CN105113034A - Regenerated cellulose fiber and preparing method thereof - Google Patents
Regenerated cellulose fiber and preparing method thereof Download PDFInfo
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- CN105113034A CN105113034A CN201510478724.1A CN201510478724A CN105113034A CN 105113034 A CN105113034 A CN 105113034A CN 201510478724 A CN201510478724 A CN 201510478724A CN 105113034 A CN105113034 A CN 105113034A
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Abstract
The invention discloses a preparing method of a regenerated cellulose fiber. The preparing method is characterized by comprising the following steps that a spinning solution is prepared through an alkali solution method, and the temperature is increased to 10-30 DEG C; then, nanometer cellulose is added in the spinning solution and is evenly dispersed, and the mass of the nanometer cellulose accounts for 0.01-5% of the mass of cellulose raw materials in the spinning solution, the length of the nanometer cellulose is smaller than or equal to 5 micrometers, and the draw ratio of the nanometer cellulose is larger than or equal to 50; then, wet method spinning is carried out to obtain a nascent cellulose fiber, and then the nascent cellulose fiber is prepared into the regenerated cellulose fiber. The invention further discloses the regenerated cellulose fiber. The preparing method of the regenerated cellulose fiber can improve the strength of the regenerated cellulose fiber.
Description
Technical field
The present invention relates to chemical fibre field, be specifically related to a kind of regenerated celulose fibre and preparation method thereof.
Background technology
Business-like regenerated celulose fibre mainly contains at present: viscose, Lyocell fibers, copper ammonia fibre etc.Viscose is that alkali cellulose and carbon disulfide react and generates cellulose sulfonate, prepare through dissolving, regeneration again, the operations such as production process comprises alkalization, squeezing, pulverizing, experienced, yellow, dissolving, maturation, filtration, deaeration, spinning, washing, desulfurization, pickling, oils, dry, complex technical process, and can CS be discharged in process of production
2and H
2the toxic gases such as S and the waste water containing heavy metal, cause severe contamination to air and water.Copper ammonia fibre take copper ammon solution as solvent, through dissolving, spray silk, solidify, fiber that decopper(ing), pickling, the operation such as drying obtain, air must be completely cut off in its production process, otherwise violent oxidative degradation can occur cellulose, copper ammon solution consumption is large in addition, reclaims difficulty, production cost is high, and seriously polluted, etching apparatus, therefore this technique is not further developed.Lyocell fibers is regenerated celulose fibre prepared by solvent with the hydrate of N-methyl morpholine oxide (be called for short NMMO), the whole circulatory system in production needs totally-enclosed, add operating cost, limit the lifting of spinning speed and the diversified development of product, reason wholely side reaction can occur and form accessory substance under not totally-enclosed condition, cause the permanent or provisional variable color of cellulose degradation, fiber, properties of product decline, NMMO obviously decomposes, stabilizing agent dosage increase, thermal runaway reaction etc.
Research finds, basic solution method prepares the pollution that regenerated celulose fibre can reduce environment greatly, found at present aqueous slkali system (as NaOH (lithium hydroxide)/urea/aqueous solution, NaOH (lithium hydroxide)/urea/sulphur urea/aqueous solution, NaOH (lithium hydroxide)/thiocarbamide/aqueous solution, NaOH (lithium hydroxide)/zinc oxide/aqueous solution, NaOH (lithium hydroxide)/polyethylene glycol/aqueous solution etc.) because of its raw material be easy to get, easily reclaim, the feature such as simple to operate, cost is low, receive more and more concern.This system is adopted to prepare the research of regenerated celulose fibre also a lot.But this system also also exists some shortcomings that cannot overcome at present: be first that its solvability is limited, can only the cellulosic material of solvent polymerization degree lower (about less than 600), the raw material that the degree of polymerization is higher can not dissolve completely in this system; Next is that the concentration of gained spinning solution is generally no more than 8wt%, otherwise easily gelation and losing flowability.Therefore, the low strength of the regenerated celulose fibre prepared by this system, seriously constrains the further industrialization development of this system.
For improving the intensity of regenerated celulose fibre, current research mainly carries out to raw material the degree of polymerization that preliminary treatment (as alkali treatment, acid treatment, steam blasting, ferment treatment etc.) reduces raw material, increase the concentration of spinning solution, but strengthen effect not obvious, intensity is too low to be caused basic solution method to prepare regenerated celulose fibre can not being applied widely, and the intensity therefore how improving regenerated celulose fibre is the problem that current basic solution method prepares that regenerated celulose fibre needs solution badly.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of regenerated celulose fibre, the TENSILE STRENGTH of regenerated celulose fibre prepared by basic solution method can be improved, make basic solution method prepare regenerated celulose fibre and applied.
A preparation method for regenerated celulose fibre, comprises the steps:
Basic solution method is adopted to prepare spinning solution and be warming up to 10-30 DEG C; Then add nano-cellulose wherein and be uniformly dispersed, described nano-cellulose quality is equivalent to the 0.01-5% of cellulosic material quality in described spinning solution, described nano-cellulose length≤5 μm, draw ratio >=50, then carry out wet spinning and obtain as-spun fibre cellulose fiber, more described as-spun fibre cellulose fiber is prepared into regenerated celulose fibre.
Further, it is characterized in that, nano-cellulose length≤2 μm.
Further, it is characterized in that, described nano-cellulose quality is equivalent to the 0.5-2% of cellulosic material quality in described spinning solution.
Further, the feed postition of described nano-cellulose is prepared into dispersion liquid for being first dispersed in aqueous slkali by nano-cellulose, the quality of described aqueous slkali is the 1-10% of aqueous slkali quality in described spinning solution, is then distributed in described spinning solution by described homogeneous dispersion.
Further, the aqueous slkali quality in described dispersion liquid is the 4-6% of the aqueous slkali quality in described spinning solution.
Further, the described concrete steps preparing spinning solution are:
Be obtain described spinning solution after dissolving under-20-0 DEG C of condition after the raw material of 300-600 mixes with aqueous slkali by the degree of polymerization of alpha-cellulose mass fraction >=90%, in described spinning solution, the mass fraction of regenerated cellulose is 3-8%.
Further, the concrete steps of described wet spinning are: have that the described spinning solution of nano-cellulose filters at 10-30 DEG C, vacuum defoamation by dispersed, and be placed in device for spinning, sprayed by spinneret orifice, enter into coagulating bath, described coagulating bath is made up of 5-15wt% sulfuric acid, 5-15wt% sodium sulphate and water, and described coagulation bath temperature is 20-60 DEG C, and in coagulating bath, coagulation forming obtains as-spun fibre element.
A kind of regenerated celulose fibre, containing the regenerated cellulose of 100 weight portions and the nano-cellulose of 0.01-5 weight portion in described regenerated celulose fibre, the TENSILE STRENGTH of described regenerated celulose fibre is 1.5-2.5cN/dtex, and elongation at break is 10-30%.
Compared with prior art, regenerated celulose fibre of the present invention and preparation method thereof has following beneficial effect:
1, prepare at basic solution method in the process of regenerated celulose fibre and add a small amount of nano-cellulose, the great amount of hydroxy group on its surface can form stable network structure with around multiple cellulose chain in hydrogen bond mode, be conducive to the compactness increasing regenerated celulose fibre, strengthen the TENSILE STRENGTH of regenerated celulose fibre.
2, the present invention adds nano-cellulose is not add together with cellulosic material, but add again be warming up to 10-30 DEG C after preparing spinning solution after, so not only ensure that the dissolving of cellulosic material but also prevent the dissolving of nano-cellulose, adopting the mode of dispersion liquid to add and ensure that being uniformly dispersed of nano-cellulose.
3, the nano-cellulose that the present invention adopts has larger draw ratio and higher degree of crystallinity, in spinning process, easy be parallel to fiber axis to align, thus improve the degree of orientation and the degree of crystallinity of regenerated fiber, and then improve the TENSILE STRENGTH of regenerated celulose fibre.
Below in conjunction with accompanying drawing, regenerated celulose fibre of the present invention and preparation method thereof is described further.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph adding nano-cellulose in regenerated celulose fibre of the present invention and do not add the regenerated celulose fibre prepared by nano-cellulose;
Wherein, Fig. 1 (a
1), 1 (a
2) and 1 (a
3) be respectively the scanning electron microscope (SEM) photograph adding the surface of regenerated celulose fibre prepared by nano-cellulose, the scanning electron microscope (SEM) photograph after the scanning electron microscope (SEM) photograph of cross-section morphology and section amplify; Fig. 1 (b
1), 1 (b
2) and 1 (b
3) be respectively the scanning electron microscope (SEM) photograph on the surface of not adding regenerated celulose fibre prepared by nano-cellulose, the scanning electron microscope (SEM) photograph after the scanning electron microscope (SEM) photograph of cross-section morphology and section amplify;
Add nano-cellulose in Fig. 2 regenerated celulose fibre of the present invention and do not add the load-deformation curve comparison diagram of the regenerated celulose fibre prepared by nano-cellulose.
Detailed description of the invention
For more clearly understanding technical scheme of the present invention, below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
A preparation method for regenerated celulose fibre, comprises the steps:
(1) basic solution method prepares spinning solution: to be 90% degree of polymerization by 3kg alpha-cellulose content be 300 needlebush dissolving pulp mix with 97kg NaOH/polyethylene glycol/aqueous solution (mass ratio is 9/1/90), the too high meeting of the degree of polymerization causes cellulosic solubility to reduce, thus affect the TENSILE STRENGTH of regenerated celulose fibre, at mixed liquor being placed in-20 DEG C after stirring, vigorous stirring, after 5 minutes, obtains homogeneous, transparent spinning solution;
(2) regenerated celulose fibre is prepared: spinning solution is warming up to 10 DEG C, because be insoluble to alkali lye under cellulose normal temperature, but the dispersion effect of nano-cellulose is bad at low temperatures, and the dissolving of nano-cellulose can be caused, therefore need dissolution in low temperature cellulosic material, after intensification, add nano-cellulose; With vigorous stirring, slowly joined in spinning solution by the nano-cellulose of 0.01wt% (relative to needlebush dissolving pulp), the length of described nano-cellulose is 5 μm, and draw ratio is 50; The length of nano-cellulose is crossed conference and is caused the conglomerate in spinning solution, causes the intensity of the regenerated celulose fibre prepared to reduce, and the too small enhancing effect that also can cause of draw ratio is bad; Continuing to stir 20min makes nano-cellulose be uniformly dispersed, dispersion is uneven can cause the intensity of regenerated celulose fibre to reduce, obtain the spinning solution containing nano-cellulose, at 10 DEG C, after spinning solution containing nano-cellulose being filtered also vacuum defoamation, be placed in device for spinning, spinning solution is sprayed by spinneret orifice, enter into the coagulating bath be made up of sulfuric acid/sodium sulphate/water (mass ratio is 8/12/80), coagulation bath temperature is 35 DEG C, the as-spun fibre of coagulation forming after repeatedly washing, drawing-off, drying, arrangement, collection, obtains regenerated celulose fibre again; The TENSILE STRENGTH of this regenerated celulose fibre is 1.5cN/dtex, and elongation at break is 10%.
Embodiment 2
A preparation method for regenerated celulose fibre, comprises the steps:
(1) basic solution method prepares spinning solution: to be 95% degree of polymerization by 5kg alpha-cellulose content be 350 cotton linter pulp mix with NaOH/urea/aqueous solution 95kg (mass ratio is 8/12/80); At mixed liquor being placed in-12 DEG C after stirring, the cellulose ratios added is crossed that I haven't seen you for ages and is caused cellulosic concentration in spinning solution to reduce, thus has influence on the TENSILE STRENGTH of regenerated celulose fibre, and vigorous stirring, after 3 minutes, obtains homogeneous, transparent spinning solution;
(2) prepare the dispersion liquid of nano-cellulose: by the nano-cellulose of 5wt% (relative to cotton linter pulp) at 15 DEG C ultrasonic disperse in the NaOH/urea/aqueous solution (mass ratio is 8/12/80) of the 10wt% quality of solvent (in relative to the spinning solution), the too low meeting of addition of nano-cellulose causes strengthening DeGrain, the length of described nano-cellulose is 2 μm, and draw ratio is 80; Obtain nano-cellulose dispersion liquid, the dispersion liquid of preparation containing nano-cellulose can make the dispersion effect of nano-cellulose better;
(3) regenerated celulose fibre is prepared: spinning solution is warming up to 15 DEG C, with vigorous stirring, dispersion liquid is dropwise slowly joined in spinning solution, continuation stirring 30min obtains the spinning solution containing nano-cellulose, spinning solution gained being contained nano-cellulose after filtration and after vacuum defoamation, be placed in device for spinning; Spinning solution is sprayed by spinneret orifice, and enter into the coagulating bath be made up of sulfuric acid/sodium sulphate/water (mass ratio is 10/10/80), coagulation bath temperature is 40 DEG C; The as-spun fibre of coagulation forming after repeatedly washing, drawing-off, drying, arrangement, collection, obtains regenerated celulose fibre again.The TENSILE STRENGTH of this regenerated celulose fibre is 2.2cN/dtex, and elongation at break is 26.3%.
Fig. 1 is interpolation nano-cellulose and the scanning electron microscope (SEM) photograph not adding the regenerated celulose fibre prepared by nano-cellulose; Wherein, Fig. 1 (a
1), 1 (a
2) and 1 (a
3) be respectively the scanning electron microscope (SEM) photograph adding the surface of regenerated celulose fibre prepared by nano-cellulose, the scanning electron microscope (SEM) photograph after the scanning electron microscope (SEM) photograph of cross-section morphology and section amplify; Fig. 1 (b
1), 1 (b
2) and 1 (b
3) be respectively the scanning electron microscope (SEM) photograph on the surface of not adding regenerated celulose fibre prepared by nano-cellulose, the scanning electron microscope (SEM) photograph after the scanning electron microscope (SEM) photograph of cross-section morphology and section amplify;
By Fig. 1 (a
1), 1 (a
2) and 1 (a
3) and Fig. 1 (b
1), 1 (b
2) and 1 (b
3) contrast can find, add nano-cellulose and do not change the exterior appearance of regenerated fiber, but add the compactness of fibrous inner structure.
Fig. 2 is interpolation nano-cellulose and the load-deformation curve comparison diagram not adding the regenerated celulose fibre prepared by nano-cellulose;
As shown in Figure 2, add the TENSILE STRENGTH that nano-cellulose can increase regenerated celulose fibre significantly, do not lose its elongation at break simultaneously.
Embodiment 3
A preparation method for regenerated celulose fibre, comprises the steps:
(1) basic solution method prepares spinning solution: to be 90% degree of polymerization by 4.5kg alpha-cellulose content be 400 cotton linter pulp mix with 95.5kg lithium hydroxide/urea/sulphur urea/aqueous solution (mass ratio is 5/7/8/80), the too low intensity step-down that also can cause the regenerated celulose fibre of preparation of the degree of polymerization, at mixed liquor being placed in-8 DEG C after stirring, vigorous stirring, after 4 minutes, obtains homogeneous, transparent spinning solution;
(2) prepare the dispersion liquid of nano-cellulose: by the nano-cellulose of 3wt% (relative to cotton linter pulp) at 20 DEG C ultrasonic disperse in the lithium hydroxide/urea/sulphur urea/aqueous solution (mass ratio is 5/7/8/780) of the 5wt% quality of solvent (in relative to the spinning solution), the length of described nano-cellulose is 3 μm, and draw ratio is 100; Obtain nano-cellulose dispersion liquid;
(3) prepare regenerated celulose fibre: spinning solution is warming up to 20 DEG C, with vigorous stirring, dropwise slowly joined in spinning solution by dispersion liquid, continuation stirring 25min obtains the spinning solution containing nano-cellulose; At 20 DEG C, spinning solution gained being contained nano-cellulose filters and vacuum defoamation, then device for spinning is placed in, spinning solution containing nano-cellulose is sprayed by spinneret orifice, enter into the coagulating bath be made up of sulfuric acid/sodium sulphate/water (mass ratio is 10/15/75), coagulation bath temperature is 50 DEG C; The as-spun fibre of coagulation forming is again after repeatedly washing, drawing-off, drying, arrangement, collection, and obtain regenerated celulose fibre, the TENSILE STRENGTH of this regenerated celulose fibre is 2.1cN/dtex, and elongation at break is 25.6%.
Embodiment 4
A preparation method for regenerated celulose fibre, comprises the steps:
(1) basic solution method prepares spinning solution: to be 98% degree of polymerization by 3.5kg alpha-cellulose content be 500 needlebush dissolving pulp mix with 96.5kg NaOH/zinc oxide/aqueous solution (mass ratio is 8/1/91), at mixed liquor being placed in 0 DEG C after stirring, vigorous stirring, after 5 minutes, obtains homogeneous, transparent spinning solution;
(2) dispersion liquid of nano-cellulose is prepared: spinning solution is warming up to 25 DEG C.By the nano-cellulose of 0.3wt% (relative to dissolving pulp) at 25 DEG C ultrasonic disperse in the NaOH/zinc oxide/aqueous solution (mass ratio is 8/1/91) of the 1wt% quality of solvent (in relative to the spinning solution), the length of described nano-cellulose is 4 μm, and draw ratio is 150; Obtain nano-cellulose dispersion liquid;
(3) prepare regenerated celulose fibre: with vigorous stirring, dispersion liquid is dropwise slowly joined in spinning solution, continue to stir 20min, obtain the spinning solution containing nano-cellulose; At 25 DEG C, after spinning solution containing nano-cellulose being filtered also vacuum defoamation, be placed in device for spinning, spinning solution is sprayed by spinneret orifice, and enter into the coagulating bath be made up of sulfuric acid/sodium sulphate/water (mass ratio is 5/10/85), coagulation bath temperature is 30 DEG C, the as-spun fibre of coagulation forming is again after repeatedly washing, drawing-off, drying, arrangement, collection, obtain regenerated celulose fibre, the TENSILE STRENGTH of this regenerated celulose fibre is 2.1cN/dtex, and elongation at break is 26.1%.
Embodiment 5
A preparation method for regenerated celulose fibre, comprises the steps:
(1) basic solution method prepares spinning solution: to be 98% degree of polymerization by 3kg alpha-cellulose content be 560 needlebush dissolving pulp mix with 97kg NaOH/polyethylene glycol/aqueous solution (mass ratio is 9/1/90), at mixed liquor being placed in-20 DEG C after stirring, vigorous stirring, after 5 minutes, obtains homogeneous, transparent spinning solution;
(2) prepare the dispersion liquid of nano-cellulose: by the nano-cellulose of 0.5wt% (relative to dissolving pulp) at 10 DEG C ultrasonic disperse in the NaOH/polyethylene glycol/aqueous solution (mass ratio is 9/1/90) of the 5wt% quality of solvent (in relative to the spinning solution), the length of described nano-cellulose is 1.8 μm, and draw ratio is 130; Obtain nano-cellulose dispersion liquid;
(3) prepare regenerated celulose fibre: spinning solution is warming up to 10 DEG C, with vigorous stirring, dispersion liquid is dropwise slowly joined in spinning solution, continue to stir 20min, obtain the spinning solution containing nano-cellulose.At 10 DEG C, after spinning solution containing nano-cellulose being filtered also vacuum defoamation, be placed in device for spinning, spinning solution containing nano-cellulose is sprayed by spinneret orifice, enter into the coagulating bath be made up of sulfuric acid/sodium sulphate/water (mass ratio is 8/12/80), coagulation bath temperature is 35 DEG C, and the as-spun fibre of coagulation forming after repeatedly washing, drawing-off, drying, arrangement, collection, obtains regenerated celulose fibre again; The TENSILE STRENGTH of this regenerated celulose fibre is 1.9cN/dtex, and elongation at break is 24.9%.
Embodiment 6
A preparation method for regenerated celulose fibre, comprises the steps:
(1) basic solution method prepares spinning solution: to be 90% degree of polymerization by 8kg alpha-cellulose content be 600 needlebush dissolving pulp mix with 92kg lithium hydroxide/thiocarbamide/aqueous solution (mass ratio is 7/12/81), at mixed liquor being placed in-6 DEG C after stirring, vigorous stirring, after 5 minutes, obtains homogeneous, transparent spinning solution;
(2) prepare the dispersion liquid of nano-cellulose: by the nano-cellulose of 5wt% (relative to dissolving pulp) at 10 DEG C ultrasonic disperse in the lithium hydroxide/thiocarbamide/aqueous solution (mass ratio is 7/12/81) of the 4wt% quality of solvent (in relative to the spinning solution), the length of described nano-cellulose is 1 μm, and draw ratio is 100; Obtain nano-cellulose dispersion liquid;
(3) prepare regenerated celulose fibre: spinning solution is warming up to 10 DEG C, with vigorous stirring, dispersion liquid is dropwise slowly joined in spinning solution, continue to stir 20min, obtain the spinning solution containing nano-cellulose.At 10 DEG C, after spinning solution containing nano-cellulose being filtered also vacuum defoamation, be placed in device for spinning, spinning solution is sprayed by spinneret orifice, enter into the coagulating bath be made up of sulfuric acid/sodium sulphate/water (mass ratio is 8/12/80), coagulation bath temperature is 35 DEG C, and the as-spun fibre of coagulation forming after repeatedly washing, drawing-off, drying, arrangement, collection, obtains regenerated celulose fibre again; The TENSILE STRENGTH of this regenerated celulose fibre is 2.5cN/dtex, and elongation at break is 30%.
Containing regenerated cellulose and nano-cellulose in the regenerated celulose fibre that above embodiment is prepared, wherein the quality of nano-cellulose is the 0.01-5% of regenerated cellulose quality.And prepared regenerated celulose fibre TENSILE STRENGTH and elongation at break all improve a lot than the regenerated celulose fibre not adding nano-cellulose, reach the object strengthening regenerated celulose fibre intensity, and reinforcing agent is nano-cellulose, do not introduce other materials outside cellulose, other harmful effects are not had to other character of regenerated celulose fibre.
Nano-cellulose used in above embodiment can be prepared by following several method and obtain:
(1) 5-20g cellulose being joined 100-200mL mass concentration is in the sulfuric acid of 40-65%, 1-4h is stirred under 50 DEG C of waters bath with thermostatic control, then 500-1000mL deionized water cessation reaction is added, high speed centrifugation (rotating speed is 10000-20000rpm) is adopted to be separated, incline supernatant liquor, gained lower sediment thing loads bag filter, dialyses in deionized water neutral to pH value, obtains Powdered nano-cellulose after freeze drying.
(2) 2g cellulose is joined 0.02-0.04g2,2,6, in 6-tetramethyl piperidine nitrogen oxide (TEMPO), 0.2-0.4g sodium bromide, 200mL deionized water, add the liquor natrii hypochloritis that 2-6mL mass fraction is 12% again, then use the hydrochloric acid solution adjust ph to 10 of 0.1mol/L, and at room temperature stir.Till adding the sodium hydroxide solution of 0.5mol/L in course of reaction, make pH value of reaction system remain on 10, no longer reduce until pH value, not needing to add sodium hydroxide solution again.Adopt high speed centrifugation (rotating speed is 10000-20000rpm) to be separated, incline supernatant liquor, and gained lower sediment thing loads bag filter, dialyses in deionized water neutral to pH value, obtain Powdered nano-cellulose after freeze drying.
(3) 1-2g cellulose being joined 100-200mL mass fraction is in the aqueous hydrochloric acid solution of 1%, 1-2h is reacted at 80-100 DEG C, react rear employing high speed centrifugation (rotating speed is 10000-20000rpm) to be separated, incline supernatant liquor, pour deionized water into, stir again, centrifugal, it is repeated multiple times until system is in neutral, then process with ultrasonic cell disruptor, power is 1000 ~ 1200W, frequency is 18-22KHz, processing time 10min-2h, suspension after process uses high speed centrifugation (rotating speed is 10000-20000rpm) to be separated again, incline supernatant liquor, nano-cellulose is obtained after the freeze drying of gained lower sediment thing.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; change can be expected easily or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of described claim.
Claims (8)
1. a preparation method for regenerated celulose fibre, is characterized in that, comprises the steps:
Basic solution method is adopted to prepare spinning solution and be warming up to 10-30 DEG C; Then add nano-cellulose wherein and be uniformly dispersed, described nano-cellulose quality is equivalent to the 0.01-5% of cellulosic material quality in described spinning solution, described nano-cellulose length≤5 μm, draw ratio >=50, then carry out wet spinning and obtain as-spun fibre cellulose fiber, more described as-spun fibre cellulose fiber is prepared into regenerated celulose fibre.
2. the preparation method of regenerated celulose fibre according to claim 1, is characterized in that, described nano-cellulose length≤2 μm.
3. the preparation method of regenerated celulose fibre according to claim 1, is characterized in that, described nano-cellulose quality is equivalent to the 0.5-2% of cellulosic material quality in described spinning solution.
4. the preparation method of regenerated celulose fibre according to claim 1, it is characterized in that, the feed postition of described nano-cellulose is prepared into dispersion liquid for being first dispersed in aqueous slkali by nano-cellulose, the quality of described aqueous slkali is the 1-10% of aqueous slkali quality in described spinning solution, is then distributed in described spinning solution by described homogeneous dispersion.
5. the preparation method of regenerated celulose fibre according to claim 4, is characterized in that, the aqueous slkali quality in described dispersion liquid is the 4-6% of the aqueous slkali quality in described spinning solution.
6. the preparation method of regenerated celulose fibre according to claim 1, it is characterized in that, the described concrete steps preparing spinning solution are:
Be obtain described spinning solution after dissolving under-20-0 DEG C of condition after the raw material of 300-600 mixes with aqueous slkali by the degree of polymerization of alpha-cellulose mass fraction >=90%, in described spinning solution, the mass fraction of regenerated cellulose is 3-8%.
7. the preparation method of regenerated celulose fibre according to claim 1, it is characterized in that, the concrete steps of described wet spinning are: have that the described spinning solution of nano-cellulose filters at 10-30 DEG C, vacuum defoamation by dispersed, and be placed in device for spinning, sprayed by spinneret orifice, enter into coagulating bath, described coagulating bath is made up of 5-15wt% sulfuric acid, 5-15wt% sodium sulphate and water, described coagulation bath temperature is 20-60 DEG C, and in coagulating bath, coagulation forming obtains as-spun fibre element.
8. a regenerated celulose fibre, it is characterized in that, described regenerated cellulose is prepared by the preparation method of claim 1-7 regenerated celulose fibre described in any one and obtains, wherein containing the regenerated cellulose of 100 weight portions and the nano-cellulose of 0.01-5 weight portion, the TENSILE STRENGTH of described regenerated celulose fibre is 1.5-2.5cN/dtex, and elongation at break is 10-30%.
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