CN110080010A - A kind of preparation method of colored fibre element fiber - Google Patents
A kind of preparation method of colored fibre element fiber Download PDFInfo
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- CN110080010A CN110080010A CN201910142338.3A CN201910142338A CN110080010A CN 110080010 A CN110080010 A CN 110080010A CN 201910142338 A CN201910142338 A CN 201910142338A CN 110080010 A CN110080010 A CN 110080010A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/30—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using sulfur dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/38—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/6025—Natural or regenerated cellulose using vat or sulfur dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/62—Natural or regenerated cellulose using direct dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/66—Natural or regenerated cellulose using reactive dyes
Abstract
The present invention relates to a kind of colored fibre element fibers and preparation method thereof, the preparation method comprises the following steps: cellulosic fibre spinning solution is squeezed out through spinning head, solidification, it stretches and washing silk is made in washing, temperature >=90 DEG C of washing, reusing temperature is that 40~90 DEG C of aqueous dye solutions handle washing silk, it finally carries out rinsing and colored fibre element fiber is made in drying, the temperature of rinsing is 20~40 DEG C, dyestuff contains X, one or more of Y and Z group, X, Y and Z group correspond to be formed the group of covalent bond with cellulose hydroxyl group, it is capable of the group of self-crosslinking reaction and the group of hydrogen bond can be formed with cellulose hydroxyl group.The quality of dyestuff is the 0.1~5.0% of cellulosic fibre substrate quality in colored fibre element fiber, and wash durability is excellent.The method of the present invention is simple and easy, and the durability of colored fibre element fiber is good.
Description
Technical field
The invention belongs to colored fibre manufacturing technology field, it is related to a kind of colored fibre element fiber and preparation method thereof.
Background technique
Cellulose fibre have natural reproducible resources advantage and it is comfortable and easy to wear, non-toxic sanitary is healthy and junk can drop
The advantages that solution, therefore, cellulose fibre, are used as the mainstream raw material of textile for a long time, lasting.However, due to native cellulose
Fiber such as cotton, numb Isoquant are limited, it is impossible to meet consumption demand, people often with natural cellulosic materials for example cotton linter, timber,
Bamboo and straw etc. are that raw material prepares regenerated celulose fibre, to reach effective use natural material and improve cellulose fibre
Supply purpose.And with the development of consumption demand, people not only increase the demand of cellulose fibre, but also require
Fibre kind, color and style varied allow it to the different demands for meeting different crowd, therefore to the product of fiber
More stringent requirements are proposed for matter, dyeability etc..
Currently, the method for preparing colored fibre cellulose fiber have it is several: first is that stoste additive process, i.e., the dyestuff in spinning solution,
Spinning preparation has colored fibre, and this method is to produce the relatively conventional technical method of colored regenerated cellulose fiber, dyeing effect
Fruit is significant, but there is also disadvantages: 1) dyestuff be easy to remain in the extrusion that fiber is influenced in spinning equipment and solidification washing system and
Forming and recycled solvent；2) degree of scatter of dyestuff and additive amount can have an adverse effect to mechanical property of fiber etc.；
3) the upper batch replacement of production is not flexible, and transition silk is more, increases production cost；Second is that fiber or fabric post treatment method, this method pair
Natural fiber and regenerated fiber are all general, advantage be batch is changeable, production conversion flexibly and adapted breed is more, but disadvantage
Be: 1) general processing method may lead to the problem of durability difference；2) while final finishing is to fiber or textile dyeing,
The feel, flexibility and gas permeability that often will affect fiber and fabric, even result in fiber or fabric is shunk；3) finished product
Microstructure fiber it is fine and close, post-process it is main fiber surface occurs, can additional dyestuff it is limited, influence dyeing effect, or
Person be swollen or activate raising reactivity, and subsequent reactions or processing solvent still need to handle, undoubtedly increase process and
Processing cost etc..
Therefore, a kind of extrusion for not influencing fiber and forming and the good colored fibre element fiber and its system of durability are studied
Preparation Method has a very important significance.
Summary of the invention
The purpose of the invention is to overcome above-mentioned problems of the prior art, providing one kind does not influence squeezing for fiber
Out and forming and the good colored fibre element fiber and preparation method thereof of durability.
In order to achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of preparation method of colored fibre element fiber, cellulosic fibre spinning solution is squeezed out through spinning head, is solidified,
Stretch and washing be made washing silk, then with aqueous dye solutions to washing silk handle after carry out rinse and drying coloured fibre is made
Tie up plain fiber；
Temperature >=90 DEG C of washing, the temperature of aqueous dye solutions is 40~90 DEG C when processing, the temperature root of aqueous dye solutions
Depending on the reaction activity of dyestuff, reaction activity Gao Shangran temperature is 40 DEG C or so, reacts the lower upper dye temperature of activity
Respectively 80~90 DEG C, the temperature of rinsing is 20~40 DEG C, and the temperature of aqueous dye solutions is greater than the temperature of rinsing when processing；Washing
Temperature, treatment temperature and rinse temperature three cooperate, and so that fibrous inside is first generated microcellular structure, then in conjunction with dyestuff, then
It shrinks, dyestuff is wrapped in fibrous inside；Method of the invention has both the advantages of stoste additive process and finishing method, simultaneously
The shortcomings that effectively preventing both methods again, great popularization；
For dyestuff containing one or more of X group, Y group and Z group, X group is that can be formed with cellulose hydroxyl group covalently
The group of key, Y group are the group for capableing of self-crosslinking reaction, and Z group is the group that hydrogen bond can be formed with cellulose hydroxyl group.
As a preferred technical scheme:
A kind of preparation method of colored fibre element fiber as described above, the concentration of cellulosic fibre spinning solution are 5
~25wt%, with the increase of concentration of dope, the diffusion coefficient of whole system is reduced, therefore concentration of dope is to spinning process
In mutually separation can have an impact, cellulosic fibre concentration of dope of the invention can appropriate adjustment, but should not too, spinning
Liquid concentration is too low, may not undergo phase transition, and can not form fiber, or has and also only form loose uneven texture when phase transformation,
Make the mechanical properties decrease of fiber；Excessive concentration is equivalent to carry out dry spinning, forms fine and close structure, is unfavorable for subsequent
Dyeing；Cellulosic fibre is regenerated celulose fibre or cellulose derivative fibres.
A kind of preparation method of colored fibre element fiber as described above, cellulosic fibre are viscose rayon, vinegar ester
Fiber, Lyocell fiber, copper ammonia fiber, the regenerated cellulose fiber prepared by solvent of ionic liquid with aqueous slkali are
The regenerated cellulose fiber of solvent preparation.Colored fibre element fiber of the invention includes but are not limited to this, can be with
For containing microcellular structure and being capable of other regenerated celulose fibres or fiber in above-mentioned treatment process in conjunction with above-mentioned dyestuff
Plain derivant fiber.
A kind of preparation method of colored fibre element fiber as described above, the termination condition of washing are as follows: wash containing for silk
Water is 40~70wt%, the present invention wash silk water content can appropriate adjustment, but should not too, water content is too low, then fiber
Drying has been carried out, internal capillary quantity is reduced, and micro-pore diameter reduces, and unfavorable and subsequent dyeing is unfavorable for dyestuff and enters fibre
Dimension is internal；Water content is high, although not densifying, there are a large amount of water in micropore, has certain pressure difference, same meeting with the external world
It is unfavorable for dyestuff and enters fibrous inside；The crystallinity of silk is washed less than 15%, micropore average diameter is 10~200 nanometers, micropore
The percentage that volume accounts for washing silk total volume is 10~30%, and washing silk crystallinity is low and has more loose microcellular structure,
Be conducive to the entrance of dyestuff.
A kind of preparation method of colored fibre element fiber as described above, X group are aldehyde radical, cyano, epoxy group, acyl
Cl radical, acid anhydrides or diisocyanate；Y group is siloxanes；Z group is sulfonic acid group or sulfate group.
A kind of preparation method of colored fibre element fiber as described above, the mass content of dyestuff is in aqueous dye solutions
2~10wt%；Since different dyestuffs itself structure is different, diffuse into that fibrous inside content is different, selection it is dense
Degree is different, and for different dyestuffs, the concentration used can be selected suitably within the above range or suitably be adjusted outside above range
It is whole, but should not too, the mass content of dyestuff is too small, even if fully entering fiber, the dyeing effect being also unable to reach, therefore
Content cannot be too low；Again due to the amount that for a certain amount of fiber, can enter internal dyestuff be it is certain, in aqueous solution
The mass content of dyestuff is too high and will cause waste, therefore content cannot be too high；Due also to dyestuff is liable to stick to fiber surface
And removed during subsequent rinse, have an adverse effect to dyeing effect, therefore, in order to ensure that (dye-uptake can for final dyeing effect
Up to 80% or more), the lower quality content of dyestuff is controlled 2% in aqueous dye solutions；
Dyestuff is more than one of direct dyes, reactive dye and sulfur dye, only enumerates some common dyestuffs herein,
Other, which meet " one or more of containing X group, Y group and Z group " and are dissolved in the dyestuff of water, is suitable for the present invention.
A kind of preparation method of colored fibre element fiber as described above, processing is by the way of impregnating or spraying, place
The time of reason is 60~600 seconds, and due to different dyestuffs, itself structure is different, diffuses into the fibrous inside time not
Together, therefore, for different dyestuffs, the processing time can suitably select within the above range or suitably adjust outside above range
It is whole, but should not too, the time is too short, then enters not comprehensively, keep dyeing effect bad, dyeing is uneven；Time is too long, at this moment
Between before arrive dyeing up to balance, waste time；The time of rinsing is 120~600 seconds.
A kind of preparation method of colored fibre element fiber as described above, dry by the way of hot-air drying, heat
The temperature of air is 105~160 DEG C, the dry temperature of the present invention can appropriate adjustment, but should not too, temperature is too low, can not make
Fiber moisture content reaches defined requirement, and it is insufficient to react progress；Temperature is too high, fiber can be made to have biggish curling, very
It may extremely make small part that carbonization occur and decompose blackening, adverse effect can be caused to fibre property；The dry water content for being dried to fiber <
15wt%, the water content of fiber of the present invention are to reach one to guarantee fiber abundant compacting by drying in 15wt% or less
As cellulose fibre using effect.
The present invention also provides using coloured fibre made from a kind of preparation method of colored fibre element fiber as described above
Plain fiber is tieed up, mainly by cellulosic fibre matrix and the intracorporal dyestuff of cellulosic fibre base is dispersed in and forms；Work as dye
When in material containing that can roll into a ball the group combined with cellulose base, on the one hand dyestuff passes through the group and cellulosic fibre of its own
Combination power between the group of matrix is fixed in cellulose fibre matrix, on the other hand passes through cellulosic fibre matrix
The embedding effect of internal micropore is fixed in cellulose fibre matrix；When being combined in dyestuff without can be rolled into a ball with cellulose base
When group, the embedding effect for the micropore for mainly passing through cellulosic fibre intrinsic silicon is fixed on cellulose fibre matrix
It is interior, can also have excellent wash durability.
As a preferred technical scheme:
Colored fibre element fiber as described above, crystallinity > 30% of colored fibre element fiber contain micropore, micropore
Average diameter is 5~50 nanometers, and the quality of dyestuff (remarks: dyes deep for the 0.1~5.0% of cellulosic fibre substrate quality
Shallow different, dye content is different, and when the depth of dye, dye content is high, conversely, then anti-)；Compared with prior art, the present invention washes
There are many micropore in rear fiber, so that the diffusion of dyestuff is adsorbed fast and be able to enter fibrous inside, then by after compacting by drying,
Dyestuff reacts with cellulose fibre, and the dyestuff of more content can anchor at the inside of cellulosic fibre matrix, dyestuff
Quality be cellulosic fibre substrate quality 0.1~5.0%, improve the durability of colored fibre element fiber.
The filament number of colored fibre element fiber is 0.5~5.0dtex, and breaking strength is 1.0~4.5cN/dtex, is broken
Splitting elongation is 5%~20%, and regain is 5%~15%, and washing color fastness is equal to 5 grades, and colour fastness to rubbing is equal to 5
Grade；
After colored fibre element fiber washs 50 times, the quality of dyestuff be cellulosic fibre substrate quality 0.08~
2.50%, washing color fastness is more than or equal to 4 grades, and colour fastness to rubbing is more than or equal to 4 grades；Compared with prior art, of the invention
Colored fibre element fiber washing fastness obtained is high, and durability is good, and dyeing effect is good；
Colored fibre element fiber be long filament, short silk or tow, for knitted fabric, woven fabric, non-woven fabrics or and other
It is fiber blended.
Invention mechanism:
Firstly, the present invention squeezes out cellulosic fibre spinning solution through spinning head, solidification, stretches and wash obtained washing
On the one hand silk, temperature >=90 DEG C of washing make the washing silk crystallinity to be formed low and have more loose microcellular structure, separately
On the one hand, diffusion velocity can be accelerated, accelerate washing, the coagulating bath equal solvent such as NMMO etc. for making to remain in inside washing silk can
It diffuses into water, reduces influence of the solvent to dyestuff and take a long time if wash temperature is too low to remove in fiber
Solvent, and residual quantity is more；
Then, the present invention is handled washing silk with aqueous dye solutions, and the temperature of processing is 40~90 DEG C, and washing silk exists
Microcellular structure is kept in the aqueous solution of 40~90 DEG C of temperature, and guarantees dyestuff solubility with higher, is diffused into using dyestuff
Enter to wash inside silk, compared to handling at normal temperature, the aqueous dye solutions processing time can be shortened, dyestuff is enable to rapidly enter fibre
Dimension is internal, and reaches diffusion balance within a short period of time, can carry out the processing of next step rinsing, temperature is excessively high, good to diffusivity
Dyestuff for, dyestuff is easy dye-uptake can be made to decline instead to external diffusion；
Finally, the present invention is to treated, washing silk rinses and dries obtained colored fibre element fiber, rinsing
Temperature is 20~40 DEG C, so that the micropore of cellulosic fibre is shunk, fiber porousness reduces, and is going for the rinsing of lower temperature
Except surface adhesion dyestuff while retain fibrous inside dyestuff, the temperature of rinsing is lower, will not due to inside and outside concentration difference and
It diffuses out internal dyestuff rapidly, will not make cellulose fibre dye inside is washed to come out, heating can also be saved
The energy, if temperature is excessively high, internal non-reacted parts dyestuff is easy to be washed out together, and fiber is in the drying process into one
Step crystallization, densification, micropore shrink, dyestuff are embedded in cellulosic fibre matrix, colored fibre element fiber is improved
Durability, especially water-wash resistance, while again since dyestuff is containing one or more of X group, Y group and Z group, with fibre
Tieing up between plain fiber macromolecular has the combination for further improving dyestuff and cellulosic fibre matrix compared with strong interaction steady
It is qualitative, the good colored fibre element fiber of durability has been made.
The temperature of fiber of the invention through using when the techniques such as washing, dye liquor dyeing and rinsing becomes in what is gradually reduced
Gesture, the first washing temperature more than or equal to 90 DEG C accelerate sovent diffusion speed, and remaining solvent in as-spun fibre can be made rapid
Washing go out, to solvent and dyestuff will not be made in the follow-up process to interact, impact effect is simultaneously greater than equal to
90 DEG C of washing temperature also increases fibrous inside hole, is conducive to the entrance of dyestuff, then uses 40~90 DEG C in dyeing
Temperature enable the microcellular structure of fiber surface be always maintained at washing after rarefaction, accelerate dye molecule and pass through fiber
Surface hole defect penetrates into the speed of fibrous inside, enables to dye molecule to rapidly enter fibrous inside, and reach within a short period of time
To balance, and then dyeing time is shortened, while at this temperature, dyestuff will not be made to react acute in water because temperature is excessively high
It is strong that dyestuff is caused to reduce.Then under subsequent lower rinse temperature, fibrous inside hole is shunk, surface unreacted can be washed away
Dyestuff without washing away fibrous inside dye molecule, keep enough and uniformly contaminate so as to internal in the fibre
Material, washing, aqueous dye solutions processing and the mutual cooperation of rinsing three's temperature, significantly improves the endurance quality of colored fibre
And mechanical performance.
In addition, the temperature that the aqueous dye solutions of the application are handled is 40~90 DEG C, the dissolution journey of dyestuff in water can guarantee
Degree is high and solution rate is fast, dissolves dyestuff rapidly and can diffuse into fiber with faster rate, moreover, in less than 40 DEG C feelings
It is dyed under condition, the product colour obtained after dyeing may be made shallow and unglazed, sun-proof degree also declines.
Beneficial effect
(1) preparation method of a kind of colored fibre element fiber of the invention carries out dyeing processing preparation using washing silk
Durability colored fibre element fiber, does not need that dyestuff is added before spinning, does not influence to squeeze out and shape, dyestuff will not influence solidifying
Solid water washes the recycling of solvent, does not influence existing spinning technique, and method is flexible, is both suitable for producing in enormous quantities, is also suitble to small
In batches, multi-item production；
(2) preparation method of a kind of colored fibre element fiber of the invention carries out dyeing processing preparation using washing silk
Durability colored fibre element fiber is handled using the open structure of washing silk, and dyestuff diffusion is fast, high production efficiency；
(3) preparation method of a kind of colored fibre element fiber of the invention carries out the Low Drift Temperature that temperature is 20~40 DEG C
The densification washed and dried is firmly combined dyestuff and fiber, improves fastness to washing；
(4) preparation method of a kind of colored fibre element fiber of the invention, durability is good, and dyeing effect is significant, washable
Fastness is high, and application prospect is good.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed range.
Embodiment 1
A kind of preparation method of colored fibre cellulose fiber, steps are as follows:
(1) degree of polymerization is 500, concentration is 20wt% viscose rayon spinning solution is squeezed out through spinning head, solidification, stretch and
Washing silk is made in 95 DEG C of washing, and the water content for washing silk is 60wt%；
(2) again with the mass content of direct scarlet 4BE be 1.5wt% aqueous solution 80 DEG C at a temperature of to washing silk into
After 200 seconds immersion treatments of row 30 DEG C at a temperature of rinsing 35 seconds and by the way of being dried using hot-air in 130 DEG C of temperature
The water content of lower drying to fiber is that colored fibre cellulose fiber is made in 10wt%.
The crystallinity of final colored fibre cellulose fiber obtained is 40%, contains micropore, and micropore average diameter is 20 nanometers,
The quality of direct dyes is the 2.0% of cellulose fibre matrix quality.
The filament number of colored fibre cellulose fiber is 2.5dtex, breaking strength 2.5cN/dtex, and elongation at break is
15%, regain 10%, after washing 50 times, the quality of direct dyes is the 1.6% of cellulosic fibre substrate quality, water-fast
Washing color fastness is 4-5 grades, and colour fastness to rubbing is 4-5 grades；
Colored fibre cellulose fiber is long filament, can be used for knitted fabric, woven fabric, non-woven fabrics or fiber blended with other.
Comparative example 1
A kind of preparation method of colored fibre cellulose fiber, it is substantially the same manner as Example 1, the difference is that, in step (1)
The temperature of washing is 88 DEG C, and the crystallinity of colored fibre cellulose fiber obtained is 38%, contains micropore, and micropore average diameter is received for 18
Rice, the quality of direct scarlet 4BE are the 1.7% of cellulose fibre matrix quality, filament number 2.4dtex, and breaking strength is
2.4cN/dtex, elongation at break 17%, regain 11%, after washing 50 times, the quality of direct scarlet 4BE is cellulose
The 0.09% of fiber substrate quality, washing color fastness are 3 grades, and colour fastness to rubbing is 3 grades.
Comparative example 2
A kind of preparation method of colored fibre cellulose fiber, it is substantially the same manner as Example 1, the difference is that, in step (2)
The temperature of immersion treatment is 35 DEG C, and the crystallinity of colored fibre cellulose fiber obtained is 39%, contains micropore, and micropore average diameter is
19 nanometers, the quality of direct scarlet 4BE is 1.6%, filament number 2.5dtex of cellulose fibre matrix quality, and fracture is strong
Degree is 2.5cN/dtex, and elongation at break 18%, regain 9%, after washing 50 times, the quality of direct scarlet 4BE is fibre
The 0.1% of plain fiber substrate quality is tieed up, washing color fastness is 3 grades, and colour fastness to rubbing is 3 grades.
Comparative example 3
A kind of preparation method of colored fibre cellulose fiber, it is substantially the same manner as Example 1, the difference is that, in step (2)
The temperature of rinsing is 46 DEG C, and the crystallinity of colored fibre cellulose fiber obtained is 36%, contains micropore, and micropore average diameter is received for 17
Rice, the quality of direct scarlet 4BE are the 1.5% of cellulose fibre matrix quality, filament number 2.3dtex, and breaking strength is
2.4cN/dtex, elongation at break 16%, regain 9%, after washing 50 times, the quality quality of direct scarlet 4BE is fibre
The 0.11% of plain fiber substrate quality is tieed up, washing color fastness is 3 grades, and colour fastness to rubbing is 3 grades.
To sum up, comparative example 1~3 and embodiment 1 are compared, it can be seen that in washing, higher washing temperature makes molten
Agent diffusion velocity is accelerated, and remaining solvent in as-spun fibre can be made rapidly to wash away, to will not make in the follow-up process
Solvent and dyestuff interact, impact effect, while higher temperature also increases fibrous inside hole, is conducive to dyestuff
Entrance；In dyeing, secondary temperature can enable the microcellular structure of fiber surface be always maintained at the rarefaction after washing, accelerate
Dye molecule penetrates into the speed of fibrous inside by fiber surface hole, and dye molecule is enabled to rapidly enter in fiber
Portion, and reach balance within a short period of time, and then shorten dyeing time, while at this temperature, it will not be excessively high because of temperature
And reacting dyestuff in water acutely causes dyestuff to reduce；In rinsing, under lower rinse temperature, fibrous inside hole is received
Contracting, washes away the unreacted dyestuff in surface without wash away fibrous inside dye molecule, fibrous inside keep it is enough and
Uniform dyestuff just makes the present invention just because of rinsing, washing and the mutual cooperation of aqueous dye solutions treatment temperature three
The durability and dyeability of colored fibre cellulose fiber obtained are fully enhanced.
Comparative example 4
A kind of preparation method of colored fibre cellulose fiber, it is substantially the same manner as Example 1, the difference is that, step (2) is right
It is directly dried after fiber immersion treatment without rinsing, the crystallinity of colored fibre cellulose fiber obtained is 38%, is contained
Micropore, micropore average diameter are 18 nanometers, and the quality of direct scarlet 4BE is the 1.4% of cellulose fibre matrix quality, and monofilament is fine
Spending is 2.5dtex, breaking strength 2.5cN/dtex, elongation at break 16%, regain 10%, after washing 50 times, directly
The quality for meeting bright red 4BE is the 0.1% of cellulosic fibre substrate quality, and washing color fastness is 3 grades, and colour fastness to rubbing is
3 grades.Comparative example 4 and embodiment 1 are compared, it can be seen that just because of rinse step is additionally arranged, in lower rinse temperature
Under, fibrous inside hole is shunk, fibrous inside dye molecule will not be made to wash away, fibrous inside is made to keep enough and equal
Even dyestuff is fully enhanced the durability of colored fibre cellulose fiber produced by the present invention and dyeability.
Embodiment 2
A kind of preparation method of colored fibre cellulose fiber, steps are as follows:
(1) the Lyocell fiber spinning solution that the degree of polymerization is 200, concentration is 5wt% squeezed out through spinning head, solidification, stretched
Washing silk is made in washing with 90 DEG C, and the water content for washing silk is 40wt%；
(2) again with the mass content of active red A-2BF be 0.5wt% aqueous solution 40 DEG C at a temperature of to washing silk into
After 5 seconds immersion treatments of row 20 DEG C at a temperature of rinsing 10 seconds and using hot-air dry by the way of 105 DEG C at a temperature of
The dry water content to fiber is that colored fibre cellulose fiber is made in 10wt%.
The crystallinity of final colored fibre cellulose fiber obtained is 35%, contains micropore, micropore average diameter is 5 nanometers, living
Property dyestuff quality be cellulose fibre matrix quality 0.1%.
The filament number of colored fibre cellulose fiber is 2.6dtex, breaking strength 4.5cN/dtex, and elongation at break is
20%, regain 5%, after washing 50 times, the quality of reactive dye is the 0.08% of cellulosic fibre substrate quality, water-fast
Washing color fastness is 4 grades, and colour fastness to rubbing is 4 grades；
Colored fibre cellulose fiber is short silk, can be used for knitted fabric, woven fabric, non-woven fabrics or fiber blended with other.
Embodiment 3
A kind of preparation method of colored fibre cellulose fiber, steps are as follows:
(1) the acetate fiber spinning solution that the degree of polymerization is 300, esterification degree 2.35, concentration are 25wt% is squeezed through spinning head
Out, washing silk is made in solidification, stretching and 95 DEG C of washing, and the water content for washing silk is 70wt%；
(2) again with the mass content of solubilised sulphur black BR be 3wt% aqueous solution 90 DEG C at a temperature of to washing silk
Carry out the at a temperature of rinsing 60 seconds and temperature by the way of drying using hot-air at 160 DEG C after 300 seconds immersion treatments at 40 DEG C
The lower dry water content to fiber of degree is that colored fibre cellulose fiber is made in 12wt%.
The crystallinity of final colored fibre cellulose fiber obtained is 55%, contains micropore, and micropore average diameter is 50 nanometers,
The quality of sulfur dye is the 5.0% of cellulose fibre matrix quality.
The filament number of colored fibre cellulose fiber is 4.0dtex, breaking strength 1.0cN/dtex, and elongation at break is
5%, regain 7%, after washing 50 times, the quality of sulfur dye is the 2.5% of cellulosic fibre substrate quality, water-fastness
Color fastness is 5 grades, and colour fastness to rubbing is 5 grades；
Colored fibre cellulose fiber is tow, can be used for knitted fabric, woven fabric, non-woven fabrics or fiber blended with other.
Embodiment 4
A kind of preparation method of colored fibre cellulose fiber, steps are as follows:
(1) degree of polymerization is 400, concentration is 10wt% copper ammonia fiber spinning solution is squeezed out through spinning head, solidification, stretch and
Washing silk is made in 98 DEG C of washing, and the water content for washing silk is 50wt%；
(2) aqueous solution for being again 1.5wt% with the mass content of water-soluble sulphur yellow GC 70 DEG C at a temperature of to water
Wash silk carry out after 60 seconds immersion treatments 25 DEG C at a temperature of rinsing 20 seconds and by the way of being dried using hot-air at 110 DEG C
At a temperature of dry to fiber water content be 12wt% be made colored fibre cellulose fiber.
The crystallinity of final colored fibre cellulose fiber obtained is 38%, contains micropore, and micropore average diameter is 10 nanometers,
The quality of sulfur dye is the 0.8% of cellulose fibre matrix quality.
The filament number of colored fibre cellulose fiber is 0.5dtex, breaking strength 4.0cN/dtex, and elongation at break is
15%, regain 12%, after washing 50 times, the quality of sulfur dye is the 0.3% of cellulosic fibre substrate quality, water-fast
Washing color fastness is 4 grades, and colour fastness to rubbing is 4 grades；
Colored fibre cellulose fiber is long filament, can be used for knitted fabric, woven fabric, non-woven fabrics or fiber blended with other.
Embodiment 5
A kind of preparation method of colored fibre cellulose fiber, steps are as follows:
(1) by the degree of polymerization is 800, concentration is 15wt% cellulose fibre (with ionic liquid 1- butyl -3- methyl miaow
Azoles villaumite is the regenerated cellulose fiber of solvent preparation) spinning solution squeezes out through spinning head, solidification, stretches and 95 DEG C of washing system
Silk must be washed, the water content for washing silk is 55wt%；
(2) again with the mass content of dyestuff (mixture of active yellow 4RFN and water-soluble sulphur yellow GC mass ratio 1:1)
For 2wt% aqueous solution 80 DEG C at a temperature of washing silk is carried out after 100 seconds spray process 30 DEG C at a temperature of rinse
Coloured fibre is made in 10 DEG C of the at a temperature of dry water content to fiber for 12wt% in 40 seconds and the mode that uses hot-air to dry
Cellulose fiber.
The crystallinity of final colored fibre cellulose fiber obtained is 40%, contains micropore, and micropore average diameter is 20 nanometers,
The quality of dyestuff is the 2.0% of cellulose fibre matrix quality.
The filament number of colored fibre cellulose fiber is 3.0dtex, breaking strength 3.5cN/dtex, and elongation at break is
20%, regain 10%, after washing 50 times, the quality of dyestuff is the 1.5% of cellulosic fibre substrate quality, water-fastness
Color fastness is 4-5 grades, and colour fastness to rubbing is 4-5 grades；
Colored fibre cellulose fiber is tow, can be used for knitted fabric, woven fabric, non-woven fabrics or fiber blended with other.
Embodiment 6
A kind of preparation method of colored fibre cellulose fiber, steps are as follows:
It (1) (is molten with carbamate/NaOH system by the cellulose fibre that the degree of polymerization is 600, concentration is 18wt%
The regenerated cellulose fiber of agent preparation) spinning solution is squeezed out through spinning head, is solidified, stretching and washing silk is made in 95 DEG C of washing,
The water content for washing silk is 60wt%；
(2) again with dyestuff (mixture of active yellow 4RFN, direct yellow R and water-soluble sulphur yellow GC mass ratio 1:1:1)
Mass content be 2wt% aqueous solution 75 DEG C at a temperature of washing silk is carried out after 200 seconds spray process at 25 DEG C
At a temperature of rinse 30 seconds and use hot-air to dry mode 140 DEG C at a temperature of the dry water content to fiber for 12wt%
Colored fibre cellulose fiber is made.
The crystallinity of final colored fibre cellulose fiber obtained is 40%, contains micropore, and micropore average diameter is 40 nanometers,
The quality of dyestuff is the 2.2% of cellulose fibre matrix quality.
The filament number of colored fibre cellulose fiber is 2.5dtex, breaking strength 3.5cN/dtex, and elongation at break is
18%, regain 15%, after washing 50 times, the quality of dyestuff is the 1.8% of cellulosic fibre substrate quality, water-fastness
Color fastness is 5 grades, and colour fastness to rubbing is 5 grades；
Colored fibre cellulose fiber is tow, can be used for knitted fabric, woven fabric, non-woven fabrics or fiber blended with other.
Embodiment 7
A kind of preparation method of colored fibre cellulose fiber, steps are as follows:
(1) degree of polymerization is 500, concentration is 22wt% viscose rayon spinning solution is squeezed out through spinning head, solidification, stretch and
Washing silk is made in 98 DEG C of washing, and the water content for washing silk is 60wt%；
(2) again with the mass content of direct scarlet 4BE be 2.8wt% aqueous solution 85 DEG C at a temperature of to washing silk into
After 250 seconds spray process of row 35 DEG C at a temperature of rinsing 50 seconds and by the way of being dried using hot-air in 150 DEG C of temperature
The water content of lower drying to fiber is that colored fibre cellulose fiber is made in 12wt%.
The crystallinity of final colored fibre cellulose fiber obtained is 45%, contains micropore, and micropore average diameter is 40 nanometers,
The quality of dyestuff is the 2.7% of cellulose fibre matrix quality.
The filament number of colored fibre cellulose fiber is 2.5dtex, breaking strength 4.0cN/dtex, and elongation at break is
19%, regain 15%, after washing 50 times, the quality of dyestuff is the 2.2% of cellulosic fibre substrate quality, water-fastness
Color fastness is 5 grades, and colour fastness to rubbing is 5 grades；
Colored fibre cellulose fiber is tow, can be used for knitted fabric, woven fabric, non-woven fabrics or fiber blended with other.
Claims (10)
1. a kind of preparation method of colored fibre element fiber, it is characterized in that: cellulosic fibre spinning solution is squeezed through spinning head
Out, it solidifies, stretch and washing silk is made in washing, then carry out rinsing after handling washing silk with aqueous dye solutions and dry make
Obtain colored fibre element fiber；
Temperature >=90 DEG C of washing, the temperature of aqueous dye solutions is a DEG C when processing, the temperature of rinsing be b DEG C, a > b, a be 40~
90, b be 20~40；
For dyestuff containing one or more of X group, Y group and Z group, X group is that can form covalent bond with cellulose hydroxyl group
Group, Y group are the group for capableing of self-crosslinking reaction, and Z group is the group that hydrogen bond can be formed with cellulose hydroxyl group.
2. a kind of preparation method of colored fibre element fiber according to claim 1, which is characterized in that cellulose family is fine
The concentration for tieing up spinning solution is 5~25wt%；Cellulosic fibre is regenerated celulose fibre or cellulose derivative fibres.
3. a kind of preparation method of colored fibre element fiber according to claim 2, which is characterized in that cellulose family is fine
Dimension is viscose rayon, acetate fiber, Lyocell fiber, copper ammonia fiber, the regenerated cellulose class prepared by solvent of ionic liquid
Fiber or the regenerated cellulose fiber prepared using aqueous slkali as solvent.
4. a kind of preparation method of colored fibre element fiber according to claim 1, which is characterized in that the termination of washing
Condition are as follows: the water content for washing silk is 40~70wt%.
5. a kind of preparation method of colored fibre element fiber according to claim 1, which is characterized in that X group is aldehyde
Base, cyano, epoxy group, acid chloride groups, acid anhydrides or diisocyanate；Y group is siloxanes；Z group is sulfonic acid group or sulphur
Acid esters group.
6. a kind of preparation method of colored fibre element fiber according to claim 5, which is characterized in that aqueous dye solutions
The mass content of middle dyestuff is 2~10wt%；Dyestuff is more than one of direct dyes, reactive dye and sulfur dye.
7. a kind of preparation method of colored fibre element fiber according to claim 1, which is characterized in that processing is using leaching
The mode of bubble or spray, the time of processing are 60~600 seconds；The time of rinsing is 120~600 seconds.
8. a kind of preparation method of colored fibre element fiber according to claim 1, which is characterized in that dry using heat
The mode of air drying, the temperature of hot-air are 105~160 DEG C, are dried to water content < 15wt% of fiber.
9. using coloured made from a kind of preparation method of colored fibre element fiber as described in any one of claims 1 to 8
Cellulosic fibre, it is characterized in that: mainly by cellulosic fibre matrix and being dispersed in the intracorporal dye of cellulosic fibre base
Material composition.
10. colored fibre element fiber according to claim 9, which is characterized in that the crystallization of colored fibre element fiber
Degree > 30% contains micropore, and micropore average diameter is 5~50 nanometers, and the quality of dyestuff is the 0.1 of cellulosic fibre substrate quality
~5.0%；
The filament number of colored fibre element fiber is 0.5~5.0dtex, and breaking strength is 1.0~4.5cN/dtex, and fracture is stretched
Long rate is 5%~20%, and regain is 5%~15%, and washing color fastness is equal to 5 grades, and colour fastness to rubbing is equal to 5 grades；
After colored fibre element fiber washs 50 times, the quality of dyestuff be cellulosic fibre substrate quality 0.08~
2.50%, washing color fastness is more than or equal to 4 grades, and colour fastness to rubbing is more than or equal to 4 grades；
Colored fibre element fiber be long filament, short silk or tow, for knitted fabric, woven fabric, non-woven fabrics or with other fibers
It is mixed.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114402098A (en) * | 2019-09-17 | 2022-04-26 | 阿尔托大学基金会 | Lyocell fiber and production method thereof |
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