylenediamine) complex compound 1-10 grams per liter that closed stablity is handled, or contain the sealer that calcium hydroxide 1-1.8 grams per liter solution constitutes, under 1-50 ℃, the time fiber carry out shower in 5-120 minute and handle, its chemical equation is as follows:
5, the described cellulose polysilicate of root a tree name claim 4 fiber production method is characterized in that: said metal (ammonia or ethylenediamine) complex compound is silver, copper, zinc, cobalt, nickel complex.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94110065 CN1037458C (en) | 1994-02-03 | 1994-02-03 | Flame-retarding fibre of cellulose polysilicate and producing method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94110065 CN1037458C (en) | 1994-02-03 | 1994-02-03 | Flame-retarding fibre of cellulose polysilicate and producing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1098149A CN1098149A (en) | 1995-02-01 |
| CN1037458C true CN1037458C (en) | 1998-02-18 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94110065 Expired - Fee Related CN1037458C (en) | 1994-02-03 | 1994-02-03 | Flame-retarding fibre of cellulose polysilicate and producing method thereof |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FI119327B (en) * | 2004-06-02 | 2008-10-15 | Sateri Internat Co Ltd | Process for manufacturing silk-containing fiber |
| CN100349970C (en) * | 2005-01-07 | 2007-11-21 | 青岛大学 | Preparation method of regenerated cellulose / nanometer SiO2 fire-retardant composite material |
| CN101210353A (en) * | 2006-12-28 | 2008-07-02 | 山东海龙股份有限公司 | Anti-flame fusion-resisting cellulose viscose and producing method thereof |
| WO2011080826A1 (en) * | 2009-12-28 | 2011-07-07 | ダイワボウホールディングス株式会社 | Flameproof rayon fiber, process for production thereof, and flameproof fiber structure |
| CN102345174B (en) * | 2011-08-12 | 2013-03-27 | 山东海龙股份有限公司 | Preparation method for flame-retardant spinning viscose |
| CN102383211B (en) * | 2011-08-30 | 2013-12-25 | 成都丽雅纤维股份有限公司 | Production technology of environmentally friendly composite flame-retardant viscose |
| CN110158176A (en) * | 2019-05-30 | 2019-08-23 | 叶小文 | A kind of preparation method of flame retardant viscose fiber |
| CN114808252B (en) * | 2021-01-21 | 2024-01-19 | 杭州安创纺织有限公司 | Flame-retardant fabric |
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1994
- 1994-02-03 CN CN 94110065 patent/CN1037458C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1098149A (en) | 1995-02-01 |
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