CN110952161B - Low-melting-point elastic polyester fiber and preparation method thereof - Google Patents
Low-melting-point elastic polyester fiber and preparation method thereof Download PDFInfo
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- CN110952161B CN110952161B CN201911293540.2A CN201911293540A CN110952161B CN 110952161 B CN110952161 B CN 110952161B CN 201911293540 A CN201911293540 A CN 201911293540A CN 110952161 B CN110952161 B CN 110952161B
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- 229920000728 polyester Polymers 0.000 title claims abstract description 148
- 239000000835 fiber Substances 0.000 title claims abstract description 106
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims abstract description 121
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 81
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims abstract description 64
- 238000009987 spinning Methods 0.000 claims abstract description 63
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000002844 melting Methods 0.000 claims abstract description 51
- 229920000909 polytetrahydrofuran Polymers 0.000 claims abstract description 37
- 230000009477 glass transition Effects 0.000 claims abstract description 30
- -1 fatty acid ester Chemical class 0.000 claims abstract description 24
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims abstract description 16
- 239000004576 sand Substances 0.000 claims abstract description 15
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 13
- 239000000194 fatty acid Substances 0.000 claims abstract description 13
- 229930195729 fatty acid Natural products 0.000 claims abstract description 13
- MLUCVPSAIODCQM-NSCUHMNNSA-N crotonaldehyde Chemical compound C\C=C\C=O MLUCVPSAIODCQM-NSCUHMNNSA-N 0.000 claims abstract description 12
- MLUCVPSAIODCQM-UHFFFAOYSA-N crotonaldehyde Natural products CC=CC=O MLUCVPSAIODCQM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 9
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 12
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical group [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 10
- 238000005886 esterification reaction Methods 0.000 claims description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 10
- 238000006068 polycondensation reaction Methods 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 150000002009 diols Chemical class 0.000 claims description 8
- OEIJHBUUFURJLI-UHFFFAOYSA-N octane-1,8-diol Chemical compound OCCCCCCCCO OEIJHBUUFURJLI-UHFFFAOYSA-N 0.000 claims description 8
- WVLBCYQITXONBZ-UHFFFAOYSA-N trimethyl phosphate Chemical compound COP(=O)(OC)OC WVLBCYQITXONBZ-UHFFFAOYSA-N 0.000 claims description 8
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical group C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 7
- MZQHAPMLAQRTTD-UHFFFAOYSA-L calcium;benzene-1,3-dicarboxylate Chemical group [Ca+2].[O-]C(=O)C1=CC=CC(C([O-])=O)=C1 MZQHAPMLAQRTTD-UHFFFAOYSA-L 0.000 claims description 6
- 239000003381 stabilizer Substances 0.000 claims description 6
- CYTQBVOFDCPGCX-UHFFFAOYSA-N trimethyl phosphite Chemical compound COP(OC)OC CYTQBVOFDCPGCX-UHFFFAOYSA-N 0.000 claims description 6
- ALQSHHUCVQOPAS-UHFFFAOYSA-N Pentane-1,5-diol Chemical compound OCCCCCO ALQSHHUCVQOPAS-UHFFFAOYSA-N 0.000 claims description 5
- SXCBDZAEHILGLM-UHFFFAOYSA-N heptane-1,7-diol Chemical compound OCCCCCCCO SXCBDZAEHILGLM-UHFFFAOYSA-N 0.000 claims description 5
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 229940043375 1,5-pentanediol Drugs 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 4
- FGYBPGJIUUUVTL-UHFFFAOYSA-N benzene-1,3-dicarboxylic acid;zinc Chemical compound [Zn].OC(=O)C1=CC=CC(C(O)=O)=C1 FGYBPGJIUUUVTL-UHFFFAOYSA-N 0.000 claims description 3
- DIHVPHOZNABKAN-UHFFFAOYSA-L magnesium;benzene-1,3-dicarboxylate Chemical compound [Mg+2].[O-]C(=O)C1=CC=CC(C([O-])=O)=C1 DIHVPHOZNABKAN-UHFFFAOYSA-L 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 238000009826 distribution Methods 0.000 claims description 2
- 125000003827 glycol group Chemical group 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 238000002788 crimping Methods 0.000 claims 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract 2
- 150000001299 aldehydes Chemical class 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- 230000003811 curling process Effects 0.000 description 9
- 238000004821 distillation Methods 0.000 description 8
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 8
- JSZBEPHXXGBFGH-UHFFFAOYSA-L calcium;2-sulfobenzene-1,3-dicarboxylate Chemical compound [Ca+2].OS(=O)(=O)C1=C(C([O-])=O)C=CC=C1C([O-])=O JSZBEPHXXGBFGH-UHFFFAOYSA-L 0.000 description 7
- MCFIAQBSNQNWQA-UHFFFAOYSA-L S(=O)(=O)(O)C1=C(C(=O)[O-])C=CC=C1C(=O)[O-].[Mg+2] Chemical compound S(=O)(=O)(O)C1=C(C(=O)[O-])C=CC=C1C(=O)[O-].[Mg+2] MCFIAQBSNQNWQA-UHFFFAOYSA-L 0.000 description 5
- 238000007259 addition reaction Methods 0.000 description 4
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 4
- 210000004177 elastic tissue Anatomy 0.000 description 3
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229920001634 Copolyester Polymers 0.000 description 1
- DUIDDZBBZIIPFX-UHFFFAOYSA-L S(=O)(=O)(O)C1=C(C(=O)[O-])C=CC=C1C(=O)[O-].[Zn+2] Chemical compound S(=O)(=O)(O)C1=C(C(=O)[O-])C=CC=C1C(=O)[O-].[Zn+2] DUIDDZBBZIIPFX-UHFFFAOYSA-L 0.000 description 1
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical group OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
Classifications
-
- 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
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/688—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur
- C08G63/6884—Polyesters containing atoms other than carbon, hydrogen and oxygen containing sulfur derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/6886—Dicarboxylic acids and dihydroxy compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to a low-melting elastic polyester fiber and a preparation method thereof, which takes phthalic acid (terephthalic acid and isophthalic acid), glycol, polytetrahydrofuran, a glass transition temperature regulator (isophthalic acid sulfonate) and a macromolecular modulus regulator (fatty acid ester or long-chain glycol with the carbon atom number more than or equal to 5) as main reaction raw materials to prepare elastic polyester, and then the elastic polyester fiber is prepared by spinning, wherein the material of metal sand in a spinning component is Ni during spinning; the prepared low-melting-point elastic polyester fiber is made of elastic polyester, a molecular chain of the elastic polyester mainly comprises a phthalic acid chain segment, an ethylene glycol chain segment, a polytetrahydrofuran chain segment, a glass transition temperature regulator chain segment and a macromolecular modulus regulator chain segment, and the total content of acetaldehyde and crotonaldehyde in the low-melting-point elastic polyester fiber is less than 0.5 ppm. The invention can avoid the adhesion phenomenon while improving the fiber softness, and reduce the content of aldehyde compounds in the fiber.
Description
Technical Field
The invention belongs to the technical field of polyester fibers, and relates to a low-melting-point elastic polyester fiber and a preparation method thereof.
Background
The polyester fiber is firm and durable, has crease resistance and good washability, has wide application, and is one of the synthetic fibers with the largest demand and the fastest development speed. Although the polyester fiber has excellent properties, conventional and single polyester fibers have failed to satisfy various needs of people. To improve such a situation, it is necessary to accelerate the diversification of polyester fibers.
The polyester elastic fiber has good dimensional stability and lower modulus, the fiber and products thereof have soft hand feeling, good wear resistance and fiber crimpability, excellent tensile elasticity and compression elasticity, good dyeing property, lower dyeing temperature, excellent color fastness and chlorine resistance, excellent chemical resistance, light resistance and heat resistance, and gradually obtain larger development space.
The polyester elastic fiber has a large market demand, is relatively late in development and relatively single in variety compared with foreign countries, has a certain gap with international leading products in raw materials, technology and equipment, is still in the development stage at present, and is difficult to realize industrialization.
The original modulus of the fiber directly reflects the softness of the fiber, and the polyester structure contains phthalic acid which is a rigid group, so that the low-melting elastic polyester fiber has hard hand feeling when being compounded with other materials to prepare underwear products, thereby influencing the comfort in use and further restricting the application field of the low-melting elastic polyester fiber.
The prior art modifies polyester to reduce the initial modulus of the fiber, and the glass transition temperature is reduced while the initial modulus is reduced. Glass transition temperature TgIs an important characteristic parameter of the material, and many characteristics of the material are changed sharply around the glass transition temperature. In terms of molecular structure, the glass transition temperature is a relaxation phenomenon of an amorphous part of a high polymer from a frozen state to a thawed state, and at the glass transition temperature, although a molecular chain cannot move, the chain segment starts to move, and the temperature is increased, so that the whole molecular chain moves and shows viscous flow property. For the low-melting elastic polyester fiber, due to the introduction of the flexible chain, the rigidity of the macromolecules is reduced, the regular structures of the macromolecules are damaged, and the adhesion phenomenon is easy to occur near the glass transition temperature. Particularly, in the processes of transportation, packaging and processing, the quality and the use of the low-melting elastic polyester fiber are seriously influenced due to more obvious conditions of temperature and extrusion.
In addition, the elastic fiber is applied to underwear and children clothes series, the requirement on the aldehyde content in the fiber is very strict, and the content of aldehyde such as acetaldehyde, crotonaldehyde and the like in the existing polyester is higher.
Therefore, it is desired to develop a method for reducing the content of aldehyde in the low-melting elastic polyester fiber, so as to reduce the initial modulus of the fiber and prevent the fiber from blocking.
Disclosure of Invention
The invention aims to solve the problems that the initial modulus of the fiber is reduced, the fiber is easy to generate the blocking phenomenon and the content of aldehyde in the low-melting-point elastic polyester fiber is too high in the prior art, and provides the low-melting-point elastic polyester fiber and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of low-melting elastic polyester fiber is characterized in that phthalic acid, ethylene glycol, polytetrahydrofuran, a glass transition temperature regulator and a macromolecular modulus regulator are used as main reaction raw materials to prepare elastic polyester, and then spinning is carried out to prepare the low-melting elastic polyester fiber;
the phthalic acid is terephthalic acid and isophthalic acid;
the glass transition temperature regulator is m-phthalic acid sulfonate;
the macromolecular modulus regulator is fatty acid ester or long-chain diol with the carbon atom number more than or equal to 5;
during spinning, the metal sand in the spinning assembly is made of Ni.
The macromolecular modulus regulator, namely fatty acid ester or long-chain diol with the carbon atom number more than or equal to 5, introduced into a molecular chain has the function of reducing the initial modulus of the fiber, and after the fatty acid ester or the long-chain diol is introduced, the flexibility, the geometric stereo structure and the interaction force among the molecular chains of the polyester molecule are changed, so the initial modulus of the fiber is reduced;
however, the introduction of the macromolecular modulus regulator can generate larger influence on the glass transition temperature of the polyester, and the glass transition temperature of the copolyester is reduced to a certain extent, so that the glass transition temperature of the low-melting-point polyester can be reduced to below 60 ℃, even lower, and the adhesion phenomenon is easy to occur;
the metal Ni is made into metal sand as a filter material, when polyester melt passes through the metal sand, the carbonyl of trace acetaldehyde and crotonaldehyde in the melt is very active, when the polyester melt is adsorbed on the heated Ni, the carbonyl of the aldehyde is in a more unstable state and is more active and can generate addition reaction with various free radicals or ions in the polyester, the metal Ni plays a role of a catalyst in the addition reaction of the aldehyde, the content of the aldehyde in the polyester is effectively reduced, the polyester is stretched in the pre-spinning process, and the polyester is stretched, washed, shaped and the like in the post-spinning process, so that the content of the aldehyde in the fiber is further reduced.
The low-melting elastic polyester fiber is a copolymer formed by block polymerization of soft and hard chain segments, wherein the hard segment is mainly polyethylene terephthalate, and the soft segment is polytetrahydrofuran, so that the low-melting elastic polyester fiber not only has higher strength and better thermal stability of the hard segment, but also has excellent elasticity of the soft segment.
As a preferred technical scheme:
in the preparation method of the elastic polyester fiber with low melting point, the number average molecular weight of the polytetrahydrofuran is 1500-2000, and the number average molecular weight of the fatty acid ester is 500-800.
In the method for preparing the low-melting elastic polyester fiber, the isophthalic acid sulfonate is calcium isophthalate sulfonate, zinc isophthalate sulfonate or magnesium isophthalate sulfonate, the fatty acid ester is polybutylene adipate or polypropylene adipate, and the long-chain diol is 1, 5-pentanediol, 1, 6-hexanediol, 1, 7-heptanediol or 1, 8-octanediol.
The preparation method of the low-melting elastic polyester fiber comprises the following steps:
(1) performing esterification reaction;
preparing phthalic acid, ethylene glycol, polytetrahydrofuran, a glass transition temperature regulator and a macromolecular modulus regulator into slurry, and reacting at 180-240 ℃ in a nitrogen atmosphere until the distilled water amount reaches more than 90% of a theoretical value;
(2) performing polycondensation reaction;
adding a catalyst and a stabilizer into the system in the step (1), reacting for 30-50 min at the temperature of 260-270 ℃ and under the pressure of 500Pa or less, and reacting for 50-90 min at the temperature of 275-280 ℃ and under the pressure of 100Pa or less to obtain the elastic polyester.
The preparation method of the elastic polyester fiber with low melting point comprises the following steps of enabling the molar ratio of terephthalic acid, isophthalic acid, ethylene glycol and a glass transition temperature regulator to be 1: 0.4-0.6: 1.5-2.0: 0.01-0.03;
the mass addition amount of the polytetrahydrofuran is 20-30% of that of the phthalic acid;
when the macromolecular modulus regulator is fatty acid ester, the mass addition amount of the macromolecular modulus regulator is 3-5% of that of the phthalic acid; when the macromolecular modulus regulator is long-chain diol, the mass addition amount of the macromolecular modulus regulator is 25-35% of that of phthalic acid;
the mass addition amount of the catalyst is 0.01-0.03 percent of that of the phthalic acid, and the catalyst is tetrabutyl titanate;
the mass addition amount of the stabilizer is 0.01-0.05% of that of the phthalic acid, and the stabilizer is triphenyl phosphate, trimethyl phosphate or trimethyl phosphite.
The preparation method of the low-melting elastic polyester fiber comprises the steps that the spinning process comprises a curling process, the post-spinning adopts a drawing-washing process, and the drawing adopts oil bath drawing; through the drawing-washing process of the post-spinning, the aldehyde content in the fiber is further reduced;
the main technological parameters of spinning are as follows: the spinning temperature is 260-270 ℃, the spinning speed is 500-800 m/min, the air temperature of circular blowing is 20-25 ℃, the air speed of circular blowing is 0.5-0.8 m/s, the oil bath temperature is 65-70 ℃, the drafting multiple is 2.7-3.0, the water washing temperature is 65-70 ℃, the curling temperature is 25-28 ℃, the main curling pressure is 0.4-0.6 MPa, and the curling backpressure is 0.2-0.4 MPa.
The invention also provides the low-melting-point elastic polyester fiber prepared by the preparation method of the low-melting-point elastic polyester fiber, the material is elastic polyester, and the molecular chain of the elastic polyester mainly comprises a phthalic acid chain segment, an ethylene glycol chain segment, a polytetrahydrofuran chain segment, a glass transition temperature regulator chain segment and a macromolecular modulus regulator chain segment;
the phthalic acid chain segment is a terephthalic acid chain segment and an isophthalic acid chain segment;
the glass transition temperature regulator chain segment is an isophthalic acid sulfonate chain segment;
the macromolecular modulus regulator chain segment is a fatty acid ester chain segment or a long-chain glycol chain segment with the carbon atom number more than or equal to 5;
the total content of acetaldehyde and crotonaldehyde in the low-melting elastic polyester fiber is less than 0.5ppm, which is far lower than the level in the prior art.
As a preferred technical scheme:
the low-melting elastic polyester fiber has the filament number of 1.5-3.0 dtex, the breaking strength of more than or equal to 2.50cN/dtex, the elongation at break of 350.0 +/-30.0 percent, the resilience of 100 percent of the fiber after stretching of 63-70 percent, the elastic modulus of 0.10-0.30 cN/dtex, the number of crimps of 8-12/25 mm and the crimpness of 12-14 percent.
The low-melting elastic polyester fiber has the melting point of the elastic polyester of 160-190 ℃, the glass transition temperature of 55-60 ℃, the number average molecular weight of 17000-30000 and the molecular weight distribution index D of 2.4-4.0.
Has the advantages that:
(1) the preparation method of the elastic polyester fiber with low melting point is simple and easy to implement, has lower cost, and can greatly reduce the content of aldehyde compounds such as acetaldehyde, crotonaldehyde and the like in the polyester fiber with low melting point;
(2) the preparation method of the low-melting elastic polyester fiber has the advantages that the softness of the fiber is improved, the adhesion phenomenon is avoided, and the preparation method has practical significance;
(3) the low-melting-point polyester fiber prepared by the preparation method of the low-melting-point elastic polyester fiber has the advantages of lower initial modulus, higher glass transition temperature, and total content of acetaldehyde and crotonaldehyde of less than 0.5ppm, which is far lower than the level in the prior art, and can be applied to underwear and children's garments.
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.
Initial length is L at normal temperature0Fixing one end of the fiber, extending the other end to a specific length L1, loosening the fiber after balancing for 10min, measuring the length Lx of the fiber after being retracted after being loosened for 60s, and calculating the rebound rate (E%) according to the following formula:
example 1
A low-melting elastic polyester fiber is prepared by the following steps:
(1) performing esterification reaction;
preparing phthalic acid (terephthalic acid and isophthalic acid), ethylene glycol, polytetrahydrofuran with the number average molecular weight of 1500, calcium isophthalate sulfonate and polybutylene adipate with the number average molecular weight of 500 into slurry, and reacting at 180 ℃ in a nitrogen atmosphere until the water distillation amount reaches 90% of a theoretical value; wherein the molar ratio of terephthalic acid to isophthalic acid to ethylene glycol to calcium sulfoisophthalate is 1:0.4:1.5:0.01, the mass addition amount of polytetrahydrofuran is 20% of the mass addition amount of the phthalic acid (namely the sum of the mass addition amounts of the terephthalic acid and the isophthalic acid), and the mass addition amount of the polybutylene adipate is 3% of the mass addition amount of the phthalic acid;
(2) performing polycondensation reaction;
adding tetrabutyl titanate and triphenyl phosphate into the system in the step (1), reacting for 50min at the temperature of 260 ℃ and the pressure of 500Pa absolute, and then reacting for 90min at the temperature of 275 ℃ and the pressure of 100Pa absolute to obtain elastic polyester; wherein the mass addition amount of the n-butyl titanate is 0.01 percent of the mass addition amount of the phthalic acid, and the mass addition amount of the triphenyl phosphate is 0.01 percent of the mass addition amount of the phthalic acid;
(3) spinning to obtain low-melting elastic polyester fiber;
the spinning process comprises a curling process, the post-spinning adopts a drawing-washing process, the drawing adopts oil bath drawing, and the metal sand in the spinning assembly is made of Ni; the spinning process parameters are shown in table 1.
The finally prepared low-melting-point elastic polyester fiber is made of elastic polyester, the molecular chain of the elastic polyester is composed of a terephthalic acid chain segment, an isophthalic acid chain segment, an ethylene glycol chain segment, a polytetrahydrofuran chain segment, a calcium isophthalate sulfonate chain segment and a polybutylene adipate chain segment, the performance indexes of the elastic polyester are shown in a table 2, and the performance indexes of the low-melting-point elastic polyester fiber are shown in a table 3.
Comparative example 1
A low-melting elastic polyester fiber was prepared in substantially the same manner as in example 1, except that calcium isophthalate was not added in the step (1), and the glass transition temperature of the finally obtained low-melting elastic polyester fiber was 53 ℃.
As can be seen by comparing comparative example 1 with example 1, the glass transition of comparative example 1 is lower because calcium isophthalate sulfonate is added in example 1, and the calcium isophthalate sulfonate introduces ionic bonds to form ionic clusters (which is equivalent to increase of cross-linking points), so that the mobility of the molecular chain segments of the polyester is inhibited, and the glass transition temperature of the polyester is improved; in contrast, in comparative example 1, no crosslinking by ionic bonds was observed, and the glass transition temperature could not be adjusted.
Comparative example 2
The preparation process of the elastic polyester fiber with the low melting point is basically the same as that in the example 1, except that the material of the metal sand in the spinning component in the step (3) is Fe, and the total content of acetaldehyde and crotonaldehyde in the finally prepared elastic polyester fiber with the low melting point is 2.3 ppm.
Comparing the comparative example 2 with the example 1, it can be seen that the total content of acetaldehyde and crotonaldehyde in the comparative example 2 is higher, because the material of the metal sand in the example 1 is Ni, and under the catalytic action of high-temperature Ni, the trace amount of acetaldehyde and carbonyl of crotonaldehyde in the melt can perform addition reaction with various free radicals or ions in the polyester, thereby effectively reducing the content of aldehyde in the polyester; the Fe in the comparative example 2 can not catalyze the addition reaction of the carbonyl of the acetaldehyde and the crotonaldehyde in the system, so that the aldehyde is retained, and the aldehyde can not be consumed and removed in the subsequent processing, so that the total content of the acetaldehyde and the crotonaldehyde in the polyester fiber in the comparative example 2 is higher.
Example 2
A low-melting elastic polyester fiber is prepared by the following steps:
(1) performing esterification reaction;
preparing phthalic acid (terephthalic acid and isophthalic acid), ethylene glycol, polytetrahydrofuran with the number average molecular weight of 1600, zinc isophthalate sulfonate and poly propylene glycol adipate with the number average molecular weight of 600 into slurry, and reacting at 200 ℃ in a nitrogen atmosphere until the water distillation amount reaches 92% of a theoretical value; wherein the molar ratio of the terephthalic acid to the isophthalic acid to the ethylene glycol to the zinc sulfoisophthalate is 1:0.5:1.7:0.01, the mass addition amount of the polytetrahydrofuran is 23% of the mass addition amount of the phthalic acid, and the mass addition amount of the polytrimethylene adipate is 3.5% of the mass addition amount of the phthalic acid;
(2) performing polycondensation reaction;
adding tetrabutyl titanate and trimethyl phosphate into the system in the step (1), reacting for 45min at the temperature of 264 ℃ and the pressure of 420Pa absolute, and then reacting for 82min at the temperature of 278 ℃ and the pressure of 80Pa absolute to obtain elastic polyester; wherein the mass addition amount of the n-butyl titanate is 0.02 percent of the mass addition amount of the phthalic acid, and the mass addition amount of the trimethyl phosphate is 0.03 percent of the mass addition amount of the phthalic acid;
(3) spinning to obtain low-melting elastic polyester fiber;
the spinning process comprises a curling process, the post-spinning adopts a drawing-washing process, the drawing adopts oil bath drawing, and the metal sand in the spinning assembly is made of Ni; the spinning process parameters are shown in table 1.
The finally prepared low-melting-point elastic polyester fiber is made of elastic polyester, the molecular chain of the elastic polyester is composed of a terephthalic acid chain segment, an isophthalic acid chain segment, an ethylene glycol chain segment, a polytetrahydrofuran chain segment, an isophthalic acid zinc sulfonate chain segment and a poly propylene glycol adipate chain segment, the performance indexes of the elastic polyester are shown in table 2, and the performance indexes of the low-melting-point elastic polyester fiber are shown in table 3.
Example 3
A low-melting elastic polyester fiber is prepared by the following steps:
(1) performing esterification reaction;
preparing phthalic acid (terephthalic acid and isophthalic acid), ethylene glycol, polytetrahydrofuran with the number average molecular weight of 1650, magnesium sulfoisophthalate and 1, 5-pentanediol into slurry, and reacting at 198 ℃ in a nitrogen atmosphere until the water distillation amount reaches 95% of a theoretical value; wherein the molar ratio of terephthalic acid to isophthalic acid to ethylene glycol to magnesium sulfoisophthalate is 1:0.6:1.8:0.03, the mass addition of polytetrahydrofuran is 25% of the mass addition of the phthalic acid, and the mass addition of 1, 5-pentanediol is 25% of the mass addition of the phthalic acid;
(2) performing polycondensation reaction;
adding tetrabutyl titanate and trimethyl phosphite into the system in the step (1), reacting for 30min at the temperature of 270 ℃ and the pressure of 400Pa absolute, and then reacting for 50min at the temperature of 280 ℃ and the pressure of 78Pa absolute to prepare elastic polyester; wherein the mass addition amount of the n-butyl titanate is 0.03 percent of the mass addition amount of the phthalic acid, and the mass addition amount of the trimethyl phosphite is 0.05 percent of the mass addition amount of the phthalic acid;
(3) spinning to obtain low-melting elastic polyester fiber;
the spinning process comprises a curling process, the post-spinning adopts a drawing-washing process, the drawing adopts oil bath drawing, and the metal sand in the spinning assembly is made of Ni; the spinning process parameters are shown in table 1.
The finally prepared low-melting-point elastic polyester fiber is made of elastic polyester, the molecular chain of the elastic polyester is composed of a terephthalic acid chain segment, an isophthalic acid chain segment, an ethylene glycol chain segment, a polytetrahydrofuran chain segment, a magnesium isophthalate sulfonate chain segment and a 1, 5-pentanediol chain segment, the performance indexes of the elastic polyester are shown in a table 2, and the performance indexes of the low-melting-point elastic polyester fiber are shown in a table 3.
Example 4
A low-melting elastic polyester fiber is prepared by the following steps:
(1) performing esterification reaction;
preparing phthalic acid (terephthalic acid and isophthalic acid), ethylene glycol, polytetrahydrofuran with the number average molecular weight of 1720, calcium sulfoisophthalate and 1, 6-hexanediol into slurry, and reacting at 240 ℃ in a nitrogen atmosphere until the water distillation amount reaches 96% of a theoretical value; wherein the molar ratio of terephthalic acid to isophthalic acid to ethylene glycol to calcium sulfoisophthalate is 1:0.6:2.0:0.03, the mass addition of polytetrahydrofuran is 30% of the mass addition of the phthalic acid, and the mass addition of 1, 6-hexanediol is 35% of the mass addition of the phthalic acid;
(2) performing polycondensation reaction;
adding tetrabutyl titanate and triphenyl phosphate into the system in the step (1), reacting for 35min at the temperature of 270 ℃ and the pressure of 410Pa, and reacting for 54min at the temperature of 280 ℃ and the pressure of 80Pa to obtain elastic polyester; wherein the mass addition amount of the n-butyl titanate is 0.02 percent of the mass addition amount of the phthalic acid, and the mass addition amount of the triphenyl phosphate is 0.03 percent of the mass addition amount of the phthalic acid;
(3) spinning to obtain low-melting elastic polyester fiber;
the spinning process comprises a curling process, the post-spinning adopts a drawing-washing process, the drawing adopts oil bath drawing, and the metal sand in the spinning assembly is made of Ni; the spinning process parameters are shown in table 1.
The finally prepared low-melting-point elastic polyester fiber is made of elastic polyester, the molecular chain of the elastic polyester is composed of a terephthalic acid chain segment, an isophthalic acid chain segment, an ethylene glycol chain segment, a polytetrahydrofuran chain segment, an isophthalic acid calcium sulfonate chain segment and a 1, 6-hexanediol chain segment, the performance indexes of the elastic polyester are shown in a table 2, and the performance indexes of the low-melting-point elastic polyester fiber are shown in a table 3.
Example 5
A low-melting elastic polyester fiber is prepared by the following steps:
(1) performing esterification reaction;
preparing phthalic acid (terephthalic acid and isophthalic acid), ethylene glycol, polytetrahydrofuran with the number average molecular weight of 1800, calcium sulfoisophthalate and 1, 7-heptanediol into slurry, and reacting at 220 ℃ in a nitrogen atmosphere until the water distillation amount reaches 92% of a theoretical value; wherein the molar ratio of terephthalic acid to isophthalic acid to ethylene glycol to calcium sulfoisophthalate is 1:0.5:1.7:0.02, the mass addition amount of polytetrahydrofuran is 27% of that of phthalic acid, and the mass addition amount of 1, 7-heptanediol is 31% of that of phthalic acid;
(2) performing polycondensation reaction;
adding tetrabutyl titanate and trimethyl phosphate into the system in the step (1), reacting for 40min at 266 ℃ and 470Pa absolute, and reacting for 70min at 279 ℃ and 92Pa absolute to obtain elastic polyester; wherein the mass addition amount of the n-butyl titanate is 0.02 percent of the mass addition amount of the phthalic acid, and the mass addition amount of the trimethyl phosphate is 0.05 percent of the mass addition amount of the phthalic acid;
(3) spinning to obtain low-melting elastic polyester fiber;
the spinning process comprises a curling process, the post-spinning adopts a drawing-washing process, the drawing adopts oil bath drawing, and the metal sand in the spinning assembly is made of Ni; the spinning process parameters are shown in table 1.
The finally prepared low-melting-point elastic polyester fiber is made of elastic polyester, the molecular chain of the elastic polyester is composed of a terephthalic acid chain segment, an isophthalic acid chain segment, an ethylene glycol chain segment, a polytetrahydrofuran chain segment, a calcium isophthalate sulfonate chain segment and a 1, 7-heptanediol chain segment, the performance indexes of the elastic polyester are shown in a table 2, and the performance indexes of the low-melting-point elastic polyester fiber are shown in a table 3.
Example 6
A low-melting elastic polyester fiber is prepared by the following steps:
(1) performing esterification reaction;
preparing phthalic acid (terephthalic acid and isophthalic acid), ethylene glycol, polytetrahydrofuran with the number average molecular weight of 2000, magnesium sulfoisophthalate and 1, 8-octanediol into slurry, and reacting at 180 ℃ in a nitrogen atmosphere until the water distillation amount reaches 90% of a theoretical value; wherein the molar ratio of terephthalic acid to isophthalic acid to ethylene glycol to magnesium sulfoisophthalate is 1:0.4:2.0:0.01, the mass addition amount of polytetrahydrofuran is 30% of that of phthalic acid, and the mass addition amount of 1, 8-octanediol is 35% of that of phthalic acid;
(2) performing polycondensation reaction;
adding tetrabutyl titanate and trimethyl phosphite into the system in the step (1), reacting for 50min at the temperature of 260 ℃ and the pressure of 500Pa absolute, and then reacting for 90min at the temperature of 275 ℃ and the pressure of 100Pa absolute to obtain elastic polyester; wherein the mass addition amount of the n-butyl titanate is 0.03 percent of the mass addition amount of the phthalic acid, and the mass addition amount of the trimethyl phosphite is 0.01 percent of the mass addition amount of the phthalic acid;
(3) spinning to obtain low-melting elastic polyester fiber;
the spinning process comprises a curling process, the post-spinning adopts a drawing-washing process, the drawing adopts oil bath drawing, and the metal sand in the spinning assembly is made of Ni; the spinning process parameters are shown in table 1.
The finally prepared low-melting-point elastic polyester fiber is made of elastic polyester, the molecular chain of the elastic polyester is composed of a terephthalic acid chain segment, an isophthalic acid chain segment, an ethylene glycol chain segment, a polytetrahydrofuran chain segment, an isophthalic acid magnesium sulfonate chain segment and a 1, 8-octanediol chain segment, the performance indexes of the elastic polyester are shown in table 2, and the performance indexes of the low-melting-point elastic polyester fiber are shown in table 3.
Example 7
A low-melting elastic polyester fiber is prepared by the following steps:
(1) performing esterification reaction;
preparing phthalic acid (terephthalic acid and isophthalic acid), ethylene glycol, polytetrahydrofuran with the number average molecular weight of 2000, magnesium isophthalate sulfonate and polybutylene adipate with the number average molecular weight of 800 into slurry, and reacting at 210 ℃ in a nitrogen atmosphere until the water distillation amount reaches 94% of a theoretical value; wherein the molar ratio of terephthalic acid to isophthalic acid to ethylene glycol to magnesium sulfoisophthalate is 1:0.4:1.5:0.01, the mass addition of polytetrahydrofuran is 25% of the mass addition of the phthalic acid, and the mass addition of polybutylene adipate is 5% of the mass addition of the phthalic acid;
(2) performing polycondensation reaction;
adding tetrabutyl titanate and trimethyl phosphate into the system in the step (1), reacting for 45min at the temperature of 264 ℃ and the pressure of 420Pa absolute, and then reacting for 82min at the temperature of 278 ℃ and the pressure of 80Pa absolute to obtain elastic polyester; wherein the mass addition amount of the n-butyl titanate is 0.02 percent of the mass addition amount of the phthalic acid, and the mass addition amount of the trimethyl phosphate is 0.03 percent of the mass addition amount of the phthalic acid;
(3) spinning to obtain low-melting elastic polyester fiber;
the spinning process comprises a curling process, the post-spinning adopts a drawing-washing process, the drawing adopts oil bath drawing, and the metal sand in the spinning assembly is made of Ni; the spinning process parameters are shown in table 1.
The finally prepared low-melting-point elastic polyester fiber is made of elastic polyester, the molecular chain of the elastic polyester is composed of a terephthalic acid chain segment, an isophthalic acid chain segment, an ethylene glycol chain segment, a polytetrahydrofuran chain segment, a magnesium isophthalate sulfonate chain segment and a polybutylene adipate chain segment, the performance indexes of the elastic polyester are shown in a table 2, and the performance indexes of the low-melting-point elastic polyester fiber are shown in a table 3.
Example 8
A low-melting elastic polyester fiber is prepared by the following steps:
(1) performing esterification reaction;
preparing phthalic acid (terephthalic acid and isophthalic acid), ethylene glycol, polytetrahydrofuran with the number average molecular weight of 1700, calcium sulfoisophthalate and 1, 8-octanediol into slurry, and reacting at 220 ℃ in a nitrogen atmosphere until the water distillation amount reaches 93 percent of a theoretical value; wherein the molar ratio of terephthalic acid to isophthalic acid to ethylene glycol to calcium sulfoisophthalate is 1:0.6:2.0:0.02, the mass addition amount of polytetrahydrofuran is 20% of the mass addition amount of phthalic acid, and the mass addition amount of 1, 8-octanediol is 30% of the mass addition amount of phthalic acid;
(2) performing polycondensation reaction;
adding tetrabutyl titanate and triphenyl phosphate into the system in the step (1), reacting for 35min under the conditions that the temperature is 270 ℃ and the pressure is 420Pa absolute, and then reacting for 55min under the conditions that the temperature is 280 ℃ and the pressure is 82Pa absolute to prepare elastic polyester; wherein the mass addition amount of the n-butyl titanate is 0.02 percent of the mass addition amount of the phthalic acid, and the mass addition amount of the triphenyl phosphate is 0.03 percent of the mass addition amount of the phthalic acid;
(3) spinning to obtain low-melting elastic polyester fiber;
the spinning process comprises a curling process, the post-spinning adopts a drawing-washing process, the drawing adopts oil bath drawing, and the metal sand in the spinning assembly is made of Ni; the spinning process parameters are shown in table 1.
The finally prepared low-melting-point elastic polyester fiber is made of elastic polyester, the molecular chain of the elastic polyester is composed of a terephthalic acid chain segment, an isophthalic acid chain segment, an ethylene glycol chain segment, a polytetrahydrofuran chain segment, an isophthalic acid calcium sulfonate chain segment and a 1, 8-octanediol chain segment, the performance indexes of the elastic polyester are shown in table 2, and the performance indexes of the low-melting-point elastic polyester fiber are shown in table 3.
TABLE 1
TABLE 2
TABLE 3
Claims (5)
1. A preparation method of low-melting elastic polyester fiber is characterized by comprising the following steps: preparing elastic polyester by using phthalic acid, ethylene glycol, polytetrahydrofuran, a glass transition temperature regulator and a macromolecular modulus regulator as main reaction raw materials, and then spinning to prepare the low-melting-point elastic polyester fiber;
the phthalic acid is terephthalic acid and isophthalic acid;
the glass transition temperature regulator is m-phthalic acid sulfonate;
the macromolecular modulus regulator is fatty acid ester or long-chain diol with the carbon atom number more than or equal to 5;
during spinning, the metal sand in the spinning assembly is made of Ni;
the number average molecular weight of the polytetrahydrofuran is 1500-2000, the number average molecular weight of the fatty acid ester is 500-800, the isophthalic acid sulfonate is calcium isophthalate sulfonate, zinc isophthalate sulfonate or magnesium isophthalate sulfonate, the fatty acid ester is polybutylene adipate or polypropylene glycol adipate, and the long-chain diol is 1, 5-pentanediol, 1, 6-hexanediol, 1, 7-heptanediol or 1, 8-octanediol;
the elastomeric polyester was prepared as follows:
(1) performing esterification reaction;
preparing phthalic acid, ethylene glycol, polytetrahydrofuran, a glass transition temperature regulator and a macromolecular modulus regulator into slurry, and reacting at 180-240 ℃ in a nitrogen atmosphere until the distilled water amount reaches more than 90% of a theoretical value;
(2) performing polycondensation reaction;
adding a catalyst and a stabilizer into the system in the step (1), reacting for 30-50 min at the temperature of 260-270 ℃ and under the pressure of less than or equal to 500Pa absolute, and then reacting for 50-90 min at the temperature of 275-280 ℃ and under the pressure of less than or equal to 100Pa absolute to obtain elastic polyester;
the molar ratio of the terephthalic acid to the isophthalic acid to the ethylene glycol to the glass transition temperature regulator is 1: 0.4-0.6: 1.5-2.0: 0.01-0.03;
the mass addition amount of the polytetrahydrofuran is 20-30% of that of the phthalic acid;
when the macromolecular modulus regulator is fatty acid ester, the mass addition amount of the macromolecular modulus regulator is 3-5% of that of the phthalic acid; when the macromolecular modulus regulator is long-chain diol, the mass addition amount of the macromolecular modulus regulator is 25-35% of that of phthalic acid;
the mass addition amount of the catalyst is 0.01-0.03 percent of that of the phthalic acid, and the catalyst is tetrabutyl titanate;
the mass addition amount of the stabilizer is 0.01-0.05% of that of the phthalic acid, and the stabilizer is triphenyl phosphate, trimethyl phosphate or trimethyl phosphite.
2. The method for preparing a low melting point elastic polyester fiber according to claim 1, wherein the spinning process comprises a crimping process and the post-spinning employs a drawing-water washing process, the drawing employs an oil bath drawing;
the main technological parameters of spinning are as follows: the spinning temperature is 260-270 ℃, the spinning speed is 500-800 m/min, the air temperature of circular blowing is 20-25 ℃, and the air speed of circular blowing is 0.5-0.8 m/s; the oil bath temperature is 65-70 ℃, the drafting multiple is 2.7-3.0, the water washing temperature is 65-70 ℃, the curling temperature is 25-28 ℃, the main curling pressure is 0.4-0.6 MPa, and the back curling pressure is 0.2-0.4 MPa.
3. The low-melting elastic polyester fiber prepared by the preparation method of the low-melting elastic polyester fiber according to any one of claims 1 to 2, which is characterized in that: the material is elastic polyester, and the molecular chain of the elastic polyester mainly comprises a phthalic acid chain segment, an ethylene glycol chain segment, a polytetrahydrofuran chain segment, a glass transition temperature regulator chain segment and a macromolecular modulus regulator chain segment;
the phthalic acid chain segment is a terephthalic acid chain segment and an isophthalic acid chain segment;
the glass transition temperature regulator chain segment is an isophthalic acid sulfonate chain segment;
the macromolecular modulus regulator chain segment is a fatty acid ester chain segment or a long-chain glycol chain segment with the carbon atom number more than or equal to 5;
the total content of acetaldehyde and crotonaldehyde in the low-melting elastic polyester fiber is less than 0.5 ppm.
4. The elastic polyester fiber with low melting point according to claim 3, wherein the elastic polyester fiber with low melting point has a single fiber fineness of 1.5 to 3.0dtex, a breaking strength of 2.50cN/dtex or more, an elongation at break of 350.0. + -. 30.0%, a resilience of 63 to 70% at 100% elongation, an elastic modulus of 0.10 to 0.30cN/dtex, a crimp number of 8 to 12/25 mm, and a crimp degree of 12 to 14%.
5. The elastic polyester fiber with low melting point according to claim 3, wherein the elastic polyester has a melting point of 160 to 190 ℃, a glass transition temperature of 61 to 65 ℃, a number average molecular weight of 17000 to 30000, and a molecular weight distribution index D of 2.4 to 4.0.
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