CN110129915A - A kind of method that original liquid coloring prepares black acid fiber by polylactic - Google Patents
A kind of method that original liquid coloring prepares black acid fiber by polylactic Download PDFInfo
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- CN110129915A CN110129915A CN201910449813.1A CN201910449813A CN110129915A CN 110129915 A CN110129915 A CN 110129915A CN 201910449813 A CN201910449813 A CN 201910449813A CN 110129915 A CN110129915 A CN 110129915A
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- polylactic
- fiber
- acid
- carbon black
- acid fiber
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Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/04—Melting filament-forming substances
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/098—Melt spinning methods with simultaneous stretching
-
- 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
- D01F1/04—Pigments
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
Abstract
The invention discloses a kind of methods that original liquid coloring prepares black acid fiber by polylactic, belong to technical field of fibre production.Modified carbon black is added pulverizer with polylactic acid and is pulverized and mixed by the present invention, is added after mixing well to the miniature mixing instrument of bipyramid and is warming up to assigned temperature, and simultaneously drawing-off is squeezed out after melt blending to up- coiler to prepare acid fiber by polylactic.The performances such as mechanical property, color depth, the fibre diameter of coloured acid fiber by polylactic can be effectively controlled by adjusting the conditions such as carbon black types, carbon black and polylactic acid ratio, winding speed and draft process in the present invention.Gained acid fiber by polylactic color fastness is high, and color depth is easy to control, and fiber differences are small between same technique different batches, is suitble to continuous production.
Description
Technical field
Present invention relates particularly to a kind of methods that original liquid coloring prepares black acid fiber by polylactic, belong to fiber production technology neck
Domain.
Background technique
Polylactic acid is that one kind derives from the natural materials such as corn and soybean, and the high molecular material of good biocompatibility,
Often it is applied to medical field such as surgical sutures, orthopaedics fixed equipment and drug controlled release etc..In recent years due to
The breakthrough of synthetic method, polylactic acid molecule amount and molecular weight distribution have obtained good control, become biomass fiber
A kind of important raw material.It matches in excellence or beauty in addition, acid fiber by polylactic has in the mechanical property of polyester fiber, while also there is easily biology drop
The advantages that solution, anti-fold, uvioresistant, limit oxygen index be higher and good hydrophilic property, is before field of textiles is paid attention to and applied the most
One of good biomass fiber of scape.
Acid fiber by polylactic is similar to terylene chemical structure, dyes frequently with disperse dyes to it.But because of its linear rouge
Fat race thermoplastic poly ester structure keeps its hydrolysis resistance poor, makes to dye polylactic acid fibre using traditional disperse dyeing process
The problem of mechanical property reduces is tieed up, the wearability of polylactic acid is affected.For example, open magazine " Journal of Applied
Polymer Science " in entitled " Comparison of disperse dye exhaustion, color yield, and
colorfastness between polylactide and poly(ethylene terephthalate)》(2010,90
(12): 3285-3290 author Yang) dyes PLA using disperse dyes, and result of study shows that improving Value in Dyeing Process has
Conducive to dye-uptake of the disperse dyes on PLA fiber, but when pH value is higher than 7, strong hydrolysis can occur for PLA fiber, seriously
Influence PLA fibrous mechanical property.
Original liquid coloring technology is that colorant is added in spinning solution or melt in one kind, obtains colored polymeric or melt,
The color method of colored fibre is directly prepared into through spinning.Pigment used is present in medium in original liquid coloring with dispersity, because
The particle size and distribution character of this pigment directly influence the color characteristics and mechanical property of coloured fiber, conventional black fiber
It is the obtained black polyester fiber using carbon black to polyester fiber original liquid coloring；United States Patent (USP) US07/099,534 discloses one kind
The black liquor colorant preparation method of original liquid coloring polyester fiber adds carbon black through liquid phase oxidation and after gaseous oxidation neutralizes
Enter into polyester liquid, obtains the aterrimus polyester with micro- blue cast.But black fiber material obtained by the above method
Mechanical property and color fastness are still weaker, need to find a kind of prepare with stronger mechanical property and superior color fastness
The method of coloured acid fiber by polylactic.
Summary of the invention
To solve the above-mentioned problems, the present invention is based on original liquid colorings is cooperated specific using modified carbon black and polylactic acid blend
Carbon black and the conditions such as polylactic acid ratio, winding speed and draft process by the partial size of control carbon black, and improve charcoal blacks
Compatibility with polylactic acid matrix is to prepare a kind of original liquid coloring black acid fiber by polylactic that thermodynamic property is excellent.
The first purpose of the invention is to provide a kind of preparation method of black acid fiber by polylactic, the method using it is non-from
Subtype modified carbon black and polylactic acid melting extrusion, then carry out drawing-off, obtain black acid fiber by polylactic；The non-ionic modification
Carbon black is 1%-2.5% with respect to the mass fraction of polylactic acid.
In one embodiment of the invention, the non-ionic modified carbon black is the polyester structural units of surface grafting
Carbon black.
In one embodiment of the invention, the polyester structural units include polylactic acid, poly terephthalic acid second two
One of alcohol ester, polypropylene terephthalate, polybutylene terephthalate (PBT), poly butylene succinate are more
Kind.
In one embodiment of the invention, the temperature of the melting extrusion is 170~210 DEG C.
In one embodiment of the invention, the melting extrusion is carried out in the miniature mixing instrument of bipyramid；Wherein, double
The temperature for boring left and right plate in miniature mixing instrument is identical, screw speed 50-80rpm.
In one embodiment of the invention, the method also includes being wound after the extrusion using up- coiler, so
After carry out drawing-off.
In one embodiment of the invention, the winding speed of the up- coiler is 5-30m/min.
In one embodiment of the invention, the drawing-off is 65~95 DEG C of progress drawing-offs in a water bath.
In one embodiment of the invention, the time of the drawing-off is 20~120s.
In one embodiment of the invention, the drafting multiple of the drawing-off is 1.5~3 times.
In one embodiment of the invention, the carbon black include MA-100 type carbon black, rubber black N110, N220,
One of N330, N550, colour carbon black R330, R400, R660 or a variety of.
The present invention is 24 hours dry in 80 DEG C of vacuum drying ovens by polylactic acid, takes a certain amount of polylactic acid and carbon black in pulverizer
In be sufficiently pulverized and mixed, be then added into the miniature mixing instrument of bipyramid, and be warming up to assigned temperature, to polylactic acid melting squeeze
First break draft is to small-sized up- coiler black acid fiber by polylactic is made out；The fiber of winding on the winder is removed, water-bath is placed in
It is more excellent to assign fiber by factors such as control bath temperature, in a water bath residence time and draft ratios for middle carry out drawing-off
Mechanical property.
A second object of the present invention is to provide a kind of black acid fiber by polylactic, the black acid fiber by polylactic is using upper
What the method for stating was prepared.
Third object of the present invention is to provide a kind of textile, the textile includes that above-mentioned black polylactic acid is fine
Dimension.
Fourth object of the present invention is that above-mentioned black acid fiber by polylactic is applied in garment industry.
Beneficial effects of the present invention are as follows:
Carbon black and polylactic acid are mixed first by the method for physical blending, are added to bipyramid by a certain percentage by the present invention
Melt blending in miniature mixing instrument squeezes out drawing-off later and prepares original liquid coloring black acid fiber by polylactic to small-sized up- coiler.It is logical
It crosses different draft process and obtains the fiber of different mechanical properties.This method has following features:
1, it is that colorant is added in the melt to obtain colored fibre to the coloring process of fiber in the method for the invention, belongs to
In physical change process.In fiber through spinning drawing preparation colorant directly by it is fixed in the fibre, eliminate fiber after stain
Colour circle section, thus the improper damage to fibrous mechanical property of dyeing condition is avoided, while reducing energy consumption, reduce color silk
Production cost, can also remove from because dyeing bring pollution problem, be a kind of green colouring method.
It 2, can be fast by the type and performance, carbon black and polylactic acid ratio of adjusting carbon black, winding in the method for the invention
The conditions such as degree and draft process, control the performances such as mechanical property, color depth, the fibre diameter of coloured acid fiber by polylactic, wherein
Up to 0.22N/tex or more, the mechanical property of fiber will not be lost in strength；Color depth it is high, and CMC DE is no more than 0.5,
Dyeing effect is highly uniform.Gained acid fiber by polylactic color fastness is high, and color depth is easy to control, fiber differences between same technique different batches
It is small, it is suitble to continuous production.
Specific embodiment
In order to be more clearly understood that technology contents of the invention, spy lifts following embodiment and is described in detail, and purpose is only
It is to be best understood from the protection scope that the contents of the present invention are not intended to limit the present invention.
Mechanics performance determining: using the mechanical property of EZ-SX type electronic universal tester test fiber；
Color characteristics measurement: using the color characteristics of CI7800 type computer colour matching instrument test fiber；Wherein CMC DE
Assessment of levels: its numerical value does not observe color change within 1, dyes more uniform.
Fastness to soaping measurement: its fastness to soaping is tested using GB/T 3921A-2008；
Non-ionic modified carbon black preparation method: 2.5g silane coupling agent and 5g carbon black are added to alcohol, water quality ratio is
The 100g in the mixed solvent of 9:1 is transferred in 40 DEG C of water-baths insulated and stirred reaction for 24 hours after being ultrasonically treated 30min.Then 1g is taken
It is added in 50g toluene solution, and the non-ionic co-monomers of 1g is added, 0.06g octoate catalyst stannous is added after heating, protect
Temperature reaction a period of time obtains non-ionic modified carbon black.Wherein non-ionic co-monomers include lactide, terephthalic acid (TPA) second
One of diol ester, propylene glycol ester terephthalate, mutual-phenenyl two acid bromide two alcohol ester, succinic acid-butanediol ester are a variety of.
Embodiment 1
Polylactic acid is placed in 80 DEG C of vacuum drying ovens dryings 24 hours, polylactic acid and 0.15g surface grafting after taking 10g dry
The non-ionic modified carbon black of polylactic acid structure is added after being thoroughly mixed in flask to the miniature mixing instrument of bipyramid, adjusts spiral shell
Left and right plate temperature is risen to 190 DEG C, to polylactic acid melting extrusion first break draft to small-sized up- coiler, winding speed to 60rpm by bar revolving speed
Degree is adjusted to 20m/min, removes the fiber of winding on the winder after a period of time, is placed in drawing-off 30 in 70 DEG C of water-bath
Second, it improves the degree of orientation of fiber and makes its length elongation to 2 times of fibrinogen.It is dried after taking-up in room temperature.
The non-ionic modified carbon black of surface grafting polylactic acid structure: 2.5g silane coupling agent and 5g carbon black are added to
Alcohol, water quality are ultrasonically treated after 30min that be transferred to insulated and stirred in 40 DEG C of water-baths anti-than the 100g in the mixed solvent for 9:1
It should for 24 hours.Then it takes 1g to be added in 50g toluene solution, and 1g lactide is added, it is sub- that 0.06g octoate catalyst is added after heating
Tin, insulation reaction obtain non-ionic modified carbon black for a period of time.
Influence of the 2 modified carbon black dosage of embodiment to fiber product
Referring to embodiment 1, by the dosage of non-ionic modified carbon black replace with respectively 0.1g, 0.2g, 0.25g, 0.3g,
1g, 2g, other conditions are constant, and corresponding fiber product is prepared.The specific results of property of product is shown in Table 1.
The results of property of fiber obtained by the dosage of the different non-ionic modified carbon blacks of table 1
| The dosage of modified carbon black | Strongly (N/tex) | Soaping fastness | K/S | CMC DE |
| 0.1g | 0.22 | 5 | 19.63 | 0.45 |
| 0.15g | 0.37 | 5 | 20.23 | 0.23 |
| 0.2g | 0.29 | 5 | 21.38 | 0.31 |
| 0.25g | 0.23 | 5 | 22.10 | 0.29 |
| 0.3g | 0.15 | 5 | 23.09 | 0.28 |
| 1g | 0.12 | 5 | 23.55 | 0.25 |
| 2g | 0.10 | 5 | 23.58 | 0.26 |
Embodiment 3
Referring to embodiment 1, the drawing-off time is replaced with into 10s, 20s, 60s, 300s respectively, other conditions are constant, are prepared into
To corresponding fiber product.Concrete outcome is shown in Table 2.
The results of property of fiber obtained by the different drawing-off times of table 2
| The drawing-off time (s) | Strongly (N/tex) | Soaping fastness | K/S | CMC DE |
| 10 | 0.27 | 5 | 20.23 | 0.25 |
| 20 | 0.30 | 5 | 20.22 | 0.23 |
| 60 | 0.35 | 5 | 20.00 | 0.23 |
| 300 | 0.33 | 5 | 20.12 | 0.21 |
Embodiment 4
Referring to embodiment 1, bath temperature is replaced with to 65 DEG C, 70 DEG C, 80 DEG C, 85 DEG C, 90 DEG C, 95 DEG C respectively, other
Part is constant, and corresponding fiber product is prepared.Concrete outcome is shown in Table 3.
The results of property of fiber obtained by the different bath temperatures of table 3
| Bath temperature (DEG C) | Strongly (N/tex) | Soaping fastness | K/S | CMC DE |
| 65 | 0.27 | 5 | 20.30 | 0.23 |
| 70 | 0.33 | 5 | 20.22 | 0.23 |
| 80 | 0.36 | 5 | 20.15 | 0.25 |
| 85 | 0.34 | 5 | 20.19 | 0.24 |
| 90 | 0.29 | 5 | 20.32 | 0.22 |
| 95 | 0.26 | 5 | 20.34 | 0.23 |
Embodiment 5
Referring to embodiment 1, winding speed is replaced with into 5m/min, 20m/min, 30m/min respectively, other conditions are constant,
Corresponding fiber product is prepared.Concrete outcome is shown in Table 4.
The results of property of fiber obtained by the different winding speeds of table 4
Comparative examples 1
Polylactic acid is placed in 80 DEG C of vacuum drying ovens are 24 hours dry, the polylactic acid and the original carbon black of 2g after taking 10g dry in
It is added after being thoroughly mixed in flask to the miniature mixing instrument of bipyramid, adjusting screw rod revolving speed to 60rpm rises to left and right plate temperature
190 DEG C, to polylactic acid melting extrusion first break draft to small-sized up- coiler, winding speed is adjusted to 10m/min, will twine after a period of time
It is removed around fiber on the winder, is placed in drawing-off 30 seconds in 70 DEG C of water-bath, improved the degree of orientation of fiber and make its length
It extends to 2 times of fibrinogen.It is dried after taking-up in room temperature.
Comparative examples 2
Polylactic acid is placed in 80 DEG C of vacuum drying ovens dryings 24 hours, the polylactic acid after taking 10g dry changes with 2g anionic
Property carbon black be thoroughly mixed in flask after be added to the miniature mixing instrument of bipyramid, adjusting screw rod revolving speed to 60rpm, by left and right plate
Temperature rises to 190 DEG C, and to polylactic acid melting extrusion first break draft to small-sized up- coiler, winding speed is adjusted to 10m/min, at one section
Between after winding fiber on the winder is removed, be placed in drawing-off 30 seconds in 70 DEG C of water-bath, improve the degree of orientation of fiber simultaneously
Make its length elongation to 2 times of fibrinogen.It is dried after taking-up in room temperature.
The preparation method of anion-modified carbon black: 2.5g silane coupling agent and 5g carbon black are added to alcohol, water quality ratio is
The 100g in the mixed solvent of 9:1 is ultrasonically treated after 30min and is transferred in 40 DEG C of water-baths insulated and stirred reaction and obtains silane for 24 hours
Coupling agent modified carbon black.Then it takes in the silane coupler modified carbon black dispersion to ethyl alcohol of 1g, is added under continuous agitation
25g sodium p styrene sulfonate, is added dropwise 5g ammonium persulfate after heating, insulation reaction obtains anionic Modified Activated Carbon for a period of time
It is black.
Comparative examples 3
Referring to embodiment 1, winding process is omitted, drawing-off 30 seconds in 70 DEG C of water-bath are placed directly within after melting extrusion, are mentioned
The degree of orientation of high microsteping simultaneously makes its length elongation to 2 times of fibrinogen.It is dried after taking-up in room temperature.
Comparative examples 4
It referring to embodiment 1, cools and solidifies, oil after melting extrusion, winding, import the drawing-off of drawing-off disk 30 seconds, improve fiber
The degree of orientation and make its length elongation to 2 times of fibrinogen.It is dried after taking-up in room temperature.
Fiber concrete outcome obtained by above-mentioned comparative examples is shown in Table 5.
The results of property of fiber obtained by 5 comparative examples of table
| Experimental result | Strongly (N/tex) | Fiber number (micron) | K/S | CMC DE |
| Comparative examples 1 | 0.26 | 48 | 21.7 | 1.44 |
| Comparative examples 2 | 0.11 | 48 | 22.462 | 1.68 |
| Comparative examples 3 | 0.20 | 48 | 21.22 | 1.83 |
| Comparative examples 4 | 0.10 | 48 | 21.9 | 0.70 |
Although the present invention has been described by way of example and in terms of the preferred embodiments, it is not intended to limit the invention, any to be familiar with this skill
The people of art can do various change and modification, therefore protection model of the invention without departing from the spirit and scope of the present invention
Enclosing subject to the definition of the claims.
Claims (10)
1. a kind of preparation method of black acid fiber by polylactic, which is characterized in that the method using non-ionic modified carbon black with
Then polylactic acid melting extrusion carries out drawing-off, obtain black acid fiber by polylactic；The non-ionic modified carbon black is with respect to polylactic acid
Mass fraction be 1%-2.5%.
2. the method according to claim 1, wherein the polyester structural units include polylactic acid, gather to benzene two
Formic acid glycol ester, polypropylene terephthalate, polybutylene terephthalate (PBT), one in poly butylene succinate
Kind is a variety of.
3. method according to claim 1 or 2, which is characterized in that the temperature of the melting extrusion is 170~210 DEG C.
4. method according to claim 1 to 3, which is characterized in that the method also includes utilizing winding after the extrusion
Machine is wound, and then carries out drawing-off.
5. method according to claim 1 to 4, which is characterized in that the winding speed of the up- coiler is 5-30m/
min。
6. -5 any method according to claim 1, which is characterized in that the time of the drawing-off is 20~120s.
7. -6 any method according to claim 1, which is characterized in that the drafting multiple of the drawing-off is 1.5~3 times.
8. the black acid fiber by polylactic that method as claimed in claim 1 to 7 is prepared.
9. textile made from black acid fiber by polylactic described in claim 8.
10. application of the black acid fiber by polylactic in garment industry described in claim 8.
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| CN111172601A (en) * | 2019-12-31 | 2020-05-19 | 神马实业股份有限公司 | Continuous production method of polyamide color yarn |
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