CN105951199A - Preparation method for regenerated cellulose fiber - Google Patents
Preparation method for regenerated cellulose fiber Download PDFInfo
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- CN105951199A CN105951199A CN201610424400.4A CN201610424400A CN105951199A CN 105951199 A CN105951199 A CN 105951199A CN 201610424400 A CN201610424400 A CN 201610424400A CN 105951199 A CN105951199 A CN 105951199A
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- spinning
- methylmorpholine
- oxide
- regenerated celulose
- celulose fibre
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to a preparation method for regenerated cellulose fiber. The preparation method comprises the following steps that pulp is subjected to preimpregnating, squeezing and smashing; the obtained mixture is added into a water solution of N-methylmorpholine-N-oxide, antioxidant is added, and the mixture is stirred to be uniform; the obtained mixture is placed into a vacuum environment, and a spinning solution is obtained under the condition that the temperature ranges from 80 DEG C to 100 DEG C; spinning is carried out on the obtained spinning solution, and the regenerated cellulose fiber is obtained, wherein during spinning, spinning bath is the water solution of the N-methylmorpholine-N-oxide. According to the method for preparing the regenerated cellulose fiber, the finally obtained regenerated cellulose fiber is high in strength, appropriate in breaking elongation, good in section form and soft and smooth in hand feeling. In addition, the whole method is simple, convenient to operate, high in repeatability, beneficial for large-scale popularization, environmentally friendly and low in cost, and the spinning bath can be recycled.
Description
Technical field
The invention belongs to textile fabric field, particularly relate to the preparation method of a kind of regenerated celulose fibre.
Background technology
Regenerated celulose fibre cellulose is that regeneration that raw material is made, that structure is cellulose I I is fine
Dimension.Due to the minimizing ploughed and exhaustion, natural fiber, the yield of synthetic fibers day by day of petroleum resources
Will more and more be restricted；People are paying attention in textile process of consumption while environmental-protecting performance,
The value of regenerated celulose fibre is re-recognized and excavated.Nowadays regenerated celulose fibre
Application has obtained a unprecedented opportunity to develop.
The production method of traditional regenerated celulose fibre takes following preparation process: by various raw materials
Pulp impregnates in alkali liquor, squeezes, pulverizes acquisition alkali fiber, then by poly-for experienced for alkali fiber fall rear with two
Nitric sulfid (CS2) reaction, generate cellulose xanthate, afterwards, cellulose xanthate is dissolved in alkali
In liquid, form viscous colloidal solution, then react with three component acid baths, prepare regenerated celulose fibre.
In the preparation technology that this is traditional, maximum defect is to use substantial amounts of CS2And zinc sulfate
(ZnSO4), discharge CS the most in process of production2And H2S toxic gas, and produce a large amount of
Zinc-containing water, causes severe contamination to air and waters, makes ecological balance be seriously damaged.
In recent years, the green spining technology research about regenerated celulose fibre constantly makes progress, example
As used the direct dissolving pulp of different dicyandiamide solutions, it is possible to resolve this restriction regenerated celulose fibre is good
The problem of sexual development.Lyocell fiber is the representative products of green fiber, in the prior art, with slurry
The dregs of rice are that raw material carries out spinning and prepares, and the product feel obtained is harder, fibrillation easily occurs, after needs
The technique that continuous increase processes fibrillation.
Summary of the invention
In order to solve the problems referred to above, present inventor has performed further investigation, found that: by pulp first
Carry out a step pretreatment, be redispersed in the aqueous solution of N-methylmorpholine-N-oxide, be then passed through
Dipping, spinning, it is thus achieved that regenerated celulose fibre, it is thus achieved that the intensity of regenerated celulose fibre high, disconnected
Splitting elongation suitable, section morphology is good, meanwhile, soft smooth, thus completes the present invention.
The elongation at break of regenerated celulose fibre needs size suitable, and elongation at break is high, fabric
Being easily generated deformation, be susceptible to fold, elongation at break is low can reduce the comfort level of fabric, research
Show that elongation at break fabric effects between 12-16% of regenerated celulose fibre is best.
It is an object of the invention to provide the preparation method of a kind of regenerated celulose fibre, including following four
Individual step.
Step one, the pretreatment of pulp, the pretreatment of pulp includes three parts:
Pulp pre-preg, joins N-methylmorpholine-N-oxide (being called for short NMMO) by pulp
Aqueous solution carries out pre-preg；Concrete, in described step one, used by pre-preg N-methyl
The mass percent of the aqueous solution of quinoline-N-oxide is 50-65%, and pre-preg temperature is 50-70 DEG C,
The pre-preg time is 15-30mim, and the bath raio of pre-preg is pulp: N-methylmorpholine-N-oxide
Aqueous solution=1:10-15；
Squeezing, squeezes the mixture after pre-preg, removes unnecessary solution, it is thus achieved that have steady
The mixture of fixed composition；Concrete, in described step one, the component of the mixture after squeezing is slurry
The dregs of rice, N-methylmorpholine-N-oxide and water, its weight ratio is 30-40:15-20:40-55；
Pulverize, the mixture after squeezing is pulverized；Concrete, in described step one, pulverize
Rear mixture particle diameter is 1-15mm.
In above-mentioned steps one, pulp is the dissolving pulp dregs of rice, and pulp methyl fiber content is more than 95%, with much money
Belong to content and be less than 0.07%, degree of polymerization 550-650DP.
And the pretreatment that the present invention is extra, i.e. with dipping and corresponding squeezing and pulverizing, it is right to be equivalent to
Pulp has done single treatment in advance, and follow-up step coordinates the NMMO being equivalent to use variable concentrations
Aqueous solution carries out after-treatment, so that the intensity of the regenerated celulose fibre prepared is high, fracture is stretched
Long suitable, section morphology is good, the soft effect such as smooth.
Step 2, mixture step one obtained join the water of N-methylmorpholine-N-oxide
In solution, add antioxidant, and stir.
In above-mentioned steps two, N-methylmorpholine-N-oxide mass percent in aqueous is
60～68%, it is further preferred that the mass percent that N-methylmorpholine-N-oxide is in aqueous
It is 60～65%, and the mixture that described step one is obtained and N-methylmorpholine-N-oxide is water-soluble
The weight ratio of liquid is 1:18-20；It is further preferred that weight ratio is preferably pulp mixture:
NMMO aqueous solution=1:19.
In above-mentioned steps two, described antioxidant is preferably propylgallate, by antioxidant
Such as after propylgallate adds, it is possible to prevent the N-methylmorpholine-N-oxide oxygen in aqueous solution
Change and decompose, thus the final quality obtaining regenerated celulose fibre of impact.It addition, when selecting Galla Turcica (Galla Helepensis)
When propyl propionate is as antioxidant, its addition is preferably the 0.2～1% of first fibre gross weight, further
Preferably, the addition of propylgallate is preferably the 0.5～1% of first fibre gross weight, and wherein first is fine
Gross weight can be understood as the gross weight that first is fine in described pulp.
When being stirred premixing in the aqueous solution that pulp is joined N-methylmorpholine-N-oxide,
Equipment, time and temperature conditions selected during stirring is conventional selection, the most special need
Ask, as long as by described pulp mix homogeneously in the aqueous solution of N-methylmorpholine-N-oxide.
Preferably, at the aqueous solution that described pulp and antioxidant are joined N-methylmorpholine-N-oxide
After in, at 90～100 DEG C, stir 20～60 minutes, obtain premixed liquid, it is further preferred that stir
The time of mixing is 20～40 minutes.Owing to premixed liquid is at 90～100 DEG C, stirs 20～60 minutes, make
Obtain pulp fully to be infiltrated in the aqueous solution of N-methylmorpholine-N-oxide, thus improve final
The performance of the regenerated celulose fibre obtained, such as can improve regenerated celulose fibre intensity and
Elongation at break.
Step 3, mixture step 2 obtained are inserted in vacuum environment, 80～100 DEG C of conditions
Under, it is thus achieved that spinning solution.
In above-mentioned steps three, the vacuum of vacuum environment is preferably-0.1MPa～-0.08MPa,
Under this vacuum degree condition, so that pulp is completely dissolved.
In above-mentioned steps three, the time that the premixed liquid obtained in step 2 is placed in vacuum environment
Can select according to the actual requirements, as long as pulp is completely dissolved.Preferably, premixed liquid is very
The time placed in Altitude is 10～20min, it is further preferred that premixed liquid is put in vacuum environment
The time put is 10～15min.
The spinning solution of acquisition can be filtered, go the removal of impurity, improve final acquisition more further
The performance of raw cellulose fibre.
First fibre content in the spinning solution obtained is preferably 10～15%, the viscosity of described spinning solution
It is preferably 13000～15000Pa S.When the first fibre content in above-mentioned spinning solution and viscosity are at above-mentioned model
When enclosing interior, it is possible to improve the performance of the final regenerated celulose fibre obtained further.If first fibre content
Too low or too high, it is unfavorable for the raising of the intensity of the regenerated celulose fibre finally obtained, same,
If viscosity is too low or too high, it is unfavorable for the raising of the intensity of the regenerated celulose fibre finally obtained.
It addition, from the point of view of more specifically, join thin film evaporation evacuation by step 2 obtains premixed liquid
In device, then at temperature is 80～90 DEG C, carry out evacuation, wherein vacuum be-0.1MPa～
-0.08MPa, finally makes pulp be completely dissolved, it is thus achieved that spinning solution.Additionally, the spinning obtained is former
Liquid can maintain spinning solution can spin state by heat exchanger heat exchange.
Step 4, the spinning solution obtained in step 3 is carried out spinning, specifically, can be by step
The spinning solution obtained in three joins and carries out spinning in spinning-drawing machine, it is thus achieved that regenerated celulose fibre, its
During middle spinning, spinning bath is N-methylmorpholine-N-oxide water solution.
It is pointed out that spinning bath is positioned at spinning-drawing machine.
In above-mentioned steps four, after spinning solution is extruded by spinning head, through air bath, then with spin
Silk bath contacts and is continued solidification, then separates out, finally obtains regenerated celulose fibre, due to head
It is introduced in air bath and solidifies, select spinning bath to proceed solidification the most again, it is possible to significantly to carry
The intensity of the high final regenerated celulose fibre obtained and elongation at break.It may also be noted that
The air gap of spinning head is preferably 15～35mm, and selecting spray webbing hole count is 20000～30000 holes, especially
Select circular spinning head.The detailed process that selection spinning-drawing machine carries out spinning is as follows: will obtain in step 2
Spinning solution, by circular spinning head ejection, enters air bath, enters spinning bath afterwards and continues solidification,
Obtain regenerated celulose fibre eventually.
In above-mentioned steps four, the aqueous solution of the N-methylmorpholine-N-oxide of described spinning bath
Mass percent is preferably 15～20%, owing to selecting the N-methylmorpholine-N-of above-mentioned mass percent
The aqueous solution of oxide, can not only make the regenerated celulose fibre obtained after air bath solidifies
Continue to solidify to improve its intensity and elongation at break, also spinning bath relatively low for mass fraction can be carried out
Enrichment, it is thus achieved that the aqueous solution of the N-methylmorpholine-N-oxide that mass fraction is higher, so that matter
N-methylmorpholine-N-the oxide that amount mark is higher is applicable in abovementioned steps one, is used for disperseing
Pulp, has reached the recycling of the aqueous solution of N-methylmorpholine-N-oxide, this external follow-up water
During washing, it is possible to recycle the aqueous solution of N-methylmorpholine-N-oxide.It addition, right
When in step 2, acquisition spinning solution carries out spinning, the temperature of spinning bath is preferably 20～30 DEG C.
In order to improve the performance of regenerated celulose fibre further, it is preferable that by regenerated celulose fibre
Carry out following process: after regenerated celulose fibre is carried out boundling, carry out successively washing, bleach, on
Oil and drying, wherein, washing can be selected for rinsing machine and washes, and drying can use chain-and-slat drying machine
Drying, the temperature of drying is preferably 100～130 DEG C, and the time of drying is preferably 10～30 minutes.
It addition, bleaching and the mode oiled are conventional method, here is omitted.
The regenerated celulose fibre that the present invention provides can be applied at field of textiles as textile fabric.
The method preparing regenerated celulose fibre that the present invention provides, first carries out pre-preg to pulp,
And squeeze, pulverize, in advance pulp is done a step pretreatment, has been redispersed in N-methylmorpholine-N-oxygen
In the aqueous solution of compound, it is then passed through dipping, spinning, it is thus achieved that regenerated celulose fibre.By this
The method preparing regenerated celulose fibre of bright offer, the quality of the final regenerated celulose fibre obtained
Good, the intensity of such as regenerated celulose fibre is high, and extension at break is suitable, and section morphology is good, same with this
Time, soft smooth.Additionally, the method preparing regenerated celulose fibre that the present invention provides is simple
Convenient, it is simple to operation, repeatable strong, be conducive to large-scale popularization, it is even more important that energy
Enough recycle spinning bath, not only environmental protection, and greatly reduce production cost.
Detailed description of the invention
Below by the present invention is described in detail, the features and advantages of the invention will be said along with these
Bright and become more apparent from, clearly.
In the following embodiments, the reagent, material and the equipment that are used such as do not have special explanation,
It is conventional reagent, conventional material and conventional equipment, the most commercially available, wherein involved former
Expect that each pulp such as also can be obtained by conventional synthesis process synthesis.
In the following embodiments,
Spinning-drawing machine: the spinning head in spinning-drawing machine is circular spinning head, and spray webbing hole count is 38000 holes, spray
The air gap of silk head is 30mm.
The preparation of embodiment regenerated celulose fibre (hereinafter referred to as fiber)
The present invention is further described below by way of instantiation.But these examples are the most exemplary,
Protection scope of the present invention is not constituted any restriction.
The preparation of embodiment 1 fiber 1
(1) pretreatment of pulp, the pretreatment of pulp includes three parts:
Pulp pre-preg, pulp is joined the aqueous solution of N-methylmorpholine-N-oxide is carried out pre-
Dipping；Concrete, the percent mass of the aqueous solution of the N-methylmorpholine-N-oxide used by pre-preg
Number is 50%, and pre-preg temperature is 70 DEG C, and the pre-preg time is 15mim, and the bath raio of pre-preg is
Pulp: the aqueous solution=1:10 of N-methylmorpholine-N-oxide；
Squeezing, squeezes the mixture after pre-preg, removes unnecessary solution, it is thus achieved that have steady
The mixture of fixed composition；Concrete, the component of the mixture after squeezing is pulp, N-methylmorpholine-N-
Oxide and water, its weight ratio is 32:17:45；
Pulverize, the mixture after squeezing is pulverized；Concrete, after pulverizing, mixture particle diameter is
1mm；
(2) mixture that step (1) is obtained is joined the water of N-methylmorpholine-N-oxide
In solution, add antioxidant-propylgallate, and stir 60 minutes at 90 DEG C so that be each
Individual raw material is sufficiently impregnated with, it is thus achieved that premixed liquid, and wherein, N-methylmorpholine-N-oxide is in aqueous
Mass fraction be 68.0%, the gross weight of step (1) obtained mixture and N-methylmorpholine-N-
The ratio 1:20 of the aqueous solution gross weight of oxide, the addition of propylgallate is first fibre gross weight
0.2%；
(3) at 90 DEG C, the premixed liquid obtained is joined thin film evaporation take out very in step (2)
In empty device, evacuation makes vacuum be-0.08MPa, places 10min, and finally each pulp is complete
CL, it is thus achieved that spinning solution, it is thus achieved that spinning solution in first fibre content be 12.1%, viscosity is
14000Pa s, filters the spinning solution obtained, goes the removal of impurity；
(4) at 98 DEG C, carry out in the spinning solution obtained is added spinning-drawing machine in step (3)
Spinning, enters air bath, afterwards with the N-methyl that mass percent is 20% after spinning liquid sprays
The aqueous solution contact of methylmorpholine-N-oxide, the temperature of spinning bath is 20 DEG C, after again separating out, obtains
Obtain regenerated celulose fibre, after then the regenerated celulose fibre of acquisition being carried out boundling, put into rinsing machine
In wash, then carry out successively bleaching, oiling, final choice chain-and-slat drying machine is at 125 DEG C
Dry 12 minutes.
The preparation of embodiment 2 fiber 2
(1) pretreatment of pulp, the pretreatment of pulp includes three parts:
Pulp pre-preg, pulp is joined the aqueous solution of N-methylmorpholine-N-oxide is carried out pre-
Dipping；Concrete, the percent mass of the aqueous solution of the N-methylmorpholine-N-oxide used by pre-preg
Number is 55%, and pre-preg temperature is 65 DEG C, and the pre-preg time is 20mim, and the bath raio of pre-preg is
Pulp: the aqueous solution=1:11 of N-methylmorpholine-N-oxide；
Squeezing, squeezes the mixture after pre-preg, removes unnecessary solution, it is thus achieved that have steady
The mixture of fixed composition；Concrete, the component of the mixture after squeezing is pulp, N-methylmorpholine-N-
Oxide and water, its weight ratio is 30:15:55；
Pulverize, the mixture after squeezing is pulverized；Concrete, after pulverizing, mixture particle diameter is
6mm；
(2) mixture that step (1) is obtained is joined the water of N-methylmorpholine-N-oxide
In solution, add antioxidant-propylgallate, and stir 58 minutes at 92 DEG C so that be each
Individual raw material is sufficiently impregnated with, it is thus achieved that premixed liquid, and wherein, N-methylmorpholine-N-oxide is in aqueous
Mass fraction be 66.9%, the gross weight of step (1) obtained mixture and N-methylmorpholine-N-
The ratio of the aqueous solution gross weight of oxide is 1:18, and the addition of propylgallate is first fibre gross weight
The 0.21% of amount；
(3) at 85 DEG C, the premixed liquid obtained is joined thin film evaporation take out very in step (2)
In empty device, evacuation makes vacuum be-0.089MPa, places 15min, and finally each pulp is complete
CL, it is thus achieved that spinning solution, it is thus achieved that spinning solution in first fibre content be 11.9%, viscosity is
14200Pa s, filters the spinning solution obtained, goes the removal of impurity；
(4) at 99 DEG C, spin in the spinning solution obtained is added spinning-drawing machine in step (3)
Silk, enters air bath, afterwards with the N-methyl that mass percent is 20% after spinning liquid sprays
The aqueous solution contact of quinoline-N-oxide, the temperature of spinning bath is 30 DEG C, after again separating out, it is thus achieved that
Regenerated celulose fibre, puts in rinsing machine after then the regenerated celulose fibre of acquisition being carried out boundling
Washing, then carry out successively bleaching, oiling, final choice chain-and-slat drying machine dries at 128 DEG C
Dry 11 minutes.
The preparation of embodiment 3 fiber 3
(1) pretreatment of pulp, the pretreatment of pulp includes three parts:
Pulp pre-preg, pulp is joined the aqueous solution of N-methylmorpholine-N-oxide is carried out pre-
Dipping；Concrete, the percent mass of the aqueous solution of the N-methylmorpholine-N-oxide used by pre-preg
Number is 60%, and pre-preg temperature is 60 DEG C, and the pre-preg time is 25mim, and the bath raio of pre-preg is
Pulp: the aqueous solution=1:12 of N-methylmorpholine-N-oxide；
Squeezing, squeezes the mixture after pre-preg, removes unnecessary solution, it is thus achieved that have steady
The mixture of fixed composition；Concrete, the component of the mixture after squeezing is pulp, N-methylmorpholine-N-
Oxide and water, its weight ratio is 35:18:45；
Pulverize, the mixture after squeezing is pulverized；Concrete, after pulverizing, mixture particle diameter is
5mm；
(2) mixture that step (1) is obtained is joined the water of N-methylmorpholine-N-oxide
In solution, add antioxidant-propylgallate, and stir 58 minutes at 92 DEG C so that be each
Individual raw material is sufficiently impregnated with, it is thus achieved that premixed liquid, and wherein, N-methylmorpholine-N-oxide is in aqueous
Mass fraction be 60.0%, the gross weight of step (1) obtained mixture and N-methylmorpholine-N-
The ratio of the aqueous solution gross weight of oxide is 1:19, and the addition of propylgallate is first fibre gross weight
The 0.216% of amount；
(3) at 88 DEG C, the premixed liquid obtained is joined thin film evaporation take out very in step (2)
In empty device, evacuation makes vacuum be-0.088MPa, places 20min, and finally each pulp is complete
CL, it is thus achieved that spinning solution, it is thus achieved that spinning solution in first fibre content be 12.2%, viscosity is
14300Pa s, filters the spinning solution obtained, goes the removal of impurity；
(4) at 100 DEG C, carry out in the spinning solution obtained is added spinning-drawing machine in step (3)
Spinning, enters air bath after spinning liquid sprays, is preferably the N-of 15% afterwards with mass percent
The aqueous solution contact of methyhnorpholine-N-oxide, the temperature of spinning bath is 25 DEG C, after again separating out,
Obtain regenerated celulose fibre, after then the regenerated celulose fibre of acquisition being carried out boundling, put into washing
Washing in machine, then carry out successively bleaching, oiling, final choice chain-and-slat drying machine is at 130 DEG C
Lower drying 10 minutes.
The preparation of embodiment 4 fiber 4
(1) pretreatment of pulp, the pretreatment of pulp includes three parts:
Pulp pre-preg, pulp is joined the aqueous solution of N-methylmorpholine-N-oxide is carried out pre-
Dipping；Concrete, the percent mass of the aqueous solution of the N-methylmorpholine-N-oxide used by pre-preg
Number is 65%, and pre-preg temperature is 50 DEG C, and the pre-preg time is 30mim, and the bath raio of pre-preg is
Pulp: the aqueous solution=1:13 of N-methylmorpholine-N-oxide；
Squeezing, squeezes the mixture after pre-preg, removes unnecessary solution, it is thus achieved that have steady
The mixture of fixed composition；Concrete, the component of the mixture after squeezing is pulp, N-methylmorpholine-N-
Oxide and water, its weight ratio is 38:20:50；
Pulverize, the mixture after squeezing is pulverized；Concrete, after pulverizing, mixture particle diameter is
10mm；
(2) mixture that step (1) is obtained is joined the water of N-methylmorpholine-N-oxide
In solution, add antioxidant-propylgallate, and stir 30 minutes at 95 DEG C so that be each
Individual raw material is sufficiently impregnated with, it is thus achieved that premixed liquid, and wherein, N-methylmorpholine-N-oxide is in aqueous
Mass fraction be 67.5%, the gross weight of step (1) obtained mixture and N-methylmorpholine-N-
The ratio of the aqueous solution gross weight of oxide is 1:19, and the addition of propylgallate is first fibre gross weight
The 0.212% of amount；
(3) at 90 DEG C, the premixed liquid obtained is joined thin film evaporation take out very in step (2)
In empty device, evacuation makes vacuum be-0.08MPa, places 20min, and finally each pulp is complete
CL, it is thus achieved that spinning solution, it is thus achieved that spinning solution in first fibre content be 15.0%, viscosity is
15000Pa s, filters the spinning solution obtained, goes the removal of impurity；
(4) at 99 DEG C, spin in the spinning solution obtained is added spinning-drawing machine in step (3)
Silk, enters air bath, afterwards with the N-methyl that mass percent is 17% after spinning liquid sprays
The aqueous solution contact of quinoline-N-oxide, the temperature of spinning bath is 23 DEG C, after again separating out, it is thus achieved that
Regenerated celulose fibre, puts in rinsing machine after then the regenerated celulose fibre of acquisition being carried out boundling
Washing, then carry out successively bleaching, oiling, final choice chain-and-slat drying machine dries at 100 DEG C
Dry 30 minutes.
The preparation of embodiment 5 fiber 5
(1) pretreatment of pulp, the pretreatment of pulp includes three parts:
Pulp pre-preg, pulp is joined the aqueous solution of N-methylmorpholine-N-oxide is carried out pre-
Dipping；Concrete, the percent mass of the aqueous solution of the N-methylmorpholine-N-oxide used by pre-preg
Number is 60%, and pre-preg temperature is 55 DEG C, and the pre-preg time is 20mim, and the bath raio of pre-preg is
Pulp: the aqueous solution=1:15 of N-methylmorpholine-N-oxide；
Squeezing, squeezes the mixture after pre-preg, removes unnecessary solution, it is thus achieved that have steady
The mixture of fixed composition；Concrete, the component of the mixture after squeezing is pulp, N-methylmorpholine-N-
Oxide and water, its weight ratio is 40:15:40；
Pulverize, the mixture after squeezing is pulverized；Concrete, after pulverizing, mixture particle diameter is
15mm；
(2) mixture that step (1) is obtained is joined the water of N-methylmorpholine-N-oxide
In solution, add antioxidant-propylgallate, and stir 20 minutes at 100 DEG C so that
Each raw material is sufficiently impregnated with, it is thus achieved that premixed liquid, and wherein, N-methylmorpholine-N-oxide is at aqueous solution
In mass fraction be 67.2%, the gross weight of step (1) obtained mixture and N-methylmorpholine-N-
The ratio of the aqueous solution gross weight of oxide is 1:19, and the addition of propylgallate is first fibre gross weight
The 1% of amount；
(3) at 80 DEG C, the premixed liquid obtained is joined thin film evaporation take out very in step (2)
In empty device, evacuation makes vacuum be-0.1MPa, places 17min, and finally each pulp is complete
Dissolve, it is thus achieved that spinning solution, it is thus achieved that spinning solution in first fibre content be 10.0%, viscosity is
13000Pa s, filters the spinning solution obtained, goes the removal of impurity；
(4) at 99 DEG C, spin in the spinning solution obtained is added spinning-drawing machine in step (3)
Silk, enters air bath, afterwards with the N-methyl that mass percent is 18% after spinning liquid sprays
The aqueous solution contact of quinoline-N-oxide, the temperature of spinning bath is 27 DEG C, after again separating out, it is thus achieved that
Regenerated celulose fibre, puts in rinsing machine after then the regenerated celulose fibre of acquisition being carried out boundling
Washing, then carry out successively bleaching, oiling, final choice chain-and-slat drying machine dries at 120 DEG C
Dry 15 minutes.
Comparative example
Comparative example 1
Commercially available regenerated celulose fibre, is designated as fiber 1#.
Comparative example 2-6
It is utilized respectively the preparation method such as embodiment 1-5 and prepares fiber, specifically during preparation,
Compared with embodiment 1-5, do not carry out step (1), only carry out step (2), (3), (4),
Respectively obtain regenerated celulose fibre, be designated as fiber 2#-6#.
Test example
According to the method be given in " GB/T 14463-2008 viscose staple fibre " in above-described embodiment
And dry strong, wet strong, the dry elongation at break of fiber that obtains in comparative example and wet elongation at break
Test.After above-mentioned test, detect each fiber institute the results obtained are as follows and state shown in table 1.
Table 1
Test result from above-mentioned table 1, fiber 1-5 and fiber 1# contrasts, is appreciated that: by this
The regenerated celulose fibre that the preparation method that invention provides prepares has the performance of excellence, such as, have
There are higher intensity and elongation at break conveniently.And fiber 1-5 and fiber 2-6# contrasts, permissible
Learning: the pretreatment that the present invention is extra, i.e. with dipping and corresponding squeezing and pulverizing, it is right to be equivalent to
Pulp has done single treatment in advance, and follow-up step coordinates the NMMO being equivalent to use variable concentrations
Aqueous solution carries out after-treatment, and does not carries out pretreatment, directly carries out subsequent step and compares, can make
The regenerated celulose fibre that must prepare has more excellent performance, such as, have higher intensity and more
Suitable elongation at break.
The announcement of book according to the above description, those skilled in the art in the invention can also be to above-mentioned reality
The mode of executing carries out suitable change and amendment.Therefore, the invention is not limited in and be disclosed above and describe
Detailed description of the invention, the right that some modifications and changes of the present invention should also be as falling into the present invention is wanted
In the protection domain asked.
Claims (10)
1. the preparation method of a regenerated celulose fibre, it is characterised in that comprise the following steps:
(1) pretreatment of pulp, joins pulp in the aqueous solution of N-methylmorpholine-N-oxide
Carry out pre-preg, the mixture after pre-preg is squeezed, remove unnecessary solution, it is thus achieved that have
The mixture of stable composition, pulverizes the mixture after squeezing；
(2) mixture that step (1) is obtained is joined the water of N-methylmorpholine-N-oxide
In solution, add antioxidant, and stir；
(3) mixture that step (2) is obtained is inserted in vacuum environment, 80～100 DEG C of conditions
Under, it is thus achieved that spinning solution；
(4) spinning solution being obtained step (3) carries out spinning, it is thus achieved that regenerated celulose fibre,
Wherein during spinning, spinning bath is the aqueous solution of N-methylmorpholine-N-oxide.
The preparation method of regenerated celulose fibre the most according to claim 1, it is characterised in that
In described step (1), the quality of the aqueous solution of the N-methylmorpholine-N-oxide used by pre-preg
Percent is 50-65%, and pre-preg temperature is 50-70 DEG C, and the pre-preg time is 15-30mim, in advance
The bath raio of dipping is pulp: the aqueous solution=1:10-15 of N-methylmorpholine-N-oxide.
The preparation method of regenerated celulose fibre the most according to claim 1, it is characterised in that
In described step (1), the component of the mixture after squeezing is pulp, N-methylmorpholine-N-oxidation
Thing and water, its weight ratio is 30-40:15-20:40-55.
The preparation method of regenerated celulose fibre the most according to claim 1, it is characterised in that
In described step (1), after pulverizing, mixture particle diameter is 1-15mm.
The preparation method of regenerated celulose fibre the most according to claim 1, it is characterised in that
In described step (2), N-methylmorpholine-N-oxide mass percent in aqueous is
60～68%, the mixture that described step (1) is obtained is water-soluble with N-methylmorpholine-N-oxide
The weight ratio of liquid is 1:18-20；Described antioxidant is propylgallate, propylgallate
Addition is the 0.2～1% of the first fibre gross weight contained in described pulp；The temperature of described stirring is
90～100 DEG C, the time is 20～60 minutes.
The preparation method of regenerated celulose fibre the most according to claim 1, it is characterised in that
In described step (3), the vacuum of vacuum environment is-0.1MPa～-0.08MPa, at vacuum ring
The time placed under border is 10～20min.
The preparation method of regenerated celulose fibre the most according to claim 1, it is characterised in that
In described step (3), the first fibre content in described spinning solution is 10～15%, and described spinning is former
The viscosity of liquid is 13000～15000Pa S.
The preparation method of regenerated celulose fibre the most according to claim 1, it is characterised in that
In described step (4), the matter of the aqueous solution of the N-methylmorpholine-N-oxide of described spinning bath
Amount percent is 15～20%, and the temperature of spinning bath is 20～30 DEG C.
The preparation method of regenerated celulose fibre the most according to claim 1, it is characterised in that
In described step (4), when spinning, the spinning solution obtained in step (3) is sprayed by spinning head
Enter air bath after going out, then contact with spinning bath.
10. according to the preparation method of the regenerated celulose fibre described in any one of claim 1 to 9,
It is characterized in that,
Also including step (5), the regenerated celulose fibre being obtained step (4) carries out following place
Reason: after regenerated celulose fibre is carried out boundling, carry out successively washing, bleach, oil and drying,
Wherein, the temperature of drying is 100～130 DEG C, and the time of drying is 10～30 minutes.
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| CN110670163A (en) * | 2019-10-12 | 2020-01-10 | 淮安天然丝纺织科技有限公司 | NMMO solution suitable for cellulose filament fiber and preparation method of cellulose filament fiber using NMMO solution |
| CN114016141A (en) * | 2021-12-09 | 2022-02-08 | 赛得利(常州)纤维有限公司 | Method for preparing fiber spinning solution by direct dissolution method |
| CN115537955A (en) * | 2022-09-27 | 2022-12-30 | 新乡化纤股份有限公司 | NMMO solvent method mycorrhiza regenerated cellulose fiber and preparation method thereof |
| CN116145449A (en) * | 2022-12-29 | 2023-05-23 | 唐山三友集团兴达化纤有限公司 | Lyocell fiber pulp fluffing liquid and preparation method thereof |
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