Produce the process of fire retardant antiflux fiber
Technical field
The present invention relates to a kind of process of producing fire retardant antiflux fiber, relate in particular to a kind of process of producing fire retardant antiflux fiber by steps such as dipping, squeezing, pulverizing, experienced, yellow, filtration, maturation, spinning, concise, oven dry.
Background technology
In vehicle, public building, family and office, fire safety problem more causes people's attention, and in order to reduce the harm of fabric fire, various countries have formulated the flame-retardant standard of various textiless and used rules.Limit non-flame-retardant textile with fabric types and field of employment, therefore, fire retardant antiflux fiber is developed rapidly.
Fiber fire-retardant mainly contains two kinds of manufacture methods.A kind of is additive process (blending method), is that fire retardant is made an addition to before spinning in the spinning solution, makes the fiber with anti-flammability.Another kind is a coating, generally is to make back or (when fiber is in gel state) in process of production at fiber, antimonous oxide is coated on the surface of fiber with the latex state with halogen-containing fire retardant.Typical fire retardant has the adhesive that polyvinyl chloride latex, polyvinyl bromide latex, chlorinated paraffin wax or bromination aromatic hydrocarbons and antimony oxide be combined into etc.
Research fire retardant antiflux fiber more, suitability for industrialized production mainly is to adopt the fire-retardant method of adding at present.The additive flame retardant of main type is as shown in table 1.
Table 1
Ignition-proof element |
Compound |
Remarks |
Phosphorus |
Alkyl and aryl phosphate ester, phosphonate ester, polyphosphonates, ExoLit 5060 |
Can mix with halide and produce cooperative effect |
Phosphorus, nitrogen |
The condensation product of phosphonitrile, phosphinylidyne or thiocarbonyl group phosphamide, spirocyclization three phosphonitriles, THPC-acid amides |
The efficient height uses nontoxic in a large number |
Phosphorus, halogen |
Halogenated alkyl or aryl phosphine acid esters or polyphosphonates, halogenation phosphite ester or phosphonitrile |
Consumption can be maximum, most of poisonous |
Silicon |
Silicate, polysilicate |
Totally nontoxic, environmental friendliness |
In recent years, several fire resistance fibres have preferably appearred on the overseas market.As the permanent fire resistance fibre (PFR Rayon) of the U.S., the permanent fire resistance fibre of company of Avis section, the HFG fiber (additive is a chlorinated phosphate) of Japan Diawabo company, clock spins the BeLL FLame fiber of company, the Lenzing fire resistance fibre of Austria Lenzing company, SandofLam 5060 (ExoLit 5060) fire retardant of Switzerland former Sandoz company (existing CLariant) and fiber etc.
A domestic climax that the development of fire resistance fibre before and after nineteen ninety, once occurred, there are many enterprises, scientific research institutions and colleges and universities to participate in, what adopt all is SandofLame5060 based flame retardants, but the quality of the fire retardant of domestic production does not reach spinning requirement because the fire retardant import price is too high, does not finally carry out suitability for industrialized production.
At present, the general two big shortcomings that exist of fire resistance fibre on the market: molten drop drippage or generation smog.Molten drop drippage junk makes the people scald easily, even the material of the low ignition point that ignites; Produce smog and be generally toxic gas, the people is produced suffocate.The flame-retardant modified research focus of present regenerated celulose fibre is to use phosphoric acid ester fire retardant and silicic acid based flame retardant, this meet fire retardant no chlorination, low toxicity, press down requirement such as cigarette, but the addition of fire retardant is bigger, generally more than 30%, the not high fibre strength of script is further reduced, have influence on the strainability of mixed viscose simultaneously.Shortcomings such as the fire resistance fibre that the silicic acid based flame retardant is produced exists alkali resistance poor, can not carry out desulfurization during the fiber post processing and handle, and the fire resistance fibre color and luster jaundice of production, feel are sent out puckery, and Practical Performance is relatively poor.
Summary of the invention
Technical problem to be solved by this invention is: a kind of process of producing fire retardant antiflux fiber is provided, the fire retardant antiflux fiber that uses this method to produce, not only anti-flame fusion-resisting is effective, the fibre strength height, and can make viscose glue keep good strainability in process of production, reduced because of viscose glue stops up the production pause that filter screen causes, improved production efficiency.
Technical scheme of the present invention is: the process of producing fire retardant antiflux fiber, with the cellulose pulp is raw material, comprise dipping, squeezing, pulverizing, experienced, yellow, filtration, maturation, spinning, concise, baking step, described concise step comprises cleans and the dehydration step that oils
In described yellow step, silicon-series five-retardant is mixed with solution, join in the alkali cellulose in the yellow, through stirring, make it fully dissolve, mix, make the viscose glue of producing fire resistance fibre;
Behind described cleaning step and dehydration oil before the step, a crosslinking Treatment step is arranged.
Described silicon-series five-retardant is sodium metasilicate or potassium silicate or its mixture, and the content of silica is that a-is cellulosic 20~60% in the described silicon-series five-retardant, is preferably 30~40%.
In described crosslinking Treatment step, the crosslinking agent of employing is a meta-aluminate, and described meta-aluminate is configured to solution, and its concentration is 2~10g/L, and described solution is heated to 70~95 ℃, and fiber is carried out crosslinking Treatment, and crosslinking time is 3~10 minutes.
After having adopted technique scheme,,, only carry out carbonization during burning, can not form fusion so its main component of making fiber is a cellulose because the present invention is raw material with the cellulose pulp.Owing in yellow, add silicon-series five-retardant, evenly mix with cellulosic molecule with molecular state this fire retardant dissolving back, has guaranteed the strainability of viscose glue behind the adding fire retardant, in filtration step, be not easy to cause the obstruction of filter screen, guaranteed carrying out smoothly of production.Simultaneously, in the spinning step, viscose glue is when the acid bath moulding, cellulose becomes macromolecular chain shape structure, micella has served as " nucleus " effect in the polymerization process of silicic acid, promoted oversaturated silicic acid molecule from solution, to separate out, all the other silicic acid generate poly-orthosilicic acid, be present in the cellulosic molecule with the web-like silicon colloidal state, fiber and fire retardant are with the molecular link strong bonded, guaranteed the stability and the follow-up anti-arrangement of fire retardant, made physical index such as fiber strength and elongation significantly better than other fire resistance fibre of producing by the fire retardant additive process.
By crosslinking Treatment, carry out chemical reaction between the linear macromolecule chain of regenerated cellulose, become net high-polymer, guaranteed the fiber alkali resistance, improved color and luster, the feel of fiber simultaneously, the intensity of regenerated fiber is to a certain degree improved.
The specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1:1.67dtex*38mm fire retardant antiflux fiber
With cellulose pulp is raw material, by known dipping, squeezing, pulverizing, experienced step, makes the 36Kg alkali cellulose, and methylcellulose is that the content of chemical cellulose is 30% in the alkali cellulose.
With 20KgSiO2 content 21% nine water sodium metasilicate (Na
2SiO
39H
2O) join in the 60L yellow dissolving water and make solution, this solution is joined in the alkali cellulose in the 36Kg yellow, make it fully dissolve, mix through stirring, making total solid content is 11.5% (quality), the viscose glue of sodium hydrate content 7.24%, after filtration, maturation makes spinning glue, at sulfuric acid content is 110g/l, sodium sulphate 330g/l, zinc sulfate 10g/l, 48 ℃ of temperature solidify the acid bath spinning, produce the 1.67dtex*38mm staple fibre through suitable drawing-off.Fiber after pickling, washing neutrality, 78 ℃ of temperature, in the crosslinked bath of concentration 3g/L meta-aluminate crosslinked 7 minutes.Make the 1.67dtex*38mm fire resistance fibre through dewatering, oil, drying.
Fiber index: do fracture strength: 2.13cN/dtex; Wet breaking strength: 1.12cN/dtex; Dried elongation at break: 20.4%; Line density deviation ratio :-1.2%; Whiteness: 79%; Oil content: 0.18%; Regain: 12.1%; Limited oxygen index (LOI) 27.5.
Embodiment 2:3.33dtex*60mm fire retardant antiflux fiber
With cellulose pulp is raw material, through known dipping, squeezing, pulverizing, experienced step, makes the 36Kg alkali cellulose, and methylcellulose is that the content of chemical cellulose is 30% in the alkali cellulose.
With 10KgSiO
2Content is 49% potassium silicate (K
2SiO
3) join in the 30L yellow dissolving water and make solution, this solution is joined in the alkali cellulose in the 36Kg yellow, make it fully dissolve, mix through stirring, making total solid content is 9.35% (quality), the viscose glue of sodium hydrate content 6.26%, after filtration, maturation makes spinning glue, at sulfuric acid content is 85g/l, sodium sulphate 320g/l, zinc sulfate 15g/l, 40 ℃ of temperature solidify the acid bath spinning, produce the 3.33dtex*60mm staple fibre through suitable drawing-off.Fiber after washing neutrality, 82 ℃ of temperature, in the crosslinked bath of the potassium metaaluminate of concentration 7g/L crosslinked 6 minutes.Make the 3.0D fire resistance fibre through dewatering, oil, drying.
Fiber index: do fracture strength: 2.03cN/dtex; Wet breaking strength: 1.01cN/dtex; Dried elongation at break: 21.0%; Line density deviation ratio :-2.8%; Whiteness: 78%; Oil content: 0.19%; Regain: 11.4%; Limited oxygen index (LOI) 28.
Embodiment 3:2.78dtex*51mm fire retardant antiflux fiber
With cellulose pulp is raw material, through known dipping, squeezing, pulverizing, experienced step, makes the 36Kg alkali cellulose, and methylcellulose is that the content of chemical cellulose is 30% in the alkali cellulose.
With 30KgSiO2 content 21% nine water sodium metasilicate (Na
2SiO
39H
2O) this solution is joined in the 70L yellow dissolving water and make solution, join in the alkali cellulose in the 36Kg yellow, making total solid content is 8.20% (quality), the viscose glue of sodium hydrate content 5.24%, after filtration, maturation makes spinning glue, is 120g/l at sulfuric acid content, sodium sulphate 330g/l, aluminum sulfate 6g/l, 48 ℃ of temperature solidify the acid bath spinning, produce the 2.78dtex*51mm staple fibre through suitable drawing-off.Fiber after washing neutrality, 85 ℃ of temperature, in the crosslinked bath of concentration 5g/L sodium metaaluminate crosslinked 7 minutes.Make the 2.78dtex*51mm fire resistance fibre through dewatering, oil, drying.
Fiber index: do fracture strength: 2.11cN/dtex; Wet breaking strength: 1.08cN/dtex; Dried elongation at break: 19.4%; Line density deviation ratio :-0.8%; Whiteness: 78%; Oil content: 0.18%; Regain: 11.1%; Limited oxygen index (LOI) 29.5.