CN108048940B - Soft polyester fiber and preparation method thereof - Google Patents

Soft polyester fiber and preparation method thereof Download PDF

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Publication number
CN108048940B
CN108048940B CN201711341960.4A CN201711341960A CN108048940B CN 108048940 B CN108048940 B CN 108048940B CN 201711341960 A CN201711341960 A CN 201711341960A CN 108048940 B CN108048940 B CN 108048940B
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polyester fiber
oil agent
terephthalic acid
oil
reaction
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CN108048940A (en
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李文刚
刘灯胜
杨超明
张群
窦弘
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Jiangsu Hengli Chemical Fiber Co Ltd
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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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
    • D01F6/84—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products from copolyesters
    • 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
    • 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
    • D01D5/096—Humidity control, or oiling, of 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
    • D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
    • D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
    • D01F11/08—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Artificial Filaments (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to a soft polyester fiber and a preparation method thereof, wherein the preparation method comprises the following steps: the soft polyester fiber is prepared from the modified polyester through metering, extruding, cooling, oiling, stretching, heat setting and winding, wherein the oiling oil agent contains crown ether, and the content of the crown ether is 67.30-85.58 wt%. The prepared soft polyester fiber is made of modified polyester with molecular chains comprising terephthalic acid chain segments, ethylene glycol chain segments and adipic acid chain segments, the initial modulus is less than or equal to 80cN/dtex, the fineness is 75-300 dtex, the breaking strength is more than or equal to 3.6cN/dtex, the elongation at break is 45.0 +/-3.0%, the CV value of the breaking strength is less than or equal to 5.0%, the CV value of the elongation at break is less than or equal to 10.0%, the shrinkage in boiling water is 7.5 +/-0.5%, and the oil content is 0.90 +/-0.20%. The preparation method is simple, and the obtained polyester fiber has good flexibility and very considerable application prospect.

Description

Soft polyester fiber and preparation method thereof
Technical Field
The invention belongs to the field of fiber preparation, and relates to a soft polyester fiber and a preparation method thereof.
Background
Polyethylene terephthalate (PET) is a polymer with excellent performance, and the PET has the advantages of high modulus, high strength, good shape retention, good barrier property and the like, so that the PET is widely applied to the fields of fibers, bottle packaging, films, sheets and the like, the yield is increased year by year, and the industrial position is remarkably improved.
Because most PET fibers have small dielectric constant, low moisture regain and high friction coefficient, a spin finish must be used in the spinning process. The main component of the oil agent is surfactant, and can form directional adsorption layer, i.e. oil film, on the surface of chemical fibre, on one hand, the hydrophilic group of the oil film is oriented to space, and can adsorb moisture in the air, and on the fibre surface a continuous water film can be formed, so that the charged ions can be migrated on the surface of the fibre, and the accumulation of static charge produced by friction between the fibres can be reduced, so that the surface resistance of the fibre can be reduced, and the conductivity of fibre can be raised, on the other hand, the oil film isolating fibre can produce a certain affinity for fibre, and can make it possess a certain concentration property and do not scatter, and in addition, the oil film also can give fibre a certain smoothness, so that the fibre can not be damaged in the course of friction, and has good hand feeling, and can smoothly pass through the operation procedures of winding, drawing and drying, etc. when spinning, the electrostatic action in the course of textile processing can be eliminated, and the, The roller, the cylinder and other adverse phenomena reduce the generation of broken filaments and broken ends, and ensure the quality of fiber products.
The friction behavior of the fiber can be changed after the oil film on the surface of the fiber is broken at high temperature, high speed and certain pressure, so that the friction force is increased, and other problems such as broken filaments and broken ends of the fiber are caused. Along with the development of high speed, super high speed and multifunctional fiber of polyester filament, the development of an oil solution with good heat resistance, low viscosity, high oil film strength, good smoothness and strong antistatic property is of great practical significance.
The softness of the fabric is a subjective feeling when a person touches and pinches the fabric, the softness is an important performance for the fiber, the fiber with good softness has fine and uniform fineness, high strength and high elasticity, soft texture and smooth and fine hand feeling, and the spun fabric has the characteristics of soft hand feeling and elegant wear. However, the oiling agent used in the prior art is difficult to meet the conditions required for producing fine denier fiber, the quality of the obtained fiber is not high, and the softness is not good.
Therefore, how to overcome the defects in the prior art and prepare a polyester fiber with good mechanical properties and softness becomes a technical problem to be solved urgently at present.
Disclosure of Invention
The invention aims to overcome the problem of poor softness of polyester fibers in the prior art, and provides soft polyester fibers with good softness and a preparation method thereof. The crown ether-containing oil agent is used, so that the heat resistance and the lubricity of the oil agent are improved, and the quality of fibers is improved; the use of the adipic acid improves the softness of the fiber.
In order to achieve the purpose, the invention adopts the technical scheme that:
the soft polyester fiber is made of modified polyester;
the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and an adipic acid chain segment, wherein the adipic acid chain segment is a longer fatty chain, so that the rigidity of the obtained polyester is reduced, and the softness of the fiber is effectively improved;
the initial modulus of the soft polyester fiber is less than or equal to 80 cN/dtex.
As a preferred technical scheme:
the soft polyester fiber has a fineness of 75-300 dtex, a breaking strength of not less than 3.6cN/dtex, an elongation at break of 45.0 +/-3.0%, a breaking strength CV value of not more than 5.0%, an elongation at break CV value of not more than 10.0%, a boiling water shrinkage of 7.5 +/-0.5%, and an oil content of 0.90 +/-0.20%.
The number average molecular weight of the modified polyester is 20000-27000, the molecular weight distribution index is 1.8-2.2, the modified polyester prepared by the method is higher in molecular weight and narrower in molecular weight distribution, the requirements of spinning processing can be met, and the preparation of fibers with excellent performance is facilitated;
the molar content of the adipic acid chain segment in the modified polyester is 5-8% of that of the terephthalic acid chain segment, and the molar content of the adipic acid chain segment in the modified polyester is low, so that the excellent performance of the polyester is maintained, the crystallinity is reduced, and the initial modulus is lower than that of the conventional polyester.
The preparation method of the modified polyester fiber comprises the following steps: uniformly mixing terephthalic acid, ethylene glycol and adipic acid, and then carrying out esterification reaction and polycondensation reaction in sequence to obtain modified polyester; the method comprises the following specific steps:
(1) performing esterification reaction;
preparing terephthalic acid, ethylene glycol and adipic acid 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 endpoint is determined when the distilled amount of water 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 a 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 260-270 ℃ for 30-50 min, then continuously pumping the vacuum to perform the polycondensation reaction in a high vacuum stage, further reducing the reaction pressure to below 100Pa, controlling the reaction temperature to 275-285 ℃ and the reaction time to be 50-90 min, and thus obtaining the modified polyester.
The soft polyester fiber is characterized in that in the step (1), the molar ratio of terephthalic acid, ethylene glycol and adipic acid is 1: 1.2-2.0: 0.03-0.06, the addition amount of the catalyst is 0.01-0.05% of the weight of the terephthalic acid, the addition amount of the delustering agent is 0.20-0.25% of the weight of the terephthalic acid, and the addition amount of the stabilizer is 0.01-0.05% of the weight of the terephthalic acid;
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.
The invention also provides a method for preparing the soft polyester fiber, which comprises the steps of metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester to obtain the soft polyester fiber;
the oiling oil agent contains crown ether, and the content of the crown ether is 67.30-85.58 wt%.
The crown ether is a heterocyclic organic compound and contains a plurality of ether groups, the wetting capacity of the crown ether surfactant is higher than that of a corresponding open-chain compound, the crown ether has better solubilization, the solubility of a salt compound in the organic compound is lower, but the addition of the crown ether can improve the solubility of the salt compound in organic matters. The common polyester or polyether compound in the oil agent has larger intermolecular action due to larger molecular weight and hydrogen bond action, and shows larger kinematic viscosity, and after the crown ether is added, the crown ether can be well compatible in the oil agent system of the polyester or polyether compound, enter between molecular chains of polyester or polyether compounds to shield acting force between the molecular chains, thereby reducing the viscosity of the oil solution system, meanwhile, the antistatic agent of the chemical fiber oil solution is mainly divided into anionic surfactant, cationic surfactant and amphoteric surfactant, most of the antistatic agent contains metal ions or exists in the form of salt, which causes poor compatibility of the antistatic agent and polyester or polyether compounds in the oil agent, and the addition of crown ether, due to the salt dissolution effect, the compatibility of the antistatic agent and polyester or polyether compounds is improved, the strength of an oil film of an oil agent is further improved, and the salt dissolution effect has great significance on the stability of spinning and the product holding capacity. Indexes of the oil agent are reflected by a comprehensive factor, so that a certain restriction is provided for the addition amount of crown ether, the advantage of the heat resistance and the oil film strength of the oil agent is not reflected by the excessively low addition amount, and other indexes are limited.
As a preferred technical scheme:
according to the method, the thermal weight loss of the oil agent after the oil agent is heated and treated at 200 ℃ for 2h is less than 15wt%, the crown ether has a higher volatile point and excellent heat-resistant stability, and the heat-resistant performance of the oil agent introduced with the crown ether is also remarkably improved;
the kinematic viscosity of the oil agent is 27.5-30.1 mm at the temperature of (50 +/-0.01) ° C2The kinematic viscosity of the oil agent prepared from water into 10wt% emulsion is 0.93-0.95 mm2The crown ether can reduce the viscosity of the oil agent mainly because the crown ether has low viscosity and is a small bead-shaped molecule, and the crown ether is used in oilAfter crown ether is introduced into the oil agent system, the crown ether can be well compatible in the polyester compound or polyether compound oil agent system and simultaneously enters between molecular chains of the polyester compound or polyether compound to shield acting force between the molecular chains, so that the viscosity of the oil agent system is reduced;
the oil film strength of the oil agent is 121-127N, the oil film strength of the oil agent in the prior art is low and is generally about 110N, the main reason is that most of antistatic agents of the chemical fiber oil agent contain metal ions or exist in the form of salt, the compatibility of the antistatic agents and polyester compounds or polyether compounds in the oil agent is poor, and the crown ether can improve the oil film strength is mainly that salt solution effect can be generated after the crown ether is added, so that the compatibility of the antistatic agents and the polyester compounds or polyether compounds is improved, and the oil film strength of the oil agent is further improved;
the surface tension of the oil agent is 23.2-26.8 cN/cm, and the specific resistance is 1.0 × 108～1.8×108Ω·cm；
After oiling, the static friction coefficient between the fibers is 0.250-0.263, and the dynamic friction coefficient is 0.262-0.273;
after oiling, the static friction coefficient between the fiber and the metal is 0.202-0.210, and the dynamic friction coefficient is 0.320-0.332.
The method as described above, wherein the crown ether is 2-hydroxymethyl-12-crown-4, 15-crown-5 or 2-hydroxymethyl-15-crown-5;
the oil agent also contains mineral oil, phosphate potassium salt, trimethylolpropane laurate and alkyl sodium sulfonate;
the mineral oil is one of 9# to 17# mineral oil;
the phosphate potassium salt is dodecyl phosphate potassium salt, isomeric tridecanol polyoxyethylene ether phosphate potassium salt or dodecatetradecanol phosphate potassium salt;
the sodium alkyl sulfonate is sodium dodecyl sulfonate, sodium pentadecyl sulfonate or sodium hexadecyl sulfonate;
when the oil agent is used, preparing an emulsion with the concentration of 10-20 wt% by using water;
the preparation method of the oil agent comprises the following steps: uniformly mixing crown ether, phosphate potassium salt, trimethylolpropane laurate and sodium alkyl sulfonate, adding the mixture into mineral oil, and uniformly stirring to obtain an oil agent; the addition amount of each component is as follows according to the parts by weight:
Figure BDA0001508556760000051
the mixing is carried out at normal temperature, the stirring temperature is 40-55 ℃, and the stirring time is 1-3 h.
In the method, the spinning process parameters of the soft polyester fiber are as follows:
spinning temperature: 280-290 ℃;
cooling temperature: 20-25 ℃;
network pressure: 0.20 to 0.30 MPa;
a roll speed: 2200 to 2600m/min
First roll temperature: 75-85 ℃;
two roll speed: 3600-3900 m/min;
temperature of the two rolls: 135-165 ℃;
speed of winding: 3580-3840 m/min.
The invention mechanism is as follows:
the crown ether is introduced into the oil agent to prepare the oil agent with low viscosity, good heat resistance and higher oil film strength. In the prior art, the higher viscosity of the oil agent is mainly due to the fact that the oil agent contains a common polyester compound or polyether compound, the intermolecular action of the compound is larger due to the larger molecular weight and the action of hydrogen bonds, the kinematic viscosity is larger, so that the viscosity of the oil agent is higher, the viscosity of the oil agent can be obviously reduced after crown ether is added, the crown ether is mainly due to the fact that the viscosity of the crown ether is lower and is bead-shaped micromolecule, the crown ether can be well compatible in a polyester compound or polyether oil agent system and simultaneously enters between molecular chains of the polyester compound or polyether compound to shield acting force between the molecular chains, and therefore the viscosity of the oil agent system is reduced. In the prior art, the oil film strength of the oil agent is low mainly because the antistatic agent of the chemical fiber oil agent mostly contains metal ions or exists in the form of salt, so that the compatibility of the antistatic agent and polyester compounds or polyethers in the oil agent is poor, and the crown ether can improve the oil film strength mainly because the crown ether can generate a salt solution effect after being added, so that the compatibility of the antistatic agent and the polyester compounds or polyethers is improved, and the oil film strength of the oil agent is further improved. In addition, the crown ether has higher volatile point and excellent heat resistance stability, and the heat resistance of the oil agent introduced with the crown ether is also obviously improved, and the crown ether has lower viscosity, higher volatile point, smaller friction coefficient and more excellent heat resistance stability compared with the conventional smoothing agent, so that the processing performance of the fiber is improved, the phenomena of fiber hairline and fiber floating are reduced, and the softness of the fiber is better.
Has the advantages that:
(1) the soft polyester fiber provided by the invention has a simple and reasonable preparation process, and the prepared soft polyester fiber has good flexibility and extremely high popularization value;
(2) according to the preparation method of the soft polyester fiber, the oxalic acid chain segment is introduced into the modified polyester, so that the rigidity of the polyester is changed, and the softness of the fiber is obviously improved;
(3) according to the preparation method of the soft polyester fiber, the oiling agent containing the crown ether used in the oiling process has the characteristics of low viscosity, good heat resistance, high oil film strength, good smoothness and strong antistatic property, and the spinning stability and the fiber processability are improved.
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 soft polyester fiber comprises the following steps:
(1) preparation of modified polyester:
(a) performing esterification reaction;
preparing terephthalic acid, ethylene glycol and adipic acid with a molar ratio of 1:1.2:0.03 into slurry, adding antimony trioxide, titanium dioxide and triphenyl phosphate, uniformly mixing, pressurizing in a nitrogen atmosphere to perform esterification reaction, wherein the pressurizing pressure is normal pressure, the esterification reaction temperature is 250 ℃, and the esterification reaction endpoint is determined when the distilled water amount in the esterification reaction reaches 90% of a theoretical value, wherein the adding amount of the antimony trioxide is 0.01% of the weight of the terephthalic acid, the adding amount of the titanium dioxide is 0.20% of the weight of the terephthalic acid, and the adding amount of the triphenyl phosphate is 0.05% of the weight of the terephthalic acid;
(b) performing 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 from normal pressure to the absolute pressure of 500Pa within 30min, controlling the reaction temperature to be 260 ℃ and the reaction time to be 40min, then continuing to pump the 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 100Pa, the reaction temperature is 275 ℃ and the reaction time is 70min, thus obtaining a modified polyester molecular chain which comprises a terephthalic acid chain segment, an ethylene glycol chain segment and an adipic acid chain segment, wherein the number average molecular weight is 20000, the molecular weight distribution index is 2.0, and the molar content of the adipic acid chain segment in the modified polyester is 3% of the molar content of the terephthalic acid chain segment;
(2) preparation of oiling oil agent: uniformly mixing 2-hydroxymethyl-12-crown-4 with dodecyl phosphate potassium salt, trimethylolpropane laurate and sodium dodecyl sulfate at normal temperature, adding into No. 9 mineral oil, and uniformly stirring at 40 ℃ for 1h to obtain an oil agent; the addition amount of each component is as follows according to the parts by weight: 2 parts of No. 9 mineral oil; 10 parts of trimethylolpropane laurate; 2-hydroxymethyl-12-crown-490 parts; 8 parts of dodecyl phosphate potassium salt; and 3 parts of sodium dodecyl sulfate. The content of crown ether in the prepared oil agent is 79.6 wt%, the high temperature resistance of the oil agent is excellent, and the thermal weight loss is 14.5 wt% after the oil agent is heated for 2 hours at 200 ℃; the viscosity of the oil agent is low, and the kinematic viscosity is 29.6mm at the temperature of (50 +/-0.01) ° C2S, usingThe kinematic viscosity of water after preparation of an emulsion with a concentration of 10% by weight is 0.93mm2The oil has high oil film strength of 125N, surface tension of 24.8cN/cm, specific resistance of 1.3 × 108Omega cm, coefficient of static friction (mu) between fibres (F/F) after oilings) 0.255, coefficient of dynamic friction (. mu.)d) 0.266, coefficient of static friction (. mu.) between fiber and metal (F/M)s) 0.203, coefficient of dynamic friction (. mu.)d) 0.320, and the prepared oil agent is prepared into an emulsion with the concentration of 15wt% by using water when in use;
(3) the soft polyester fiber is prepared by metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester, and the main spinning process parameters of the soft polyester fiber are shown in table 1.
The finally obtained soft polyester fiber has the initial modulus of 80cN/dtex, the fineness of 80dtex, the breaking strength of 3.6cN/dtex, the elongation at break of 42.0 percent, the CV value of the breaking strength of 4.7 percent, the CV value of the elongation at break of 9.8 percent, the shrinkage in boiling water of 7.5 percent and the oil content of 1.10 percent.
Example 2
A preparation method of soft polyester fiber comprises the following steps:
(1) preparation of modified polyester:
(a) performing esterification reaction;
preparing terephthalic acid, ethylene glycol and adipic acid with a molar ratio of 1:1.4:0.05 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 0.1MPa, the esterification reaction temperature is 252 ℃, the esterification reaction endpoint is determined when the distilled amount of water in the esterification reaction reaches 92% of a theoretical value, wherein the adding amount of antimony acetate is 0.03% of the weight of the terephthalic acid, the adding amount of titanium dioxide is 0.23% of the weight of the terephthalic acid, and the adding amount of trimethyl phosphite is 0.01% of the weight of the terephthalic acid;
(b) performing 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 from normal pressure to absolute pressure of 495Pa within 40min, controlling the reaction temperature to 263 ℃ and the reaction time to 45min, then continuing to pump the vacuum, and carrying out the polycondensation reaction in the high vacuum stage, so that the reaction pressure is further reduced to absolute pressure of 95Pa, the reaction temperature is 278 ℃ and the reaction time is 60min, thus obtaining a modified polyester molecular chain which comprises a terephthalic acid chain segment, an ethylene glycol chain segment and an adipic acid chain segment, wherein the number average molecular weight is 21000, the molecular weight distribution index is 2.2, and the molar content of the adipic acid chain segment in the modified polyester is 4% of the molar content of the terephthalic acid chain segment;
(2) preparation of oiling oil agent: uniformly mixing 15-crown ether-5, isotridecanol polyoxyethylene ether phosphate potassium salt, trimethylolpropane laurate and sodium pentadecylsulfonate at normal temperature, adding into 10# mineral oil, and uniformly stirring at 43 ℃ for 1.5h to obtain an oil agent; the addition amount of each component is as follows according to the parts by weight: 2 parts of No. 10 mineral oil; 15 parts of trimethylolpropane laurate; 15-crown ether-570 parts; 10 parts of isomeric tridecanol polyoxyethylene ether phosphate potassium salt; and 7 parts of sodium pentadecylsulfonate. The prepared oil agent has crown ether content of 67.30 wt%, excellent high temperature resistance, thermal weight loss of 13 wt% after heating treatment at 200 deg.C for 2h, low viscosity, and kinematic viscosity of 28.1mm at (50 + -0.01) ° C2(s) a kinematic viscosity of 0.93mm after preparation with water as an emulsion having a concentration of 10% by weight2(s) 123N, which is a high oil film strength of the oil agent, 25.1cN/cm, which is a surface tension of the oil agent, and 1.5 × 10 which is a specific resistance8Omega cm, coefficient of static friction (mu) between fibres (F/F) after oilings) 0.257, coefficient of dynamic friction (. mu.)d) 0.265, coefficient of static friction (. mu.m) between fiber and metal (F/M) after oilings) 0.205, coefficient of dynamic friction (. mu.)d) 0.323, the prepared oil agent is prepared into emulsion with the concentration of 14 weight percent by water when in use;
(3) the soft polyester fiber is prepared by metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester, and the main spinning process parameters of the soft polyester fiber are shown in table 1.
The finally obtained soft polyester fiber has the initial modulus of 79cN/dtex, the fineness of 120dtex, the breaking strength of 3.8cN/dtex, the elongation at break of 45.0 percent, the CV value of the breaking strength of 4.7 percent, the CV value of the elongation at break of 9.9 percent, the shrinkage in boiling water of 7.0 percent and the oil content of 1.10 percent.
Example 3
A preparation method of soft polyester fiber comprises the following steps:
(1) preparation of modified polyester:
(a) performing esterification reaction; preparing terephthalic acid, ethylene glycol and adipic acid with a molar ratio of 1:1.4:0.05 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 0.1MPa, the esterification reaction temperature is 252 ℃, the esterification reaction endpoint is determined when the distilled amount of water in the esterification reaction reaches 92% of a theoretical value, wherein the adding amount of antimony acetate is 0.03% of the weight of the terephthalic acid, the adding amount of titanium dioxide is 0.23% of the weight of the terephthalic acid, and the adding amount of trimethyl phosphite is 0.01% of the weight of the terephthalic acid;
(b) performing 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 from normal pressure to absolute pressure of 495Pa within 40min, controlling the reaction temperature to 263 ℃ and the reaction time to 45min, then continuing to pump the vacuum, and carrying out the polycondensation reaction in the high vacuum stage, so that the reaction pressure is further reduced to absolute pressure of 95Pa, the reaction temperature is 278 ℃ and the reaction time is 60min, the molecular chain of the prepared modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and an adipic acid chain segment, the number average molecular weight is 21000, the molecular weight distribution index is 2.2, and the molar content of the adipic acid chain segment in the modified polyester is 4% of the molar content of the terephthalic acid chain segment;
(2) preparation of oiling oil agent: uniformly mixing 2-hydroxymethyl-15-crown-5 with potassium dodecatetradecanol phosphate, trimethylolpropane laurate and sodium pentadecylsulfonate at normal temperature, adding into No. 11 mineral oil, and uniformly stirring at 48 ℃ for 3h to obtain an oil solution; the addition amount of each component is as follows according to the parts by weight: 8 parts of No. 11 mineral oil; 10 parts of trimethylolpropane laurate; 2-hydroxymethyl-15-crown-585 parts; phosphoric ester of dodecatetradecanol11 parts of potassium salt; 5 parts of sodium pentadecylsulfonate. The prepared oil agent has crown ether content of 70.83 wt%, excellent high temperature resistance, thermal weight loss of 11 wt% after heating treatment at 200 deg.C for 2h, low viscosity, and kinematic viscosity of 30.1mm at (50 + -0.01) ° C2(s) a kinematic viscosity of 0.94mm after preparation with water as an emulsion having a concentration of 10% by weight2(s) 125N, the oil film strength is high, the surface tension of the oil is 23.2cN/cm, and the specific resistance is 1.8 × 108Omega cm, coefficient of static friction (mu) between fibres (F/F) after oilings) 0.250, coefficient of dynamic friction (. mu.)d) 0.272, coefficient of static friction (. mu.) between fiber and metal (F/M) after oilings) 0.209, coefficient of dynamic friction (. mu.)d) 0.329, and the prepared oil agent is prepared into an emulsion with the concentration of 15wt% by using water when in use;
(3) the soft polyester fiber is prepared by metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester, and the main spinning process parameters of the soft polyester fiber are shown in table 1.
The finally obtained soft polyester fiber has the initial modulus of 77cN/dtex, the fineness of 250dtex, the breaking strength of 3.9cN/dtex, the elongation at break of 48.0 percent, the CV value of the breaking strength of 4.7 percent, the CV value of the elongation at break of 9.6 percent, the shrinkage in boiling water of 8.0 percent and the oil content of 0.90 percent.
Example 4
A preparation method of soft polyester fiber comprises the following steps:
(1) preparation of modified polyester:
(a) performing esterification reaction; preparing terephthalic acid, ethylene glycol and adipic acid with a molar ratio of 1:1.5:0.06 into slurry, adding antimony trioxide, 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 255 ℃, and the esterification reaction end point is determined when the distilled amount of water in the esterification reaction reaches 95% of a theoretical value, wherein the adding amount of the antimony trioxide is 0.04% of the weight of the terephthalic acid, the adding amount of the titanium dioxide is 0.25% of the weight of the terephthalic acid, and the adding amount of the triphenyl phosphate is 0.01% of the weight of the terephthalic acid;
(b) performing 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 from normal pressure to the absolute pressure of 400Pa within 50min, controlling the reaction temperature to be 265 ℃ and the reaction time to be 33min, then continuing to pump the 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 90Pa, the reaction temperature is 280 ℃ and the reaction time is 50min, the molecular chain of the prepared modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and an adipic acid chain segment, the number average molecular weight is 23000, the molecular weight distribution index is 1.9, and the molar content of the adipic acid chain segment in the modified polyester is 3.5 percent of the molar content of the terephthalic acid chain segment;
(2) preparation of oiling oil agent: uniformly mixing 2-hydroxymethyl-12-crown-4 with dodecyl phosphate potassium salt, trimethylolpropane laurate and sodium hexadecylsulfonate at normal temperature, adding into 12# mineral oil, and uniformly stirring at 40 ℃ for 2.5h to obtain an oil agent; the addition amount of each component is as follows according to the parts by weight: 5 parts of No. 12 mineral oil; 2-hydroxymethyl-12-crown-495 parts; 9 parts of dodecyl phosphate potassium salt; and 2 parts of sodium hexadecyl sulfonate. The prepared oil agent has crown ether content of 85.58wt%, excellent high temperature resistance, thermal weight loss of 9 wt% after heating treatment at 200 deg.C for 2h, low viscosity, and kinematic viscosity of 29.5mm at (50 + -0.01) ° C2(s) a kinematic viscosity of 0.93mm after preparation with water as an emulsion having a concentration of 10% by weight2(s) the oil film strength of the oil agent is high and is 121N, the surface tension of the oil agent is 24.3cN/cm, and the specific resistance is 1.0 × 108Omega cm, coefficient of static friction (mu) between fibres (F/F) after oilings) 0.260, coefficient of dynamic friction (. mu.)d) 0.263, coefficient of static friction (. mu.m) between fiber and metal (F/M) after oilings) 0.202, coefficient of dynamic friction (. mu.)d) 0.330, and the prepared oil agent is prepared into 16 wt% emulsion by water when in use;
(3) the soft polyester fiber is prepared by metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester, and the main spinning process parameters of the soft polyester fiber are shown in table 1.
The finally obtained soft polyester fiber has the initial modulus of 80cN/dtex, the fineness of 190dtex, the breaking strength of 4.0cN/dtex, the elongation at break of 44.0 percent, the CV value of the breaking strength of 5.0 percent, the CV value of the elongation at break of 9.3 percent, the shrinkage in boiling water of 7.4 percent and the oil content of 0.80 percent.
Example 5
A preparation method of soft polyester fiber comprises the following steps:
(1) preparation of modified polyester:
(a) performing esterification reaction;
preparing terephthalic acid, ethylene glycol and adipic acid with a molar ratio of 1:1.6:0.03 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 normal pressure, the esterification reaction temperature is 257 ℃, and the esterification reaction endpoint is determined when the water distillation amount in the esterification reaction reaches 92% of a theoretical value, wherein the adding amount of the ethylene glycol antimony is 0.05% of the weight of the terephthalic acid, the adding amount of the titanium dioxide is 0.20% of the weight of the terephthalic acid, and the adding amount of the trimethyl phosphate is 0.04% of the weight of the terephthalic acid;
(b) performing 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 from normal pressure to the absolute pressure of 450Pa within 33min, controlling the reaction temperature to be 270 ℃ and the reaction time to be 30min, then continuing to pump the 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 95Pa, the reaction temperature is 275 ℃ and the reaction time is 60min, the molecular chain of the prepared modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and an adipic acid chain segment, the number average molecular weight is 25000, the molecular weight distribution index is 2.1, and the molar content of the adipic acid chain segment in the modified polyester is 5% of the molar content of the terephthalic acid chain segment;
(2) preparation of oiling oil agent: mixing 15-crown ether-5, isotridecanol polyoxyethylene ether phosphate potassium salt, trimethylolpropane laurate and sodium dodecyl sulfate at normal temperatureAdding into 13# mineral oil and stirring at 52 deg.C for 2h to obtain oil solution; the addition amount of each component is as follows according to the parts by weight: 10 parts of No. 13 mineral oil; 5 parts of trimethylolpropane laurate; 15-crown ether-570 parts; 8 parts of isomeric tridecanol polyoxyethylene ether phosphate potassium salt; 6 parts of sodium dodecyl sulfate. The prepared oil agent has crown ether content of 70.70 wt%, excellent high temperature resistance, thermal weight loss of 13.5 wt% after heating treatment at 200 ℃ for 2h, low viscosity of the oil agent, and kinematic viscosity of 28.6mm at (50 +/-0.01) ° C2(s) a kinematic viscosity of 0.95mm after preparation with water as an emulsion having a concentration of 10% by weight2The oil has high oil film strength of 126N, surface tension of 24.9cN/cm, and specific resistance of 1.2 × 108Omega cm, coefficient of static friction (mu) between fibres (F/F) after oilings) 0.251, coefficient of dynamic friction (. mu.)d) 0.262, coefficient of static friction (. mu.m) between fiber and metal (F/M) after oilings) 0.202, coefficient of dynamic friction (. mu.)d) 0.332, and when the prepared oil agent is used, water is used for preparing an emulsion with the concentration of 15 wt%;
(3) the soft polyester fiber is prepared by metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester, and the main spinning process parameters of the soft polyester fiber are shown in table 1.
The finally obtained soft polyester fiber has an initial modulus of 75cN/dtex, a fineness of 130dtex, a breaking strength of 4.4cN/dtex, an elongation at break of 43.2%, a CV value of the breaking strength of 4.8%, a CV value of the elongation at break of 9.5%, a shrinkage in boiling water of 7.8% and an oil content of 1.00%.
Example 6
A preparation method of soft polyester fiber comprises the following steps:
(1) preparation of modified polyester:
(a) performing esterification reaction;
preparing terephthalic acid, ethylene glycol and adipic acid with a molar ratio of 1:1.7:0.05 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 253 ℃, and the esterification reaction end point is determined when the distilled amount of water in the esterification reaction reaches 96% of a theoretical value, wherein the adding amount of antimony acetate is 0.01% of the weight of the terephthalic acid, the adding amount of titanium dioxide is 0.20% of the weight of the terephthalic acid, and the adding amount of trimethyl phosphite is 0.05% of the weight of the terephthalic acid;
(b) performing 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 from normal pressure to absolute pressure of 480Pa within 38min, controlling the reaction temperature to be 262 ℃ and the reaction time to be 38min, then continuing to pump the vacuum, and carrying out the polycondensation reaction in the high vacuum stage, so that the reaction pressure is further reduced to absolute pressure of 98Pa, the reaction temperature is 279 ℃ and the reaction time is 80min, the molecular chain of the prepared modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and an adipic acid chain segment, the number average molecular weight is 27000, the molecular weight distribution index is 2.2, and the molar content of the adipic acid chain segment in the modified polyester is 4% of the molar content of the terephthalic acid chain segment;
(2) preparation of oiling oil agent: uniformly mixing 2-hydroxymethyl-15-crown-5 with potassium dodecatetradecanol phosphate, trimethylolpropane laurate and sodium pentadecylsulfonate at normal temperature, adding into 14# mineral oil, and uniformly stirring at 55 ℃ for 1h to obtain an oil agent; the addition amount of each component is as follows according to the parts by weight: 3 parts of No. 14 mineral oil; 10 parts of trimethylolpropane laurate; 2-hydroxymethyl-15-crown-575 parts; 14 parts of potassium dodecatetradecanol phosphate; and 7 parts of sodium pentadecylsulfonate. The prepared oil agent has the crown ether content of 68.80 wt%, excellent high temperature resistance, thermal weight loss of 12 wt% after heat treatment at 200 ℃ for 2h, low viscosity, and kinematic viscosity of 27.5mm at (50 +/-0.01) ° C2(s) a kinematic viscosity of 0.95mm after preparation with water as an emulsion having a concentration of 10% by weight2The oil has a high oil film strength of 126N, a surface tension of 25.4cN/cm and a specific resistance of 1.6 × 108Omega cm, coefficient of static friction (mu) between fibres (F/F) after oilings) 0.255, coefficient of dynamic friction (. mu.)d) 0.267, coefficient of static friction (. mu.) between fiber and metal (F/M) after oilings) 0.203, coefficient of dynamic friction (. mu.)d) 0.330, and the prepared oil agent is prepared into an emulsion with the concentration of 17 wt% by using water when in use;
(3) the soft polyester fiber is prepared by metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester, and the main spinning process parameters of the soft polyester fiber are shown in table 1.
The finally obtained soft polyester fiber has an initial modulus of 71cN/dtex, a fineness of 75dtex, a breaking strength of 3.7cN/dtex, an elongation at break of 45.5%, a CV value of the breaking strength of 4.9%, a CV value of the elongation at break of 10.0%, a shrinkage in boiling water of 7.3% and an oil content of 0.92%.
Example 7
A preparation method of soft polyester fiber comprises the following steps:
(1) preparation of modified polyester:
(a) performing esterification reaction;
preparing terephthalic acid, ethylene glycol and adipic acid with a molar ratio of 1:1.8:0.03 into slurry, adding antimony trioxide, 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 250 ℃, and the esterification reaction end point is determined when the distilled amount of water in the esterification reaction reaches 90% of a theoretical value, wherein the adding amount of the antimony trioxide is 0.03% of the weight of the terephthalic acid, the adding amount of the titanium dioxide is 0.24% of the weight of the terephthalic acid, and the adding amount of the triphenyl phosphate is 0.02% of the weight of the terephthalic acid;
(b) performing polycondensation reaction;
after the esterification reaction is finished, starting the polycondensation reaction in the low vacuum stage under the negative pressure condition, smoothly pumping the pressure from normal pressure to the absolute pressure of 455Pa within 42min, the reaction temperature of 264 ℃ and the reaction time of 45min, then continuing to pump the vacuum, and carrying out the polycondensation reaction in the high vacuum stage to further reduce the reaction pressure to the absolute pressure of 85Pa, the reaction temperature of 285 ℃ and the reaction time of 75min, wherein the molecular chain of the prepared modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and an adipic acid chain segment, the number average molecular weight of 26500 and the molecular weight distribution index of 2.2, and the molar content of the adipic acid chain segment in the modified polyester is 4.5 percent of the molar content of the terephthalic acid;
(2) preparation of oiling oil agent: uniformly mixing 15-crown ether-5 with dodecyl phosphate potassium salt, trimethylolpropane laurate and sodium hexadecylsulfonate at normal temperature, adding the mixture into 15# mineral oil, and uniformly stirring the mixture for 2 hours at 41 ℃ to obtain an oil agent; the addition amount of each component is as follows according to the parts by weight: 8 parts of No. 15 mineral oil; 20 parts of trimethylolpropane laurate; 15-crown ether-5100 parts; 15 parts of dodecyl phosphate potassium salt; and 2 parts of sodium hexadecyl sulfonate. The prepared oil agent has the crown ether content of 68.97 wt%, excellent high temperature resistance, thermal weight loss of 8.5 wt% after 2h of heat treatment at 200 ℃, low viscosity of the oil agent, and kinematic viscosity of 28.4mm at (50 +/-0.01) ° C2(s) a kinematic viscosity of 0.94mm after preparation with water as an emulsion having a concentration of 10% by weight2(s) 122N, the oil film strength is high, the surface tension of the oil is 26.8cN/cm, and the specific resistance is 1.8 × 108Omega cm, coefficient of static friction (mu) between fibres (F/F) after oilings) 0.263, coefficient of dynamic friction (. mu.)d) 0.268, coefficient of static friction (. mu.M) between fiber and metal (F/M) after oilings) 0.210, coefficient of dynamic friction (. mu.)d) 0.320, and the prepared oil agent is prepared into 16 wt% emulsion by water when in use;
(3) the soft polyester fiber is prepared by metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester, and the main spinning process parameters of the soft polyester fiber are shown in table 1.
The finally obtained soft polyester fiber has the initial modulus of 72cN/dtex, the fineness of 72dtex, the breaking strength of 3.7cN/dtex, the elongation at break of 45.0 percent, the CV value of the breaking strength of 4.9 percent, the CV value of the elongation at break of 10.0 percent, the shrinkage in boiling water of 7.0 percent and the oil content of 0.90 percent.
Example 8
A preparation method of soft polyester fiber comprises the following steps:
(1) preparation of modified polyester:
(a) performing esterification reaction;
preparing terephthalic acid, ethylene glycol and adipic acid with a molar ratio of 1:1.9:0.04 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 amount of water in the esterification reaction reaches 93% of a theoretical value, wherein the adding amount of the ethylene glycol antimony is 0.04% of the weight of the terephthalic acid, the adding amount of the titanium dioxide is 0.21% of the weight of the terephthalic acid, and the adding amount of the trimethyl phosphate is 0.03% of the weight of the terephthalic acid;
(b) performing 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 from normal pressure to absolute pressure of 475Pa within 45min, the reaction temperature of 265 ℃ and the reaction time of 48min, then continuing to pump the vacuum, and carrying out the polycondensation reaction in the high vacuum stage, so that the reaction pressure is further reduced to absolute pressure of 88Pa, the reaction temperature is 283 ℃ and the reaction time is 80min, the molecular chain of the prepared modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and an adipic acid chain segment, the number average molecular weight is 23000, the molecular weight distribution index is 2.0, and the molar content of the adipic acid chain segment in the modified polyester is 3% of the molar content of the terephthalic acid chain segment;
(2) preparation of oiling oil agent: uniformly mixing 2-hydroxymethyl-12-crown-4 with potassium dodecatetradecanol phosphate, trimethylolpropane laurate and sodium pentadecylsulfonate at normal temperature, adding into 16# mineral oil, and uniformly stirring at 45 ℃ for 3h to obtain an oil solution; the addition amount of each component is as follows according to the parts by weight: 9 parts of No. 16 mineral oil; 2-hydroxymethyl-12-crown-480 parts; 12 parts of potassium dodecatetradecanol phosphate; 5 parts of sodium pentadecylsulfonate. The prepared oil agent has crown ether content of 83.33 wt%, excellent high temperature resistance, thermal weight loss of 14 wt% after heating treatment at 200 deg.C for 2h, low viscosity of the oil agent, and kinematic viscosity of 30.0mm at (50 + -0.01) ° C2(s) a kinematic viscosity of 0.93mm after preparation with water as an emulsion having a concentration of 10% by weight2The oil film strength of the oil agent was 127N. The surface tension of the oil agent is23.5cN/cm, specific resistance 1.5 × 108Omega cm, coefficient of static friction (mu) between fibres (F/F) after oilings) 0.262, coefficient of dynamic friction (. mu.)d) 0.273, coefficient of static friction (. mu.M) between fiber and metal (F/M) after oilings) 0.208, coefficient of dynamic friction (. mu.)d) 0.328, and the prepared oil agent is prepared into emulsion with the concentration of 18 wt% by using water when in use;
(3) the soft polyester fiber is prepared by metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester, and the main spinning process parameters of the soft polyester fiber are shown in table 1.
The finally obtained soft polyester fiber has the initial modulus of 80cN/dtex, the fineness of 200dtex, the breaking strength of 3.8cN/dtex, the elongation at break of 42.0 percent, the CV value of the breaking strength of 4.2 percent, the CV value of the elongation at break of 9.5 percent, the shrinkage in boiling water of 8.0 percent and the oil content of 0.90 percent.
Example 9
A preparation method of soft polyester fiber comprises the following steps:
(1) preparation of modified polyester:
(a) performing esterification reaction;
preparing terephthalic acid, ethylene glycol and adipic acid with a molar ratio of 1:2.0:0.05 into slurry, adding antimony acetate, titanium dioxide and trimethyl phosphate, uniformly mixing, pressurizing in a nitrogen atmosphere to perform esterification reaction, wherein the pressurizing pressure is normal pressure MPa, the esterification reaction temperature is 251 ℃, and the esterification reaction endpoint is determined when the water distillation amount in the esterification reaction reaches 96% of a theoretical value, wherein the adding amount of the antimony acetate is 0.05% of the weight of the terephthalic acid, the adding amount of the titanium dioxide is 0.22% of the weight of the terephthalic acid, and the adding amount of the trimethyl phosphate is 0.04% of the weight of the terephthalic acid;
(b) performing 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 from normal pressure to the absolute pressure of 420Pa within 30min, controlling the reaction temperature to 267 ℃, controlling the reaction time to 50min, then continuing to pump the 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 280 ℃, and the reaction time is 90min, the molecular chain of the prepared modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and an adipic acid chain segment, the number average molecular weight is 24000, the molecular weight distribution index is 2.2, and the molar content of the adipic acid chain segment in the modified polyester is 4% of the molar content of the terephthalic acid chain segment;
(2) preparation of oiling oil agent: uniformly mixing 2-hydroxymethyl-15-crown-5 with dodecyl phosphate potassium salt, trimethylolpropane laurate and sodium dodecyl sulfate at normal temperature, and uniformly stirring at 55 ℃ for 3 hours to obtain an oil agent; the addition amount of each component is as follows according to the parts by weight: 15 parts of trimethylolpropane laurate; 2-hydroxymethyl-15-crown-590 parts; 8 parts of dodecyl phosphate potassium salt; 7 parts of sodium dodecyl sulfate. The prepared oil agent has the crown ether content of 81.81 wt%, excellent high temperature resistance, thermal weight loss of 10wt% after heating treatment at 200 ℃ for 2h, low viscosity of the oil agent, and kinematic viscosity of 29.7mm at (50 +/-0.01) ° C2(s) a kinematic viscosity of 0.94mm after preparation with water as an emulsion having a concentration of 10% by weight2The oil has a high oil film strength of 126N, a surface tension of 24.8cN/cm and a specific resistance of 1.8 × 108Omega cm, coefficient of static friction (mu) between fibres (F/F) after oilings) 0.250, coefficient of dynamic friction (. mu.)d) 0.264, coefficient of static friction (. mu.m) between fiber and metal (F/M) after oilings) 0.210, coefficient of dynamic friction (. mu.)d) 0.321, preparing the prepared oil agent into an emulsion with the concentration of 17 wt% by using water when in use;
(3) the soft polyester fiber is prepared by metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester, and the main spinning process parameters of the soft polyester fiber are shown in table 1.
The finally obtained soft polyester fiber has the initial modulus of 76cN/dtex, the fineness of 240dtex, the breaking strength of 3.9cN/dtex, the elongation at break of 42.0 percent, the CV value of the breaking strength of 5.0 percent, the CV value of the elongation at break of 9.4 percent, the shrinkage in boiling water of 7.0 percent and the oil content of 0.70 percent.
Example 10
A preparation method of soft polyester fiber comprises the following steps:
(1) preparation of modified polyester:
(a) performing esterification reaction;
preparing terephthalic acid, ethylene glycol and adipic acid with a molar ratio of 1:1.2:0.06 into slurry, adding ethylene glycol antimony, titanium dioxide and trimethyl phosphite, uniformly mixing, pressurizing in a nitrogen atmosphere to perform esterification reaction, wherein the pressurizing pressure is 0.1MPa, the esterification reaction temperature is 255 ℃, and the esterification reaction endpoint is determined when the distilled amount of water in the esterification reaction reaches 92% of a theoretical value, wherein the adding amount of the ethylene glycol antimony is 0.01% of the weight of the terephthalic acid, the adding amount of the titanium dioxide is 0.20% of the weight of the terephthalic acid, and the adding amount of the trimethyl phosphite is 0.01% of the weight of the terephthalic acid;
(b) performing 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 from normal pressure to absolute pressure of 490Pa within 50min, the reaction temperature of 269 ℃, the reaction time of 30min, then continuing to pump the vacuum, and carrying out the polycondensation reaction in the high vacuum stage, so that the reaction pressure is further reduced to absolute pressure of 100Pa, the reaction temperature of 281 ℃, and the reaction time of 55min, the molecular chain of the prepared modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and an adipic acid chain segment, the number average molecular weight is 20000, the molecular weight distribution index is 1.9, and the molar content of the adipic acid chain segment in the modified polyester is 3.5% of the molar content of the terephthalic acid chain segment;
(2) preparation of oiling oil agent: uniformly mixing 2-hydroxymethyl-15-crown-5 with dodecyl phosphate potassium salt, trimethylolpropane laurate and sodium dodecyl sulfate at normal temperature, and uniformly stirring at 55 ℃ for 3 hours to obtain an oil agent; the addition amount of each component is as follows according to the parts by weight: 15 parts of trimethylolpropane laurate; 2-hydroxymethyl-15-crown-590 parts; 8 parts of dodecyl phosphate potassium salt; 7 parts of sodium dodecyl sulfate. The prepared oil agent has the crown ether content of 81.81 wt%, excellent high temperature resistance, thermal weight loss of 10wt% after heating treatment at 200 ℃ for 2h, low viscosity (50 +/-0)01) DEG C, the kinematic viscosity is 29.7mm2(s) a kinematic viscosity of 0.94mm after preparation with water as an emulsion having a concentration of 10% by weight2The oil has high oil film strength of 126N, surface tension of 24.8cN/cm, and specific resistance of 1.8 × 108Omega cm, coefficient of static friction (mu) between fibres (F/F) after oilings) 0.250, coefficient of dynamic friction (. mu.)d) 0.264, coefficient of static friction (. mu.m) between fiber and metal (F/M) after oilings) 0.210, coefficient of dynamic friction (. mu.)d) 0.321, the prepared oil agent is prepared into emulsion with 16 wt% concentration by water when in use;
(3) the soft polyester fiber is prepared by metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester, and the main spinning process parameters of the soft polyester fiber are shown in table 1.
The finally obtained soft polyester fiber has the initial modulus of 74cN/dtex, the fineness of 150dtex, the breaking strength of 4.5cN/dtex, the elongation at break of 48.0 percent, the CV value of the breaking strength of 4.4 percent, the CV value of the elongation at break of 9.7 percent, the shrinkage in boiling water of 7.5 percent and the oil content of 0.70 percent.
Example 11
A preparation method of soft polyester fiber comprises the following steps:
(1) preparation of modified polyester:
(a) performing esterification reaction;
preparing terephthalic acid, ethylene glycol and adipic acid with a molar ratio of 1:2.0:0.03 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 250 ℃, and the esterification reaction endpoint is determined when the water distillation amount in the esterification reaction reaches 97% of a theoretical value, wherein the adding amount of antimony acetate is 0.01% of the weight of the terephthalic acid, the adding amount of titanium dioxide is 0.23% of the weight of the terephthalic acid, and the adding amount of trimethyl phosphite is 0.05% of the weight of the terephthalic acid;
(b) performing polycondensation reaction;
after the esterification reaction is finished, starting the polycondensation reaction in the low vacuum stage under the condition of negative pressure, stably pumping the pressure from normal pressure to the absolute pressure of 500Pa within 45min, controlling the reaction temperature to be 260 ℃ and the reaction time to be 40min, then continuing to pump the vacuum, and carrying out the polycondensation reaction in the high vacuum stage to further reduce the reaction pressure to the absolute pressure of 92Pa, controlling the reaction temperature to be 277 ℃ and the reaction time to be 80min, wherein the molecular chain of the prepared modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and a 3 adipic acid chain segment, the number average molecular weight is 25500, the molecular weight distribution index is 1.8, and the molar content of the adipic acid chain segment in the modified polyester is 5% of the molar content of the terephthalic acid chain segment.
(2) Preparation of oiling oil agent: uniformly mixing 2-hydroxymethyl-12-crown-4 with dodecyl phosphate potassium salt, trimethylolpropane laurate and sodium dodecyl sulfate at normal temperature, adding into No. 9 mineral oil, and uniformly stirring at 40 ℃ for 1h to obtain an oil agent; the addition amount of each component is as follows according to the parts by weight: 2 parts of No. 9 mineral oil; 10 parts of trimethylolpropane laurate; 2-hydroxymethyl-12-crown-490 parts; 8 parts of dodecyl phosphate potassium salt; and 3 parts of sodium dodecyl sulfate. The prepared oil agent has crown ether content of 79.6 wt%, excellent high temperature resistance, thermal weight loss of 14.5 wt% after heating treatment at 200 ℃ for 2h, low viscosity of the oil agent, and kinematic viscosity of 29.6mm at (50 +/-0.01) ° C2(s) a kinematic viscosity of 0.93mm after preparation with water as an emulsion having a concentration of 10% by weight2(s) the oil has high oil film strength of 125N, surface tension of 24.8cN/cm, and specific resistance of 1.3 × 108Omega cm, coefficient of static friction (mu) between fibres (F/F) after oilings) 0.255, coefficient of dynamic friction (. mu.)d) 0.266, after oiling, the coefficient of static friction (μ) between fiber and metal (F/M)s) 0.203, coefficient of dynamic friction (. mu.)d) 0.320, and the prepared oil agent is prepared into an emulsion with the concentration of 15wt% by using water when in use;
(3) the soft polyester fiber is prepared by metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester, and the main spinning process parameters of the soft polyester fiber are shown in table 1.
The finally obtained soft polyester fiber has the initial modulus of 79cN/dtex, the fineness of 300dtex, the breaking strength of 3.8cN/dtex, the elongation at break of 48.0 percent, the CV value of the breaking strength of 4.7 percent, the CV value of the elongation at break of 9.9 percent, the shrinkage in boiling water of 8.0 percent and the oil content of 1.10 percent.
TABLE 1
Figure BDA0001508556760000191
Figure BDA0001508556760000201

Claims (6)

1. The preparation method of the soft polyester fiber is characterized by comprising the following steps: metering, extruding, cooling, oiling, stretching, heat setting and winding the modified polyester to obtain soft polyester fiber;
the molecular chain of the modified polyester comprises a terephthalic acid chain segment, an ethylene glycol chain segment and an adipic acid chain segment;
the oiling oil agent contains crown ether, and the content of the crown ether is 67.30-85.58 wt%;
the crown ether is 2-hydroxymethyl-12-crown-4, 15-crown ether-5 or 2-hydroxymethyl-15-crown-5;
when the oil agent is used, preparing an emulsion with the concentration of 10-20 wt% by using water;
the thermal weight loss of the oil agent after heating treatment for 2 hours at 200 ℃ is less than 15 wt%;
the kinematic viscosity of the oil agent is 27.5-30.1 mm at the temperature of (50 +/-0.01) ° C2The kinematic viscosity of the oil agent prepared from water into 10wt% emulsion is 0.93-0.95 mm2/s；
The oil film strength of the oil agent is 121-127N;
the surface tension of the oil agent is 23.2-26.8 cN/cm, and the specific resistance is 1.0 × 108~1.8×108Ω·cm；
After oiling, the static friction coefficient between the fibers is 0.250-0.263, and the dynamic friction coefficient is 0.262-0.273;
after oiling, the static friction coefficient between the fiber and the metal is 0.202-0.210, and the dynamic friction coefficient is 0.320-0.332;
the soft polyester fiber is made of modified polyester;
the initial modulus of the soft polyester fiber is less than or equal to 80 cN/dtex;
the fineness of the soft polyester fiber is 75-300 dtex, the breaking strength is more than or equal to 3.6cN/dtex, the elongation at break is 45.0 +/-3.0%, the CV value of the breaking strength is less than or equal to 5.0%, the CV value of the elongation at break is less than or equal to 10.0%, the boiling water shrinkage is 7.5 +/-0.5%, and the oil content is 0.90 +/-0.20%.
2. The method for preparing the soft polyester fiber according to claim 1, wherein the following components are added to the finish in parts by weight:
0-10 parts of mineral oil;
0-20 parts of trimethylolpropane laurate;
70-100 parts of crown ether;
8-15 parts of phosphate potassium salt;
2-7 parts of sodium alkylsulfonate;
the preparation method of the oil agent comprises the following steps: uniformly mixing all the components and then uniformly stirring to obtain an oil agent;
the mixing is carried out at normal temperature, the stirring temperature is 40-55 ℃, and the stirring time is 1-3 h.
3. The method for preparing the soft polyester fiber according to any one of claims 1 to 2, wherein the spinning process parameters of the soft polyester fiber are as follows:
spinning temperature: 280-290 ℃;
cooling temperature: 20-25 ℃;
network pressure: 0.20 to 0.30 MPa;
a roll speed: 2200 to 2600m/min
First roll temperature: 75-85 ℃;
two roll speed: 3600-3900 m/min;
temperature of the two rolls: 135-165 ℃;
speed of winding: 3580-3840 m/min.
4. The method for producing a soft polyester fiber according to claim 1, wherein the modified polyester has a number average molecular weight of 20000 to 27000 and a molecular weight distribution index of 1.8 to 2.2;
the molar content of the adipic acid chain segment in the modified polyester is 5-8% of that of the terephthalic acid chain segment.
5. The method for preparing a soft polyester fiber according to claim 4, wherein the modified polyester is prepared by: uniformly mixing terephthalic acid, ethylene glycol and adipic acid, and then carrying out esterification reaction and polycondensation reaction in sequence to obtain modified polyester; the method comprises the following specific steps:
(1) performing esterification reaction;
preparing terephthalic acid, ethylene glycol and adipic acid into slurry, adding a catalyst, a delustering agent and a stabilizer, uniformly mixing, and pressurizing in a nitrogen atmosphere to perform esterification reaction, wherein the pressurizing pressure is normal pressure-0.3 MPa, the esterification reaction temperature is 250-260 ℃, and the esterification reaction end point is determined when the distilled amount of water 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 a 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 260-270 ℃ for 30-50 min, then continuously pumping the vacuum to perform the polycondensation reaction in a high vacuum stage, further reducing the reaction pressure to below 100Pa, controlling the reaction temperature to 275-285 ℃ and the reaction time to be 50-90 min, and thus obtaining the modified polyester.
6. The method for preparing the soft polyester fiber according to claim 5, wherein in the step (1), the molar ratio of the terephthalic acid, the ethylene glycol and the adipic acid is 1: 1.2-2.0: 0.03-0.06, the addition amount of the catalyst is 0.01-0.05% of the weight of the terephthalic acid, the addition amount of the delustering agent is 0.20-0.25% of the weight of the terephthalic acid, and the addition amount of the stabilizer is 0.01-0.05% of the weight of the terephthalic acid;
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.
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