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CN101545150A - Method for manufacturing modal fiber - Google Patents

Method for manufacturing modal fiber Download PDF

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Publication number
CN101545150A
CN101545150A CN200910098209A CN200910098209A CN101545150A CN 101545150 A CN101545150 A CN 101545150A CN 200910098209 A CN200910098209 A CN 200910098209A CN 200910098209 A CN200910098209 A CN 200910098209A CN 101545150 A CN101545150 A CN 101545150A
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viscose glue
pulp
cellulose
steeping
plasticizing
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CN200910098209A
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CN101545150B (en
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冉国庆
郑睿敏
李文峰
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Hangzhou Aotong new material Intelligent Technology Co.,Ltd.
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Hangzhou Autoon Science & Technology Co Ltd
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Abstract

The invention discloses a method for manufacturing modal fiber, which comprises basification reaction, ageing reaction, yellowing reaction, dissolution of viscose glue, filter of the viscose glue, defoaming of the viscose glue, ripening of the viscose glue, wet spinning, drawing and other related process steps. The method adopts cellulose pulp with alpha cellulose content of less than 95 percent as a raw material, uses common equipment for producing common viscose glue short fiber, and adopts the technology to control a simple and practical special process formulation and a spinning drawing mode to manufacture the modal fiber capable of reaching international standards. The method has the advantages of little investment, easily obtained and low-cost raw materials, high productivity and simple process operation; and the manufactured modal fiber has good quality and stable performance.

Description

A kind of method for manufacturing modal fiber
Technical field:
The present invention relates to the manufacture method of a kind of regenerated cellulose, particularly Modal fibre.
In this explanation, defined Modal fibre among the international standard ISO 2076:1999 (E), be high wet modulus, high breaking strength by specific viscose glue and the regenerated celulose fibre made of regeneration bath composition, when this tensile fiber condenses, can reach the molecularly oriented of higher degree.
Background technology:
The gloss of Modal fibre, flexibility, hygroscopicity, dyeability, dyefastness all are better than textile product; With the fabric that it is made, showed that a kind of face gloss has pleasant soft touch sensation and dangle sense and fabulous endurable performance.
Define according to BISFA: Modal fibre is the regenerated cellulose that obtains high strength and high wet modulus by process, and its wet breaking strength is more than 2.20CN/dtex, and wet elongation at break is less than 15%.At present homemade and push the high wet modulus fibrid in market, can not reach the Modal fibre international standard.Therefore the fabric made from it can't reach the model properties of product.
The general Modal fibre of producing needs high alpha cellulose content pulp, and for dipping effect is good, hemicellulose level is low in the maceration extract, and the viscose solution filtration and the spinning property that make are good.And in the cellulose pulp of low alpha cellulose content<95%, impurity such as hemicellulose are on the high side, will influence viscose glue manufacturing and spinning as effectively not removing, and are difficult to produce Modal fibre.Chinese patent application " koplon and preparation method thereof " as publication number CN101024907 discloses a kind of method that is used to prepare koplon, but its production process is to the ingredient requirement harshness, require pulp alpha cellulose content 〉=95%, this pulp needs special processing, cost and difficulty that pulp is made have been increased, especially wood pulp, the corresponding cost of material that increases fiber production greatly.But generally produce the pulp of viscose, the raw material that employing easily obtains, cost is low, its alpha cellulose content is generally 88%~93%.
Summary of the invention:
The cellulose pulp (comprising wood pulp, cotton pulp or wet pulp etc.) of alpha cellulose content that the object of the present invention is to provide common<95% of a kind of employing is for raw material, reduce cost of material greatly, and can on common viscose glue production equipment, produce, have small investment, the high advantage of production capacity, adopt special process prescription and spinning drafting method and technology controlling and process simple and practical simultaneously, the manufacture method of the Modal fibre that meets international standards.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: at method for manufacturing modal fiber, it is characterized in that adopting successively following steps:
A. quaternization: adopt single-steeping or double-steeping alkalization respectively according to raw material condition, when the alpha cellulose content of pulp more than 93% and less than 95% the time (also can adopt the inventive method) greater than 95% adopt single-steeping technology, pulp floods in the NaOH of concentration 200g/l~300g/l solution, quaternization takes place, dipping temperature is 40 ℃~60 ℃, dip time is 0.5~3 hour, slurry congee concentration is 2.0%~6.0%, generate alkali cellulose, reacted slurry congee is through squeezing, unnecessary NaOH solution is extruded, and press ratio is 2.5~3.5.Through pulverizing, degree of grinding is that 120~220g/l makes alkali cellulose to the alkali cellulose that press dry again; Double-steeping is carrying out carrying out (do not require These parameters to press ratio and degree of grinding this moment) after first time dipping and squeezing are pulverized according to above-mentioned condition, double-steeping does not require the alpha cellulose upper content limit of pulp, the alpha cellulose content that is particularly useful for pulp is less than 95%, particularly the alpha cellulose content of pulp adopts the double-steeping step when following 93%, the NaOH solution concentration is 120g/l~200g/l during double-steeping, the double-steeping temperature is 40 ℃~55 ℃, the double-steeping time is 0.5~1.5 hour, double-steeping slurry congee concentration is 2.0%~6.0%, the double-steeping press ratio is 2.5~3.5, the double-steeping degree of grinding is 100~200g/l, so that hemicellulose in the pulp is tried one's best stripping in maceration extract, and the hemicellulose in the pressed liquor removed, and make alkali cellulose.Usually, this alkali cellulose contains alpha cellulose 25~35%, and containing NaOH is 14~18%.
B. experienced reaction: according to the cellulose macromolecule degree of polymerization of pulp raw material, with its oxidation scission, control ageing time by alkali cellulose material amount in the experienced equipment and alkali cellulose discharging speed, wind pushing temperature is controlled at 20 ℃~45 ℃ in the experienced equipment, reduce the degree of polymerization to 350~550 scopes,, be beneficial to viscose filtration and the spinning that makes thereafter and make fiber reach high brute force at 60~120mps with the alkali cellulose cuprammonium viscosity that reaches experienced equipment;
C. yellow reaction: with above-mentioned alkali cellulose that makes (about 8000kg/ criticizes) and CS 2Reaction (CS 2Addition is 650~8501/ batches), the yellow time is 0.5~2.5 hour, generate cellulose xanthate, add 2 ℃~12 ℃ of temperature, the alpha cellulose content 5.0~8.0% that this viscose glue is formed is formed in the NaOH solution dissolving of concentration 10g/l~80g/l with the viscose glue that reaches the spinning Modal fibre, NaOH content 4.0~7.0%, cellulose xanthate add the alkylene oxide adduct denaturant of 1.0~4.0% nitrogen compound of relative alpha cellulose weight in course of dissolution;
D. the dissolving of viscose glue: adopt continuously or batch (-type) viscose glue grinding dissolution mechanism 8 ℃~25 ℃ of solution temperatures, dissolution time 0.5~3 hour;
E. the filtration of viscose glue: the mode that viscose filtration adopts wire sintering screen pack continuous filter to filter two roads or three roads, filter turnover pressure differential is between 0.1~0.4Mpa;
F. the deaeration of viscose glue: adopt the continuously and rapidly defoaming method, viscose glue turnover temperature difference T is 3 ℃~7 ℃, and deaeration vacuum≤40mbar removes bubble in the viscose glue;
G. the maturation of viscose glue: viscose glue is the low temperature maturation in the maturation bucket, 10 ℃~25 ℃ of glue temperature, and the maturation time is 3~10 hours;
H. spinning: will make falling ball viscosity is 70~130S, degree of ripeness (10%NH 4Cl)〉20ml, esterification degree 45~65, alpha cellulose content 5.0~8.0%, the viscose solution of NaOH content 4.0~7.0% solidification forming in spinning coagulation bath, the coagulating bath composition comprises the H of 40~110g/l 2SO 4, 30~80g/l ZnSO 4, 80~160g/l Na 2SO 4, all the other are water, 35~48 ℃ of coagulation bath temperatures, and spinning speed 20~40m/min, the strand Immersion time in coagulating bath was at 0.5~1.6 second;
I. drawing-off: strand is bathed drawing-off through spinneret draft, draw-off godet drawing-off, plasticizing two, draw-off godet speed 20~50m/min, two bathe drawing roller speed 22~80m/min, strand total draft rate reaches 50~200%, strand be immersed in plasticizing two when bathing in the mixed liquors drawing-off plasticizing two bathe the H that mixed liquors comprise concentration 10.0~50.0g/l 2SO 4, the ZnSO of concentration 5.0~15.0g/l 4, all the other are water, it is 80~99 ℃ that drawing temperature is bathed in plasticizing two;
J. post-processed.
Drawing-off of the present invention also comprises plasticizing three bath drawing-offs, and plasticizing three bath drawing-offs are stretched after drawing-off is bathed in plasticizing two and carried out, and plastify three and bathe the H that mixed liquors comprise concentration 10.0~30.0g/l 2SO 4, concentration 2.0~10.0g/l ZnSO 4, all the other are water, and it is 75~98 ℃ that drawing temperature is bathed in plasticizing three, and three bathe drawing roller speed 30~100m/min.
Pulp of the present invention hemicellulose level<30g/l in the maceration extract when the NaOH solution impregnation adopts membrane filtering method to remove hemicellulose too much in the immersion liquid.
Pulp of the present invention adds the fatty alcohol ether that is equivalent to alpha cellulose weight 0.05~0.20% in alkalization process (when single-steeping or double-steeping).
The extra coagulating bath of spinning step of the present invention becomes height and contains zincic acid bath shunting to the general fibre production line behind pervaporation, do zinc sulfate and add use, thereby reduce because of low Na 2SO 4The acid bath amount that the content acid bath can't crystallization need be discharged.
Post-processed of the present invention be strand again through desulfurization, bleaching, wash, oil, dry and obtain finished fiber, it is main finish that the finish of the operation that wherein oils is selected fatty acid polyglycol ethylene glycol especially, can spin by the single mark when the high-speed spinning to adapt to, and when washing, the pH value of washing lotion is regulated, the pH value that makes fiber is 6.0~7.5.
The present invention adopts the pulp raw material, can for the pulp of alpha cellulose content<95% (comprising one or more the combination in wood pulp, cotton pulp or the wet pulp) or with the combination of (comprising one or more the combination in wood pulp, cotton pulp or the wet pulp) of the pulp of alpha cellulose content 〉=95%; The present invention utilizes double-steeping the effective stripping of the hemicellulose in the pulp because in the cellulose pulp of alpha cellulose content<95%, impurity such as hemicellulose are on the high side, will be able to be influenced glue and spinning as effectively not removing, and is difficult to produce Modal fibre; The present invention adds the fatty alcohol ether to alpha cellulose weight 0.05~0.20% when alkali cellulose prepares, with respect to present domestic employed viscose glue auxiliary agent-polyalkylene glycol alkyl amine, can obtain better crushing effect, thereby reduce the weight of every liter of alkali cellulose, and help xanthation, this auxiliary agent can make the insoluble matter on dipping, squeezing and the pulverizer obtain reducing more effective raising yellow reaction effect and viscose filtration performance.Thereby obtain higher esterification degree, the viscose glue of high viscosity and Geng Gao degree of ripeness more; The present invention adds the alkylene oxide adduct of 1.0~4.0% nitrogen compound of relative alpha cellulose weight in the course of dissolution of cellulose xanthate, with respect to present domestic employed denaturant-polyoxyethylene fatty amine, delay the speed of viscose glue regenerative response in coagulating bath more, stop the decomposition of xanthate acid, reduce thereby strand has been solidified in the expanded raising of as-spun fibre in the coagulating bath stretching and dehydration, owing to have good and couplings resin and other water insoluble byproducts, make viscose glue clarify and the raising strainability, reduce the interfacial tension of viscose glue and prevent to stop up spinneret orifice, so can carry out bigger drawing-off to strand, thereby make the degree of orientation of fiber and degree of crystallinity increase brute force and the wet modulus that improves fiber greatly.
The present invention adopts coagulating bath low speed wet spinning moulding under lower temperature of the low high zinc of sodium of low acid, further slows down the regenerative response of cellulose xanthate, and guarantees that the length of immersion of strand and reaction time are to increase fibrocortex thickness; The present invention adopts plasticizing in the diluted acid of heat is bathed (two bathe or three baths) drawing-off, to obtain the brute force of the bigger degree of orientation of fiber and Geng Gao; The present invention is in the operation that oils of refining, the special fatty acid polyglycol ethylene glycol of selecting is main finish, contain in the finish low friction performance component, high embrace and and antistatic ingredient, give fiber good embracing and degree and significant scrooping feel, the spinning processing characteristics is good can be spun by the single mark when the high-speed spinning to adapt to; When washing, the pH value of washing lotion is regulated, made the pH value of fiber be neutral (pH value is 6.0~7.5).
In addition, selected equipment and technology are the same with the production common viscose fiber, and other process conditions are the conventional requirement of production common viscose fiber, and technological parameter of the present invention can be optimized it according to production equipment.
The obtained fiber of the present invention, its dried fracture strength 3.10~4.50CN/dtex;
Dried elongation at break 12~17%
Wet breaking strength 1.80~3.50CN/dtex;
Wet elongation at break 13~18%
Wet modulus 0.30~0.55CN/dtex.
(×20)6~11
The every index of the obtained Modal fibre of this method reaches the Modal fibre international standard.Its fabric that is made into has advantages such as intensity height, washing is indeformable, dyeing is bright-coloured.
The specific embodiment
Embodiment 1:
Adopting alpha cellulose content is that 92% lignose pulp carries out the single-steeping alkalization through the NaOH of 230g/l solution, slurry congee concentration is 4.5%, dipping temperature is 50 ℃, add viscose glue auxiliary agent---the fatty alcohol ether (code name EBZ) that is equivalent to methylcellulose amount 0.1% when dipping, dip time is 1.5 hours for the first time.Again through the alkalization of the NaOH of 160g/l solution double-steeping, slurry congee concentration is 4.0% after squeezing is pulverized, and dipping temperature is 42 ℃, and dip time is 1 hour for the second time, makes hemicellulose stripping in the steeping liquor, its content<20g/l.Making press ratio after squeezing is pulverized once more is 2.8, and degree of grinding is the alkali cellulose of 120g/l.Alkali cellulose 30 ℃ experienced 4 hours, make the alkali cellulose that cuprammonium viscosity is 70mps.With 7500kg alkali cellulose and 790 liters of CS 2Yellow reaction 45min generates cellulose xanthate, after yellow finishes, adds 30g/lNaOH solution, dissolves under 5 ℃ temperature.Obtaining alpha cellulose content is 6.5%, and the cellulose viscose glue of NaOH5.0% adds 1.0% viscose glue denaturant---the alkylene oxide adduct (code name EB) of nitrogen compound be equivalent to alpha cellulose weight in the course of dissolution of cellulose xanthate.The cellulose viscose glue is after dissolving, and more after filtration, operations such as deaeration, maturation, wherein viscose filtration adopts the mode that KKF filter three roads filter, filter turnover pressure differential 0.35Mpa; Continuously and rapidly defoaming is adopted in the deaeration of viscose glue, and viscose glue turnover temperature difference T is 5 ℃, and deaeration vacuum≤30mbar sloughs bubble in the viscose glue; The maturation of viscose glue is the low temperature maturation in bucket, 10 ℃~18 ℃ of glue temperature, and the maturation time is 8 hours; Obtaining viscosity is 90s, and degree of ripeness is 30.0ml (10%NH 4Cl), esterification degree is 58 cellulose rayon spinning stoste.The wet spinning moulding (spinning) of cellulose rayon spinning stoste, be pressed into sulfuric acid 85g/L, zinc sulfate 40g/l, sodium sulphate 150g/l through spray orifice, react moulding in the coagulating bath that the acid bath temperature is 40 ℃, immersion length is not less than 60mm in the coagulating bath, and Immersion time is at 0.5~1.6s.Strand is bathed drawing-off, plasticizing three bath drawing-off secondary plasticizing drawing-offs, retraction etc. through shower nozzle drawing-off, draw-off godet drawing-off, plasticizing two, plasticizing-bath comprises that two bathe and three baths, plasticizing two is bathed mixed liquor and is comprised sulfuric acid concentration 35g/l, zinc sulfate concentration 10g/l, and all the other are water, 98 ℃ of temperature; Plasticizing three is bathed mixed liquor and is comprised sulfuric acid concentration 25g/l, zinc sulfate concentration 5g/l, and all the other are water, 90 ℃ of temperature.The suffered total stretch ratio of strand is 120%, again through desulfurization, bleaching, wash, oil, make finished fiber after the operation such as oven dry, resultant fibre number is 1.33dtex, does strong 3.30cN/dtex, wet strong 2.25cN/dtex, the hygrometric state elastic modelling quantity is 0.38cN/dtex.
Embodiment 2:
Adopting alpha cellulose content is that 89% the lignose pulp and 94% the cotton pulp dregs of rice (each 50%) carry out the single-steeping alkalization through the NaOH of 240g/L solution, slurry congee concentration is 4.8%, dipping temperature is 52 ℃, dip time is 1 hour, adds viscose glue auxiliary agent---the fatty alcohol ether (code name EBZ) to the fine content 0.1% of first when pulverizing.Again through the alkalization of the NaOH of 170g/l solution double-steeping, slurry congee concentration is 4.5% after squeezing is pulverized, and dipping temperature is 48 ℃, and dip time is 1.5 hours, makes hemicellulose stripping in the steeping liquor, its content<25g/l.Make press ratio after squeezing is pulverized once more and be 3.0 alkali cellulose.Alkali cellulose 25 ℃ experienced 5 hours, make the alkali cellulose that cuprammonium viscosity is 90mps.With 7800kg alkali cellulose and 810 liters of CS 2Yellow reaction 1 hour, generate cellulose xanthate, after yellow finishes, add 40g/LNaOH solution 7 ℃ of dissolvings, obtaining alpha cellulose content is 5.5%, the viscose solution of NaOH5.5%, 4.0% of the relative alpha cellulose weight of adding viscose glue denaturant---the alkylene oxide adduct (code name MI07) of nitrogen compound in the course of dissolution of cellulose xanthate.The cellulose viscose glue is after dissolving, and more after filtration, operations such as deaeration, maturation, wherein the mode that KKF filter two roads filter is adopted in the filtration of viscose glue, filter turnover pressure differential 0.30Mpa; Continuously and rapidly defoaming is adopted in the deaeration of viscose glue, and viscose glue turnover temperature difference T is 4 ℃, and deaeration vacuum≤20mbar sloughs bubble in the viscose glue; The maturation of viscose glue is the low temperature maturation in bucket, 12 ℃~20 ℃ of glue temperature, and the maturation time is 4 hours; Making viscosity is that 120s, degree of ripeness are that 45ml (10%NH4Cl), esterification degree are 55 cellulose rayon spinning stoste.Cellulose rayon spinning stoste adopts the wet spinning moulding, is pressed in the coagulating bath (acid bath) of sulfuric acid 80g/l, zinc sulfate 50g/l, sodium sulphate 125g/l through spray orifice, and the acid bath temperature is 35 ℃, the reaction moulding, and immersion length is not less than 60mm in the coagulating bath.Plasticizing-bath is sulfuric acid concentration 45g/l, zinc sulfate concentration 25g/l, 96 ℃ of temperature.Strand is through shower nozzle drawing-off, draw-off godet drawing-off, plasticizing drawing-off, retraction etc., the suffered total stretch ratio of strand institute bar is 80%, again through desulfurization, bleaching, wash, oil, make finished fiber after the operation such as oven dry, resultant fiber is 1.67dtex for degree, dry state fracture strength 3.80CN/dtex, the hygrometric state fracture strength is at 2.55CN/dtex, hygrometric state elastic modelling quantity 0.42CN/dtex.
Embodiment 3:
Adopting the fine content of first is that 94.5% the cotton pulp dregs of rice carry out the single-steeping alkalization through the NaOH of 235g/l solution, and slurry congee concentration is 3.8%, and dipping temperature is 52 ℃, adds viscose glue auxiliary agent---the fatty alcohol ether (code name EBZ) to methylcellulose amount 0.2% when dipping.Dip time is 2.5 hours, makes hemicellulose stripping in the steeping liquor, its content<30g/l.After pulverizing, squeezing makes press ratio and is 3.2 alkali cellulose.Alkali cellulose 35 ℃ experienced 2.5 hours, make the alkali cellulose that cuprammonium viscosity is 80mps.With 8000kg alkali cellulose and 840 liters of CS 2Yellow reaction 55min, generate cellulose xanthate, after yellow finishes, add the 48g/lNaOH sig water 8 ℃ of dissolvings, obtaining alpha cellulose content is 7.0%, the cellulose viscose glue of NaOH6.5%, 2.0% of the relative alpha cellulose weight of adding viscose glue denaturant---the alkylene oxide adduct (code name EB) of nitrogen compound in the course of dissolution of cellulose xanthate.The cellulose viscose glue is after dissolving, and more after filtration, operations such as deaeration, maturation, wherein the mode that KKF filter three roads filter is adopted in the filtration of viscose glue, filter turnover pressure differential 0.25Mpa; Continuously and rapidly defoaming is adopted in the deaeration of viscose glue, and viscose glue turnover temperature difference T is 6 ℃, and deaeration vacuum≤25mbar sloughs bubble in the viscose glue; The maturation of viscose glue is the low temperature maturation in bucket, 15 ℃~22 ℃ of glue temperature, and the maturation time is 6 hours; Obtaining viscosity is 90s, and degree of ripeness is 40ml (10%NH 4Cl), esterification degree is 55 cellulose rayon spinning stoste.Cellulose rayon spinning stoste adopts the wet spinning moulding, is pressed into sulfuric acid 90g/l, zinc sulfate 45g/l, sodium sulphate 150g/l through spray orifice, reacts moulding in the coagulating bath that the acid bath temperature is 45 ℃, and immersion length is not less than 60mm in the coagulating bath, and Immersion time is at 0.5-1.6s.The plasticizing of employing secondary, plasticizing-bath comprise that two bathe and three baths, and plasticizing two is bathed mixed liquor and comprised sulfuric acid concentration 38g/l, zinc sulfate concentration 12g/l, and all the other are water, 96 ℃ of temperature; Plasticizing three is bathed mixed liquor and is comprised sulfuric acid concentration 20g/l, zinc sulfate concentration 6g/l, and all the other are water, 92 ℃ of temperature.Strand is bathed secondary plasticizing drawing-off, retraction etc. through shower nozzle drawing-off, draw-off godet drawing-off, plasticizing-bath two, three, the suffered total draft rate of strand institute bar is 170%, again through desulfurization, bleaching, wash, oil, make finished fiber after the operation such as oven dry, resultant fibre number is 1.33dtex, do strong 3.50CN/dtex, wet strong 2.28CN/dtex, the hygrometric state elastic modelling quantity is 0.40CN/dtex.
More than be the concrete enforcement under the technical solution of the present invention framework, the simple deformation or the combination of every embodiment of the invention technical scheme and technical characterictic all should be thought to fall into protection scope of the present invention.

Claims (7)

1, a kind of method for manufacturing modal fiber is characterized in that adopting successively following steps:
A. quaternization: adopt single-steeping or double-steeping alkalization respectively according to raw material condition, when the alpha cellulose content of pulp is adopting single-steeping more than 93% and less than 95% the time, pulp floods in the NaOH of concentration 200g/l~300g/l solution, quaternization takes place, dipping temperature is 40 ℃~60 ℃, dip time is 0.5~3 hour, slurry congee concentration is 2.0%~6.0%, generate alkali cellulose, reacted slurry congee extrudes unnecessary NaOH solution through squeezing, and press ratio is 2.5~3.5, through pulverizing, degree of grinding is 120~220g/l to the alkali cellulose that press dry again; Double-steeping carries out after dipping and squeezing are pulverized for the first time, double-steeping NaOH solution concentration is 120g/l~200g/l, the double-steeping temperature is 40 ℃~55 ℃, the double-steeping time is 0.5~1.5 hour, and double-steeping slurry congee concentration is 2.0%~6.0%, and the double-steeping press ratio is 2.5~3.5, the double-steeping degree of grinding is 100~200g/l, so that hemicellulose in the pulp is tried one's best stripping in maceration extract, and the hemicellulose in the pressed liquor is removed, and made alkali cellulose;
B. experienced reaction: according to the cellulose macromolecule degree of polymerization of pulp raw material, with its oxidation scission, control ageing time by alkali cellulose material amount in the experienced equipment and alkali cellulose discharging speed, wind pushing temperature is controlled at 20 ℃~45 ℃ in the experienced equipment, reduce the degree of polymerization to 350~550 scopes,, be beneficial to viscose filtration and the spinning that makes thereafter and make fiber reach high brute force at 60~120mps with the alkali cellulose cuprammonium viscosity that reaches experienced equipment;
C. yellow reaction: with above-mentioned alkali cellulose that makes and CS 2Reaction, the yellow time is 0.5~2.5 hour, generate cellulose xanthate, add 2 ℃~12 ℃ of temperature, the alpha cellulose content 5.0~8.0% that this viscose glue is formed is formed in the NaOH solution dissolving of concentration 10g/l~80g/l with the viscose glue that reaches the spinning Modal fibre, NaOH content 4.0~7.0%, cellulose xanthate add the alkylene oxide adduct denaturant of 1.0~4.0% nitrogen compound of relative alpha cellulose weight in course of dissolution;
D. the dissolving of viscose glue: adopt continuously or batch (-type) viscose glue grinding dissolution mechanism 8 ℃~25 ℃ of solution temperatures, dissolution time 0.5~3 hour;
E. the filtration of viscose glue: the mode that viscose filtration adopts wire sintering screen pack continuous filter to filter two roads or three roads, filter turnover pressure differential is between 0.1~0.4Mpa;
F. the deaeration of viscose glue: adopt the continuously and rapidly defoaming method, viscose glue turnover temperature difference T is 3 ℃~7 ℃, and deaeration vacuum≤40mbar removes bubble in the viscose glue;
G. the maturation of viscose glue: viscose glue is the low temperature maturation in the maturation bucket, 10 ℃~25 ℃ of glue temperature, and the maturation time is 3~10 hours;
H. spinning: will make falling ball viscosity is 70~130S, degree of ripeness 10%NH 4The Cl value〉20ml, esterification degree 45~65, alpha cellulose content 5.0~8.0%, the viscose solution of NaOH content 4.0~7.0% solidification forming in spinning coagulation bath, the coagulating bath composition comprises the H of 40~110g/l 2SO 4, 30~80g/l ZnSO 4, 80~160g/l Na 2SO 4, all the other are water, 35~48 ℃ of coagulation bath temperatures, and spinning speed 20~40m/min, the strand Immersion time in coagulating bath was at 0.5~1.6 second;
I. drawing-off: strand is bathed drawing-off through spinneret draft, draw-off godet drawing-off, plasticizing two, draw-off godet speed 20~50m/min, two bathe drawing roller speed 22~80m/min, strand total draft rate reaches 50~200%, strand be immersed in plasticizing two when bathing in the mixed liquors drawing-off plasticizing two bathe the H that mixed liquors comprise concentration 10.0~50.0g/l 2SO 4, the ZnSO of concentration 5.0~15.0g/l 4, all the other are water, it is 80~99 ℃ that drawing temperature is bathed in plasticizing two;
J. post-processed.
2, method for manufacturing modal fiber according to claim 1 is characterized in that: described drawing-off also comprises plasticizing three bath drawing-offs, and plasticizing three bath drawing-offs are stretched after drawing-off is bathed in plasticizing two and carried out, and plastify three and bathe the H that mixed liquors comprise concentration 10.0~30.0g/l 2SO 4, concentration 2.0~10.0g/l ZnSO 4, all the other are water, and it is 75~98 ℃ that drawing temperature is bathed in plasticizing three, and three bathe drawing roller speed 30~100m/min.
3, method for manufacturing modal fiber according to claim 1 and 2, it is characterized in that: raw material adopts the pulp of alpha cellulose content<95%, comprise a kind of in wood pulp, cotton pulp or the wet pulp or their combination, the perhaps combination of the pulp of the pulp of alpha cellulose content<95% and alpha cellulose content 〉=95%, the degree of polymerization of pulp is 450~1250.
4, method for manufacturing modal fiber according to claim 1 and 2 is characterized in that: pulp hemicellulose level<30g/l in the maceration extract when the NaOH solution impregnation, adopt membrane filtering method to remove hemicellulose too much in the immersion liquid.
5, method for manufacturing modal fiber according to claim 1 and 2 is characterized in that: pulp adds the fatty alcohol ether that is equivalent to alpha cellulose weight 0.05~0.20% in the alkalization process.
6, method for manufacturing modal fiber according to claim 1 is characterized in that: the extra coagulating bath of described spinning step becomes height and contains zincic acid bath shunting to the general fibre production line behind pervaporation, do zinc sulfate and add use, thereby reduce because of low Na 2SO 4The acid bath amount that the content acid bath can't crystallization need be discharged.
7, method for manufacturing modal fiber according to claim 1 and 2, it is characterized in that: described post-processed be strand again through desulfurization, bleaching, wash, oil, dry and obtain finished fiber, it is main finish that the finish of the operation that wherein oils is selected fatty acid polyglycol ethylene glycol especially, can spin by the single mark when the high-speed spinning to adapt to, and when washing, the pH value of washing lotion is regulated, the pH value that makes fiber is 6.0~7.5.
CN2009100982095A 2009-04-30 2009-04-30 Method for manufacturing modal fiber Active CN101545150B (en)

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CN102337604A (en) * 2011-01-30 2012-02-01 唐山三友集团兴达化纤有限公司 Method for producing modal fiber from cotton pulp
US20130161861A1 (en) * 2011-12-21 2013-06-27 E. I. Du Pont De Nemours And Company Process for preparing polysaccharide fibers from aqueous alkali metal hydroxide solution
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US10059778B2 (en) 2014-01-06 2018-08-28 E I Du Pont De Nemours And Company Production of poly alpha-1,3-glucan films
US10106626B2 (en) 2014-01-17 2018-10-23 Ei Du Pont De Nemours And Company Production of poly alpha-1,3-glucan formate films
CN103924315A (en) * 2014-03-20 2014-07-16 绍兴文理学院 Aloe fiber preparation method
CN111885992A (en) * 2018-05-17 2020-11-03 松下知识产权经营株式会社 Selectively permeable membrane for biological adhesion, transdermal absorption kit, and cosmetic method
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CN109280987A (en) * 2018-09-20 2019-01-29 武汉纺织大学 A kind of method that bamboo raw material prepares Modal fibre
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CN112442775A (en) * 2019-09-02 2021-03-05 连津格股份公司 Applying draw in a modal spinning process
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CN112831856A (en) * 2020-07-13 2021-05-25 太极石股份有限公司 Preparation method of Tai Ji stone modal fiber

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