CN101851802A - Method for producing functional high wet modulus fiber by using hemp-containing pulp - Google Patents
Method for producing functional high wet modulus fiber by using hemp-containing pulp Download PDFInfo
- Publication number
- CN101851802A CN101851802A CN 201010181300 CN201010181300A CN101851802A CN 101851802 A CN101851802 A CN 101851802A CN 201010181300 CN201010181300 CN 201010181300 CN 201010181300 A CN201010181300 A CN 201010181300A CN 101851802 A CN101851802 A CN 101851802A
- Authority
- CN
- China
- Prior art keywords
- cellulose
- pulp
- hemp
- viscose glue
- viscose
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a method for producing functional high wet modulus fiber by using hemp-containing pulp. The functional high wet modulus fiber is manufactured by adopting a mixture of pure hemp pulp or hemp pulp and other pulp as a raw material, using common equipment for producing common viscose staple and adopting a process-controlled simple and practical special process formula and a spinning drafting mode through alkalization reaction, ageing reaction, yellowing reaction, viscose dissolution, viscose filter, viscose de-foaming, viscose ageing, wet spinning, drafting and other related process steps. The method has the advantages of low investment, adoption of easily obtained and low-cost raw materials, high capacity and simple process operation; and the manufactured hemp cellulose functional high wet modulus fiber has good quality and stable performance.
Description
Technical field:
The present invention relates to a kind of method of producing functional high wet modulus fiber with the plain pulp of novel plant raw material flax fibre.
Background technology:
The gloss of high-wet-modulus 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; Functional high wet modulus fiber with jute pulp is made not only has the characteristics of common high-wet-modulus fibre, also have because of the distinctive bacteria resistance function of the antibacterial material that has in its flax fibre, and the cunning with flax fibre very, nice and cool, fine and smooth, smooth characteristics.
High wet modulus fibrid in the market, its raw material are the wood pulps of high alpha-cellulose content, and product is is not with functional medium-sized textile fiber.The present invention is 200910098913.0 at the application number of our company application, and name is called on the basis of " a kind of manufacture method of high-wet-modulus fibre " to be expanded.
Summary of the invention:
The object of the present invention is to provide a kind of plain pulp of common flax fibre (comprise with mixing of wood pulp, cotton pulp or wet pulp etc.) that adopts to be raw material, to reduce cost of material greatly, and can on common viscose glue production equipment, produce, adopt special process prescription and spinning drafting method and technology controlling and process simple and practical, meet international standards and with functional high-wet-modulus fibre manufacture method.
The technical solution adopted in the present invention is: this is characterized in that adopting successively following steps with the method that hemp-containing pulp is produced functional high wet modulus fiber:
A. pulp floods in the NaOH of 200-300g/l solution, 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, press ratio is 2.5～3.5, and through pulverizing, degree of grinding is 120～220g/l to the alkali cellulose after the squeezing again, carry out the dipping second time, the NaOH solution concentration of double-steeping is 120g/l～200g/l, and dipping temperature is 40 ℃～55 ℃, and dip time is 0.5～1.5 hour, dipping slurry congee concentration is 2.0%～6.0%, behind the double-steeping again through the squeezing, pulverize, press ratio is 2.5～3.5, and degree of grinding is 100～200g/l, so that hemicellulose in the pulp is tried one's best stripping in pressed liquor, and the hemicellulose in the pressed liquor removed, to contain the alpha-cellulose percentage by weight be 25～35% and make, and contains the NaOH percentage by weight and be 14～18% 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, at 60～120mps, guarantee viscose filtration performance and spinnability preferably with the cuprammonium viscosity of the alkali cellulose that reaches experienced equipment, satisfy the needs of fiber high-strength power simultaneously;
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 NaOH solution dissolving of concentration 10g/l～80g/l, form with the viscose glue that reaches the spinning high-wet-modulus fibre, it is 5.0～8.0% that viscose glue consists of the alpha-cellulose percentage by weight, and the NaOH percentage by weight is 4.0～7.0%; Cellulose xanthate in the described yellow reaction adds the alkylene oxide adduct denaturant of 0.5～1.0% 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, the filter pressure differential is 0.1～0.4Mpa;
F. the deaeration of viscose glue: adopt the continuously and rapidly defoaming method, the viscose glue turnover temperature difference 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 be that the alkylene oxide adduct denaturant of 1～3% nitrogen compound injects with injection method before spinning to alpha cellulose content, making falling ball viscosity be 70～130S, degree of ripeness (10%NH
4Cl)＞and 20ml, esterification degree 45～65, alpha-cellulose percentage by weight are 5.0～8.0%, the NaOH percentage by weight is 4.0～7.0% viscose solution, solidification forming in spinning coagulation bath then, the coagulating bath composition comprises the H of 40～110g/l
2SO
4, 30～80g/l ZnSO
4, 80～160g/l Na
2SO
4All the other are water, 35～48 ℃ of coagulation bath temperatures, spinning speed 20～40m/min, the strand Immersion time in coagulating bath added phosphoric acid formicester defoamer to defoam at 0.5～1.6 second in coagulating bath, on the circulating line of coagulating bath, install simultaneously the foam catcher additional to eliminate foam, because the foam in the viscose glue too much can influence spinning technique, the degassing of coagulating bath, waste gas are reclaimed and evaporation etc. causes adverse effect, the stable operation that serious meeting influence is produced;
I. drawing-off: strand is through spinneret draft, draw-off godet drawing-off, plasticizing drawing-off, the plasticizing drawing-off comprises that two bathe drawing-off, draw-off godet speed 20～50m/min, two bathe drawing roller speed 22～80m/min, strand total draft rate reaches 50～200%, and strand is immersed in two and two bathes the H that mixed liquors comprise concentration 10.0～50.0g/l when bathing in the mixed liquors drawing-off
2SO
4, the ZnSO of concentration 5.0～15.0g/l
4, all the other are water, two bath drawing temperatures are 80～99 ℃;
J. post-processed.
Drawing-off of the present invention comprises that also three bathe drawing-off, and plasticizing three bath drawing-offs are stretched after drawing-offs are bathed in plasticizing two and carried out, and the H that mixed liquor comprises concentration 10.0～30.0g/l is bathed in plasticizing three
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.
Raw material of the present invention adopts hemp dissolving pulp, the perhaps combination of hemp dissolving pulp and wood pulp, cotton pulp.
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.
Hemp dissolving pulp of the present invention adds the fatty alcohol ether with respect to alpha cellulose weight 0.05～0.20% in the alkalization process.
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 plain high-wet-modulus fibre of flax fibre that the present invention makes with said method is characterized in that doing fracture strength: 3.10～4.00CN/dtex; Wet breaking strength: 1.80～3.00CN/dtex; Dried elongation at break: 11～16%; Wet elongation at break 11～16%; Wet modulus: 0.45～0.55CN/dtex, (* 20) 6～11; Line density deviation ratio: ± 7.00%; Length variation rate: ± 7.0%; Overcut fibre :≤1.0%; Over-length fibre :≤20.0mg/100g; Residual sulfur content :≤10mg/100g; Fault :≤12mg/100g.
The every index of the plain high-wet-modulus fibre of the obtained flax fibre of this method reaches the high-wet-modulus fibre international standard.Its fabric that is made into has intensity height, indeformable, the dyeing advantage such as bright-coloured of washing, and the cunning with flax fibre very, nice and cool, fine and smooth, smooth and antibiotic characteristics.
The specific embodiment
The embodiment of the invention adopts hemp dissolving pulp through NaOH solution once or double-steeping, quaternization takes place, again through squeezing, pulverizing, adopting dipping temperature is 40 ℃～60 ℃, dip time is 0.5～3 hour, slurry congee concentration is 2.0%～6.0%, and press ratio is 2.5～3.5, and degree of grinding is that 100～200g/l makes alkali cellulose.The alkali cellulose that makes is according to the cellulose macromolecule degree of polymerization of hemp dissolving pulp raw material, suitably with its oxidation scission, by alkali cellulose material amount and discharging speed experienced (oxidation) time of control in the experienced equipment, wind pushing temperature is controlled at 20 ℃～45 ℃, reduce the degree of polymerization to 350～550 to reach experienced outlet cuprammonium viscosity 60～120mps, the viscose filtration performance and the spinning property that make are good, and guarantee that fiber reaches high brute force.With above-mentioned alkali cellulose that makes (7500～8000kg/ criticizes) and CS
2Reaction (CS
2Addition is that 650～850l/ criticizes), the yellow time is 0.5～2.5 hour, generates cellulose xanthate, adds 2 ℃～12 ℃ of temperature, the dissolving alkali lye of concentration 20g/l～60g/l, dissolving alkali addition is 25m
3～35m
3, form with the viscose glue that reaches the spinning functional high wet modulus fiber.In the processing procedure of viscose glue, adopt continuously or batch (-type) viscose glue dissolution mechanism 8 ℃～25 ℃ of solution temperatures, dissolution time 0.5～3h.The mode that the filtration of viscose glue adopts wire sintering screen pack continuous filter to filter two roads or three roads, filter---advance-export pressure reduction=0.1～0.4Mpa.Continuously and rapidly defoaming is adopted in the deaeration of viscose glue, and the temperature difference---advancing-go out Δ T=is 3 ℃～7 ℃, and deaeration vacuum≤40mbar sloughs bubble in the viscose glue in the viscose glue turnover.Viscose glue low temperature maturation in bucket simultaneously, 10 ℃～25 ℃ of glue temperature, the maturation time is 3～10 hours.Making falling ball viscosity is 70～130S, and degree of ripeness is＞20ml (10%NH
4Cl) viscose solution, viscose glue is solidification forming in spinning coagulation bath, coagulating bath (acid bath) composition H
2SO
440～110g/l, ZnSO
430～80g/l, Na
2SO
480～160g/l, all the other are water.35～48 ℃ of coagulation bath temperatures.Spinning speed 20～40m/min, draw-off godet speed 20～50m/min, two bathe drawing roller speed 22～80m/min, and three bathe drawing roller speed 30～100m/min.Strand after the shaping is through spinneret draft, draw-off godet drawing-off, plasticizing (two bathe) drawing-off, or in addition three bathes drawing-offs again, and brute force is improved.Strand is immersed in plasticizing two and bathes drawing-off in the mixed liquor, H
2SO
4Concentration 10.0～50.0g/l, ZnSO
4Concentration 5.0～15.0g/l, all the other are water, 80～99 ℃ of temperature.Or bathe drawing-off in the mixed liquor, H three again
2SO
4Concentration 10.0～30.0g/l, ZnSO
4Concentration 2.0～10.0g/l, all the other are water, 75～98 ℃ of temperature.Again through desulfurization, bleaching, wash, oil, postprocessing working procedures such as oven dry obtains finished fiber.
The present invention adopts the hemp dissolving pulp raw material, can be the hemp dissolving pulp combination of (comprising one or more the combination in wood pulp, cotton pulp or the wet pulp); The present invention utilizes the double-steeping can be with the effective stripping of the hemicellulose in the hemp dissolving pulp, and impurity such as hemicellulose are on the high side, will influence glue and spinning as effectively not removing, and is difficult to produce high-wet-modulus 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 the course of dissolution of cellulose xanthate with spin before inject the alkylene oxide adduct (English name: Alkylene oxide adducts ofnitrogen compounds) of 1.0～4.0% the nitrogen compound that adds relative alpha-cellulose weight in the viscose glue, with respect to present domestic employed denaturant-polyoxyethylene fatty amine (English name: Polyoxyethylene fatty amine), can 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 denaturant of bringing in the viscose glue and produce foam, foam too much can influence spinning technique, and the degassing, the waste gas of coagulating bath is reclaimed and evaporation etc. causes adverse effect, the stable operation that serious meeting influence is produced.The alkylene oxide adduct denaturant that during spinning technique with relative alpha cellulose content is 1～3% nitrogen compound injects viscose solution with injection method before spinning, and can reduce the generation of foam, improves the quality of products.But still have the part foam to be difficult to eliminate, the present invention adds in coagulating bath that existing phosphoric acid formicester defoamer installs the foam catcher simultaneously additional with the elimination foam further to defoam in the prior art on the circulating line of coagulating bath.
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.Ratio of the present invention or content all refer to weight or percentage by weight.
The every index of the plain high-wet-modulus fibre of the obtained flax fibre of this method reaches the high-wet-modulus fibre international standard.Its fabric that is made into has intensity height, indeformable, the dyeing advantage such as bright-coloured of washing, and the cunning with flax fibre very, nice and cool, fine and smooth, smooth and antibiotic characteristics.
Embodiment 1:
Adopting alpha-cellulose content is that 90% the plain pulp of flax fibre 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 STOKOMIN EBZ) 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, and dipping temperature is 42 ℃, and dip time is 0.5 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 7.0%, the cellulose viscose glue of NaOH5.0%, 1.0% of the relative alpha-cellulose weight of adding viscose glue denaturant---the alkylene oxide adduct (code name STOKOMIN 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 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 cellulose viscose glue is after the alkylene oxide adduct denaturant (code name STOKOMIN EB) of 1.5% nitrogen compound injects with injection method before spinning to alpha cellulose content, spinning solution wet spinning moulding (spinning), 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 ℃, the defoamer addition is the 0.2kg/T fiber in the coagulating bath.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, three through shower nozzle drawing-off, draw-off godet drawing-off, two and is bathed drawing-off secondary plasticizing drawing-off, retraction etc., and plasticizing-bath comprises that two bathe and three baths, and two baths are sulfuric acid concentration 35g/l, zinc sulfate concentration 10g/l, 98 ℃ of temperature; Three baths are sulfuric acid concentration 25g/l, zinc sulfate concentration 5g/l, 90 ℃ of temperature.The suffered total stretch ratio of strand is 100%, again through desulfurization, bleaching, wash, oil, make finished fiber after the operation such as oven dry, resultant fibre number is 1.33dtex, does strong 3.10cN/dtex, wet strong 1.90cN/dtex, wet modulus is 0.48cN/dtex.
Embodiment 2:
Adopting alpha-cellulose content is that 89% the plain pulp of flax fibre and 93% the cotton pulp dregs of rice (each 50%) carry out the single-steeping alkalization through the NaOH of 238g/L solution, slurry congee concentration is 4.5%, dipping temperature is 52 ℃, dip time is 1 hour, adds viscose glue auxiliary agent---the fatty alcohol ether (code name STOKOMIN EBZ) to the fine content 0.15% of first when pulverizing.Again through the alkalization of the NaOH of 175g/l solution double-steeping, slurry congee concentration is 4.2% after squeezing, and dipping temperature is 46 ℃, and dip time is 0.35 hour, 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 1.5 hours, make the alkali cellulose that cuprammonium viscosity is 78mps.With 7800kg alkali cellulose and 810 liters of CS
2Yellow reaction 1 hour, generate cellulose xanthate, after yellow finishes, add 40g/LNaOH solution 8 ℃ of dissolvings, obtaining alpha-cellulose content is 5.6%, the viscose solution of NaOH5.6%, 0.5% of the relative alpha-cellulose weight of adding viscose glue denaturant---the alkylene oxide adduct (code name STOKOMIN EBT) 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 ℃～18 ℃ of glue temperature, and the maturation time is 3.5 hours; Making viscosity is that 120s, degree of ripeness are 45ml (10%NH
4Cl), esterification degree is 55 cellulose rayon spinning stoste.The cellulose viscose glue is after the alkylene oxide adduct denaturant (code name STOKOMIN EBT) of 2% nitrogen compound injects with injection method before spinning to alpha cellulose content, spinning solution adopts the wet spinning moulding, be pressed in the acid bath of sulfuric acid 72g/l, zinc sulfate 48g/l, sodium sulphate 133g/l through spray orifice, the acid bath temperature is 38 ℃, the reaction moulding, the defoamer addition is the 0.15kg/T fiber in the coagulating bath.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 3.22CN/dtex, hygrometric state fracture strength be at 2.18CN/dtex, wet modulus 0.50CN/dtex.
Embodiment 3:
Adopting alpha-cellulose content is that 88% hemp dissolving pulp and alpha-cellulose content are 94% wood pulps, jute pulp: wood pulp=60%: 40%, carry out the single-steeping alkalization through the NaOH of 235g/l solution, slurry congee concentration is 3.6%, dipping temperature is 53 ℃, adds viscose glue auxiliary agent---the fatty alcohol ether (code name STOKOMIN 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 3.3 alkali cellulose.Alkali cellulose 35 ℃ experienced 2.0 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 6.0%, the cellulose viscose glue of NaOH6.0%, 1.0% of the relative alpha-cellulose weight of adding viscose glue denaturant---the alkylene oxide adduct (code name STOKOMIN 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 4 hours; Making viscosity is 90s, and degree of ripeness is 35ml (10%NH
4Cl), esterification degree is 55 cellulose rayon spinning stoste.The cellulose viscose glue is after the alkylene oxide adduct denaturant (code name STOKOMIN EB) of 2% nitrogen compound injects with injection method before spinning to alpha cellulose content, spinning solution adopts the wet spinning moulding, be pressed into sulfuric acid 90g/l, zinc sulfate 45g/l, sodium sulphate 150g/l through spray orifice, react moulding in the coagulating bath that the acid bath temperature is 45 ℃, the defoamer addition is the 0.25kg/T fiber in the coagulating bath.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 two baths are sulfuric acid concentration 38g/l, zinc sulfate concentration 12g/l, 94 ℃ of temperature; Three baths are sulfuric acid concentration 20g/l, zinc sulfate concentration 6g/l, 90 ℃ 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 120%, again through desulfurization, bleaching, wash, oil, make finished fiber after the operation such as oven dry, resultant fibre number is 1.33dtex, do strong 3.38CN/dtex, wet strong 2.08CN/dtex, wet modulus is 0.47CN/dtex.
The simple deformation or the combination of every embodiment of the invention technical scheme and technical characterictic all should be thought all within protection scope of the present invention.
Claims (6)
1. method of producing functional high wet modulus fiber with hemp-containing pulp is characterized in that adopting successively following steps:
A. raw material floods in the NaOH of 200-300g/l solution, 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, press ratio is 2.5～3.5, and through pulverizing, degree of grinding is 120～220g/l to the alkali cellulose after the squeezing again, carry out the dipping second time, the NaOH solution concentration of double-steeping is 120g/l～200g/l, and dipping temperature is 40 ℃～55 ℃, and dip time is 0.5～1.5 hour, dipping slurry congee concentration is 2.0%～6.0%, behind the double-steeping again through the squeezing, pulverize, press ratio is 2.5～3.5, and degree of grinding is 100～200g/l, so that hemicellulose in the pulp is tried one's best stripping in pressed liquor, and the hemicellulose in the pressed liquor removed, to contain the alpha-cellulose percentage by weight be 25～35% and make, and contains the NaOH percentage by weight and be 14～18% alkali cellulose;
B. experienced reaction: according to the cellulose macromolecule degree of polymerization of 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, at 60～120mps, guarantee viscose filtration performance and spinnability preferably with the cuprammonium viscosity of the alkali cellulose that reaches experienced equipment, satisfy the needs of fiber high-strength power simultaneously;
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 NaOH solution dissolving of concentration 10g/l～80g/l, form with the viscose glue that reaches the spinning high-wet-modulus fibre, it is 5.0～8.0% that viscose glue consists of the alpha-cellulose percentage by weight, and the NaOH percentage by weight is 4.0～7.0%; Cellulose xanthate in the described yellow reaction adds the alkylene oxide adduct denaturant of 0.5～1.0% 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,
The filter pressure differential is 0.1～0.4Mpa;
F. the deaeration of viscose glue: adopt the continuously and rapidly defoaming method, the viscose glue turnover temperature difference 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 be that the alkylene oxide adduct denaturant of 1～3% nitrogen compound injects with injection method before spinning that to make falling ball viscosity be 70～130S to alpha cellulose content, degree of ripeness 10%NH
4Cl value＞20ml, esterification degree 45～65, alpha-cellulose percentage by weight are 5.0～8.0%, the NaOH percentage by weight is 4.0～7.0% viscose solution, solidification forming in spinning coagulation bath then, 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, spinning speed 20～40m/min, the Immersion time of strand in coagulating bath added phosphoric acid formicester defoamer to defoam at 0.5～1.6 second in coagulating bath, install the foam catcher simultaneously additional to eliminate foam on the circulating line of coagulating bath;
I. drawing-off: strand is through spinneret draft, draw-off godet drawing-off, plasticizing drawing-off, the plasticizing drawing-off comprises that two bathe drawing-off, draw-off godet speed 20～50m/min, two bathe drawing roller speed 22～80m/min, strand total draft rate reaches 50～200%, and strand is immersed in two and two bathes the H that mixed liquors comprise concentration 10.0～50.0g/l when bathing in the mixed liquors drawing-off
2SO
4, the ZnSO of concentration 5.0～15.0g/l
4, all the other are water, two bath drawing temperatures are 80～99 ℃;
J. post-processed;
The plain high-wet-modulus fibre of the flax fibre that said method is made, its dried fracture strength: 3.10～4.00CN/dtex; Wet breaking strength: 1.80～3.00CN/dtex; Dried elongation at break: 11～16%; Wet elongation at break 11～16%; Wet modulus: 0.45～0.55CN/dtex; Line density deviation ratio: ± 7.00%; Length variation rate: ± 7.0%; Overcut fibre :≤1.0%; Over-length fibre :≤20.0mg/100g; Residual sulfur content :≤10mg/100g; Fault :≤12mg/100g.
2. method of producing functional high wet modulus fiber with hemp-containing pulp according to claim 1 is characterized in that: described drawing-off comprises that also three bathe drawing-off, and three bath drawing-offs are stretched after two bath drawing-offs and carried out, and three 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 three bath drawing temperatures are 75～98 ℃, and three bathe drawing roller speed 30～100m/min.
3. method of producing functional high wet modulus fiber with hemp-containing pulp according to claim 1 is characterized in that: raw material adopts hemp dissolving pulp, the perhaps combination of hemp dissolving pulp and wood pulp, cotton pulp.
4. according to the described method of producing functional high wet modulus fiber with hemp-containing pulp of the arbitrary claim of claim 1～3, it is characterized in that: raw material 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. according to the described method of producing functional high wet modulus fiber with hemp-containing pulp of the arbitrary claim of claim 1～3, it is characterized in that: hemp dissolving pulp adds the fatty alcohol ether with respect to alpha cellulose weight 0.05～0.20% in the alkalization process.
6. according to the described method of producing functional high wet modulus fiber with hemp-containing pulp of the arbitrary claim of claim 1～3, 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010181300 CN101851802A (en) | 2010-05-24 | 2010-05-24 | Method for producing functional high wet modulus fiber by using hemp-containing pulp |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010181300 CN101851802A (en) | 2010-05-24 | 2010-05-24 | Method for producing functional high wet modulus fiber by using hemp-containing pulp |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101851802A true CN101851802A (en) | 2010-10-06 |
Family
ID=42803473
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010181300 Pending CN101851802A (en) | 2010-05-24 | 2010-05-24 | Method for producing functional high wet modulus fiber by using hemp-containing pulp |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101851802A (en) |
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011205A (en) * | 2010-10-19 | 2011-04-13 | 山东海龙股份有限公司 | Germanium viscose fiber and preparation method thereof |
| CN102295705A (en) * | 2011-07-04 | 2011-12-28 | 山东雅美科技有限公司 | Method for preparing alkali cellulose by wet pulp method |
| CN102535221A (en) * | 2012-01-09 | 2012-07-04 | 成都丽雅纤维股份有限公司 | Process for crushing pulp dregs in production of viscose fibers |
| CN102851776A (en) * | 2012-09-24 | 2013-01-02 | 成都丽雅纤维股份有限公司 | Production method of colored cotton, wood and bamboo composite pulp viscose |
| CN104831387A (en) * | 2015-05-27 | 2015-08-12 | 宜宾丝丽雅集团有限公司 | Delustering high-strength low-elongation viscose fiber preparation technology |
| CN104831392A (en) * | 2015-05-27 | 2015-08-12 | 宜宾丝丽雅集团有限公司 | High-strength low-elongation viscose and preparing method thereof |
| CN104831388A (en) * | 2015-04-30 | 2015-08-12 | 湖州珠力纳米材料科技开发有限公司 | Preparation method of temperature regulating fiber |
| CN104846455A (en) * | 2015-05-27 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | High-tenacity and low-elongation viscose fibers, as well as preparation method and application thereof |
| CN104846453A (en) * | 2015-05-27 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | Superfine viscose fiber and preparation method thereof |
| CN104862802A (en) * | 2015-05-27 | 2015-08-26 | 宜宾丝丽雅集团有限公司 | Process method for preparing high-tenacity and low-elongation viscose |
| CN104894670A (en) * | 2015-05-27 | 2015-09-09 | 宜宾丝丽雅集团有限公司 | High-strength viscose fibers and preparation method and application of high-strength viscose fibers |
| CN104911726A (en) * | 2015-05-27 | 2015-09-16 | 宜宾丝丽雅集团有限公司 | Flatting ultra-fine type high-strength and low-stretching viscose fibers and preparation method thereof |
| CN104928786A (en) * | 2015-05-27 | 2015-09-23 | 宜宾丝丽雅集团有限公司 | Preparation process of semi-dull high-strength low-elongation viscose fibers |
| WO2016188274A1 (en) * | 2015-05-27 | 2016-12-01 | 宜宾丝丽雅集团有限公司 | Matte high-strength, low-stretch viscose fiber and manufacturing method therefor |
| CN107574491A (en) * | 2017-09-01 | 2018-01-12 | 恒天海龙（潍坊）新材料有限责任公司 | A kind of numb material high-tenacity regenerated celulose fibre and its production method |
| CN107938010A (en) * | 2017-10-30 | 2018-04-20 | 宜宾丝丽雅股份有限公司 | A kind of high-intensity fine denier flame retardant viscose fiber and its production technology |
| CN107964693A (en) * | 2017-10-30 | 2018-04-27 | 宜宾丝丽雅股份有限公司 | A kind of production technology of high-strength anti-flaming viscose rayon |
| CN107974722A (en) * | 2017-10-30 | 2018-05-01 | 宜宾丝丽雅股份有限公司 | A kind of production technology of high-intensity fine denier flame retardant viscose fiber |
| CN109913967A (en) * | 2019-03-19 | 2019-06-21 | 阿拉尔市富丽达纤维有限公司 | A kind of technique preparing viscose rayon using low polymerizing degree pulp |
| CN109930412A (en) * | 2017-12-15 | 2019-06-25 | 中国制浆造纸研究院有限公司 | A method of regulation cellulose pulp viscosity |
| CN110042489A (en) * | 2019-04-30 | 2019-07-23 | 阜宁澳洋科技有限责任公司 | A kind of preparation method of high crimp viscose |
| CN111206290A (en) * | 2020-02-28 | 2020-05-29 | 上海棉芙生物科技有限公司 | Making method of beautiful sesame fiber |
| CN112521517A (en) * | 2020-12-10 | 2021-03-19 | 宜宾丝丽雅股份有限公司 | Yellowing jacket control system and method in viscose fiber production |
| CN113388910A (en) * | 2021-06-17 | 2021-09-14 | 百事基材料（青岛）股份有限公司 | Viscose macrobio-fiber containing hemp active ingredient and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565863A (en) * | 2009-05-15 | 2009-10-28 | 云南瑞升烟草技术（集团）有限公司 | Preparation method of hemp dissolving pulp |
| CN101591814A (en) * | 2009-05-25 | 2009-12-02 | 杭州奥通科技有限公司 | A kind of manufacture method of high-wet-modulus fibre |
-
2010
- 2010-05-24 CN CN 201010181300 patent/CN101851802A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101565863A (en) * | 2009-05-15 | 2009-10-28 | 云南瑞升烟草技术（集团）有限公司 | Preparation method of hemp dissolving pulp |
| CN101591814A (en) * | 2009-05-25 | 2009-12-02 | 杭州奥通科技有限公司 | A kind of manufacture method of high-wet-modulus fibre |
Non-Patent Citations (1)
| Title |
|---|
| 《化纤与纺织技术》 19861231 钱以竑 粘胶纤维生产中的助剂应用技术 第4部分 1-6 , 第3期 2 * |
Cited By (31)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102011205B (en) * | 2010-10-19 | 2012-03-28 | 山东海龙股份有限公司 | Germanium viscose fiber and preparation method thereof |
| CN102011205A (en) * | 2010-10-19 | 2011-04-13 | 山东海龙股份有限公司 | Germanium viscose fiber and preparation method thereof |
| CN102295705A (en) * | 2011-07-04 | 2011-12-28 | 山东雅美科技有限公司 | Method for preparing alkali cellulose by wet pulp method |
| CN102535221A (en) * | 2012-01-09 | 2012-07-04 | 成都丽雅纤维股份有限公司 | Process for crushing pulp dregs in production of viscose fibers |
| CN102535221B (en) * | 2012-01-09 | 2014-11-26 | 成都丽雅纤维股份有限公司 | Process for crushing pulp dregs in production of viscose fibers |
| CN102851776A (en) * | 2012-09-24 | 2013-01-02 | 成都丽雅纤维股份有限公司 | Production method of colored cotton, wood and bamboo composite pulp viscose |
| CN102851776B (en) * | 2012-09-24 | 2014-07-09 | 成都丽雅纤维股份有限公司 | Production method of colored cotton, wood and bamboo composite pulp viscose |
| CN104831388A (en) * | 2015-04-30 | 2015-08-12 | 湖州珠力纳米材料科技开发有限公司 | Preparation method of temperature regulating fiber |
| CN104911726A (en) * | 2015-05-27 | 2015-09-16 | 宜宾丝丽雅集团有限公司 | Flatting ultra-fine type high-strength and low-stretching viscose fibers and preparation method thereof |
| CN104846453B (en) * | 2015-05-27 | 2017-10-03 | 宜宾丝丽雅集团有限公司 | A kind of superfine type viscose rayon and preparation method thereof |
| CN104846455A (en) * | 2015-05-27 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | High-tenacity and low-elongation viscose fibers, as well as preparation method and application thereof |
| CN104846453A (en) * | 2015-05-27 | 2015-08-19 | 宜宾丝丽雅集团有限公司 | Superfine viscose fiber and preparation method thereof |
| CN104862802A (en) * | 2015-05-27 | 2015-08-26 | 宜宾丝丽雅集团有限公司 | Process method for preparing high-tenacity and low-elongation viscose |
| CN104894670A (en) * | 2015-05-27 | 2015-09-09 | 宜宾丝丽雅集团有限公司 | High-strength viscose fibers and preparation method and application of high-strength viscose fibers |
| CN104831387A (en) * | 2015-05-27 | 2015-08-12 | 宜宾丝丽雅集团有限公司 | Delustering high-strength low-elongation viscose fiber preparation technology |
| CN104928786A (en) * | 2015-05-27 | 2015-09-23 | 宜宾丝丽雅集团有限公司 | Preparation process of semi-dull high-strength low-elongation viscose fibers |
| WO2016188275A1 (en) * | 2015-05-27 | 2016-12-01 | 宜宾丝丽雅集团有限公司 | High-strength, low-stretch viscose fiber and manufacturing method therefor |
| WO2016188274A1 (en) * | 2015-05-27 | 2016-12-01 | 宜宾丝丽雅集团有限公司 | Matte high-strength, low-stretch viscose fiber and manufacturing method therefor |
| CN104894670B (en) * | 2015-05-27 | 2017-09-15 | 宜宾丝丽雅集团有限公司 | A kind of high tenacity viscose fiber and its preparation method and application |
| CN104831392A (en) * | 2015-05-27 | 2015-08-12 | 宜宾丝丽雅集团有限公司 | High-strength low-elongation viscose and preparing method thereof |
| CN107574491A (en) * | 2017-09-01 | 2018-01-12 | 恒天海龙（潍坊）新材料有限责任公司 | A kind of numb material high-tenacity regenerated celulose fibre and its production method |
| CN107574491B (en) * | 2017-09-01 | 2020-10-23 | 恒天海龙（潍坊）新材料有限责任公司 | Hemp high-strength regenerated cellulose fiber and production method thereof |
| CN107938010A (en) * | 2017-10-30 | 2018-04-20 | 宜宾丝丽雅股份有限公司 | A kind of high-intensity fine denier flame retardant viscose fiber and its production technology |
| CN107964693A (en) * | 2017-10-30 | 2018-04-27 | 宜宾丝丽雅股份有限公司 | A kind of production technology of high-strength anti-flaming viscose rayon |
| CN107974722A (en) * | 2017-10-30 | 2018-05-01 | 宜宾丝丽雅股份有限公司 | A kind of production technology of high-intensity fine denier flame retardant viscose fiber |
| CN109930412A (en) * | 2017-12-15 | 2019-06-25 | 中国制浆造纸研究院有限公司 | A method of regulation cellulose pulp viscosity |
| CN109913967A (en) * | 2019-03-19 | 2019-06-21 | 阿拉尔市富丽达纤维有限公司 | A kind of technique preparing viscose rayon using low polymerizing degree pulp |
| CN110042489A (en) * | 2019-04-30 | 2019-07-23 | 阜宁澳洋科技有限责任公司 | A kind of preparation method of high crimp viscose |
| CN111206290A (en) * | 2020-02-28 | 2020-05-29 | 上海棉芙生物科技有限公司 | Making method of beautiful sesame fiber |
| CN112521517A (en) * | 2020-12-10 | 2021-03-19 | 宜宾丝丽雅股份有限公司 | Yellowing jacket control system and method in viscose fiber production |
| CN113388910A (en) * | 2021-06-17 | 2021-09-14 | 百事基材料（青岛）股份有限公司 | Viscose macrobio-fiber containing hemp active ingredient and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101851802A (en) | Method for producing functional high wet modulus fiber by using hemp-containing pulp | |
| CN101545150B (en) | Method for manufacturing modal fiber | |
| CN101591814B (en) | Method for manufacturing high wet modulus fiber | |
| CN101851804B (en) | Method for producing fire-retardant anti-melt viscose fibers | |
| CN103556281B (en) | The method of high wet modulus regenerated celulose fibre is produced with bamboo pulp | |
| CN1282773C (en) | Method for preparing regenerative cellulose fiber by two-step coagulating bath process | |
| CN109930225B (en) | Chlorine-bleaching-free high-whiteness viscose fiber and preparation method thereof | |
| CN1247838C (en) | Preparation method of polyacrylonitrile carbon raw yarn | |
| CN101857983A (en) | Production method of high wet modulus synthetic fiber containing bamboo | |
| CN105517955A (en) | Alkali recycling in cellulose spinning process | |
| CN101200819A (en) | High-strength high-wet-modulus bamboo fibre and preparation method thereof | |
| CN102337604B (en) | Method for producing modal fiber from cotton pulp | |
| CN104831392A (en) | High-strength low-elongation viscose and preparing method thereof | |
| CN104831387A (en) | Delustering high-strength low-elongation viscose fiber preparation technology | |
| CN102443868B (en) | Method for manufacturing regenerated cellulose fibers | |
| CN104846453B (en) | A kind of superfine type viscose rayon and preparation method thereof | |
| CN104846459A (en) | Extinction type high-strength low-elongation viscose and preparation method thereof | |
| CN104862802A (en) | Process method for preparing high-tenacity and low-elongation viscose | |
| CN100359050C (en) | High whiteness and strength adhesive short fiber and process for making same | |
| CN106498527A (en) | A kind of process for producing high-wet-modulus fibre cellulose fiber | |
| CN1706995A (en) | Denatured bamboo pulp viscose short fiber and its production process | |
| CN112708954B (en) | Rose plant extract cellulose fiber and preparation method thereof | |
| CN1085749C (en) | Shaped viscose staple and its preparing process and spinneret | |
| CN112680807B (en) | Cellulose fiber containing collagen component and preparation method thereof | |
| CN103305939B (en) | A kind of production technology of fine denier viscose staple fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20101006 |