CN107723831B - Dope-dyed polyester fiber and preparation method thereof - Google Patents
Dope-dyed polyester fiber and preparation method thereof Download PDFInfo
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- CN107723831B CN107723831B CN201610653035.4A CN201610653035A CN107723831B CN 107723831 B CN107723831 B CN 107723831B CN 201610653035 A CN201610653035 A CN 201610653035A CN 107723831 B CN107723831 B CN 107723831B
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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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
- 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
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Abstract
The invention belongs to the technical field of spinning, and particularly relates to dope-dyed polyester fiber and a preparation method thereof. The preparation method comprises the following steps: (1) adding a colorant into a carrier polyester polyol to prepare uniform coloring mother liquor; (2) adding the coloring mother liquor into a polyester oligomer, uniformly mixing, and then feeding into a polycondensation system to sequentially carry out a pre-polycondensation reaction and a final polycondensation reaction to obtain a coloring polyester melt; (3) spinning and drafting the obtained colored polyester melt to obtain the dope colored polyester fiber. The invention realizes the uniform dispersion of the colorant in the polyester component, effectively solves the problem of the compatibility of the polyester component and the colorant carrier, eliminates the influence of the colorant and the carrier thereof on the spinning performance of the colored polyester melt, and the prepared stock solution colored polyester fiber has high colorant content, stable quality, no color difference, soft hand feeling and good mechanical property.
Description
Technical Field
The invention belongs to the technical field of spinning, and particularly relates to dope-dyed polyester fiber and a preparation method thereof.
Background
The polyester fiber has the advantages of high breaking strength, stable shape, good stiffness, crease resistance, easy washing and drying, and the like, and is an ideal textile fiber. These excellent physical and mechanical properties of the polyester fiber depend on its highly stereoregular macromolecular chain structure and highly crystalline and oriented condensed state structure, but these structural characteristics also pose a problem that the polyester fiber is not easily dyed. At present, the polyester fiber is dyed mainly by adopting a disperse dye high-temperature high-pressure dyeing process, and the process has the outstanding problems of high equipment requirement, high investment, difficult three-waste treatment and the like. Therefore, the energy-saving and environment-friendly coloring technology is important for promoting the sustainable development of the polyester fiber.
The polyester fiber stock solution coloring has the advantages of simple process, good color fastness, uniform coloring, energy conservation, less three wastes and the like, and is particularly suitable for mass production and development of polyester fiber interwoven fabrics. The dope-dyed polyester fiber is a colored fiber obtained by adding a colorant into a polyester melt and spinning, and is also called a non-dyed fiber or a spun-dyed fiber. The subsequent application of the dope-dyed polyester fiber can save the printing and dyeing process, avoid the generation of a large amount of printing and dyeing wastewater, and has outstanding environment-friendly characteristics.
The Chinese patent with the application number of 200710118294.8 discloses a black polyester chip and a preparation method of the black polyester chip, and particularly designs a black color paste of carbon black after treatment added in the esterification reaction process or before the ester exchange reaction to prepare the black polyester chip and the preparation method thereof. The black polyester prepared by the method has the advantages that carbon black particles in the slices are easy to agglomerate, and a spinning assembly is blocked during spinning, so that the period of the spinning assembly is short; in addition, the carbon black particles can also act as a matting agent in the polyester, resulting in a lower brightness of the spun fibers.
The Chinese patent with the application number of 201310147346.X discloses a method for preparing colored polyester fibers by dope-dyeing, wherein liquid color paste consisting of dye, liquid polyester carrier, plasticizer and dispersant is injected before entering a spinning manifold and is uniformly mixed, and then melt direct spinning is carried out to prepare the colored polyester fibers. The compatibility of the liquid polyester carrier and the polyester melt and the existence of low molecular substances such as a plasticizer, a dispersing agent and the like in the invention greatly influence the spinnability of the colored polyester melt.
The Chinese patent with application number 201310150118.8 discloses a dope dyeing process for polyester fiber before spinning by solvent carrier, which comprises injecting dye dope prepared by blending dye and solvent carrier polyester polyol before entering a spinning manifold, mixing uniformly, and carrying out melt spinning to prepare colored polyester fiber. The compatibility of the melt carrier polyester polyol and the polyester melt and the reduction of the intrinsic viscosity of the polyester melt caused by the alcoholysis reaction between the polyester polyol and the polyester in the invention can cause the serious deterioration of the spinning performance of the colored polyester melt.
Chinese patent application No. 201410709477.7 discloses a method for preparing black polyester fiber by stock solution coloring, which comprises adding black pigment carbon black into a liquid dispersion medium, fully grinding, adding a compound capable of chemically reacting with carbon black surface groups, and carrying out grafting reaction under the action of a catalyst at a certain temperature to obtain uniformly dispersed black slurry; adding the black slurry into a polyester oligomer, uniformly mixing, carrying out pre-polycondensation and final polycondensation to obtain a polyester melt, and carrying out direct melt spinning through a spinning manifold. According to the method, when the coloring mother liquor is prepared, the carbon black pigment and the pigment carrier are subjected to a grafting reaction, so that in a further reaction, the pre-polymerization of the carrier and the polyester oligomer is influenced to a certain extent, and the carrier is unevenly distributed in a product and has poor mechanical property; the method is only suitable for carbon black pigment, and cannot be widely applied to other types of dyes when the process for preparing the polyester fiber by stock solution coloring is carried out, so that the method has limitation.
The invention is provided to overcome the defects in the prior art.
Disclosure of Invention
As described in the background art section, in the prior art, there has been a problem that colored polyester melts are deteriorated in spinnability due to agglomeration of a colorant, poor compatibility of a colorant carrier with a polyester component, addition of low molecular substances such as a plasticizer and a dispersant for dispersing the colorant, and the like.
In order to solve the problems, the invention provides a preparation method of a dope dyed polyester fiber and the dope dyed polyester fiber, so as to eliminate the influence of a coloring agent and a carrier thereof on the spinning performance of a dyed polyester melt and prepare the dope dyed polyester fiber with soft hand feeling and high coloring agent content.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the dope-dyed polyester fiber is characterized by comprising the following steps:
(1) adding a colorant into a carrier polyester polyol to prepare a uniform coloring mother solution, wherein the content of the colorant is 5-40 wt%;
when the content of the coloring agent in the coloring mother liquor is 5-40 wt%, the coloring agent can be fully dissolved in the polyester polyol carrier, so that the coloring agent molecules of the obtained coloring mother liquor can be uniformly dispersed.
(2) Injecting the coloring mother liquor prepared in the step (1) and a catalyst into a polyester oligomer pipeline on line, uniformly mixing the coloring mother liquor and the catalyst with a polyester oligomer with a polymerization degree of 1-8 from an esterification system through a dynamic mixer, and then feeding the mixture into a pre-polycondensation system for pre-polycondensation reaction to obtain a coloring prepolymer with a viscosity of 0.15-0.45 dL/g;
the polyester oligomer includes, but is not limited to, an ethylene terephthalate oligomer, a trimethylene terephthalate oligomer, and a tetramethylene terephthalate oligomer. The polymerization degree of the polyester oligomer is 1 to 8. The polymerization degree of the polyester oligomer is controlled in the range, which is beneficial to the copolycondensation reaction of the polyester oligomer and the carrier aliphatic polyester polyol, and the uniform distribution of aliphatic polyester polyol chain segments in a polyester molecular chain is realized, so that the prepared colored polyester melt has good spinnability.
In the step (2) of the preparation method, the coloring mother liquor is injected into the polyester oligomer pipeline on line and then is mixed with the polyester oligomer from the esterification system through the dynamic mixer, so that the efficient and uniform dispersion of the colorant in the main material polyester oligomer can be realized. Compare in the mixing assembly of traditional pipeline formula static mixer, the mixing assembly of dynamic mixer can provide powerful shearing force through high-speed rotation and realize the high-efficient broken mixing of material. Such dynamic mixers include, but are not limited to, high shear homogenizing pumps
(3) Filtering the colored prepolymer prepared in the step (2) by using a prepolymer filter, and then, allowing the filtered colored prepolymer to enter a final polycondensation system for final polycondensation reaction to obtain a colored polyester melt with the viscosity of 0.50-1.20 dL/g;
the intrinsic viscosity of the colored polyester melt is controlled within the range, so that the colored polyester melt can have good spinnability in the subsequent melt spinning process, and the mechanical property of the prepared fiber can meet the requirement of subsequent processing.
(4) And (4) filtering the colored polyester melt prepared in the step (3) by a melt filter, and then, spinning and drafting the colored polyester melt in a spinning manifold to obtain the dope colored polyester fiber.
In the preparation method provided by the invention, the ester-soluble colorant is used as the colorant for coloring the polyester stock solution, so that the colorant molecules are uniformly dispersed in the polyester polymer, the influence of the dispersion degree of the colorant on the spinnability of the colored polyester melt is effectively eliminated, and the preparation of the stock solution colored polyester fiber with high colorant content can be realized. Meanwhile, the aliphatic polyester polyol is used as a colorant carrier, so that the ester-soluble colorant can be dissolved in the aliphatic polyester polyol to obtain uniform coloring mother liquor, and the precise addition of the colorant can be realized in an online adding mode of a coloring mother liquor polyester oligomer pipeline, so that the prepared stock solution coloring polyester fiber has stable quality and no color difference. In addition, the polyester polyol with a flexible molecular chain structure as a colorant carrier can be embedded into a polyester molecular main chain with a polyester oligomer through a copolycondensation reaction in a polycondensation reaction process, so that the compatibility problem between the colorant carrier and the polyester polymer can be thoroughly solved, and the colored polyester melt has good spinnability; on the other hand, the regularity of the polyester molecular chain can be damaged, the flexibility of the molecular chain is improved, the prepared fiber is endowed with soft hand feeling, and the comfort level of the fabric is improved.
In the above production method, the colorant in the step (1) is an ester-soluble colorant.
The invention uses ester-soluble colorant as the colorant for coloring the polyester stock solution, and the colorant can be dissolved in the polyester matrix to realize the uniform dispersion of colorant molecules so as to eliminate the influence of the colorant on the spinnability of colored polyester melt. And the ester-soluble colorant has good thermal stability, and is not decomposed or sublimated in the polymerization and spinning processes of the colored polyester. The above-mentioned ester-soluble colorants include, but are not limited to, c.i. solvent blue 83, 90, 94, 97, 101, 104, 102, 105, 130, 132, c.i. solvent yellow 116, 117, 125, 156, 158, 163, 167, c.i. solvent red 135, 138, 145, 146, 150, 151, 155, 168, 172, 169, 175, 181, 207, 222, c.i. solvent black 3, 5, 7, 27, 45, 47.
In the preparation method, the polyester polyol in the step (1) is an aliphatic polyester polyol with the molecular weight of 300-10000, and is preferably one of polybutylene adipate, polyethylene glycol succinate, polypropylene glycol sebacate, polyethylene glycol adipate, polypropylene glycol adipate, polyethylene glycol sebacate, polybutylene succinate and polyethylene glycol adipate.
The invention uses aliphatic polyester polyol as a colorant carrier, so that the ester-soluble colorant can be dissolved in the carrier to prepare uniform coloring mother liquor, and the precise proportion addition of the colorant is convenient. And after the aliphatic polyester polyol with a flexible molecular chain structure as a carrier is injected into a polyester oligomer pipeline along with a coloring agent, the aliphatic polyester polyol and the polyester oligomer can be embedded into a polyester molecular chain through copolycondensation reaction in the subsequent polycondensation reaction process, so that the problem of compatibility of the carrier polyester polyol and polyester components is solved, meanwhile, the regularity of the polyester molecular chain can be damaged, the flexibility of the molecular chain is improved, and the prepared fiber has soft hand feeling. The molecular weight of the aliphatic polyester polyol is 300-10000, and the polyester polyol in the molecular weight range has moderate dynamic viscosity, so that the coloring mother liquor is convenient to configure and convey. Aliphatic dibasic acids for synthesizing the aliphatic polyester polyol include, but are not limited to, succinic acid, adipic acid, sebacic acid; aliphatic diols include, but are not limited to, ethylene glycol, propylene glycol, butylene glycol, hexylene glycol, decylene glycol, diethylene glycol.
In the preparation method, the adding amount of the catalyst in the step (2) is 0.003-0.2 wt% of the mass of the polyester oligomer, and the catalyst is at least one of antimony catalyst, titanium catalyst and germanium catalyst.
Under the catalytic action of antimony catalyst and/or titanium catalyst and/or germanium catalyst, the aliphatic polyester polyol and polyester oligomer as colorant carrier can be subjected to copolycondensation reaction to generate copolyester, so that aliphatic polyester polyol molecular chains are embedded into polyester molecular chains. The amount of the catalyst added is controlled within the above range, which is favorable for balancing the reaction efficiency and the production cost. The antimony-based catalyst includes, but is not limited to, ethylene glycol antimony, antimony acetate or antimony trioxide, the titanium-based catalyst includes, but is not limited to, ethylene glycol titanium, tetrabutyl titanate, tetraisopropyl titanate, and the germanium-based catalyst includes, but is not limited to, germanium oxide.
In the preparation method, the blending temperature of the coloring mother liquor in the step (1) is 100-200 ℃, and the supply temperature is 50-150 ℃. Under the temperature condition, the colorant can be fully dissolved, and the thermal decomposition of the colorant and the carrier polyester polyol can be avoided.
In the preparation method, the online injection amount of the coloring mother liquor in the step (2) is 3-20 wt% of the mass of the polyester oligomer. At this ratio, the colored polyester melt produced can maintain good spinnability.
In the preparation method, the reaction temperature of the pre-polycondensation reaction in the step (2) is 230-275 ℃, the reaction time is 40-120 min, the preferable reaction temperature is 240-265 ℃, and the reaction time is 60-90 min. Under the condition of the pre-polycondensation reaction process, the prepolymer meeting the requirement of the subsequent final polycondensation reaction process can be prepared.
In the preparation method, the reaction temperature of the final polycondensation reaction in the step (3) is 240-285 ℃, the reaction time is 60-240 min, the preferable reaction temperature is 245-270 ℃, and the reaction time is 90-180 min. .
In the preparation method, the spinning temperature of the dope-dyed polyester fiber in the step (4) is 235-295 ℃, and the preferable spinning temperature is 245-280 ℃. The dope-dyed polyester fiber formed at the spinning temperature has uniform diameter and good fiber appearance.
After the colored polyester melt provided by the invention is spun, different types of fibers, such as short fibers, Fully Drawn Yarns (FDY) or false twist textured yarns (DTY), can be prepared by adjusting the drafting and winding processes. The specific spinning process of each type of fiber is as follows:
the process for preparing the dope-dyed polyester fiber short fiber comprises the following specific steps:
the spinning speed is 600-1800 m/min, the drawing temperature is 50-130 ℃, the primary drawing multiplying power is 2-4 times, the secondary drawing multiplying power is 1.05-2 times, the crimping temperature is 50-90 ℃, and the setting temperature is 80-200 ℃.
The process for preparing the dope dyed polyester fiber fully drawn yarn FDY comprises the following steps:
the spinning speed is 3500-5200 m/min, the speed of the hot roller GR1 is 1400-3000 m/min, the temperature is 50-100 ℃, the speed of the hot roller GR2 is 3500-5200 m/min, and the temperature is 105-150 ℃.
The process for preparing the dope dyed polyester fiber false twist textured yarn DTY comprises the following steps:
spinning speed is 2000-4000 m/min, and pre-oriented yarn POY is prepared. The pre-oriented yarn POY is subjected to texturing to prepare false twist textured yarn DTY, and the texturing process comprises the following steps: the processing speed is 300-1200 m/min, the stretching multiple is 1.3-3 times, the deformation temperature is 120-210 ℃, the setting temperature is 100-200 ℃, and the D/Y is 1.2-2.5.
The invention also provides the dope dyed polyester fiber prepared by the preparation method, wherein the dope dyed polyester fiber has the colorant content of 0.5-7.5 wt%, the color uniformity of 3-5 level and the modulus of 20-90 cN/dtex.
The invention provides a dope-dyed polyester fiber and a preparation method thereof. In the preparation method, the ester-soluble colorant is used as the colorant for coloring the polyester stock solution, so that the colorant molecules are uniformly dispersed in the polyester polymer, the influence of the dispersion degree of the colorant on the spinnability of the colored polyester melt is effectively eliminated, and the preparation of the stock solution colored polyester fiber with high colorant content can be realized.
Meanwhile, the aliphatic polyester polyol is used as a colorant carrier, so that the ester-soluble colorant can be dissolved in the aliphatic polyester polyol to obtain uniform coloring mother liquor, and the precise addition of the colorant can be realized in an online adding mode of a coloring mother liquor polyester oligomer pipeline, so that the prepared stock solution coloring polyester fiber has stable quality and no color difference.
In addition, the aliphatic polyester polyol with a flexible molecular chain structure as a colorant carrier can be subjected to polycondensation reaction with the polyester oligomer in a pre-polycondensation process to be embedded into a polyester molecular main chain, so that the compatibility problem between the colorant carrier and the polyester polymer can be thoroughly solved, and the colored polyester melt has good spinnability; on the other hand, the regularity of the polyester molecular chain can be damaged, the flexibility of the molecular chain is improved, the prepared fiber is endowed with soft hand feeling, and the comfort level of the fabric is improved.
Detailed Description
The present invention is described in further detail below with reference to specific examples, which are not to be construed as limiting the scope of the invention as claimed.
Example 1
Adding the colorant C.I. solvent red 135 and the polybutylene adipate polyol with the molecular weight of 4000 into a coloring mother liquor preparation tank according to the weight ratio of 30:70, and fully dissolving the colorant C.I. solvent red 135 into the polybutylene adipate polyol by stirring under the condition that the preparation temperature is 150 ℃ to obtain the coloring mother liquor with the colorant C.I. solvent red 135 content of 30 wt%. And then transferring the prepared coloring mother liquor into a coloring mother liquor supply tank for standby, wherein the supply temperature of the coloring mother liquor is 100 ℃.
The coloring mother liquor with the mass of 12 wt% and the antimony catalyst with the mass of 0.05 wt% are injected into the ethylene terephthalate oligomer with the polymerization degree of 5 from the esterification system, the materials are uniformly mixed by a high shear homogenizing pump and then enter a pre-polycondensation system for pre-polycondensation reaction, the pre-polycondensation reaction temperature is 265 ℃, the reaction time is 90min, and the coloring prepolymer with the intrinsic viscosity of 0.25dL/g is obtained.
And filtering the colored prepolymer by a prepolymer filter, and then feeding the filtered colored prepolymer into a final polycondensation system for final polycondensation reaction, wherein the final polycondensation reaction temperature is 270 ℃, and the reaction time is 120min, so that a colored polyester melt with the intrinsic viscosity of 0.67dL/g is obtained.
And (3) filtering the colored polyester melt by a melt filter, and then, spinning the colored polyester melt in a spinning manifold at the spinning temperature of 280 ℃ and the winding speed of 4500m/min to obtain the dope colored polyester fiber fully drawn yarn FDY. Wherein the speed of the hot roller GR1 is 1700m/min, the temperature is 80 ℃, the speed of the hot roller GR2 is 4550m/min, and the temperature is 125 ℃.
Example 2
Adding a colorant C.I. solvent red 168 and polyethylene glycol succinate polyol with the molecular weight of 300 into a coloring mother liquor preparation tank according to the weight ratio of 10:90, and stirring to fully dissolve the colorant C.I. solvent red 168 into the polyethylene glycol succinate polyol at the preparation temperature of 100 ℃ to obtain the coloring mother liquor with the colorant C.I. solvent red 168 content of 10 wt%. And then transferring the prepared coloring mother liquor into a coloring mother liquor supply tank for standby application, wherein the supply temperature of the coloring mother liquor is 50 ℃.
The coloring mother liquor with the mass of 5.3 wt% and the titanium catalyst with the mass of 0.1 wt% are injected into the butylene terephthalate oligomer with the polymerization degree of 3 from the esterification system, the materials are uniformly mixed by a high shear homogenizing pump and then enter a pre-polycondensation system for pre-polycondensation reaction, the pre-polycondensation reaction temperature is 245 ℃, the reaction time is 40min, and the coloring prepolymer with the intrinsic viscosity of 0.35dL/g is obtained.
And filtering the colored prepolymer by a prepolymer filter, and then feeding the filtered colored prepolymer into a final polycondensation system for final polycondensation reaction, wherein the final polycondensation reaction temperature is 250 ℃, and the reaction time is 120min, so that a colored polyester melt with the intrinsic viscosity of 1.05dL/g is obtained.
And (3) filtering the colored polyester melt by a melt filter, and then, spinning the colored polyester melt in a spinning manifold at the spinning temperature of 255 ℃ and the winding speed of 5200m/min to obtain the dope-colored polyester fiber fully drawn yarn FDY. Wherein the speed of the hot roller GR1 is 2400m/min, the temperature is 60 ℃, the speed of the hot roller GR2 is 5250m/min, and the temperature is 120 ℃.
Example 3
Adding a colorant C.I. solvent yellow 116 and polypropylene sebacate polyol with molecular weight of 2000 into a coloring mother liquor blending tank according to the weight ratio of 10:90, and fully dissolving the colorant C.I. solvent yellow 116 into the polypropylene sebacate polyol by stirring under the condition that the blending temperature is 100 ℃ to obtain the coloring mother liquor with the colorant C.I. solvent yellow 116 content of 10 wt%. And then transferring the prepared coloring mother liquor into a coloring mother liquor supply tank for standby application, wherein the supply temperature of the coloring mother liquor is 80 ℃.
The coloring mother liquor with the mass of 10 wt% and the titanium catalyst with the mass of 0.2wt% are injected into the trimethylene terephthalate oligomer with the polymerization degree of 3 from the esterification system, the materials are uniformly mixed by a high shear homogenizing pump and then enter a pre-polycondensation system for pre-polycondensation reaction, the pre-polycondensation reaction temperature is 230 ℃, the reaction time is 60min, and the coloring prepolymer with the intrinsic viscosity of 0.35dL/g is obtained.
And filtering the colored prepolymer by a prepolymer filter, and then feeding the filtered colored prepolymer into a final polycondensation system for final polycondensation reaction, wherein the final polycondensation reaction temperature is 240 ℃, and the reaction time is 180min, so that a colored polyester melt with the intrinsic viscosity of 1.00dL/g is obtained.
And (3) filtering the colored polyester melt by a melt filter, and then, spinning in a spinning box at the spinning temperature of 250 ℃ and the winding speed of 3500m/min to obtain the dope colored polyester fiber fully drawn yarn FDY. Wherein the speed of the hot roller GR1 is 1400m/min, the temperature is 50 ℃, the speed of the hot roller GR2 is 3550m/min, and the temperature is 105 ℃.
Example 4
Adding the colorant C.I. solvent black 3 and polyethylene glycol adipate with molecular weight of 2000 into a coloring mother liquor preparation tank according to the weight ratio of 15:85, and fully dissolving the colorant C.I. solvent black 3 in the polyethylene glycol adipate by stirring under the condition that the preparation temperature is 100 ℃ to obtain the coloring mother liquor with the colorant C.I. solvent black 3 content of 15 wt%. And then transferring the prepared coloring mother liquor into a coloring mother liquor supply tank for standby, wherein the supply temperature of the coloring mother liquor is 70 ℃.
The coloring mother liquor with the mass of 20wt% and the titanium catalyst with the mass of 0.003 wt% are injected into the ethylene terephthalate oligomer with the polymerization degree of 1 from the esterification system, the materials are uniformly mixed by a high shear homogenizing pump and then enter a pre-polycondensation system for pre-polycondensation reaction, the pre-polycondensation reaction temperature is 245 ℃, the reaction time is 120min, and the coloring prepolymer with the intrinsic viscosity of 0.20dL/g is obtained.
And filtering the colored prepolymer by a prepolymer filter, and then feeding the filtered colored prepolymer into a final polycondensation system for final polycondensation reaction, wherein the final polycondensation reaction temperature is 250 ℃, and the reaction time is 120min, so that a colored polyester melt with the intrinsic viscosity of 0.74dL/g is obtained.
And (3) filtering the colored polyester melt by a melt filter, and then, spinning in a spinning box at the spinning temperature of 260 ℃ and the winding speed of 3000m/min to obtain the stock solution colored polyester fiber pre-oriented yarn POY. The fiber was drawn on a draw texturing machine at a processing speed of 600m/min by a factor of 1.6. Wherein the deformation temperature is 140 ℃, the setting temperature is 120 ℃, and the D/Y is 1.8, thus obtaining the dope dyed polyester fiber false twist textured yarn DTY.
Example 5
Adding a colorant C.I. solvent blue 104 and polybutylene adipate polyol with the molecular weight of 10000 into a coloring mother liquor preparation tank according to the weight ratio of 45:55, and fully dissolving the colorant C.I. solvent blue 104 into the polybutylene adipate polyol by stirring under the condition that the preparation temperature is 200 ℃ to obtain the coloring mother liquor with the colorant C.I. solvent blue 104 content of 45 wt%. And then transferring the prepared coloring mother liquor into a coloring mother liquor supply tank for standby, wherein the supply temperature of the coloring mother liquor is 150 ℃.
The coloring mother liquor with the mass of 3 wt% and the titanium catalyst with the mass of 0.1 wt% are injected into the butylene terephthalate oligomer with the polymerization degree of 3 from the esterification system, the materials are uniformly mixed by a high shear homogenizing pump and then enter a pre-polycondensation system for pre-polycondensation reaction, the pre-polycondensation reaction temperature is 255 ℃, the reaction time is 60min, and the coloring prepolymer with the intrinsic viscosity of 0.45dL/g is obtained.
And filtering the colored prepolymer by a prepolymer filter, and then feeding the filtered colored prepolymer into a final polycondensation system for final polycondensation reaction, wherein the final polycondensation reaction temperature is 260 ℃ and the reaction time is 120min, so as to obtain a colored polyester melt with the intrinsic viscosity of 1.20 dL/g.
And (3) filtering the colored polyester melt by a melt filter, and then, spinning in a spinning box at 270 ℃ at a winding speed of 3200m/min to obtain the stock solution colored polyester fiber pre-oriented yarn POY. The fiber was drawn on a draw texturing machine at a processing speed of 520m/min by a factor of 1.5. Wherein the deformation temperature is 150 ℃, the setting temperature is 130 ℃, and the D/Y is 2.0, thus obtaining the dope dyed polyester fiber false twist textured yarn DTY.
Example 6
Adding the colorant C.I. solvent blue 132 and the polypropylene glycol adipate with the molecular weight of 4000 into a coloring mother liquor preparation tank according to the weight ratio of 40:60, and fully dissolving the colorant C.I. solvent blue 132 into the polypropylene glycol adipate by stirring under the condition that the preparation temperature is 150 ℃ to obtain the coloring mother liquor with the colorant C.I. solvent blue 132 content of 40 wt%. And then transferring the prepared coloring mother liquor into a coloring mother liquor supply tank for standby, wherein the supply temperature of the coloring mother liquor is 100 ℃.
The coloring mother liquor with the mass of 13 wt% and the titanium catalyst with the mass of 0.15 wt% are injected into the polytrimethylene terephthalate oligomer with the polymerization degree of 8 from the esterification system, the materials are uniformly mixed by a high shear homogenizing pump and then enter a pre-polycondensation system for pre-polycondensation reaction, the pre-polycondensation reaction temperature is 235 ℃, the reaction time is 90min, and the coloring prepolymer with the intrinsic viscosity of 0.40dL/g is obtained.
And filtering the colored prepolymer by a prepolymer filter, and then feeding the filtered colored prepolymer into a final polycondensation system for final polycondensation reaction, wherein the final polycondensation reaction temperature is 245 ℃ and the reaction time is 120min, so as to obtain a colored polyester melt with the intrinsic viscosity of 1.10 dL/g.
And filtering the colored polyester melt by a melt filter, and then, spinning in a spinning box at 235 ℃ at a winding speed of 2800m/min to obtain the stock solution colored polyester fiber pre-oriented yarn POY. The fiber was drawn on a draw texturing machine at a processing speed of 400m/min by a factor of 1.8. Wherein the texturing temperature is 120 ℃, the setting temperature is 100 ℃, and the D/Y is 1.8, thus obtaining the dope dyed polyester fiber false twist textured yarn DTY.
Example 7
Adding a colorant C.I. solvent black 47 and polysebacic acid sebacic ester polyol with the molecular weight of 10000 into a coloring mother liquor preparation tank according to the weight ratio of 40:60, and stirring to fully dissolve the colorant C.I. solvent black 47 into the polysebacic acid sebacic ester polyol at the preparation temperature of 200 ℃ to obtain the coloring mother liquor with the colorant C.I. solvent black 47 content of 40 wt%. And then transferring the prepared coloring mother liquor into a coloring mother liquor supply tank for standby, wherein the supply temperature of the coloring mother liquor is 150 ℃.
The coloring mother liquor with the mass of 5wt% and the germanium catalyst with the mass of 0.08 wt% are injected into the ethylene terephthalate oligomer with the polymerization degree of 6 from the esterification system, the materials are uniformly mixed by a high shear homogenizing pump and then enter a pre-polycondensation system for pre-polycondensation reaction, the pre-polycondensation reaction temperature is 275 ℃, the reaction time is 40min, and the coloring prepolymer with the intrinsic viscosity of 0.15dL/g is obtained.
And filtering the colored prepolymer by a prepolymer filter, and then feeding the filtered colored prepolymer into a final polycondensation system for final polycondensation reaction, wherein the final polycondensation reaction temperature is 285 ℃, and the reaction time is 60min, so that a colored polyester melt with the intrinsic viscosity of 0.50dL/g is obtained.
And (3) filtering the colored polyester melt by a melt filter, and then, spinning in a spinning box at 295 ℃ at a winding speed of 1000m/min to obtain the dope-colored polyester fiber undrawn yarn. Then, primary drawing was carried out at 70 ℃ at a draft ratio of 2.5 times, secondary drawing was carried out at 90 ℃ at a draft ratio of 1.2 times, and then the fiber was crimped at a temperature of 90 ℃. Then heat-set at 120 ℃ for 15 minutes. And cutting the shaped fiber on a cutting machine, and packaging to obtain the stock solution coloring polyester fiber short fiber.
Example 8
Adding the colorant C.I. solvent red 207 and the polybutylene succinate polyol with the molecular weight of 2000 into a coloring mother liquor preparation tank according to the weight ratio of 45:55, and stirring to fully dissolve the colorant C.I. solvent red 207 into the polybutylene succinate polyol at the preparation temperature of 120 ℃ to obtain the coloring mother liquor with the colorant C.I. solvent red 207 content of 45 wt%. And then transferring the prepared coloring mother liquor into a coloring mother liquor supply tank for standby application, wherein the supply temperature of the coloring mother liquor is 50 ℃.
The coloring mother liquor with the mass of 20wt% and the titanium catalyst with the mass of 0.1 wt% are injected into the butylene terephthalate oligomer with the polymerization degree of 5 from the esterification system, the materials are uniformly mixed by a high shear homogenizing pump and then enter a pre-polycondensation system for pre-polycondensation reaction, the pre-polycondensation reaction temperature is 240 ℃, the reaction time is 40min, and the coloring prepolymer with the intrinsic viscosity of 0.30dL/g is obtained.
And filtering the colored prepolymer by a prepolymer filter, and then feeding the filtered colored prepolymer into a final polycondensation system for final polycondensation reaction, wherein the final polycondensation reaction temperature is 245 ℃ and the reaction time is 90min, so as to obtain a colored polyester melt with the intrinsic viscosity of 0.95 dL/g.
And filtering the colored polyester melt by a melt filter, and then, spinning in a spinning box at the spinning temperature of 245 ℃ at the winding speed of 1500m/min to obtain the dope-colored polyester fiber undrawn yarn. Then, primary drawing is carried out at 50 ℃, the drawing multiple is 2 times, secondary drawing is carried out at 70 ℃, the drawing multiple is 1.5 times, and then the fiber is curled, wherein the curling temperature is 50 ℃. Then heat-set at 80 ℃ for 15 minutes. And cutting the shaped fiber on a cutting machine, and packaging to obtain the stock solution coloring polyester fiber short fiber.
Example 9
Adding the colorant C.I. solvent yellow 163 and the polyethylene glycol adipate polyol with the molecular weight of 2000 into a coloring mother liquor preparation tank according to the weight ratio of 40:60, and fully dissolving the colorant C.I. solvent yellow 163 into the polyethylene glycol adipate polyol by stirring under the condition that the preparation temperature is 120 ℃ to obtain the coloring mother liquor with the colorant C.I. solvent yellow 163 content of 40 wt%. And then transferring the prepared coloring mother liquor into a coloring mother liquor supply tank for standby application, wherein the supply temperature of the coloring mother liquor is 60 ℃.
The coloring mother liquor with the mass of 15 wt% and the titanium catalyst with the mass of 0.1 wt% are injected into the polytrimethylene terephthalate oligomer with the polymerization degree of 5 from the esterification system, the materials are uniformly mixed by a high shear homogenizing pump and then enter a pre-polycondensation system for pre-polycondensation reaction, the pre-polycondensation reaction temperature is 230 ℃, the reaction time is 120min, and the coloring prepolymer with the intrinsic viscosity of 0.35dL/g is obtained.
And filtering the colored prepolymer by a prepolymer filter, and then feeding the filtered colored prepolymer into a final polycondensation system for final polycondensation reaction, wherein the final polycondensation reaction temperature is 240 ℃, and the reaction time is 240min, so that a colored polyester melt with the intrinsic viscosity of 1.20dL/g is obtained.
And (3) filtering the colored polyester melt by a melt filter, and then, spinning in a spinning box at 235 ℃ at a winding speed of 800m/min to obtain the dope-colored polyester fiber undrawn yarn. Then, primary drawing is carried out at 60 ℃, the drawing multiple is 3 times, secondary drawing is carried out at 80 ℃, the drawing multiple is 1.8 times, and then the fiber is curled, wherein the curling temperature is 60 ℃. Then heat-set at 90 ℃ for 15 minutes. And cutting the shaped fiber on a cutting machine, and packaging to obtain the stock solution coloring polyester fiber short fiber.
Comparative example 1
Adding the colorant C.I. solvent red 135 and the polybutylene adipate polyol with the molecular weight of 4000 into a coloring mother liquor preparation tank according to the weight ratio of 30:70, and fully dissolving the colorant C.I. solvent red 135 into the polybutylene adipate polyol by stirring under the condition that the preparation temperature is 150 ℃ to obtain the coloring mother liquor with the colorant C.I. solvent red 135 content of 30 wt%. And then transferring the prepared coloring mother liquor into a coloring mother liquor supply tank for standby, wherein the supply temperature of the coloring mother liquor is 100 ℃.
The coloring mother solution with the mass of 12 wt% is injected into polyethylene glycol terephthalate melt with the intrinsic viscosity of 0.67dL/g from a final polycondensation system, the materials are filtered by a melt filter after being uniformly mixed and then enter a spinning manifold for spinning, the spinning temperature is 280 ℃, the winding speed is 4500m/min, and the dope coloring polyester fiber fully drawn yarn FDY is obtained. Wherein the speed of the hot roller GR1 is 1700m/min, the temperature is 80 ℃, the speed of the hot roller GR2 is 4500m/min, and the temperature is 125 ℃.
Comparative example 2
Adding a colorant C.I. solvent red 168 and polyethylene glycol succinate polyol with the molecular weight of 300 into a coloring mother liquor preparation tank according to the weight ratio of 10:90, and stirring to fully dissolve the colorant C.I. solvent red 168 into the polyethylene glycol succinate polyol at the preparation temperature of 100 ℃ to obtain the coloring mother liquor with the colorant C.I. solvent red 168 content of 10 wt%. And then transferring the prepared coloring mother liquor into a coloring mother liquor supply tank for standby application, wherein the supply temperature of the coloring mother liquor is 50 ℃.
Injecting the coloring mother solution with the mass of 5.3 wt% into polybutylene terephthalate melt with the intrinsic viscosity of 1.05dL/g from a final polycondensation system, uniformly mixing the materials, filtering the materials by a melt filter, and then feeding the materials into a spinning manifold for spinning at the spinning temperature of 255 ℃ and the winding speed of 5200m/min to obtain the dope-colored fully drawn polyester fiber FDY. Wherein the speed of the hot roller GR1 is 2400m/min, the temperature is 60 ℃, the speed of the hot roller GR2 is 5250m/min, and the temperature is 120 ℃.
Comparative example 3
Adding a colorant C.I. solvent yellow 116 and polypropylene sebacate polyol with molecular weight of 2000 into a coloring mother liquor blending tank according to the weight ratio of 10:90, and fully dissolving the colorant C.I. solvent yellow 116 into the polypropylene sebacate polyol by stirring under the condition that the blending temperature is 100 ℃ to obtain the coloring mother liquor with the colorant C.I. solvent yellow 116 content of 10 wt%. And then transferring the prepared coloring mother liquor into a coloring mother liquor supply tank for standby application, wherein the supply temperature of the coloring mother liquor is 80 ℃.
And (2) injecting 10 wt% of the coloring mother solution into a polybutylene terephthalate melt with the intrinsic viscosity of 1.00dL/g from a final polycondensation system, uniformly mixing the materials, filtering the materials by a melt filter, and then feeding the filtered materials into a spinning manifold for spinning at the spinning temperature of 250 ℃ and the winding speed of 3500m/min to obtain the dope-colored fully drawn polyester fiber FDY. Wherein the speed of the hot roller GR1 is 1400m/min, the temperature is 50 ℃, the speed of the hot roller GR2 is 3550m/min, and the temperature is 105 ℃.
Comparative example 4
5kg of rubber carbon black is put into a special reaction kettle
Adding 5kg of rubber carbon black N322 into 70kg of water as a dispersion medium, fully grinding, slowly heating to boil, adding a graft compound of butylene terephthalate, simultaneously adding a proper amount of catalyst tetrapropyl titanate, and fully reacting by stirring at the blending temperature of 230 ℃ to obtain the carbon black slurry with low twist.
And (2) metering and adding the carbon black slurry into a polybutylene terephthalate oligomer conveying pipeline on line through a slurry adding system, uniformly mixing through a homogenizing system, and respectively entering a pre-polycondensation kettle and a final polycondensation kettle for reaction to obtain a black polyester melt with the intrinsic viscosity of 1.20 dL/g.
And (3) filtering the colored polyester melt by a melt filter, and then, spinning the colored polyester melt in a spinning manifold at the spinning temperature of 280 ℃ and the winding speed of 4500m/min to obtain the dope colored polyester fiber fully drawn yarn FDY. Wherein the speed of the hot roller GR1 is 1700m/min, the temperature is 80 ℃, the speed of the hot roller GR2 is 4550m/min, and the temperature is 125 ℃.
Test example 1
The following test method is adopted to carry out performance characterization test on the dope-dyed polyester fiber:
the intrinsic viscosity is η (dL/g), and the test method refers to GB/T14190-2008.
Line density (dtex), test method: the short fibers refer to GB/T14335-;
breaking strength (cN/dtex) and elongation at break (%), test method: the short fibers refer to GB/T14337-;
modulus (cN/dtex), test method: the short fibers refer to GB/T14337-;
color uniformity (gray card) (grade) test method: reference is made to GB/T6508-2001.
Colorant content (wt%) test method: reference GB/T9337-
The dope-dyed polyester fibers prepared in examples 1 to 9 and comparative examples 1 to 4 were subjected to a performance characterization test, and the test results are shown in table 1:
TABLE 1 Performance test results for dope-dyed polyester fibers prepared in examples 1 to 9 and comparative examples 1 to 4
As can be seen from Table 1, the test results of the dope dyed polyester fibers of comparative examples 1 to 3 and comparative examples 1 to 3 show that the breaking strength and the breaking elongation of examples 1 to 3, which adopt the pre-polycondensation process of the dyed mother liquid and the polyester oligomer, are improved, and the strength of the fibers is enhanced; the modulus is reduced, and the softness of the fiber is improved; the content of the coloring agent and the color uniformity are improved, which shows that the coloring effect of the polyester pre-polycondensation polyester; further analyzing the change of the intrinsic viscosity of the polyester fiber from the colored polyester melt to the spun finished product, it can be seen that the viscosity of the spun finished product prepared in examples 1-3 is reduced less than that of the spun finished product prepared in comparative examples 1-3, the product has larger relative molecular mass, and the property tends to be more stable. In conclusion, the process of pre-polycondensation of the coloring mother liquor and the polyester oligomer has excellent effects of improving the mechanical property, flexibility, color uniformity and stability of the dope coloring polyester fiber product.
Further analysis, comparing the fiber properties of example 1 and comparative example 4 prepared by the method disclosed in chinese patent application No. 201410709477.7, although comparative example 4 is superior to example 1 in elongation at break, the fiber prepared in example 1 is inferior in breaking strength, modulus, and more important colorant content and color uniformity, and the viscosity of comparative example 4 is remarkably decreased, so it can be considered that although the process of pre-polycondensation of the coloring mother liquor and the polyester oligomer is also used, the coloring mother liquor of comparative example 4 needs to perform grafting reaction on the pigment and the carrier, resulting in non-ideal combination effect with the polyester oligomer when entering into the polycondensation reaction, and thus causing inferior mechanical properties and color; in contrast to example 1 of the present invention, in the coloring mother liquor stage, the polyester polyol and the ester-soluble pigment are physically mixed, and in the polycondensation process with the polyester oligomer, the polyester polyol can be used as a block for increasing the flexibility of a molecular chain to enter a main chain, so that the flexibility of a fiber product is improved and the use hand feeling is improved on the premise of not affecting the compatibility of the coloring mother liquor and the polyester oligomer.
Further analyzing that the aliphatic polyester polyols with different polymerization degrees are used in the false twist textured yarn DTY prepared in examples 4 to 9 and examples 4 to 6, the obtained polyester melt viscosity and the polymerization degree of the aliphatic polyester polyol show the same change trend, and the polyester melt viscosity and the polymerization degree of the aliphatic polyester polyol show the opposite change trend when the aliphatic polyester polyols with different polymerization degrees are used in the dope dyed polyester fiber short fiber prepared in examples 7 to 9, it can be seen that the polymerization degree of the aliphatic polyester polyol has certain influence on the product performance in different fiber products produced by the method of the present invention.
Further, as a result of analyzing examples 1 to 3 and 4 to 6, it was found that the content of the catalyst added in the step of prepolycondensation of the coloring mother liquor and the polyester oligomer and the change in modulus of the product are in a reverse trend, and the modulus decrease trend is more remarkable as the content of the catalyst is increased, and thus it was found that the prepolycondensation reaction of the coloring mother liquor and the polyester oligomer has a large influence on the modulus of the product because the degree of bonding of the aliphatic polyester polyol and the polyester oligomer affects the modulus of the product.
Further analyzing examples 2, 3, 5 and 6, it can be seen that the breaking strength and the breaking elongation of the colored prepolymer and the colored polyester melt change obviously with the changes of the reaction time, the reaction temperature, the viscosity of the colored prepolymer and the colored polyester melt during the pre-polycondensation and final polycondensation reaction of the colored mother liquor and the polyester oligomer, and the reaction conditions of the pre-polycondensation and the final polycondensation have a great influence on the mechanical properties of the product, and can be adjusted according to the requirements of the product during the actual production process.
In summary, the method for preparing the dope-dyed polyester fiber provided by the invention uses the ester-soluble colorant and the aliphatic polyester polyol as the coloring mother liquor, so that the colorant molecules are uniformly dispersed in the polyester polymer, the influence of the dispersion degree of the colorant on the spinnability of the colored polyester melt is effectively eliminated, and the prepared dope-dyed polyester fiber has stable quality and no color difference. In addition, the aliphatic polyester polyol with a flexible molecular chain structure can be subjected to polycondensation reaction with the polyester oligomer in the pre-polycondensation process to be embedded into a polyester molecular main chain, so that the compatibility problem between a colorant carrier and the polyester polymer can be thoroughly solved, and the colored polyester melt has good spinnability; on the other hand, the regularity of the polyester molecular chain can be damaged, the flexibility of the molecular chain is improved, the prepared fiber is endowed with soft hand feeling, and the comfort level of the fabric is improved. The polymerization degree of the aliphatic polyester polyol, the catalyst content of the pre-polycondensation reaction, and the selection of the temperature, time and melt viscosity in the pre-polycondensation reaction and the final polycondensation reaction are all important factors in the preparation method of the invention.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the dope-dyed polyester fiber is characterized by comprising the following steps:
(1) adding a colorant into a carrier polyester polyol to prepare a uniform coloring mother solution, wherein the content of the colorant is 5-40 wt%;
(2) injecting the coloring mother liquor prepared in the step (1) and a catalyst into a polyester oligomer pipeline on line, uniformly mixing the coloring mother liquor and the catalyst with a polyester oligomer with a polymerization degree of 1-8 from an esterification system through a dynamic mixer, and then feeding the mixture into a pre-polycondensation system for pre-polycondensation reaction to obtain a coloring prepolymer with a viscosity of 0.15-0.45 dL/g;
(3) filtering the colored prepolymer prepared in the step (2) by using a prepolymer filter, and then, allowing the filtered colored prepolymer to enter a final polycondensation system for final polycondensation reaction to obtain a colored polyester melt with the viscosity of 0.50-1.20 dL/g;
(4) filtering the colored polyester melt prepared in the step (3) by a melt filter, and then, spinning and drafting the colored polyester melt in a spinning manifold to obtain stock solution colored polyester fibers;
the colorant in the step (1) is an ester-soluble colorant;
the polyester polyol in the step (1) is aliphatic polyester polyol with the molecular weight of 300-10000, and the aliphatic polyester polyol is one of polybutylene adipate, polyethylene glycol succinate, polypropylene glycol sebacate, polyethylene glycol adipate, polypropylene glycol adipate, polyethylene glycol sebacate, polybutylene succinate and polyethylene glycol adipate;
in the step (2), the online injection amount of the coloring mother liquor is 3-20 wt% of the mass of the polyester oligomer;
in the step (2), the polyester oligomer is selected from one of ethylene terephthalate oligomer, trimethylene terephthalate oligomer and butylene terephthalate oligomer.
2. The method for preparing a dope-dyed polyester fiber as claimed in claim 1, wherein the amount of the catalyst added in the step (2) is 0.003 to 0.2wt% based on the mass of the polyester oligomer, and the catalyst is at least one of an antimony-based catalyst, a titanium-based catalyst and a germanium-based catalyst.
3. The method for preparing dope-dyed polyester fiber according to claim 1, wherein in the step (1), the blending temperature of the dyeing mother liquor is 100-200 ℃ and the supply temperature is 50-150 ℃.
4. The method for preparing dope-dyed polyester fiber according to claim 1, wherein in the step (2), the reaction temperature of the pre-polycondensation reaction is 230 to 275 ℃, and the reaction time is 40 to 120 min.
5. The method for preparing dope-dyed polyester fiber according to claim 4, wherein the reaction temperature of the pre-polycondensation is 240-265 ℃ and the reaction time is 60-90 min.
6. The method for preparing dope-dyed polyester fiber according to claim 1, wherein in the step (3), the reaction temperature of the final polycondensation is 240 to 285 ℃, and the reaction time is 60 to 240 min.
7. The method for preparing dope-dyed polyester fiber as claimed in claim 6, wherein in the step (3), the reaction temperature of the final polycondensation is 245-270 ℃ and the reaction time is 90-180 min.
8. The method for preparing the dope-dyed polyester fiber as claimed in claim 1, wherein in the step (4), the spinning temperature of the dope-dyed polyester fiber is 235-295 ℃.
9. The method for preparing the dope-dyed polyester fiber as claimed in claim 8, wherein in the step (4), the spinning temperature of the dope-dyed polyester fiber is 245-280 ℃.
10. The dope dyed polyester fiber produced by the process according to any one of claims 1 to 9, wherein the dope dyed polyester fiber has a colorant content of 0.5 to 7.5wt%, a color uniformity of 3 to 5 steps, and a modulus of 20 to 90 cN/dtex.
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| CN108774312B (en) * | 2018-06-29 | 2020-09-04 | 浙江尤夫高新纤维股份有限公司 | Low-viscosity polyester and preparation method thereof |
| CN109385920B (en) * | 2018-10-25 | 2021-04-16 | 绍兴九洲化纤有限公司 | Dyeing process of poly (butylene succinate) fibers |
| CN112176447B (en) * | 2020-10-20 | 2022-12-20 | 苏州世名科技股份有限公司 | Colored polyester fiber and preparation method thereof |
| CN112962156B (en) * | 2021-02-01 | 2022-05-17 | 杭州飞来创意设计有限公司 | Zero-emission high-fastness stock solution coloring process |
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