CN105951199B - The preparation method of regenerated celulose fibre - Google Patents
The preparation method of regenerated celulose fibre Download PDFInfo
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- CN105951199B CN105951199B CN201610424400.4A CN201610424400A CN105951199B CN 105951199 B CN105951199 B CN 105951199B CN 201610424400 A CN201610424400 A CN 201610424400A CN 105951199 B CN105951199 B CN 105951199B
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- spinning
- methylmorpholine
- oxides
- 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
Abstract
The present invention relates to a kind of preparation methods of regenerated celulose fibre, comprise the following steps：Pulp is subjected to pre-preg, and squeezes, crush；The mixture obtained is added in the aqueous solution of N methyl morpholine N oxides, adds in antioxidant, and stir evenly；The mixture obtained is inserted in vacuum environment, under the conditions of 80~100 DEG C, obtains spinning solution；Spinning is carried out to the spinning solution of acquisition, when obtaining regenerated celulose fibre, wherein spinning, spinning bath is the aqueous solution of N methyl morpholine N oxides.By the method provided by the invention for preparing regenerated celulose fibre, the intensity of the regenerated celulose fibre finally obtained is high, and extension at break is suitable, and section morphology is good, soft smooth.In addition, entire method is simple and easy, easy to operation, repeatability is strong, is conducive to promote on a large scale, additionally it is possible to spinning bath is recycled, it is environmentally friendly and of low cost.
Description
Technical field
The invention belongs to textile fabric field more particularly to a kind of preparation methods of regenerated celulose fibre.
Background technology
The regenerated fiber that regenerated celulose fibre is made of cellulose is raw material, structure is cellulose I I.Due to arable land
Reduction and petroleum resources increasingly depleted, natural fiber, the yield of synthetic fibers will be restricted more and more；People
While environmental-protecting performance in paying attention to textile process of consumption, the value of regenerated celulose fibre is re-recognized and sent out
Pick.Nowadays the application of regenerated celulose fibre has obtained a unprecedented opportunity to develop.
The production method of traditional regenerated celulose fibre takes following preparation process：By the pulp of various raw materials in lye
It is middle to impregnate, squeeze, crushing acquisition alkali fiber, then the experienced drop of alkali fiber is gathered into rear and carbon disulfide (CS2) reaction, generate cellulose
Xanthate acid, afterwards, cellulose xanthate are dissolved in lye, form viscous colloidal solution, are then reacted with three component acid baths, system
Obtain regenerated celulose fibre.In this traditional preparation process, it is maximum the defects of be using substantial amounts of CS2And zinc sulfate
(ZnSO4), CS is then released in process of production2And H2S toxic gases, and a large amount of zinc-containing waters are generated, to air and waters
It causes seriously to pollute, the ecological balance is made to be seriously damaged.
In recent years, the green spining technology research on regenerated celulose fibre constantly makes progress, for example with difference
The direct dissolving pulp of dicyandiamide solution, can solve the problems, such as this restriction regenerated celulose fibre benign development.Lyocell fiber
The representative products of green fiber, in the prior art, using pulp as raw material carry out spinning preparation, the product feel obtained compared with
Firmly, fibrillation easily occurs, it is necessary to subsequently increase the technique of processing fibrillation.
The content of the invention
To solve the above-mentioned problems, present inventor has performed further investigation, it turns out that：Pulp is first carried out to a step in advance to locate
Reason, is redispersed in the aqueous solution of N-methylmorpholine-N- oxides, and then by dipping, spinning, it is fine to obtain regenerated cellulose
Dimension, the intensity of the regenerated celulose fibre of acquisition is high, and extension at break is suitable, and section morphology is good, at the same time, soft refreshing
It is sliding, thereby completing the present invention.
The elongation at break of regenerated celulose fibre needs size appropriate, and elongation at break is high, and fabric is also easy to produce deformation,
Fold, the low comfort level that can reduce fabric of elongation at break easily occurs, research shows that the fracture of regenerated celulose fibre is stretched
Long rate fabric effects between 12-16% are best.
It is an object of the invention to provide a kind of preparation method of regenerated celulose fibre, including following four step.
Step 1: the pretreatment of pulp, the pretreatment of pulp includes three parts：
Pulp is added in the aqueous solution of N-methylmorpholine-N- oxides (abbreviation NMMO) and carries out in advance by pulp pre-preg
Dipping；Specifically, in the step 1, the quality percentage of the aqueous solution of the N-methylmorpholine-N- oxides used in pre-preg
Number is 50-65%, and pre-preg temperature is 50-70 DEG C, and the pre-preg time is 15-30mim, and the bath raio of pre-preg is pulp：N- first
Aqueous solution=1 of base methylmorpholine-N-oxide：10-15；
Squeezing, squeezes the mixture after pre-preg, removes extra solution, obtains with the mixing for stablizing composition
Object；Specifically, in the step 1, the component of the mixture after squeezing is pulp, N-methylmorpholine-N- oxides and water,
Its weight ratio is 30-40：15-20：40-55；
It crushes, the mixture after squeezing is crushed；Specifically, in the step 1, mixture grain size after crushing
For 1-15mm.
In above-mentioned steps one, pulp is the dissolving pulp dregs of rice, and pulp methyl fiber content is more than 95%, and content of beary metal is less than
0.07%, degree of polymerization 550-650DP.
And the pretreatment that the present invention is additional, i.e., with dipping and corresponding squeezing and crushing, it is equivalent to and pulp is done in advance
Single treatment and the cooperation of follow-up step are equivalent to carries out after-treatment using the NMMO aqueous solutions of various concentration, can make
Regenerated celulose fibre obtained intensity it is high, extension at break is suitable, and section morphology is good, soft smooth and other effects.
Step 2: the mixture that step 1 is obtained is added in the aqueous solution of N-methylmorpholine-N- oxides, add in
Antioxidant, and stir evenly.
In above-mentioned steps two, the mass percent of N-methylmorpholine-N- oxides in aqueous solution is 60~68%, into
Preferably, the mass percent of N-methylmorpholine-N- oxides in aqueous solution is 60~65% to one step, and the step 1 institute
The weight ratio of the mixture of acquisition and the aqueous solution of N-methylmorpholine-N- oxides is 1：18-20；It is further preferred that weight
The ratio between be preferably pulp mixture：NMMO aqueous solution=1：19.
In above-mentioned steps two, the antioxidant is preferably propylgallate, by antioxidant such as nutgall
After propyl propionate adds in, it can prevent the N-methylmorpholine-N- oxides in aqueous solution from decomposing, so as to influence finally to obtain again
The quality of raw cellulose fibre.In addition, when selecting propylgallate as antioxidant, additive amount is preferably that first is fine total
The 0.2~1% of weight, it is further preferred that the additive amount of propylgallate is preferably the 0.5~1% of first fibre total weight,
Middle first fibre total weight can be understood as the total weight of the first fibre in the pulp.
Pulp is added to be stirred premixing in the aqueous solution of N-methylmorpholine-N- oxides when, stirring when institute
Equipment, time and the temperature conditionss of selection are conventional selection, there is no special demand, as long as by the pulp in N- first
It is uniformly mixed in the aqueous solution of base methylmorpholine-N-oxide.Preferably, the pulp and antioxidant are being added to N- first
After in the aqueous solution of base methylmorpholine-N-oxide, at 90~100 DEG C, stir 20~60 minutes, obtain premixed liquid, it is further excellent
Selection of land, mixing time are 20~40 minutes.Since premixed liquid is at 90~100 DEG C, stir 20~60 minutes so that pulp is in N-
It is fully infiltrated in the aqueous solution of methyhnorpholine-N-oxide, so as to improve the property of the regenerated celulose fibre finally obtained
Can, such as the intensity and elongation at break of regenerated celulose fibre can be improved.
Step 3: the mixture that step 2 is obtained is inserted in vacuum environment, under the conditions of 80~100 DEG C, spun
Silk stock solution.
In above-mentioned steps three, the vacuum degree of vacuum environment is preferably -0.1MPa~-0.08MPa, in this vacuum degree condition
Under, can pulp be completely dissolved.
In above-mentioned steps three, the time that the premixed liquid that is obtained in step 2 is placed in vacuum environment can be according to reality
Demand makes choice, as long as pulp is completely dissolved.Preferably, the time that premixed liquid is placed in vacuum environment for 10~
20min, it is further preferred that the time that premixed liquid is placed in vacuum environment is 10~15min.
The spinning solution of acquisition can be filtered, remove impurity, it is fine to further improve the regenerated cellulose finally obtained
The performance of dimension.
First fibre content in the spinning solution of acquisition is preferably 10~15%, and the viscosity of the spinning solution is preferably
13000~15000PaS.When the first fibre content in above-mentioned spinning solution and viscosity within the above range when, can further carry
The performance for the regenerated celulose fibre that height finally obtains.If first fibre content is too low or excessively high, it is unfavorable for the regeneration finally obtained
The raising of the intensity of cellulose fibre likewise, if viscosity is too low or excessively high, is unfavorable for the regenerated cellulose finally obtained fibre
The raising of the intensity of dimension.
In addition, for more specifically, it is added to premixed liquid is obtained in step 2 in thin film evaporation vacuum extractor, then
It in the case where temperature is 80~90 DEG C, is vacuumized, wherein vacuum degree is -0.1MPa~-0.08MPa, finally so that pulp is complete
Dissolving obtains spinning solution.Maintain spinning solution that can spin state in addition, the spinning solution obtained can be exchanged heat by heat exchanger.
Step 4: spinning, specifically, the spinning that can will be obtained in step 3 are carried out to the spinning solution obtained in step 3
Silk stock solution, which is added in spinning-drawing machine, carries out spinning, and when obtaining regenerated celulose fibre, wherein spinning, spinning bath is N- methyl
Quinoline-N- oxide water solutions.
It is pointed out that spinning bath is located in spinning-drawing machine.
In above-mentioned steps four, after spinning solution is extruded by spinning head, by air bath, then it is in contact with spinning bath
To continue to cure, then it is precipitated, finally obtains regenerated celulose fibre, cured due to initially entering in air bath, then
Spinning bath is selected to continue to cure again, the intensity and fracture that can greatly improve the regenerated celulose fibre finally obtained are stretched
Long rate.It may also be noted that the air gap of spinning head is preferably 15~35mm, it is 20000~30000 holes to select spinneret hole count,
Especially select circular spinning head.Select the detailed process that spinning-drawing machine carries out spinning as follows：Will in step 2 obtain spinning solution by
Circular spinning head sprays, and into air bath, continues to cure into spinning bath afterwards, finally obtains regenerated celulose fibre.
In above-mentioned steps four, the mass percent of the aqueous solution of the N-methylmorpholine-N- oxides of the spinning bath
Preferably 15~20%, the aqueous solution of the N-methylmorpholine-N- oxides due to selecting above-mentioned mass percent can not only make
The regenerated celulose fibre that must be obtained after air bath cures continues to cure to improve its intensity and elongation at break, can also incite somebody to action
The relatively low spinning bath of mass fraction carries out enrichment, obtains the aqueous solution of the higher N-methylmorpholine-N- oxides of mass fraction, from
And N-methylmorpholine-N- the oxides for causing mass fraction higher are applicable in abovementioned steps one, for disperseing pulp, are reached
The recycling of the aqueous solution of N-methylmorpholine-N- oxides has been arrived, in addition during follow-up washing, also recoverable
The aqueous solution of N-methylmorpholine-N- oxides.In addition, when obtaining spinning solution progress spinning in step 2, spinning bath
Temperature is preferably 20~30 DEG C.
In order to further improve the performance of regenerated celulose fibre, it is preferable that regenerated celulose fibre is carried out following place
Reason：After regenerated celulose fibre is carried out boundling, washed, bleached, oiled and dried successively, wherein, it washes and water can be selected
Washing machine is washed, and chain-and-slat drying machine, which can be used, in drying is dried, and the temperature of drying is preferably 100~130 DEG C, drying
Time is preferably 10~30 minutes.In addition, bleaching and the mode to oil are conventional method, details are not described herein again.
Regenerated celulose fibre provided by the invention can be applied as textile fabric in field of textiles.
The method provided by the invention for preparing regenerated celulose fibre first carries out pulp carry out pre-preg, and squeezes, powder
It is broken, step pretreatment has been done to pulp in advance, has been redispersed in the aqueous solution of N-methylmorpholine-N- oxides, then by leaching
Stain, spinning obtain regenerated celulose fibre.It is final to obtain by the method provided by the invention for preparing regenerated celulose fibre
Regenerated celulose fibre quality it is good, such as the intensity of regenerated celulose fibre is high, and extension at break is suitable, and section morphology is good,
At the same time, it is soft smooth.In addition, it is provided by the invention prepare regenerated celulose fibre method it is simple and easy, be convenient for
Operation, repeatability is strong, is conducive to promote on a large scale, it is even more important that spinning bath can be recycled, it is not only environmentally friendly,
And greatly reduce production cost.
Specific embodiment
Below by the present invention is described in detail, the features and advantages of the invention will become more with these explanations
To be clear, clear and definite.
In the following embodiments, reagent, material and the equipment used is as being conventional examination without special explanation
Agent, conventional material and conventional equipment, it is commercially available, wherein for example each pulp of involved raw material can also pass through conventional conjunction
It synthesizes and obtains into method.
In the following embodiments,
Spinning-drawing machine：Spinning head in spinning-drawing machine is circular spinning head, and spinneret hole count is 38000 holes, and the air gap of spinning 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 specific example.But these examples are only exemplary, not to this
The protection domain of invention forms any restrictions.
The preparation of 1 fiber 1 of embodiment
(1) pretreatment of pulp, the pretreatment of pulp include three parts：
Pulp is added in the aqueous solution of N-methylmorpholine-N- oxides and carries out pre-preg by pulp pre-preg；Specifically
, the mass percent of the aqueous solution of the N-methylmorpholine-N- oxides used in pre-preg is 50%, and pre-preg temperature is 70
DEG C, the pre-preg time is 15mim, and the bath raio of pre-preg is pulp：Aqueous solution=1 of N-methylmorpholine-N- oxides：10；
Squeezing, squeezes the mixture after pre-preg, removes extra solution, obtains with the mixing for stablizing composition
Object；Specifically, the component of the mixture after squeezing is pulp, N-methylmorpholine-N- oxides and water, weight ratio 32：17：
45；
It crushes, the mixture after squeezing is crushed；Specifically, mixture grain size is 1mm after crushing；
(2) mixture that step (1) is obtained is added in the aqueous solution of N-methylmorpholine-N- oxides, added in anti-
Oxidant-propylgallate, and stirred 60 minutes at 90 DEG C so that each raw material is sufficiently impregnated, and obtains premixed liquid,
In, the mass fraction of N-methylmorpholine-N- oxides in aqueous solution is 68.0%, and step (1) obtains the total weight of mixture
With the ratio between the aqueous solution total weight of N-methylmorpholine-N- oxides 1：20, the addition of propylgallate is first fibre total weight
0.2%；
(3) at 90 DEG C, the premixed liquid obtained in step (2) is added in thin film evaporation vacuum extractor, is vacuumized
So that vacuum degree is -0.08MPa, 10min is placed, final each pulp is completely dissolved, and obtains spinning solution, and the spinning of acquisition is former
First fibre content in liquid is 12.1%, viscosity 14000Pas, and the spinning solution of acquisition is filtered, and removes impurity；
(4) at 98 DEG C, the spinning solution obtained in step (3) is added in, spinning is carried out in spinning-drawing machine, when spinning solution sprays
Into air bath after going out, contacted afterwards with aqueous solution of the mass percent for 20% N-methylmorpholine-N- oxides, spinning bath
Temperature for 20 DEG C, after being precipitated again, obtain regenerated celulose fibre, then collect the regenerated celulose fibre of acquisition
It is put into rinsing machine and is washed after beam, then bleached, oiled successively, final choice chain-and-slat drying machine dries at 125 DEG C
It is 12 minutes dry.
The preparation of 2 fiber 2 of embodiment
(1) pretreatment of pulp, the pretreatment of pulp include three parts：
Pulp is added in the aqueous solution of N-methylmorpholine-N- oxides and carries out pre-preg by pulp pre-preg；Specifically
, the mass percent of the aqueous solution of the N-methylmorpholine-N- oxides used in pre-preg is 55%, and pre-preg temperature is 65
DEG C, the pre-preg time is 20mim, and the bath raio of pre-preg is pulp：Aqueous solution=1 of N-methylmorpholine-N- oxides：11；
Squeezing, squeezes the mixture after pre-preg, removes extra solution, obtains with the mixing for stablizing composition
Object；Specifically, the component of the mixture after squeezing is pulp, N-methylmorpholine-N- oxides and water, weight ratio 30：15：
55；
It crushes, the mixture after squeezing is crushed；Specifically, mixture grain size is 6mm after crushing；
(2) mixture that step (1) is obtained is added in the aqueous solution of N-methylmorpholine-N- oxides, added in anti-
Oxidant-propylgallate, and stirred 58 minutes at 92 DEG C so that each raw material is sufficiently impregnated, and obtains premixed liquid,
In, the mass fraction of N-methylmorpholine-N- oxides in aqueous solution is 66.9%, and step (1) obtains the total weight of mixture
It is 1 with the ratio between the aqueous solution total weight of N-methylmorpholine-N- oxides：18, the additive amount of propylgallate is first fibre gross weight
The 0.21% of amount；
(3) at 85 DEG C, the premixed liquid obtained in step (2) is added in thin film evaporation vacuum extractor, is vacuumized
So that vacuum degree is -0.089MPa, 15min is placed, final each pulp is completely dissolved, and obtains spinning solution, the spinning of acquisition
First fibre content in stoste is 11.9%, viscosity 14200Pas, and the spinning solution of acquisition is filtered, and removes impurity；
(4) at 99 DEG C, the spinning solution obtained in step (3) is added in, spinning is carried out in spinning-drawing machine, when spinning solution sprays
Into air bath after going out, contacted afterwards with aqueous solution of the mass percent for 20% N-methylmorpholine-N- oxides, spinning bath
Temperature for 30 DEG C, after being precipitated again, obtain regenerated celulose fibre, then collect the regenerated celulose fibre of acquisition
It is put into rinsing machine and is washed after beam, then bleached, oiled successively, final choice chain-and-slat drying machine dries at 128 DEG C
It is 11 minutes dry.
The preparation of 3 fiber 3 of embodiment
(1) pretreatment of pulp, the pretreatment of pulp include three parts：
Pulp is added in the aqueous solution of N-methylmorpholine-N- oxides and carries out pre-preg by pulp pre-preg；Specifically
, the mass percent of the aqueous solution of the N-methylmorpholine-N- oxides used in pre-preg is 60%, and pre-preg temperature is 60
DEG C, the pre-preg time is 25mim, and the bath raio of pre-preg is pulp：Aqueous solution=1 of N-methylmorpholine-N- oxides：12；
Squeezing, squeezes the mixture after pre-preg, removes extra solution, obtains with the mixing for stablizing composition
Object；Specifically, the component of the mixture after squeezing is pulp, N-methylmorpholine-N- oxides and water, weight ratio 35：18：
45；
It crushes, the mixture after squeezing is crushed；Specifically, mixture grain size is 5mm after crushing；
(2) mixture that step (1) is obtained is added in the aqueous solution of N-methylmorpholine-N- oxides, added in anti-
Oxidant-propylgallate, and stirred 58 minutes at 92 DEG C so that each raw material is sufficiently impregnated, and obtains premixed liquid,
In, the mass fraction of N-methylmorpholine-N- oxides in aqueous solution is 60.0%, and step (1) obtains the total weight of mixture
It is 1 with the ratio between the aqueous solution total weight of N-methylmorpholine-N- oxides：19, the addition of propylgallate is first fibre gross weight
The 0.216% of amount；
(3) at 88 DEG C, the premixed liquid obtained in step (2) is added in thin film evaporation vacuum extractor, is vacuumized
So that vacuum degree is -0.088MPa, 20min is placed, final each pulp is completely dissolved, and obtains spinning solution, the spinning of acquisition
First fibre content in stoste is 12.2%, viscosity 14300Pas, and the spinning solution of acquisition is filtered, and removes impurity；
(4) at 100 DEG C, the spinning solution obtained in step (3) is added in, spinning is carried out in spinning-drawing machine, when spinning solution sprays
Into air bath after going out, it is preferably that the aqueous solutions of 15% N-methylmorpholine-N- oxides is contacted with mass percent afterwards, spins
The temperature of silk bath is 25 DEG C, after being precipitated again, obtains regenerated celulose fibre, then by the regenerated celulose fibre of acquisition into
It is put into rinsing machine and is washed after row boundling, then bleached, oiled successively, final choice chain-and-slat drying machine is at 130 DEG C
Lower drying 10 minutes.
The preparation of 4 fiber 4 of embodiment
(1) pretreatment of pulp, the pretreatment of pulp include three parts：
Pulp is added in the aqueous solution of N-methylmorpholine-N- oxides and carries out pre-preg by pulp pre-preg；Specifically
, the mass percent of the aqueous solution of the N-methylmorpholine-N- oxides used in pre-preg is 65%, and pre-preg temperature is 50
DEG C, the pre-preg time is 30mim, and the bath raio of pre-preg is pulp：Aqueous solution=1 of N-methylmorpholine-N- oxides：13；
Squeezing, squeezes the mixture after pre-preg, removes extra solution, obtains with the mixing for stablizing composition
Object；Specifically, the component of the mixture after squeezing is pulp, N-methylmorpholine-N- oxides and water, weight ratio 38：20：
50；
It crushes, the mixture after squeezing is crushed；Specifically, mixture grain size is 10mm after crushing；
(2) mixture that step (1) is obtained is added in the aqueous solution of N-methylmorpholine-N- oxides, added in anti-
Oxidant-propylgallate, and stirred 30 minutes at 95 DEG C so that each raw material is sufficiently impregnated, and obtains premixed liquid,
In, the mass fraction of N-methylmorpholine-N- oxides in aqueous solution is 67.5%, and step (1) obtains the total weight of mixture
It is 1 with the ratio between the aqueous solution total weight of N-methylmorpholine-N- oxides：19, the addition of propylgallate is first fibre gross weight
The 0.212% of amount；
(3) at 90 DEG C, the premixed liquid obtained in step (2) is added in thin film evaporation vacuum extractor, is vacuumized
So that vacuum degree is -0.08MPa, 20min is placed, final each pulp is completely dissolved, and obtains spinning solution, and the spinning of acquisition is former
First fibre content in liquid is 15.0%, viscosity 15000Pas, and the spinning solution of acquisition is filtered, and removes impurity；
(4) at 99 DEG C, the spinning solution obtained in step (3) is added in, spinning is carried out in spinning-drawing machine, when spinning solution sprays
Into air bath after going out, contacted afterwards with aqueous solution of the mass percent for 17% N-methylmorpholine-N- oxides, spinning bath
Temperature for 23 DEG C, after being precipitated again, obtain regenerated celulose fibre, then collect the regenerated celulose fibre of acquisition
It is put into rinsing machine and is washed after beam, then bleached, oiled successively, final choice chain-and-slat drying machine dries at 100 DEG C
It is 30 minutes dry.
The preparation of 5 fiber 5 of embodiment
(1) pretreatment of pulp, the pretreatment of pulp include three parts：
Pulp is added in the aqueous solution of N-methylmorpholine-N- oxides and carries out pre-preg by pulp pre-preg；Specifically
, the mass percent of the aqueous solution of the N-methylmorpholine-N- oxides used in pre-preg is 60%, and pre-preg temperature is 55
DEG C, the pre-preg time is 20mim, and the bath raio of pre-preg is pulp：Aqueous solution=1 of N-methylmorpholine-N- oxides：15；
Squeezing, squeezes the mixture after pre-preg, removes extra solution, obtains with the mixing for stablizing composition
Object；Specifically, the component of the mixture after squeezing is pulp, N-methylmorpholine-N- oxides and water, weight ratio 40：15：
40；
It crushes, the mixture after squeezing is crushed；Specifically, mixture grain size is 15mm after crushing；
(2) mixture that step (1) is obtained is added in the aqueous solution of N-methylmorpholine-N- oxides, added in anti-
Oxidant-propylgallate, and stirred 20 minutes at 100 DEG C so that each raw material is sufficiently impregnated, and obtains premixed liquid,
In, the mass fraction of N-methylmorpholine-N- oxides in aqueous solution is 67.2%, and step (1) obtains the total weight of mixture
It is 1 with the ratio between the aqueous solution total weight of N-methylmorpholine-N- oxides：19, the addition of propylgallate is first fibre gross weight
The 1% of amount；
(3) at 80 DEG C, the premixed liquid obtained in step (2) is added in thin film evaporation vacuum extractor, is vacuumized
So that vacuum degree is -0.1MPa, 17min is placed, final each pulp is completely dissolved, and obtains spinning solution, and the spinning of acquisition is former
First fibre content in liquid is 10.0%, viscosity 13000Pas, and the spinning solution of acquisition is filtered, and removes impurity；
(4) at 99 DEG C, the spinning solution obtained in step (3) is added in, spinning is carried out in spinning-drawing machine, when spinning solution sprays
Into air bath after going out, contacted afterwards with aqueous solution of the mass percent for 18% N-methylmorpholine-N- oxides, spinning bath
Temperature for 27 DEG C, after being precipitated again, obtain regenerated celulose fibre, then collect the regenerated celulose fibre of acquisition
It is put into rinsing machine and is washed after beam, then bleached, oiled successively, final choice chain-and-slat drying machine dries at 120 DEG C
It is 15 minutes dry.
Comparative example
Comparative example 1
Commercially available regenerated celulose fibre is denoted as fiber 1#.
Comparative example 2-6
It is utilized respectively the preparation method of embodiment 1-5 such as and prepares fiber, specifically during preparation, with embodiment 1-5
It compares, without step (1), only carries out step (2), (3), (4), respectively obtain regenerated celulose fibre, be denoted as fiber 2#-
6#。
Test example
According to《GB/T 14463-2008 viscose staple fibres》In the method that provides in above-described embodiment and in comparative example
Dry strong, wet strong, the dry elongation at break of the fiber of acquisition and wet elongation at break are tested.After above-mentioned test, detection
The results obtained are as follows states shown in table 1 for each fiber institute.
Table 1
Test result from above-mentioned table 1, fiber 1-5 and fiber 1# are compared, can learnt：Preparation provided by the present invention
The regenerated celulose fibre that method is prepared has excellent performance, such as is stretched with higher intensity and convenient fracture
Long rate.And fiber 1-5 and fiber 2-6# is compared, and can be learnt：The additional pretreatment of the present invention, i.e., with dipping and corresponding pressure
Squeeze and crush, be equivalent to pulp has been done in advance single treatment and follow-up step cooperation be equivalent to using various concentration
NMMO aqueous solutions carry out after-treatment, with without pretreatment, directly carrying out subsequent step and comparing, can cause regeneration obtained
Cellulose fibre has more excellent performance, such as with higher intensity and elongation at break preferably.
The announcement of book according to the above description, those skilled in the art in the invention can also carry out the above embodiment
Appropriate change and modification.Therefore, the invention is not limited in specific embodiment disclosed and described above, to the present invention's
Some modifications and changes should also be as falling into the scope of the claims of the present invention.
Claims (8)
1. a kind of preparation method of regenerated celulose fibre, which is characterized in that comprise the following steps：
（1）Pulp is added in the aqueous solution of N-methylmorpholine-N- oxides and carries out pre-preg, to pre- by the pretreatment of pulp
Mixture after dipping is squeezed, and removes extra solution, is obtained with the mixture for stablizing composition, to the mixing after squeezing
Object crushes；Wherein, the mass percent of the aqueous solution of the N-methylmorpholine-N- oxides used in pre-preg is 50 ~ 65%,
Pre-preg temperature is 50 ~ 70 DEG C, and the pre-preg time is 15 ~ 30min, and the bath raio of pre-preg is pulp：N-methylmorpholine-N- is aoxidized
Aqueous solution=1 of object：10~15；The component of mixture after squeezing be pulp, N-methylmorpholine-N- oxides and water, weight
Than for 30 ~ 40：15~20：40~55；
（2）By step（1）The mixture obtained is added in the aqueous solution of N-methylmorpholine-N- oxides, is added in anti-oxidant
Agent, and stir evenly；
（3）By step（2）The mixture obtained is inserted in vacuum environment, under the conditions of 80 ~ 100 DEG C, obtains spinning solution；
（4）To step（3）The spinning solution obtained carries out spinning, when obtaining regenerated celulose fibre, wherein spinning, spinning bath
For the aqueous solution of N-methylmorpholine-N- oxides.
2. the preparation method of regenerated celulose fibre according to claim 1, which is characterized in that in the step（1）In,
Mixture grain size is 1 ~ 15mm after crushing.
3. the preparation method of regenerated celulose fibre according to claim 1, which is characterized in that in the step（2）In,
The mass percent of N-methylmorpholine-N- oxides in aqueous solution is 60 ~ 68%, the step（1）The mixture that is obtained with
The weight ratio of the aqueous solution of N-methylmorpholine-N- oxides is 1：18~20；The antioxidant is propylgallate, is not eaten
The additive amount of sub- propyl propionate is the 0.2 ~ 1% of the first fibre total weight contained in the pulp；The temperature of the stirring is 90 ~ 100
DEG C, the time is 20 ~ 60 minutes.
4. the preparation method of regenerated celulose fibre according to claim 1, which is characterized in that in the step（3）In,
The vacuum degree of vacuum environment is -0.1MPa~-0.08MPa, and the time placed under vacuum conditions is 10 ~ 20min.
5. the preparation method of regenerated celulose fibre according to claim 1, which is characterized in that in the step（3）In,
First fibre content in the spinning solution is 10 ~ 15%, and the viscosity of the spinning solution is 13000 ~ 15000PaS.
6. the preparation method of regenerated celulose fibre according to claim 1, which is characterized in that in the step（4）In,
The mass percent of the aqueous solution of the N-methylmorpholine-N- oxides of the spinning bath is 15 ~ 20%, and the temperature of spinning bath is
20~30℃。
7. the preparation method of regenerated celulose fibre according to claim 1, which is characterized in that in the step（4）In,
In spinning, step（3）The spinning solution of middle acquisition enters air bath after being sprayed by spinning head, is then contacted with spinning bath.
8. the preparation method of regenerated celulose fibre according to any one of claims 1 to 7, which is characterized in that
Further include step（5）, to step（4）The regenerated celulose fibre obtained carries out following processing：Regenerated cellulose is fine
After dimension carries out boundling, washed, bleached, oiled and dried successively, wherein, the temperature of drying is 100 ~ 130 DEG C, drying when
Between be 10 ~ 30 minutes.
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