CN109666990B - Super-soft polyester composite yarn and preparation method thereof - Google Patents

Super-soft polyester composite yarn and preparation method thereof Download PDF

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CN109666990B
CN109666990B CN201811615736.4A CN201811615736A CN109666990B CN 109666990 B CN109666990 B CN 109666990B CN 201811615736 A CN201811615736 A CN 201811615736A CN 109666990 B CN109666990 B CN 109666990B
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modified polyester
tert
polyester
butyl
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CN109666990A (en
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汤方明
尹立新
陈锋
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Jiangsu Hengli Chemical Fiber Co Ltd
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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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • 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
    • C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
    • C08G63/695—Polyesters containing atoms other than carbon, hydrogen and oxygen containing silicon
    • C08G63/6954—Polyesters containing atoms other than carbon, hydrogen and oxygen containing silicon derived from polxycarboxylic acids and polyhydroxy compounds
    • C08G63/6956—Dicarboxylic acids and dihydroxy compounds
    • 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
    • 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
    • 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
    • D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
    • 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
    • D01D5/12—Stretch-spinning methods
    • D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)
  • Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)

Abstract

The invention relates to an ultra-soft polyester composite yarn and a preparation method thereof, wherein the preparation method comprises the following steps: firstly introducing dihydric alcohol with silicon in a main chain and dibasic acid with a tert-butyl side group into polyester to prepare modified polyester, then preparing modified polyester FDY yarns and modified polyester POY yarns from modified polyester melts according to an FDY process and a POY process respectively, and then doubling the modified polyester FDY yarns and the modified polyester POY yarns, wherein the dihydric alcohol with silicon in the main chain is dimethyl silicon glycol, dimethyl diphenyl disiloxane glycol or tetramethyl disiloxane glycol, the dibasic acid with the tert-butyl side group is 5-tert-butyl-1, 3-phthalic acid, 2-tert-butyl-1, 6-hexanedicarboxylic acid, 3-tert-butyl-1, 6-hexanedicarboxylic acid or 2, 5-di-tert-butyl-1, 6-hexanedicarboxylic acid, the dye uptake of the ultra-soft polyester composite yarns at the temperature of 123 ℃ is 86.3-90.2%, and the K/S value is 21.15-23.4. The method of the invention has simple operation, and the prepared fiber has good dyeing property.

Description

Super-soft polyester composite yarn and preparation method thereof
Technical Field
The invention belongs to the technical field of modified fibers, and relates to an ultra-soft polyester composite yarn and a preparation method thereof.
Background
The polyester fiber has good physical and chemical properties due to the unique chemical structure of the polyester macromolecular chain, and the fabric prepared from the polyester fiber is stiff and smooth, but the unique chemical structure of the polyester fiber endows the polyester fiber and the fabric thereof with the defects of low hygroscopicity, poor antistatic property, easiness in fluffing and pilling, stiff hand feeling, poor hair feeling, strong wax texture and the like. Along with the improvement of living standard of people, the wearing requirement of clothes is continuously improved, and the defects of the clothes are increasingly revealed. With the fine denier of the fiber, the specific surface area of the fiber is increased, the adsorption capacity is increased, and the prepared fabric has small and many micropores and has the characteristics of soft hand feeling, good drapability, good air permeability and the like. The fine denier of the fiber overcomes the inherent disadvantages of the polyester fiber.
According to the results of the current research, the ultra-fine denier fiber mainly has the following six characteristics: 1) the diameter is small, the bending resistance is small, and the yarn is softer; 2) the specific surface area is increased, and the water absorption and oil absorption are improved; 3) the specific surface area is increased, and the fluffiness and the coverage are improved; 4) the high filling density generates a microclimate effect, and the heat retention is improved; 5) the wicking property of the capillary is improved, and the moisture permeability of the fabric is improved; 6) the strength of the monofilament is low, which is beneficial to post-treatment processing such as sanding. The super fine denier polyester fiber is most used in clothing, is an important raw material of high-quality fabrics, and can be blended with nylon micro fine denier fiber or cotton fiber and the like or used independently to weave materials with excellent hand feeling, such as artificial chamois and peach skin, or produce fabrics with reduced friction resistance, such as ski and skating clothes, or produce moisture-absorbing and sweat-releasing fabrics, such as high-grade sportswear and other high-grade fabrics.
The smaller diameter of the individual fibers, i.e. the lower fiber titer, results in a rapid increase in the total surface area of the finished yarn and textile, which increases exponentially, especially when the fiber titer is less than 1 dtex. The refracted light after the fiber is dyed depends only on the refracted light returning to the outside from the inside of the fiber, and the hue and shade of the light depends on the light directly reflected by the surface and the refracted light returning to the outside from the inside of the dyed fiber. Fine or ultra-fine denier fibers having a large surface reflection are much lighter in color than large denier fibers dyed with the same amount of dye. This is mainly because the finer the fineness of the fiber, the greater the surface reflection light, and the more difficult it is to dye a deep color. The larger the specific surface area of the fiber, the lighter the color development of the fine-denier yarn fabric, and if the fabric is dyed in a dark color, the larger the dye dosage is needed.
Therefore, a fine denier soft fiber that is easily dyed in a dark color is urgently under study.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides the ultra-soft polyester composite yarn easy to be dyed in dark color and the preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
the preparation method of the super-soft polyester-polyester composite filament comprises the steps of preparing modified polyester FDY filaments and modified polyester POY filaments from modified polyester melts according to an FDY process and a POY process respectively, and then doubling the modified polyester FDY filaments and the modified polyester POY filaments to obtain the super-soft polyester-polyester composite filament;
the preparation method of the modified polyester comprises the following steps: uniformly mixing terephthalic acid, ethylene glycol, dihydric alcohol with a silicon-containing main chain and dibasic acid with a tert-butyl side group, and then sequentially carrying out esterification reaction and polycondensation reaction;
the dihydric alcohol with silicon in the main chain is dimethyl silicon glycol, dimethyl diphenyl disiloxane glycol or tetramethyl disiloxane glycol, and the dibasic acid with tertiary butyl side group is 5-tertiary butyl-1, 3-phthalic acid, 2-tertiary butyl-1, 6-hexanedicarboxylic acid, 3-tertiary butyl-1, 6-hexanedicarboxylic acid or 2, 5-di-tertiary butyl-1, 6-hexanedicarboxylic acid.
According to the invention, terephthalic acid, ethylene glycol, dihydric alcohol with silicon-containing main chain and dibasic acid with tertiary butyl side group are uniformly mixed and then are subjected to esterification reaction and polycondensation reaction, namely, the dibasic acid with tertiary butyl side group and the dihydric alcohol with silicon-containing main chain are introduced into a polyester molecular chain, so that the free volume of the hollow cavity of the polyester is obviously increased. Disperse dyes are a class of dyes that are relatively small in molecule and structurally free of water-soluble groups, mostly in the form of particles, with a particle size of between a few hundred nanometers and a micron. When the modified polyester begins to dye, along with the continuous improvement of temperature, because the polyester macromolecular chain contains-Si-O-Si-bonds, the silicon-oxygen bonds are longer than the carbon-oxygen bonds, the internal rotation activation energy is lower, the molecular chain containing the carbon-oxygen bonds starts to move firstly, when the dye bath temperature needs to be improved to 120-130 ℃, the intensity of the movement of the macromolecular chain containing the silicon-oxygen bonds is larger than that of the molecular chain containing only the carbon-oxygen bonds, simultaneously, because the cavity free volume is larger, the cavity free volume formed by the macromolecular chain containing the silicon-oxygen bonds is higher than that of the molecular chain containing only the carbon-oxygen bonds, simultaneously, the dibasic acid chain segment with the tertiary butyl side group in the polyester macromolecular chain starts to move before the molecular chain starts to dye, when the dye bath temperature is improved, the intensity of the dibasic acid chain segment with the tertiary butyl side group is larger than that of the molecular chain, and simultaneously, because the cavity free volume formed by the tertiary butyl side group is larger than that of the, therefore, the diffusion rate of the granular dye to the inside of the fiber is remarkably improved, the small dye molecules can be more easily permeated into the modified polyester macromolecules, the dyeing and the like of the fiber are positively influenced, the dyeing temperature can be reduced, the dyeing time is shortened, the energy consumption is reduced, the dye-uptake and the color depth of the fiber are improved, and the fine-denier soft polyester fiber can be easily dyed in deep color.
As a preferred technical scheme:
in the preparation method of the super soft polyester-polyester composite filament, the synthesis method of the 2-tert-butyl-1, 6-hexanedicarboxylic acid, the 3-tert-butyl-1, 6-hexanedicarboxylic acid and the 2, 5-di-tert-butyl-1, 6-hexanedicarboxylic acid comprises the following steps:
firstly, mixing tungstic acid and hydrogen peroxide, stirring for 10-15 min at room temperature, then adding raw material alcohol, reacting for 1-2 h at the temperature of 80-85 ℃, then heating to 90-95 ℃ and reacting for 2-3 h, wherein reactants are always in a reflux state in the reaction process, and finally cooling, crystallizing, washing and refining;
when the reaction starts, the molar ratio of the tungstic acid to the raw material alcohol to the hydrogen peroxide is 1: 30-40: 120-150;
the raw material alcohols corresponding to the 2-tert-butyl-1, 6-hexanedicarboxylic acid, the 3-tert-butyl-1, 6-hexanedicarboxylic acid and the 2, 5-di-tert-butyl-1, 6-hexanedicarboxylic acid are respectively 2-tert-butylcyclohexanol, 4-tert-butylcyclohexanol and 2, 4-di-tert-butylcyclohexanol.
The preparation method of the super-soft polyester-polyester composite yarn comprises the following steps:
(1) performing esterification reaction;
preparing terephthalic acid, ethylene glycol, dihydric alcohol with a silicon-containing main chain and dibasic acid with a tert-butyl side group into slurry, adding a catalyst, a delustering agent and a stabilizer, uniformly mixing, pressurizing in a nitrogen atmosphere to perform esterification reaction, wherein the pressurizing pressure is normal pressure to 0.3MPa, the esterification reaction temperature is 250-260 ℃, and the esterification reaction end point is determined when the water distillation amount in the esterification reaction reaches more than 90% of a theoretical value;
(2) performing polycondensation reaction;
and after the esterification reaction is finished, starting the polycondensation reaction in the low vacuum stage under the negative pressure condition, stably pumping the pressure in the low vacuum stage from normal pressure to below 500Pa in 30-50 min at the reaction temperature of 250-260 ℃ for 30-50 min, then continuously pumping the vacuum to perform the polycondensation reaction in the high vacuum stage, so that the reaction pressure is further reduced to below 100Pa, the reaction temperature is 270-275 ℃, and the reaction time is 50-90 min.
The mole ratio of the terephthalic acid to the ethylene glycol is 1: 1.2-2.0, the sum of the addition amounts of the dibasic acid with the silicon-containing main chain and the dibasic acid with the tertiary butyl side group is 3.5-5 mol% (mole percentage) of the addition amount of the terephthalic acid, the addition amount of the dibasic acid with the tertiary butyl side group and the dibasic acid with the silicon-containing main chain of the invention is preferably in the range, so that the modified fiber has good mechanical property and crystallinity, the dyeing property of the fiber can be obviously improved, the production and the application of the fiber are facilitated, the addition amounts of the dibasic acid with the tertiary butyl side group and the dibasic acid with the silicon-containing main chain can be properly adjusted according to the actual needs, but are not too large, the excessively high addition amount has too much damage to the regularity of a polyester macromolecular structure, and has too much influence on the crystallinity and the mechanical property of the fiber, and is not favorable for the production and the application of the fiber, if the dyeing rate is too low, the dyeing effect is not obviously improved; the mole ratio of the dihydric alcohol with silicon in the main chain to the dibasic acid with the tertiary butyl side group is 1.5-2: 2-3, the addition amounts of the catalyst, the flatting agent and the stabilizer are respectively 0.03-0.05 wt%, 0.20-0.25 wt% and 0.01-0.05 wt% of the addition amount of the terephthalic acid, the dibasic alcohol with silicon in the main chain and the dibasic acid with the tertiary butyl side group provide cavity free volume, the two are matched with each other, and when the effects of the two are exerted, the effect is optimal.
According to the preparation method of the super-soft polyester composite filament, the catalyst is antimony trioxide, ethylene glycol antimony or antimony acetate, the flatting agent is titanium dioxide, and the stabilizer is triphenyl phosphate, trimethyl phosphate or trimethyl phosphite.
According to the preparation method of the super-soft polyester-polyester composite filament, the number average molecular weight of the modified polyester is 25000-30000, and the molecular weight distribution index is 1.8-2.2.
According to the preparation method of the super-soft polyester-polyester composite filament, the process of the FDY process comprises the following steps: metering, spinneret plate extruding, cooling, oiling, stretching, heat setting and winding;
the FDY process comprises the following parameters: the spinning temperature is 285-300 ℃, the cooling temperature is 20-25 ℃, the network pressure is 0.20-0.30 MPa, the first roller speed is 850-950 m/min, the first roller temperature is 98-110 ℃, the two roller speed is 3250-3670 m/min, and the two roller temperature is 120-135 ℃;
the POY process comprises the following steps: metering, spinneret plate extrusion, cooling, oiling and winding;
the parameters of the POY process are as follows: the spinning temperature is 280-290 ℃, and the cooling temperature is 18-22 ℃;
the winding speed during doubling is 3200-3600 m/min.
The invention also provides the super-soft polyester composite filament prepared by the preparation method of the super-soft polyester composite filament, which is mainly formed by compounding modified polyester FDY filaments and modified polyester POY filaments;
the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment, a dihydric alcohol chain segment with a silicon-containing main chain and a dibasic acid chain segment with a tert-butyl side group;
the filament number of the modified polyester FDY yarn and the filament number of the modified polyester POY yarn are respectively 0.30-0.50 dtex and 0.28-0.35 dtex.
As a preferred technical scheme:
the titer of the super-soft polyester-polyester composite filament is 75-90 dtex, and the titer ratio of the modified polyester FDY filament to the modified polyester POY filament in the super-soft polyester-polyester composite filament is 2-3: 3-5;
the breaking strength of the super-soft polyester composite filament is more than or equal to 2.0cN/dtex, the elongation at break is 43.0 +/-3.0%, the linear density CV value is less than or equal to 1.00%, the breaking strength CV value is less than or equal to 5.00%, the elongation at break CV value is less than or equal to 8.00%, the boiling water shrinkage is 55.0 +/-8.0%, the oil content is 0.80 +/-0.20 wt%, and the yarn evenness CV value is less than or equal to 2.50%.
According to the super-soft polyester-polyester composite yarn, the dye uptake of the super-soft polyester-polyester composite yarn at the temperature of 123 ℃ is 86.3-90.2%, the K/S value is 21.15-23.4, the soaping color fastness reaches 5 level, the dry rubbing fastness reaches 5 level, and the wet rubbing fastness is higher than 4 level; under the same other test conditions, the dye uptake of a comparison sample under the temperature condition of 130 ℃ is 84.7%, the K/S value is 19.56, the soaping-resistant color fastness is less than grade 5, the dry rubbing fastness is grade 4-5, the wet rubbing fastness is grade 3-4, and the comparison sample is different from the super-soft polyester composite yarn only in that the material is common polyester.
The invention mechanism is as follows:
the macromolecular chains in the polymer are not completely tightly packed, and voids always exist among the macromolecular chains, and the void volume is the free volume. Since small molecules are allowed to penetrate into the polymer, voids are sufficiently large in the polymer or between the polymers, the permeability and diffusivity of the small molecules are related to the size of the voids (i.e., the size of free volume) in the polymer structure, and within a certain range, the larger the size of the free volume, the higher the permeability of the small molecules, and the better the diffusivity. The free volume is divided into a cavity free volume and a slit free volume, the cavity free volume has larger space size than the slit free volume, and the effect of increasing the cavity free volume and increasing the slit free volume is more obvious for improving the permeability of small molecules.
The size and type of free volume depends mainly on the structure of the polymer, and the main factors influencing the structure of the polymer are steric hindrance, the size of the side group, the structure of the side group and the like. When a certain position on the main chain of the polymer is substituted by a side group, the activity change of the main chain is inevitably caused, so that the interaction force between chains is changed, the distance between the chains is also correspondingly changed, and consequently, the cohesive energy and the free volume are changed, and the polarity, the size, the length and the like of the substituent on the side chain of the macromolecule have certain influences on the rigidity of the molecular chain, the interaction between molecules and the free volume fraction of the polymer structure, so that the effects generated by different substituents are different, and the osmotic separation performance of the polymer is often different.
According to the invention, terephthalic acid, ethylene glycol, dihydric alcohol with silicon-containing main chain and dibasic acid with tertiary butyl lateral group are uniformly mixed and then subjected to esterification reaction and polycondensation reaction, namely, the dibasic acid with tertiary butyl lateral group and the dihydric alcohol with silicon-containing main chain are introduced into a polyester molecular chain, so that the dyeing property of the super soft polyester composite yarn is remarkably improved, and the method comprises the following steps:
for straight chain molecules such as isophthalic acid and adipic acid, when the H atom on the benzene ring of isophthalic acid or the H atom on the methylene group of adipic acid is replaced by a methyl group (-CH)3) When in substitution, the C atoms on the side groups and the main chain C atoms are not in the same plane, so that four sp3 hybridized orbitals on the center C are respectively overlapped with empty orbitals on the four surrounding C atoms to form four completely same sigma bonds which are arranged in a regular tetrahedron, the four carbon atoms are respectively positioned at four vertexes of the regular tetrahedron, when three hydrogen of a methyl group is further substituted by the methyl group, the three hydrogen is equivalent to tert-butyl to be substituted to form a larger tetrahedron structure, molecular chains arranged in the regular tetrahedron are relatively arranged in a zigzag manner, the free volume of the empty holes is obviously increased by a lot, and the permeability and diffusivity of small molecules can be obviously improved; when the H atom on the benzene ring of the isophthalic acid or the H atom on the methylene of the adipic acid is replaced by the long branched chain substituent, the slit free volume is mainly increased, the increase amplitude is small, the improvement effect on the permeability and the diffusivity of the small molecule is limited, and meanwhile, the long branched chain substituent has small rigidity, the molecular chains are easy to tangle, and the increase of the free volume is not facilitated.
The dibasic acid with the tertiary butyl side group is 5-tertiary butyl-1, 3-phthalic acid, 2-tertiary butyl-1, 6-adipic acid, 3-tertiary butyl-1, 6-adipic acid or 2, 5-di-tertiary butyl-1, 6-adipic acid, wherein the 2-tertiary butyl-1, 6-adipic acid, 3-tertiary butyl-1, 6-adipic acid and 2, 5-di-tertiary butyl-1, 6-adipic acid are adipic acid, and the adipic acid is fatty acid, the rigidity of the fatty acid is less than that of the 5-tertiary butyl-1, 3-phthalic acid, which is beneficial to improving the softness of a polyester chain segment, and the existence of the tertiary butyl in the dibasic acid with the tertiary butyl side group can cause the change of the activity of a main chain so as to change the interaction force among chain units, the distance between molecular chain units is also changed correspondingly, which leads to the increase of the free volume of the hollow of the modified polyester. Compared with short-chain substituent groups (such as methyl, ethyl and the like), the tertiary butyl group occupies a larger spatial position, and a larger free volume is obtained in the molecular chain arrangement mode; compared with the long-branched-chain substituent, on one hand, the tertiary butyl group has the increased free volume of a cavity, the long-branched-chain substituent has the increased free volume of a slit, and on the other hand, the rigidity of the tertiary butyl group is higher than that of the long-branched-chain substituent, so that entanglement among molecular chains is reduced, and the tertiary butyl group has more free volume than the long-branched-chain substituent in the arrangement mode of the molecular chains. In addition, when the dibasic acid with the tertiary butyl side group is 5-tertiary butyl-1, 3-phthalic acid, a benzene ring connected with the m-phthalic acid forms a larger asymmetric chain segment, so that the steric hindrance of inter-chain-segment migration is increased, the steric hindrance of rotation around a m-connection bond in the chain segment is increased, the introduction of the m-isomer is favorable for increasing the free volume, and the introduction of the dibasic acid with the tertiary butyl side group increases the free volume of a cavity of the modified polyester.
The dihydric alcohol with the silicon-containing main chain is dimethyl silicon glycol, dimethyl diphenyl disiloxane glycol or tetramethyl disiloxane glycol, and the structural formulas are respectively as follows:
Figure BDA0001925792120000071
the rigidity of the high molecular chain is determined by the size of a rotation potential barrier in the molecular chain, the main chain structures are different, wherein the bond angles and bond lengths are different or the bonding modes are different, the rigidity is also different, after the diatomic alcohol with silicon in the main chain is introduced, the high molecular main chain contains-Si-O-Si-bonds, the silicon-oxygen bond gaps are larger, the internal rotation activation energy is lower, the free rotation of atoms is facilitated, and meanwhile, the Si atoms and-CH on the high molecular main chain3Is connected to-CH3Perpendicular to the plane of the Si-O-Si atom, the-CH results from the Si-C bond being longer than the C-C bond3Three of H are in a spread state, -CH3Three propped H atoms in the polymer material can freely rotate to increase the distance between adjacent Si-O molecular chain segments, and in addition, the inert methyl of the side chain blocks the approach of the high polymer, so that the high polymer material is very flexible, and the free volume of the cavity is obviously increased compared with the high polymer material without introducing the dihydric alcohol containing silicon in the main chain; when the Si atom on the main chain of the macromolecule is connected with the long branched chain substituent, the slit free volume is mainly increased, the increase amplitude is smaller, and the small molecule is infiltratedThe improvement effect of the permeability and the diffusivity are limited, meanwhile, due to the fact that the rigidity of the long branched chain substituent is small, molecular chains are easy to tangle, the increase of the free volume is not facilitated, and the introduction of the dihydric alcohol with silicon in the main chain also enables the cavity free volume of the modified polyester to be increased.
The increase of the free volume of the cavity enables water or other molecules such as dye to be easier to permeate into the modified polyester macromolecules, has positive influence on the dyeing of the modified polyester and the like, can reduce the dyeing temperature, shorten the dyeing time, reduce the energy consumption and simultaneously improve the dye uptake of the fiber.
In addition, the oxidation degradation and hydrolysis rate of the high polymer material are closely related to the rate of oxygen permeation into the material, the rigidity of the macromolecular structure of the polyester is high, the free volume fraction is low, the oxygen permeation rate is very low, the oxidation and hydrolysis of the polyester in the natural environment are mainly carried out on the surface of the polyester, which is one of the main reasons for the slow degradation of the polyester in the natural environment, the increase of the free volume of the space is also beneficial to the permeation of oxygen into the polyester macromolecules, and further the oxidation degradation and hydrolysis rate of the polyester is further beneficial to improvement.
The fine denier soft polyester fiber in the prior art has large specific surface area and large surface reflected light, and meanwhile, because polyester molecular chains are arranged more tightly and dye molecules are not easy to permeate into the fiber, more refracted light returns from the inside of the dyed fiber to the outside, and the fine denier soft polyester fiber is difficult to dye deep color.
Has the advantages that:
(1) the preparation method of the super-soft polyester-polyester composite yarn has simple process and low cost, and the dibasic acid with the tertiary butyl side group and the dihydric alcohol polyester with the silicon-containing main chain are introduced into the polyester for modification, so that the dyeing temperature is reduced, the dyeing time is shortened, the dye uptake of the fiber is improved, the energy consumption is reduced, and the spinnability is improved;
(2) according to the preparation method of the super-soft polyester-polyester composite filament, the cavity free volume of the modified polyester is large, so that dye small molecules can easily enter the interior of the fiber, and the fiber is easy to have a dark color;
(3) according to the preparation method of the super-soft polyester-polyester composite yarn, the cavity free volume of the modified polyester is larger, so that water and oxygen-containing micromolecules can easily permeate into the polyester to carry out oxidative degradation and hydrolysis on the polyester, the degradability of the fiber is improved, and the polyester fiber can be recycled;
(4) the super-soft polyester composite yarn has the advantages of excellent dyeing performance, good mechanical performance and good application prospect.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
A preparation method of super-soft polyester composite yarn comprises the following steps:
(1) preparing modified polyester;
(1.1) esterification reaction;
preparing terephthalic acid, ethylene glycol, dimethyl silicon glycol and 5-tert-butyl-1, 3-phthalic acid into slurry, adding antimony trioxide, titanium dioxide and triphenyl phosphate, uniformly mixing, then carrying out esterification reaction at normal pressure in a nitrogen atmosphere, wherein the temperature of the esterification reaction is 255 ℃, the end point of the esterification reaction is when the distilled amount of water in the esterification reaction reaches 95% of a theoretical value, the molar ratio of the terephthalic acid to the ethylene glycol is 1:1.8, the sum of the adding amounts of the dimethyl silicon glycol and the 5-tert-butyl-1, 3-phthalic acid is 5mol% of the adding amount of the terephthalic acid, the molar ratio of the dibasic acid of the dimethyl silicon glycol and the 5-tert-butyl-1, 3-phthalic acid is 2:2, the adding amounts of the antimony trioxide, the titanium dioxide and the triphenyl phosphate are respectively 0.05wt% of the adding amount of the terephthalic acid, 0.25wt% and 0.05 wt%;
(1.2) polycondensation reaction;
after the esterification reaction is finished, starting the polycondensation reaction in the low vacuum stage under the negative pressure condition, wherein the pressure in the stage is stably pumped from normal pressure to absolute pressure of 490Pa within 40min, the reaction temperature is 255 ℃, the reaction time is 35min, then continuing to pump vacuum, and carrying out the polycondensation reaction in the high vacuum stage, so that the reaction pressure is further reduced to absolute pressure of 90Pa, the reaction temperature is 270 ℃, and the reaction time is 70 min;
the molecular chain of the modified polyester comprises a terephthalic acid chain segment, a glycol chain segment, a dimethyl silicon glycol chain segment and a 5-tert-butyl-1, 3-phthalic acid chain segment, the number average molecular weight of the modified polyester is 26000, and the molecular weight distribution index is 2.1;
(2) preparing modified polyester FDY yarns;
the modified polyester melt is subjected to metering, spinneret plate extrusion, cooling, oiling, stretching, heat setting and winding to obtain modified polyester FDY yarns, the filament number of the modified polyester FDY yarns is 0.4dtex, and the parameters of the FDY process are as follows: the spinning temperature is 290 ℃, the cooling temperature is 25 ℃, the network pressure is 0.30MPa, the speed of one roller is 900m/min, the temperature of one roller is 100 ℃, the speed of two rollers is 3500m/min, and the temperature of two rollers is 130 ℃;
(3) preparing modified polyester POY (polyester pre-oriented yarn);
the modified polyester POY is obtained after the modified polyester melt is subjected to metering, extrusion by a spinneret plate, cooling, oiling and winding, the filament number of the modified polyester POY is 0.3dtex, wherein the parameters of the POY process are as follows: the spinning temperature is 285 ℃, and the cooling temperature is 120 ℃;
(4) preparing super-soft polyester composite yarn;
and doubling the modified polyester FDY yarns and the modified polyester POY yarns to obtain the super-soft polyester-polyester composite yarns, wherein the winding speed during doubling is 3400 m/min.
The fineness of the finally prepared super-soft polyester-polyester composite filament is 80dtex, the fineness ratio of modified polyester FDY filaments to modified polyester POY filaments in the super-soft polyester-polyester composite filament is 3:3, the breaking strength of the super-soft polyester-polyester composite filament is 2.2cN/dtex, the elongation at break is 46%, the linear density CV value is 0.6%, the breaking strength CV value is 4.0%, the elongation at break CV value is 7.2%, the boiling water shrinkage rate is 50%, the oil content is 0.90 wt%, and the yarn evenness CV value is 2.2%.
The dye uptake of the super-soft polyester composite yarn at the temperature of 123 ℃ is 90.2%, the K/S value is 23.2, the soaping-resistant color fastness reaches 5 grades, the dry rubbing fastness reaches 5 grades, and the wet rubbing fastness reaches 5 grades.
Comparative example 1
A composite polyester yarn, which was prepared in substantially the same manner as in example 1, except that dimethyl silicon glycol and 5-tert-butyl-1, 3-phthalic acid were not added in step (1.1), and the composite polyester yarn had a breaking strength of 2.2cN/dtex, an elongation at break of 45%, a linear density CV value of 0.6%, a breaking strength CV value of 3.8%, an elongation at break CV value of 7.0%, a boiling water shrinkage of 52%, an oil content of 0.90 wt%, and a yarn evenness CV value of 2.2%. Under the same conditions as other test conditions of example 1, the dye uptake under the temperature condition of 130 ℃ is 84.7%, the K/S value is 19.56, the soaping fastness is grade 4-5, the dry rubbing fastness is grade 4-5, and the wet rubbing fastness is grade 3-4.
Comparative example 2
The preparation steps of the composite polyester yarn are basically the same as those of example 1, except that dimethyl silicon glycol is not added in the step (1.1), the breaking strength of the prepared composite polyester yarn is 2.3cN/dtex, the elongation at break is 44%, the linear density CV value is 0.6%, the breaking strength CV value is 3.7%, the elongation at break CV value is 7.1%, the boiling water shrinkage rate is 51%, the oil content is 0.90 wt%, the yarn evenness CV value is 2.2%, the dye uptake under the temperature condition of 130 ℃ is 87.8%, the K/S value is 21.77, the color fastness to washing is 5 grade, the dry rubbing fastness is 5 grade, and the wet rubbing fastness is 4 grade under the same conditions as other testing conditions of example 1.
Comparative example 3
A polyester composite yarn, which is prepared by the substantially same procedure as in example 1, except that 5-tert-butyl-1, 3-phthalic acid is not added in the procedure (1.1), the breaking strength of the prepared polyester composite yarn is 2.0cN/dtex, the elongation at break is 45%, the linear density CV value is 0.7%, the breaking strength CV value is 3.9%, the elongation at break CV value is 7.2%, the boiling water shrinkage is 50%, the oil content is 0.90 wt%, the yarn evenness CV value is 2.2%, the dye uptake under the same conditions as other test conditions of example 1 at a temperature of 130 ℃ is 88.1%, the K/S value is 22.53, the soaping color fastness is grade 5, the dry rubbing fastness is grade 5, and the wet rubbing fastness is grade 4.
Comprehensive analysis of example 1 and comparative examples 1 to 3 shows that the invention significantly improves the dyeing property of the fiber by introducing a dimethylsilanediol chain segment and a 5-tert-butyl-1, 3-phthalic acid chain segment, i.e., a diol chain segment with a silicon-containing main chain and a diacid chain segment with a tert-butyl side group, into the polyester molecular chain, and the dimethylsilanediol and the 5-tert-butyl-1, 3-phthalic acid have a synergistic effect, so that the free volume of the cavity of the polyester is increased, water or other molecules such as dyes can more easily permeate into the modified polyester macromolecules, and further the dyeing property of the fiber is improved, and in addition, the addition of the dimethylsilanediol and the 5-tert-butyl-1, 3-phthalic acid has little influence on other properties of the fiber, and does not influence the processability and the mechanical properties thereof.
Comparative example 4
The preparation steps of the composite polyester yarn are basically the same as those of the example 1, except that 1, 6-hexanediol is used for replacing dimethyl silicon glycol in the step (1.1), the prepared composite polyester yarn has the breaking strength of 2.1cN/dtex, the elongation at break of 43%, the linear density CV value of 0.7%, the breaking strength CV value of 3.6%, the elongation at break CV value of 7.0%, the boiling water shrinkage of 50%, the oil content of 0.90 wt%, the yarn evenness CV value of 2.2%, the dye uptake under the temperature condition of 130 ℃ of 87.5%, the K/S value of 21.56, the soaping color fastness of 5 grade, the dry rubbing fastness of 5 grade and the wet rubbing fastness of 4 grade under the same test conditions as those of the example 1. Compared with the embodiment 1, the introduction of the dihydric alcohol with silicon in the main chain can lead the main chain of the macromolecule to contain-Si-O-Si-bonds, so that the silicon-oxygen bond gap is larger, the internal rotation activation energy is lower, and the free rotation of atoms is facilitated, thereby increasing the free volume of cavities, and being more favorable for improving the dyeing property of the fiber compared with a long branched chain substituent.
Comparative example 5
A polyester composite yarn, the preparation steps are basically the same as example 1, except that 1, 2-dodecyl glycol is used to replace 5-tert-butyl-1, 3-phthalic acid in step (1.1), the breaking strength of the prepared polyester composite yarn is 2.3cN/dtex, the elongation at break is 42%, the linear density CV value is 0.7%, the breaking strength CV value is 3.8%, the elongation at break CV value is 7.2%, the boiling water shrinkage is 53%, the oil content is 0.90 wt%, the yarn evenness CV value is 2.2%, the dye uptake under the temperature condition of 130 ℃ is 87.9%, the K/S value is 22.03, the soaping color fastness is grade 5, the dry rubbing fastness is grade 5, and the wet rubbing fastness is grade 4 under the same conditions as other test conditions in example 1.
Compared with example 1, it can be found that the diacid with the tertiary butyl side group is more favorable for improving the dyeing performance of the fiber compared with the 1, 2-dodecyl glycol containing the long-branched substituent group, mainly because the free volume increased by the tertiary butyl group in the diacid with the tertiary butyl side group on one side is more hollow free volume, the free volume increased by the long-branched substituent group is more slit free volume, and the rigidity of the tertiary butyl group in the diacid with the tertiary butyl side group on the other side is more than that of the long-branched substituent group, so that the entanglement between molecular chains is reduced, and therefore, the diacid with the tertiary butyl side group has more free volume in the molecular chain arrangement mode compared with the 1, 2-dodecyl glycol containing the long-branched substituent group, and is more favorable for improving the dyeing performance of the fiber.
Example 2
A preparation method of super-soft polyester composite yarn comprises the following steps:
(1) preparing modified polyester;
(1.1) esterification reaction;
preparing terephthalic acid, ethylene glycol, dimethyl diphenyl disiloxane diol and 5-tert-butyl-1, 3-phthalic acid into slurry, adding ethylene glycol antimony, titanium dioxide and trimethyl phosphate, uniformly mixing, pressurizing in a nitrogen atmosphere to perform esterification reaction, wherein the pressurizing pressure is 0.3MPa, the esterification reaction temperature is 250 ℃, and the esterification reaction endpoint is determined when the distilled water amount in the esterification reaction reaches 92% of a theoretical value, wherein the molar ratio of the terephthalic acid to the ethylene glycol is 1:1.2, the sum of the adding amounts of the dimethyl diphenyl disiloxane diol and the 5-tert-butyl-1, 3-phthalic acid is 3.5 mol% of the adding amount of the terephthalic acid, the molar ratio of the dimethyl diphenyl disiloxane diol to the dibasic acid of the 5-tert-butyl-1, 3-phthalic acid is 1.5:3, and the ethylene glycol antimony, the titanium dioxide and the trimethyl phosphate are added into the slurry, The addition amounts of titanium dioxide and trimethyl phosphate are 0.03 wt%, 0.25wt% and 0.05wt% of the addition amount of terephthalic acid, respectively;
(1.2) polycondensation reaction;
after the esterification reaction is finished, starting the polycondensation reaction in the low vacuum stage under the negative pressure condition, wherein the pressure in the stage is stably pumped from normal pressure to the absolute pressure of 400Pa within 50min, the reaction temperature is 250 ℃, the reaction time is 50min, then continuing to pump vacuum, and carrying out the polycondensation reaction in the high vacuum stage, so that the reaction pressure is further reduced to the absolute pressure of 80Pa, the reaction temperature is 275 ℃, and the reaction time is 90 min;
the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment, a dimethyl diphenyl disiloxane glycol chain segment and a 5-tert-butyl-1, 3-phthalic acid chain segment, the number average molecular weight of the modified polyester is 30000, and the molecular weight distribution index is 2.2;
(2) preparing modified polyester FDY yarns;
the modified polyester melt is subjected to metering, spinneret plate extrusion, cooling, oiling, stretching, heat setting and winding to obtain modified polyester FDY yarns, the filament number of the modified polyester FDY yarns is 0.30dtex, and the parameters of the FDY process are as follows: the spinning temperature is 285 ℃, the cooling temperature is 20 ℃, the network pressure is 0.20MPa, the first roller speed is 850m/min, the first roller temperature is 98 ℃, the two roller speed is 3250m/min, and the two roller temperature is 120 ℃;
(3) preparing modified polyester POY (polyester pre-oriented yarn);
the modified polyester POY is obtained by metering, extruding by a spinneret plate, cooling, oiling and winding the modified polyester melt, the filament number of the modified polyester POY is 0.28dtex, wherein the parameters of the POY process are as follows: the spinning temperature is 280 ℃, and the cooling temperature is 18 ℃;
(4) preparing super-soft polyester composite yarn;
and doubling the modified polyester FDY yarns and the modified polyester POY yarns to obtain the super-soft polyester-polyester composite yarns, wherein the winding speed in doubling is 3200 m/min.
The fineness of the finally prepared super-soft polyester-polyester composite filament is 75dtex, the fineness ratio of modified polyester FDY filaments to modified polyester POY filaments in the super-soft polyester-polyester composite filament is 2:5, the breaking strength of the super-soft polyester-polyester composite filament is 2.0cN/dtex, the elongation at break is 40.0%, the linear density CV value is 1.00%, the breaking strength CV value is 5.00%, the elongation at break CV value is 8.00%, the boiling water shrinkage is 63%, the oil content is 1.0 wt%, and the yarn evenness CV value is 2.5%.
The dye uptake of the super-soft polyester composite yarn at the temperature of 123 ℃ is 86.3%, the K/S value is 21.15, the soaping-resistant color fastness reaches 5 grades, the dry rubbing fastness reaches 5 grades, and the wet rubbing fastness reaches 4-5 grades.
Example 3
A preparation method of super-soft polyester composite yarn comprises the following steps:
(1) preparing modified polyester;
(1.1) preparing 2-tert-butyl-1, 6-hexanedicarboxylic acid;
firstly, mixing tungstic acid and hydrogen peroxide, stirring for 12min at room temperature, then adding 2-tert-butylcyclohexanol, reacting for 1.5h at 83 ℃, then heating to 92 ℃ for reacting for 2.5h, wherein reactants are always in a reflux state in the reaction process, and finally cooling, crystallizing, washing and refining to obtain 2-tert-butyl-1, 6-hexanedicarboxylic acid, wherein the molar ratio of tungstic acid, 2-tert-butylcyclohexanol and hydrogen peroxide is 1:35:140 at the beginning of the reaction;
(1.2) esterification reaction;
preparing terephthalic acid, ethylene glycol, tetramethyldisiloxane diol and 2-tert-butyl-1, 6-hexanedioic acid into slurry, adding antimony acetate, titanium dioxide and trimethyl phosphite, uniformly mixing, pressurizing in a nitrogen atmosphere to perform esterification reaction, wherein the pressurizing pressure is 0.2MPa, the esterification reaction temperature is 260 ℃, and the esterification reaction endpoint is determined when the distilled water amount in the esterification reaction reaches 98% of a theoretical value, wherein the molar ratio of the terephthalic acid to the ethylene glycol is 1:2.0, the sum of the adding amounts of the tetramethyldisiloxane diol and the 2-tert-butyl-1, 6-hexanedioic acid is 3.7 mol% of the adding amount of the terephthalic acid, the molar ratio of the tetramethyldisiloxane diol to the 2-tert-butyl-1, 6-hexanedioic acid is 1.5:2.1, and the adding amounts of the antimony acetate, the titanium dioxide and the trimethyl phosphite are respectively 0.05wt% of the adding amount of the terephthalic acid, 0.20wt% and 0.01 wt%;
(1.3) a polycondensation reaction;
after the esterification reaction is finished, starting the polycondensation reaction in the low vacuum stage under the negative pressure condition, wherein the pressure in the stage is stably pumped from normal pressure to absolute pressure of 490Pa within 30min, the reaction temperature is 260 ℃, the reaction time is 30min, then continuing to pump vacuum, and carrying out the polycondensation reaction in the high vacuum stage, so that the reaction pressure is further reduced to absolute pressure of 90Pa, the reaction temperature is 275 ℃, and the reaction time is 50 min;
the molecular chain of the modified polyester comprises a terephthalic acid chain segment, a glycol chain segment, a tetramethyldisiloxane glycol chain segment and a 2-tert-butyl-1, 6-hexanedicarboxylic acid chain segment, the number average molecular weight of the modified polyester is 25000, and the molecular weight distribution index is 1.8;
(2) preparing modified polyester FDY yarns;
the modified polyester melt is subjected to metering, spinneret plate extrusion, cooling, oiling, stretching, heat setting and winding to obtain modified polyester FDY yarns, the filament number of the modified polyester FDY yarns is 0.50dtex, and the parameters of the FDY process are as follows: the spinning temperature is 2300 ℃, the cooling temperature is 25 ℃, the network pressure is 0.30MPa, the first roller speed is 950m/min, the first roller temperature is 110 ℃, the second roller speed is 3670m/min, and the second roller temperature is 135 ℃;
(3) preparing modified polyester POY (polyester pre-oriented yarn);
the modified polyester POY is obtained by metering, extruding by a spinneret plate, cooling, oiling and winding the modified polyester melt, the filament number of the modified polyester POY is 0.35dtex, wherein the parameters of the POY process are as follows: the spinning temperature is 290 ℃, and the cooling temperature is 22 ℃;
(4) preparing super-soft polyester composite yarn;
and doubling the modified polyester FDY yarns and the modified polyester POY yarns to obtain the super-soft polyester-polyester composite yarns, wherein the winding speed during doubling is 3600 m/min.
The titer of the finally prepared super-soft polyester-polyester composite filament is 90dtex, the titer ratio of the modified polyester FDY filament to the modified polyester POY filament in the super-soft polyester-polyester composite filament is 2:5, the breaking strength of the super-soft polyester-polyester composite filament is 2.2cN/dtex, the elongation at break is 46%, the linear density CV value is 1.50%, the breaking strength CV value is 4.20%, the elongation at break CV value is 4.40%, the boiling water shrinkage is 47%, the oil content is 0.6 wt%, and the yarn evenness CV value is 2.80%.
The dye uptake of the super-soft polyester composite yarn at the temperature of 123 ℃ is 86.7%, the K/S value is 21.5, the soaping-resistant color fastness reaches 5 grades, the dry rubbing fastness reaches 5 grades, and the wet rubbing fastness reaches 4-5 grades.
Example 4
A preparation method of super-soft polyester composite yarn comprises the following steps:
(1) preparing modified polyester;
(1.1) preparing 3-tert-butyl-1, 6-hexanedicarboxylic acid;
firstly, mixing tungstic acid and hydrogen peroxide, stirring for 15min at room temperature, then adding 4-tert-butylcyclohexanol, reacting for 2h at the temperature of 80 ℃, heating to 90 ℃ and reacting for 3h, wherein reactants are always in a reflux state in the reaction process, and finally cooling, crystallizing, washing and refining to obtain 3-tert-butyl-1, 6-hexanedicarboxylic acid, wherein the molar ratio of the tungstic acid to the 4-tert-butylcyclohexanol to the hydrogen peroxide is 1:30:150 at the beginning of the reaction;
(1.2) esterification reaction;
preparing terephthalic acid, ethylene glycol, dimethyl silicon glycol and 3-tert-butyl-1, 6-hexanedicarboxylic acid into slurry, adding antimony acetate, titanium dioxide and triphenyl phosphate, uniformly mixing, pressurizing in a nitrogen atmosphere to perform esterification reaction, wherein the pressurizing pressure is 0.25MPa, the esterification reaction temperature is 250 ℃, and the esterification reaction end point is determined when the distilled water amount in the esterification reaction reaches 95% of a theoretical value, wherein the molar ratio of the terephthalic acid to the ethylene glycol is 1:1.4, the sum of the addition amounts of the dimethyl silicon glycol and the 3-tert-butyl-1, 6-hexanedicarboxylic acid is 4.0 mol% of the addition amount of the terephthalic acid, the molar ratio of the dimethyl silicon glycol to the dibasic acid of the 3-tert-butyl-1, 6-hexanedicarboxylic acid is 1.8, and the addition amounts of the antimony acetate, the titanium dioxide and the triphenyl phosphate are respectively 0.035 wt% of the addition amount of the terephthalic acid, 0.21 wt% and 0.025 wt%;
(1.3) a polycondensation reaction;
after the esterification reaction is finished, starting the polycondensation reaction in the low vacuum stage under the negative pressure condition, stably pumping the pressure in the stage from normal pressure to absolute pressure 490 within 40min, wherein the reaction temperature is 255 ℃ and the reaction time is 35min, then continuously pumping vacuum to perform the polycondensation reaction in the high vacuum stage, further reducing the reaction pressure to absolute pressure 90Pa, the reaction temperature is 270 ℃ and the reaction time is 60 min;
the molecular chain of the modified polyester comprises a terephthalic acid chain segment, a glycol chain segment, a dimethyl silicon glycol chain segment and a 3-tert-butyl-1, 6-hexanedicarboxylic acid chain segment, the number average molecular weight of the modified polyester is 26000, and the molecular weight distribution index is 1.9;
(2) preparing modified polyester FDY yarns;
the modified polyester melt is subjected to metering, spinneret plate extrusion, cooling, oiling, stretching, heat setting and winding to obtain modified polyester FDY yarns, the filament number of the modified polyester FDY yarns is 0.35dtex, and the parameters of the FDY process are as follows: the spinning temperature is 290 ℃, the cooling temperature is 22 ℃, the network pressure is 0.25MPa, the one-roller speed is 900m/min, the one-roller temperature is 100 ℃, the two-roller speed is 3350m/min, and the two-roller temperature is 125 ℃;
(3) preparing modified polyester POY (polyester pre-oriented yarn);
the modified polyester POY is obtained after the modified polyester melt is subjected to metering, extrusion by a spinneret plate, cooling, oiling and winding, the filament number of the modified polyester POY is 0.3dtex, wherein the parameters of the POY process are as follows: the spinning temperature is 285 ℃, and the cooling temperature is 20 ℃;
(4) preparing super-soft polyester composite yarn;
and doubling the modified polyester FDY yarns and the modified polyester POY yarns to obtain the super-soft polyester-polyester composite yarns, wherein the winding speed in doubling is 3300 m/min.
The fineness of the finally prepared super-soft polyester-polyester composite filament is 80dtex, the fineness ratio of modified polyester FDY filaments to modified polyester POY filaments in the super-soft polyester-polyester composite filament is 2.5:3, the breaking strength of the super-soft polyester-polyester composite filament is 2.1cN/dtex, the elongation at break is 42%, the linear density CV value is 0.8%, the breaking strength CV value is 4.5%, the elongation at break CV value is 7.4%, the boiling water shrinkage rate is 52%, the oil content is 0.7 wt%, and the yarn evenness CV value is 2.20%.
The dye uptake of the super-soft polyester composite yarn at the temperature of 123 ℃ is 87.3 percent, the K/S value is 22.2, the soaping-resistant color fastness reaches 5 grades, the dry rubbing fastness reaches 5 grades, and the wet rubbing fastness reaches 4-5 grades.
Example 5
A preparation method of super-soft polyester composite yarn comprises the following steps:
(1) preparing modified polyester;
(1.1) preparing 2, 5-di-tert-butyl-1, 6-hexanedicarboxylic acid;
firstly, mixing tungstic acid and hydrogen peroxide, stirring for 10min at room temperature, then adding 2, 4-di-tert-butylcyclohexanol, reacting for 1h at 85 ℃, then heating to 90 ℃ for reaction for 3h, wherein reactants are always in a reflux state in the reaction process, and finally cooling, crystallizing, washing and refining to obtain 2, 5-di-tert-butyl-1, 6-hexanedicarboxylic acid, wherein the molar ratio of tungstic acid, 2, 4-di-tert-butylcyclohexanol and hydrogen peroxide is 1:40:120 at the beginning of the reaction;
(1.2) esterification reaction;
preparing terephthalic acid, ethylene glycol, dimethyl silicon glycol and 2, 5-di-tert-butyl-1, 6-hexanedicarboxylic acid into slurry, adding antimony acetate, titanium dioxide and triphenyl phosphate, uniformly mixing, pressurizing in a nitrogen atmosphere to perform esterification reaction, wherein the pressurizing pressure is 0.3MPa, the esterification reaction temperature is 260 ℃, and the esterification reaction end point is reached when the distilled water amount in the esterification reaction reaches 96% of a theoretical value, wherein the molar ratio of the terephthalic acid to the ethylene glycol is 1:1.5, the sum of the addition amounts of the dimethyl silicon glycol and the 2, 5-di-tert-butyl-1, 6-hexanedicarboxylic acid is 4.2 mol% of the addition amount of the terephthalic acid, the molar ratio of the dimethyl silicon glycol to the dibasic acid of the 2, 5-di-tert-butyl-1, 6-hexanedicarboxylic acid is 1.8:2, and the addition amounts of the antimony acetate, the titanium dioxide and the triphenyl phosphate are respectively 0.035 wt% of the addition amount of the terephthalic acid, 0.22 wt% and 0.02 wt%;
(1.3) a polycondensation reaction;
after the esterification reaction is finished, starting the polycondensation reaction in the low vacuum stage under the negative pressure condition, wherein the pressure in the stage is stably pumped from normal pressure to absolute pressure of 440Pa within 50min, the reaction temperature is 255 ℃, the reaction time is 50min, then continuing to pump vacuum, and carrying out the polycondensation reaction in the high vacuum stage, so that the reaction pressure is further reduced to absolute pressure of 80Pa, the reaction temperature is 275 ℃, and the reaction time is 70 min;
the molecular chain of the modified polyester comprises a terephthalic acid chain segment, a glycol chain segment, a dimethyl silicon glycol chain segment and a 2, 5-di-tert-butyl-1, 6-hexanedicarboxylic acid chain segment, the number average molecular weight of the modified polyester is 27000, and the molecular weight distribution index is 2.0;
(2) preparing modified polyester FDY yarns;
the modified polyester melt is subjected to metering, spinneret plate extrusion, cooling, oiling, stretching, heat setting and winding to obtain modified polyester FDY yarns, the filament number of the modified polyester FDY yarns is 0.4dtex, and the parameters of the FDY process are as follows: the spinning temperature is 295 ℃, the cooling temperature is 25 ℃, the network pressure is 0.30MPa, the first roller speed is 850m/min, the first roller temperature is 105 ℃, the second roller speed is 3400m/min, and the second roller temperature is 125 ℃;
(3) preparing modified polyester POY (polyester pre-oriented yarn);
the modified polyester POY is obtained after the modified polyester melt is subjected to metering, extrusion by a spinneret plate, cooling, oiling and winding, the filament number of the modified polyester POY is 0.32dtex, wherein the parameters of the POY process are as follows: the spinning temperature is 285 ℃, and the cooling temperature is 22 ℃;
(4) preparing super-soft polyester composite yarn;
and doubling the modified polyester FDY yarns and the modified polyester POY yarns to obtain the super-soft polyester-polyester composite yarns, wherein the winding speed during doubling is 3450 m/min.
The fineness of the finally prepared super-soft polyester-polyester composite filament is 85dtex, the fineness ratio of modified polyester FDY filaments to modified polyester POY filaments in the super-soft polyester-polyester composite filament is 3:5, the breaking strength of the super-soft polyester-polyester composite filament is 2.3cN/dtex, the elongation at break is 44%, the linear density CV value is 0.8%, the breaking strength CV value is 4.4%, the elongation at break CV value is 7.5%, the boiling water shrinkage rate is 55%, the oil content is 0.8 wt%, and the yarn evenness CV value is 2.3%.
The dye uptake of the super-soft polyester composite yarn at the temperature of 123 ℃ is 88.5%, the K/S value is 22.5, the soaping-resistant color fastness reaches 5 grade, the dry rubbing fastness reaches 5 grade, and the wet rubbing fastness reaches 5 grade.
Example 6
A preparation method of super-soft polyester composite yarn comprises the following steps:
(1) preparing modified polyester;
(1.1) preparing 2, 5-di-tert-butyl-1, 6-hexanedicarboxylic acid;
firstly, mixing tungstic acid and hydrogen peroxide, stirring for 15min at room temperature, then adding 2, 4-di-tert-butylcyclohexanol, reacting for 2h at the temperature of 80 ℃, then heating to 90 ℃ for reacting for 3h, wherein reactants are always in a reflux state in the reaction process, and finally cooling, crystallizing, washing and refining to obtain 2, 5-di-tert-butyl-1, 6-hexanedicarboxylic acid, wherein the molar ratio of the tungstic acid to the 2, 4-di-tert-butylcyclohexanol to the hydrogen peroxide is 1:35:140 at the beginning of the reaction;
(1.2) esterification reaction;
preparing terephthalic acid, ethylene glycol, dimethyl diphenyl disiloxane diol and 2, 5-di-tert-butyl-1, 6-hexanedioic acid into slurry, adding ethylene glycol antimony, titanium dioxide and trimethyl phosphate, uniformly mixing, pressurizing in a nitrogen atmosphere to perform esterification reaction, wherein the pressurizing pressure is 0.3MPa, the esterification reaction temperature is 250 ℃, and the esterification reaction endpoint is determined when the distilled water amount in the esterification reaction reaches 95% of a theoretical value, wherein the molar ratio of the terephthalic acid to the ethylene glycol is 1:1.8, the sum of the addition amounts of the dimethyl diphenyl disiloxane diol and the 2, 5-di-tert-butyl-1, 6-hexanedioic acid is 4.5 mol% of the addition amount of the terephthalic acid, and the molar ratio of the 2, 5-di-tert-butyl-1, 6-hexanedioic acid to the 2, 5-di-tert-butyl-1, 6-hexanedioic acid is 1.5:2.5, the addition amounts of ethylene glycol antimony, titanium dioxide and trimethyl phosphate are 0.05wt%, 0.25wt% and 0.01 wt% of the addition amount of terephthalic acid, respectively;
(1.3) a polycondensation reaction;
after the esterification reaction is finished, starting the polycondensation reaction in the low vacuum stage under the negative pressure condition, wherein the pressure in the stage is stably pumped from normal pressure to the absolute pressure of 400Pa within 30min, the reaction temperature is 260 ℃, the reaction time is 50min, then continuing to pump vacuum, and carrying out the polycondensation reaction in the high vacuum stage, so that the reaction pressure is further reduced to the absolute pressure of 80Pa, the reaction temperature is 275 ℃, and the reaction time is 80 min;
the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment, dimethyl diphenyl disiloxane diol and a 2, 5-di-tert-butyl-1, 6-hexanedicarboxylic acid chain segment, the number average molecular weight of the modified polyester is 28000, and the molecular weight distribution index is 2.0;
(2) preparing modified polyester FDY yarns;
the modified polyester melt is subjected to metering, spinneret plate extrusion, cooling, oiling, stretching, heat setting and winding to obtain modified polyester FDY yarns, the filament number of the modified polyester FDY yarns is 0.50dtex, and the parameters of the FDY process are as follows: the spinning temperature is 300 ℃, the cooling temperature is 20 ℃, the network pressure is 0.20MPa, the speed of one roller is 850m/min, the temperature of one roller is 100 ℃, the speed of two rollers is 3600m/min, and the temperature of two rollers is 130 ℃;
(3) preparing modified polyester POY (polyester pre-oriented yarn);
the modified polyester POY is obtained after the modified polyester melt is subjected to metering, extrusion by a spinneret plate, cooling, oiling and winding, the filament number of the modified polyester POY is 0.3dtex, wherein the parameters of the POY process are as follows: the spinning temperature is 280 ℃, and the cooling temperature is 20 ℃;
(4) preparing super-soft polyester composite yarn;
and doubling the modified polyester FDY yarns and the modified polyester POY yarns to obtain the super-soft polyester-polyester composite yarns, wherein the winding speed in doubling is 3500 m/min.
The fineness of the finally prepared super-soft polyester-polyester composite filament is 85dtex, the fineness ratio of modified polyester FDY filaments to modified polyester POY filaments in the super-soft polyester-polyester composite filament is 2:3, the breaking strength of the super-soft polyester-polyester composite filament is 2.4cN/dtex, the elongation at break is 45%, the linear density CV value is 0.9%, the breaking strength CV value is 4.6%, the elongation at break CV value is 7.8%, the boiling water shrinkage is 50%, the oil content is 1.0 wt%, and the yarn evenness CV value is 2.50%.
The dye uptake of the super-soft polyester composite yarn at the temperature of 123 ℃ is 89.5%, the K/S value is 23.0, the soaping-resistant color fastness reaches 5 grades, the dry rubbing fastness reaches 5 grades, and the wet rubbing fastness reaches 5 grades.
Example 7
A preparation method of super-soft polyester composite yarn comprises the following steps:
(1) preparing modified polyester;
(1.1) preparing 2-tert-butyl-1, 6-hexanedicarboxylic acid;
firstly, mixing tungstic acid and hydrogen peroxide, stirring for 10min at room temperature, then adding 2-tert-butylcyclohexanol, reacting for 2h at the temperature of 80 ℃, heating to 95 ℃ for reaction for 2h, wherein reactants are always in a reflux state in the reaction process, and finally cooling, crystallizing, washing and refining to obtain 2-tert-butyl-1, 6-hexanedicarboxylic acid, wherein the molar ratio of the tungstic acid to the 2-tert-butylcyclohexanol to the hydrogen peroxide is 1:40:150 at the beginning of the reaction;
(1.2) esterification reaction;
preparing terephthalic acid, ethylene glycol, tetramethyldisiloxane diol and 2-tert-butyl-1, 6-hexanedioic acid into slurry, adding ethylene glycol antimony, titanium dioxide and trimethyl phosphate, uniformly mixing, pressurizing in a nitrogen atmosphere to perform esterification reaction, wherein the pressurizing pressure is 0.3MPa, the esterification reaction temperature is 260 ℃, and the esterification reaction endpoint is determined when the distilled water amount in the esterification reaction reaches 95% of a theoretical value, wherein the molar ratio of the terephthalic acid to the ethylene glycol is 1:2.0, the sum of the adding amounts of the tetramethyldisiloxane diol and the 2-tert-butyl-1, 6-hexanedioic acid is 4.8 mol% of the adding amount of the terephthalic acid, the molar ratio of the tetramethyldisiloxane diol to the 2-tert-butyl-1, 6-hexanedioic acid is 2:3, and the adding amounts of the ethylene glycol antimony, the titanium dioxide and the trimethyl phosphate are respectively 0.05wt% of the adding amount of the terephthalic acid, 0.25wt% and 0.04 wt%;
(1.3) a polycondensation reaction;
after the esterification reaction is finished, starting the polycondensation reaction in the low vacuum stage under the negative pressure condition, wherein the pressure in the stage is stably pumped from normal pressure to the absolute pressure of 410Pa within 50min, the reaction temperature is 250 ℃, the reaction time is 50min, then continuing to pump vacuum, and carrying out the polycondensation reaction in the high vacuum stage, so that the reaction pressure is further reduced to the absolute pressure of 80Pa, the reaction temperature is 275 ℃, and the reaction time is 90 min;
the molecular chain of the modified polyester comprises a terephthalic acid chain segment, a glycol chain segment, a tetramethyldisiloxane glycol chain segment and a 2-tert-butyl-1, 6-hexanedicarboxylic acid chain segment, the number average molecular weight of the modified polyester is 29000, and the molecular weight distribution index is 2.2;
(2) preparing modified polyester FDY yarns;
the modified polyester melt is subjected to metering, spinneret plate extrusion, cooling, oiling, stretching, heat setting and winding to obtain modified polyester FDY yarns, the filament number of the modified polyester FDY yarns is 0.45dtex, and the parameters of the FDY process are as follows: the spinning temperature is 300 ℃, the cooling temperature is 25 ℃, the network pressure is 0.30MPa, the one-roller speed is 900m/min, the one-roller temperature is 100 ℃, the two-roller speed is 3670m/min, and the two-roller temperature is 135 ℃;
(3) preparing modified polyester POY (polyester pre-oriented yarn);
the modified polyester POY is obtained by metering, extruding by a spinneret plate, cooling, oiling and winding the modified polyester melt, the filament number of the modified polyester POY is 0.35dtex, wherein the parameters of the POY process are as follows: the spinning temperature is 290 ℃, and the cooling temperature is 18 ℃;
(4) preparing super-soft polyester composite yarn;
and doubling the modified polyester FDY yarns and the modified polyester POY yarns to obtain the super-soft polyester-polyester composite yarns, wherein the winding speed during doubling is 3600 m/min.
The fineness of the finally prepared super-soft polyester-polyester composite filament is 90dtex, the fineness ratio of modified polyester FDY filaments to modified polyester POY filaments in the super-soft polyester-polyester composite filament is 3:5, the breaking strength of the super-soft polyester-polyester composite filament is 2.5cN/dtex, the elongation at break is 46%, the linear density CV value is 1.00%, the breaking strength CV value is 4.5%, the elongation at break CV value is 7.5%, the boiling water shrinkage is 60%, the oil content is 1.0 wt%, and the yarn evenness CV value is 2.20%.
The dye uptake of the super-soft polyester composite yarn at the temperature of 123 ℃ is 90%, the K/S value is 23.2, the soaping-resistant color fastness reaches 5 grade, the dry rubbing fastness reaches 5 grade, and the wet rubbing fastness reaches 5 grade.

Claims (10)

1. The preparation method of the super-soft polyester composite yarn is characterized by comprising the following steps: preparing modified polyester FDY yarns and modified polyester POY yarns from the modified polyester melt according to an FDY process and a POY process respectively, and then doubling the modified polyester FDY yarns and the modified polyester POY yarns to obtain super-soft polyester composite yarns;
the preparation method of the modified polyester comprises the following steps: uniformly mixing terephthalic acid, ethylene glycol, dihydric alcohol with a silicon-containing main chain and dibasic acid with a tert-butyl side group, and then sequentially carrying out esterification reaction and polycondensation reaction;
the dihydric alcohol with silicon in the main chain is dimethyl silicon glycol, dimethyl diphenyl disiloxane glycol or tetramethyl disiloxane glycol, and the dibasic acid with tertiary butyl side group is 5-tertiary butyl-1, 3-phthalic acid, 2-tertiary butyl-1, 6-hexanedicarboxylic acid, 3-tertiary butyl-1, 6-hexanedicarboxylic acid or 2, 4-di-tertiary butyl-1, 6-hexanedicarboxylic acid.
2. The method for preparing the ultra-soft polyester composite filament according to claim 1, wherein the synthesis method of the 2-tert-butyl-1, 6-hexanedicarboxylic acid, the 3-tert-butyl-1, 6-hexanedicarboxylic acid and the 2, 4-di-tert-butyl-1, 6-hexanedicarboxylic acid comprises the following steps:
firstly, mixing tungstic acid and hydrogen peroxide, stirring for 10-15 min at room temperature, then adding raw material alcohol, reacting for 1-2 h at the temperature of 80-85 ℃, then heating to 90-95 ℃ and reacting for 2-3 h, wherein reactants are always in a reflux state in the reaction process, and finally cooling, crystallizing, washing and refining;
when the reaction starts, the molar ratio of the tungstic acid to the raw material alcohol to the hydrogen peroxide is 1: 30-40: 120-150;
the raw material alcohols corresponding to the 2-tert-butyl-1, 6-hexanedicarboxylic acid, the 3-tert-butyl-1, 6-hexanedicarboxylic acid and the 2, 4-di-tert-butyl-1, 6-hexanedicarboxylic acid are respectively 2-tert-butylcyclohexanol, 4-tert-butylcyclohexanol and 2, 4-di-tert-butylcyclohexanol.
3. The preparation method of the super soft polyester composite filament according to claim 2, wherein the modified polyester is prepared by the following steps:
(1) performing esterification reaction;
preparing terephthalic acid, ethylene glycol, dihydric alcohol with a silicon-containing main chain and dibasic acid with a tert-butyl side group into slurry, adding a catalyst, a delustering agent and a stabilizer, uniformly mixing, pressurizing in a nitrogen atmosphere to perform esterification reaction, wherein the pressurizing pressure is normal pressure to 0.3MPa, the esterification reaction temperature is 250-260 ℃, and the esterification reaction end point is determined when the water distillation amount in the esterification reaction reaches more than 90% of a theoretical value;
(2) performing polycondensation reaction;
and after the esterification reaction is finished, starting the polycondensation reaction in the low vacuum stage under the negative pressure condition, stably pumping the pressure in the low vacuum stage from normal pressure to below 500Pa in 30-50 min at the reaction temperature of 250-260 ℃ for 30-50 min, then continuously pumping the vacuum to perform the polycondensation reaction in the high vacuum stage, so that the reaction pressure is further reduced to below 100Pa, the reaction temperature is 270-275 ℃, and the reaction time is 50-90 min.
4. The preparation method of the ultra-soft polyester composite filament according to claim 3, wherein the molar ratio of terephthalic acid to ethylene glycol is 1: 1.2-2.0, the sum of the addition amounts of the main chain silicon-containing diol and the dibasic acid with the tertiary butyl side group is 3.5-5 mol% of the addition amount of terephthalic acid, the molar ratio of the main chain silicon-containing diol to the dibasic acid with the tertiary butyl side group is 1.5-2: 2-3, and the addition amounts of the catalyst, the delustering agent and the stabilizer are 0.03-0.05 wt%, 0.20-0.25 wt% and 0.01-0.05 wt% of the addition amount of terephthalic acid, respectively.
5. The method for preparing the ultra-soft polyester composite filament according to claim 4, wherein the catalyst is antimony trioxide, ethylene glycol antimony or antimony acetate, the delustering agent is titanium dioxide, and the stabilizer is triphenyl phosphate, trimethyl phosphate or trimethyl phosphite.
6. The preparation method of the super-soft polyester composite filament according to claim 5, wherein the modified polyester has a number average molecular weight of 25000 to 30000 and a molecular weight distribution index of 1.8 to 2.2.
7. The preparation method of the ultra-soft polyester-polyester composite filament according to claim 1, wherein the FDY process comprises the following steps: metering, spinneret plate extruding, cooling, oiling, stretching, heat setting and winding;
the FDY process comprises the following parameters: the spinning temperature is 285-300 ℃, the cooling temperature is 20-25 ℃, the network pressure is 0.20-0.30 MPa, the first roller speed is 850-950 m/min, the first roller temperature is 98-110 ℃, the two roller speed is 3250-3670 m/min, and the two roller temperature is 120-135 ℃;
the POY process comprises the following steps: metering, spinneret plate extrusion, cooling, oiling and winding;
the parameters of the POY process are as follows: the spinning temperature is 280-290 ℃, and the cooling temperature is 18-22 ℃;
the winding speed during doubling is 3200-3600 m/min.
8. The super-soft polyester composite yarn prepared by the preparation method of the super-soft polyester composite yarn as claimed in any one of claims 1 to 7 is characterized in that: mainly compounded by modified polyester FDY yarns and modified polyester POY yarns;
the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment, a dihydric alcohol chain segment with a silicon-containing main chain and a dibasic acid chain segment with a tert-butyl side group;
the filament number of the modified polyester FDY yarn and the filament number of the modified polyester POY yarn are respectively 0.30-0.50 dtex and 0.28-0.35 dtex.
9. The super soft polyester composite filament according to claim 8, wherein the titer of the super soft polyester composite filament is 75-90 dtex, and the titer ratio of the modified polyester FDY filament to the modified polyester POY filament in the super soft polyester composite filament is 2-3: 3-5;
the breaking strength of the super-soft polyester composite filament is more than or equal to 2.0cN/dtex, the elongation at break is 43.0 +/-3.0%, the linear density CV value is less than or equal to 1.00%, the breaking strength CV value is less than or equal to 5.00%, the elongation at break CV value is less than or equal to 8.00%, the boiling water shrinkage is 55.0 +/-8.0%, the oil content is 0.80 +/-0.20 wt%, and the yarn evenness CV value is less than or equal to 2.50%.
10. The super soft polyester composite filament according to claim 9, wherein the dye uptake of the super soft polyester composite filament at a temperature of 123 ℃ is 86.3-90.2%, the K/S value is 21.15-23.4, the soaping color fastness reaches 5 level, the dry rubbing fastness reaches 5 level, and the wet rubbing fastness is higher than 4 level.
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