CN111349980A - Method for manufacturing microporous polyester fiber - Google Patents

Method for manufacturing microporous polyester fiber Download PDF

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Publication number
CN111349980A
CN111349980A CN202010078232.4A CN202010078232A CN111349980A CN 111349980 A CN111349980 A CN 111349980A CN 202010078232 A CN202010078232 A CN 202010078232A CN 111349980 A CN111349980 A CN 111349980A
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China
Prior art keywords
polyester
fiber
polyester fiber
double salt
hot water
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Pending
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CN202010078232.4A
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Chinese (zh)
Inventor
李革
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Jiangsu Yinzhao New Material Technology Co ltd
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Jiangsu Yinzhao New Material Technology Co ltd
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Priority to CN202010078232.4A priority Critical patent/CN111349980A/en
Publication of CN111349980A publication Critical patent/CN111349980A/en
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
    • 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)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Textile Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention discloses a manufacturing method of microporous polyester fiber, which is prepared by further polymerizing terephthalic acid and/or terephthalic dicarboxylic ester and dihydric alcohol monomer in the presence of oxalic acid double salt and conventional polycondensation catalyst after esterification or ester exchange. The polyester is sliced, granulated and melt spun to obtain the polyester fiber. The obtained polyester fiber is treated by high-temperature hot water, so that the obtained fiber contains a large number of through micropores on the surface and in the interior, and the fiber density is 1.15-1.30g/cm3The cloth made of the fiber has good moisture absorption and air permeability.

Description

Method for manufacturing microporous polyester fiber
Technical Field
The invention relates to the technical field of polyester fiber manufacturing, in particular to a manufacturing method of microporous polyester fiber.
Background
The polyester fiber has excellent physical and chemical properties, and is widely applied to textiles such as clothing and the like. However, the polyester fiber has hydrophobic surface, poor moisture absorption and air permeability, which leads to stuffiness and poor comfort for the wearer. In order to improve the moisture absorption and air permeability of polyester fibers, the physical or chemical structure of the interior and the surface of the polyester fibers is often modified by a modification method, so as to obtain better performance and comfort.
Microporosity is one of the modification methods that change the structure of the interior and surface of a fiber by physical methods, thereby changing some basic properties of the original fiber. The introduction of pores, especially through pores, into the fiber interior and surface can not only change the density and specific surface area of the fiber, but also change the surface hydrophilic property, moisture absorption property and water conductivity of the fiber. Compared with the common polyester fiber, the fabric made of the microporous polyester fiber has better moisture absorption and moisture conductivity, and a wearer feels dry and comfortable. In addition, as the pores contain a large amount of still air, the heat retention property of the cloth made of the fiber is also obviously improved.
Chinese patent CN100424241C discloses a method for preparing porous polyester fiber. The method uses a mixed polyester of a conventional polyester and a readily hydrolyzable polyester as a raw material to carry out melt spinning, and then uses an aqueous solution of sodium hydroxide to carry out alkali weight reduction treatment to dissolve the readily hydrolyzable polyester, thereby obtaining a polyester fiber having a microporous structure. Chinese patent CN101144206A discloses a similar method for making porous polyester fiber. The method also uses a mixed raw material of a conventional polyester and a water-soluble polyester to carry out melt spinning, and then the water-soluble polyester is dissolved out to prepare the porous polyester fiber. Another chinese patent CN107502990A discloses a similar method for making porous fiber. The difference is that the fiber is added with water-soluble polymer and inorganic substances such as calcium carbonate. In the subsequent dissolution treatment, the water-soluble polymer is dissolved with water, and then the calcium carbonate is dissolved with acid. Similar patent publications can be cited in many cases, but in any case, the common thing is that a polymer and/or other additives added must be dissolved out, which causes unnecessary waste and also imposes an additional burden on the environment, particularly when acid or alkali treatment is required. Therefore, an improved technique for solving the problem in the prior art is desired.
Disclosure of Invention
The invention aims to provide a method for manufacturing microporous polyester fiber, wherein oxalate double salt is put in the synthesis stage of polyester, no special requirement is made on existing equipment, the obtained polyester is uniform, other soluble substances are not required to be added, the later spinning process is easy to override, the oxalate double salt plays the role of a pore-forming agent, but the oxalate double salt is not decomposed or dissolved out in the hot water treatment process, and is not decomposed by acid or alkali or dissolved out by a solvent unlike other pore-forming agents, so unnecessary waste is not generated, no extra burden is brought to the environment, the fiber after the hot water treatment has a through microporous structure, the manufactured fabric has good moisture absorption and moisture conductivity, particularly the fabric made of hydrophilic polyester, the water absorption performance of the fabric exceeds that of pure cotton, and the easy drying performance of the polyester fiber is still maintained, to solve the problems set forth in the background art described above.
In order to achieve the purpose, the invention provides the following technical scheme:
a method of making a microporous polyester fiber comprising the steps of:
the method comprises the following steps: after terephthalic acid and/or terephthalic dicarboxylic acid ester and dihydric alcohol monomer are esterified or subjected to ester exchange, further polymerizing in the presence of oxalic acid double salt and a conventional polycondensation catalyst to prepare polyester;
step two: slicing and granulating the obtained polyester, and then carrying out melt spinning to obtain polyester fiber;
step three: the obtained polyester fiber is treated by high-temperature hot water, the surface and the inside of the prepared fiber contain a large number of through micropores, and the fiber density is 1.15-1.30g/cm3。
Preferably, the terephthalic dicarboxylic acid ester is a dibasic ester compound of terephthalic acid with a lower saturated fatty acid, such as dimethyl terephthalate, diethyl terephthalate, dipropyl terephthalate, or the like.
Preferably, the diol monomer has the following formula: HO- (CH)2)n-OH；
Wherein n represents an integer of 2 to 10.
Preferably, the oxalic acid double salt is added in an amount of 2-10% of the total weight of the polyester, and has the following molecular formula: mnZ(C2O4)m；
Wherein M represents alkali metal elements such as lithium, sodium, potassium, rubidium or cesium;
wherein Z represents polyvalent metal elements such as magnesium, aluminum, calcium, strontium, barium, scandium, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, zinc, gallium, indium, tin or antimony;
wherein m and n represent integers of 1, 2, 3, 4, etc.
Preferably, the temperature of the high-temperature hot water treatment is 110-140-oC, the treatment time is 10-60 minutes.
Compared with the prior art, the invention has the beneficial effects that:
(1) the oxalic acid double salt is put into the polyester synthesis stage, no special requirement is required for existing equipment, the obtained polyester is uniform, other soluble substances are not required to be added, and the later spinning process is easy to override.
(2) The oxalic acid double salt serves as a pore-forming agent, but is not decomposed or dissolved out in the hot water treatment process, and is not decomposed by acid or alkali or dissolved out by a solvent unlike other pore-forming agents, so that unnecessary waste is not generated, and extra burden is not brought to the environment.
(3) The fiber after hot water treatment has a through microporous structure, and the prepared cloth has good moisture absorption and moisture conductivity, particularly the cloth prepared from hydrophilic polyester has the moisture absorption performance exceeding that of pure cotton, and simultaneously the dryness performance of the polyester fiber is still maintained.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples do not specify particular techniques or conditions, and are carried out according to the techniques or conditions described in the literature in the art or according to the product specifications.
The invention provides a technical scheme that:
a method of making a microporous polyester fiber comprising the steps of:
the method comprises the following steps: after terephthalic acid and/or terephthalic dicarboxylic acid ester and dihydric alcohol monomer are esterified or subjected to ester exchange, further polymerizing in the presence of oxalic acid double salt and a conventional polycondensation catalyst to prepare polyester;
step two: slicing and granulating the obtained polyester, and then carrying out melt spinning to obtain polyester fiber;
step three: the obtained polyester fiber is treated by high-temperature hot water,the fiber obtained thereby has a large number of through-holes on the surface and inside, and a fiber density of 1.15-1.30g/cm3。
The fabric made of the fiber has good moisture absorption and air permeability.
The terephthalic dicarboxylic acid ester is a dibasic ester compound of terephthalic acid with a lower saturated fatty acid, such as dimethyl terephthalate, diethyl terephthalate, dipropyl terephthalate, or the like.
The diol monomer has the following formula: HO- (CH)2)n-OH; wherein n represents an integer of 2 to 10.
The addition amount of the oxalic acid double salt is 1-20% of the total weight of the polyester, preferably 2-10% of the total weight of the polyester, and the oxalic acid double salt has the following molecular formula: mnZ(C2O4)m(ii) a Wherein M represents alkali metal elements such as lithium, sodium, potassium, rubidium or cesium; wherein Z represents polyvalent metal elements such as magnesium, aluminum, calcium, strontium, barium, scandium, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, zinc, gallium, indium, tin or antimony; wherein m and n represent integers of 1, 2, 3, 4, etc.
The temperature of the high-temperature hot water treatment is 100-160 DEG CoC, preferably 110-oAnd C, the treatment time is 5 to 100 minutes, and preferably 10 to 60 minutes.
Example 1:
weighing equal single amount of dimethyl terephthalate and ethylene glycol, adding into a reaction kettle, and gradually heating to 220-230-oAnd C, carrying out ester exchange reaction. After the transesterification reaction was completed, K was added in an amount of 8wt% based on the total weight of the polyester3Al(C2O4)3And proper amount of antimony trioxide catalyst and triphenyl phosphate stabilizer, and the temperature is gradually increased to 280 ℃ under vacuumoC, performing polycondensation reaction. The obtained polyester is sliced, granulated and melt-spun to obtain the polyester fiber with the density of 1.39g/cm3。
Placing the obtained fiber at 140oC, taking out after hot water heat treatment for 10 minutes, and measuring the fiber density to be 1.25g/cm3The porosity was 10%. The fibers are at 34oC. Relative to each otherThe moisture regain in an environment with a humidity of 92% was 8%. And the moisture regain of the common polyester fiber under the same condition is only 0.6 percent, which shows that the fiber prepared by the method has better moisture absorption performance than the common polyester fiber under the high-humidity environment.
Example 2:
weighing equal single amount of terephthalic acid and ethylene glycol, adding into a reaction kettle, and gradually heating to 220-230-oAnd C, carrying out esterification reaction. After the esterification had proceeded to 90% of theory, K was added in succession in an amount corresponding to 4% by weight of the total weight of the polyester3Al(C2O4)3And proper amount of antimony trioxide catalyst and triphenyl phosphate stabilizer, and the temperature is gradually increased to 280 ℃ under vacuumoC, performing polycondensation reaction. The obtained polyester is sliced, granulated and melt-spun to obtain the polyester fiber with the density of 1.39g/cm3。
Placing the obtained fiber at 150 deg.CoC, taking out after hot water heat treatment for 10 minutes, and measuring the fiber density to be 1.28g/cm3The porosity was 8%. The fibers are at 34oC. The moisture regain in an environment with a relative humidity of 92% was 5.5%. And the moisture regain of the common polyester fiber under the same condition is only 0.6 percent, which shows that the fiber prepared by the method has better moisture absorption performance than the common polyester fiber under the high-humidity environment.
Comparative example 1:
weighing equal single amount of dimethyl terephthalate and ethylene glycol, adding into a reaction kettle, and gradually heating to 220-230-oAnd C, carrying out ester exchange reaction. Al is added in an amount of 8wt% based on the total weight of the polyester2(C2O4)3And proper amount of antimony trioxide catalyst and triphenyl phosphate stabilizer are gradually heated to 280 ℃ under vacuumoC, performing polycondensation reaction. The obtained polyester is sliced, granulated and melt-spun to obtain the polyester fiber with the density of 1.39g/cm3。
Placing the obtained fiber at 140oC, taking out after hot water heat treatment for 10 minutes, and measuring the fiber density to be 1.39g/cm3The porosity was 0%. The fibers are at 34oC. Phase (C)The moisture regain of the polyester fiber in the environment with the humidity of 92 percent is 0.6 percent, and the polyester fiber has no difference with the common polyester fiber products and has no obvious moisture absorption in the high-humidity environment.
The results of comparative example 1 show that when the oxalic acid double salt of the present invention was substituted with a common oxalate, the fiber obtained by the same method had no microporous structure and could not be modified.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (5)

1. A method for manufacturing microporous polyester fibers is characterized in that: the method comprises the following steps:
the method comprises the following steps: after terephthalic acid and/or terephthalic dicarboxylic acid ester and dihydric alcohol monomer are esterified or subjected to ester exchange, further polymerizing in the presence of oxalic acid double salt and a conventional polycondensation catalyst to prepare polyester;
step two: slicing and granulating the obtained polyester, and then carrying out melt spinning to obtain polyester fiber;
step three: the obtained polyester fiber is treated by high-temperature hot water, the surface and the inside of the prepared fiber contain a large number of through micropores, and the fiber density is 1.15-1.30g/cm3。
2. The terephthalic acid dicarboxylate monomer according to claim 1, wherein: the monomer is a dibasic ester compound of terephthalic acid and lower saturated fatty acid, such as dimethyl terephthalate, diethyl terephthalate, dipropyl terephthalate, etc.
3. The diol monomer according to claim 1, wherein: the monomer has the following molecular formula: HO- (CH)2)n-OH；
Wherein n represents an integer of 2 to 10.
4. The double salt of oxalic acid according to claim 1, wherein: the addition amount of the oxalic acid double salt is 1-20% of the total weight of the polyester, and the oxalic acid double salt has the following molecular formula: mnZ(C2O4)m；
Wherein M represents alkali metal elements such as lithium, sodium, potassium, rubidium or cesium;
wherein Z represents polyvalent metal elements such as magnesium, aluminum, calcium, strontium, barium, scandium, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, zinc, gallium, indium, tin or antimony;
wherein m and n represent integers of 1, 2, 3, 4, etc.
5. High temperature hot water treatment of polyester fiber according to claim 1, characterized in that: the temperature of the high-temperature hot water treatment is 100-160 DEG CoC, the treatment time is 5-100 minutes.
CN202010078232.4A 2020-02-03 2020-02-03 Method for manufacturing microporous polyester fiber Pending CN111349980A (en)

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CN202010078232.4A CN111349980A (en) 2020-02-03 2020-02-03 Method for manufacturing microporous polyester fiber

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Application Number Priority Date Filing Date Title
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5407752A (en) * 1991-08-28 1995-04-18 Mitsubishi Rayon Company Ltd. Polyester resin
CN101144206A (en) * 2007-10-23 2008-03-19 浙江理工大学 Multi-micropore polyester fiber and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5407752A (en) * 1991-08-28 1995-04-18 Mitsubishi Rayon Company Ltd. Polyester resin
CN101144206A (en) * 2007-10-23 2008-03-19 浙江理工大学 Multi-micropore polyester fiber and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
张树钧等: "《改性纤维与特种纤维》", 31 October 1995, 中国石化出版社 *
美国国家环境环保局文件: "《美国有机化工行业污染物排放估算协议》", 31 May 2017, 中国环境出版社 *

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