CN113403709B - Composite spandex and preparation method thereof - Google Patents

Composite spandex and preparation method thereof Download PDF

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Publication number
CN113403709B
CN113403709B CN201910111392.1A CN201910111392A CN113403709B CN 113403709 B CN113403709 B CN 113403709B CN 201910111392 A CN201910111392 A CN 201910111392A CN 113403709 B CN113403709 B CN 113403709B
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polyurethane
composite
spandex
solution
core
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CN113403709A (en
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杨晓印
陈厚翔
王建波
杨从登
梁红军
蒋曙
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Huafeng Chemical Co ltd
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

Abstract

The invention discloses a preparation method of composite spandex, which comprises the steps of uniformly mixing polyurethane urea, thermoplastic polyurethane and dipropylene glycol dibenzoate in dimethylacetamide according to different weight proportions to prepare polyurethane solution A and polyurethane solution B, and respectively carrying out dry spinning through a skin feed inlet and a core feed inlet of a skin-core composite component. The invention also provides the composite spandex prepared by the method, the cross section of the composite spandex has no skin-core interface and presents a single area when observed under an optical microscope, and meanwhile, the composite spandex has no spiral yarn phenomenon and has more uniform and stable performance.

Description

Composite spandex and preparation method thereof
Technical Field
The invention relates to a composite spandex and a preparation method thereof. More specifically, the composite spandex is prepared from two polyurethane solutions prepared from polyurethane urea, thermoplastic polyurethane and dipropylene glycol dibenzoate in different proportions through a sheath-core composite assembly and by adopting dry spinning, and the cross section of the composite spandex is observed to have a sheath-core-free interface under an optical microscope and shows a single area, so that the composite spandex has excellent uniformity and is widely applied to the fields of silk stockings, seamless underwear and the like.
Background
The weft knitted fabric is formed by mutually sleeving loops formed by the same yarn along the weft direction of the fabric, based on the special structure, the weft knitted fabric has bidirectional stripping property, can be stripped in the reverse knitting direction, and can be stripped in the knitting direction, and in the process of fabric wearing, using or washing, yarn breakage or damage to the loop structure is often caused by scratching, cutting, repeated stretching and the like, so that fibers are stripped from the breakage along the longitudinal direction, the appearance and uniformity of the fabric are seriously affected, the fabric is finally damaged and discarded, and meanwhile, the weft knitted fabric also has hemming and yarn hooking phenomena, particularly for the spandex-containing weft knitted flat knitted fabric, the phenomenon is more remarkable, mainly because the spandex has high elasticity. In order to improve the above phenomenon, a spandex having excellent heat adhesiveness is demanded, which can provide a large number of network bonding points for a fabric, so that the phenomena of raveling, curling and hooking of the fabric can be suppressed.
There have been a number of reports on spandex having the above-described functions. CN1957125 and CN1723307 mainly describe that highly fusible spandex having a melting point of 180 ℃ or lower is produced by a melt spinning technique, and at the same time, the strength retention after a dry heat treatment at 150 ℃ for 45 seconds in a 100% elongation state is 50% or more, specifically, a polymer obtained by melt spinning an isocyanate-terminated prepolymer obtained by reacting a polymer diol with a diisocyanate and a hydroxy-terminated prepolymer obtained by reacting a polymer diol, a diisocyanate and a low molecular weight diol. JP patent No. 2007-177359 reports that thermoplastic polyurethane with a softening point of 50-140 ℃ accounting for 5% -60% of the total amount of fibers is added into polyurethane urea, polyurethane is prepared by a dry spinning technology after being uniformly mixed, and after the polyurethane is subjected to dry heat treatment, the thermal bonding stripping stress of the mutually crossed polyurethane reaches more than 0.2 cN/dt. CN101484620 discloses a spandex having high recovery, heat resistance and a function of preventing the yarn-off of clothing articles, which is a special polyurethane compound containing 5 to 40% by weight of the fiber, and has a low hard segment ratio, a loose hard segment structure, and a low crystallinity, i.e., a sharp change of the fiber structure due to a sharp melting of the hard segment at a specific temperature is not generated, and good performance can be maintained. The spandex prepared by the technology has the same problem that both heat resistance and thermal adhesion are difficult to obtain, and the subsequent wide application of the product is limited.
An effective method for solving the problems in the industry is to adopt a skin-core composite structure, and rely on special performance requirements such as thermal adhesion provided by skin, and the core provides basic performance support such as heat resistance to solve the contradiction. CN102257195A, CN102257198A, CN105431579A, CN102257194A, CN106222795a discloses a sheath-core composite spandex prepared by dry spinning technology, the cross section of which comprises at least a sheath region and a core region, and a well-defined boundary is provided between the two regions, the sheath region contains at least a fusible polyurethane with a low melting point, the core region contains at least a polyurethane or polyurethane urea with a high melting point, the spandex has a steam setting efficiency of more than 50% and a fusion strength of more than 0.15CN/dt, but due to the obvious change of the sheath and core structures, the great difference of the sheath elastic property and the core elastic property is brought, the sheath and the core of the fiber cross section are separated, and the fiber shows a spiral phenomenon on a macroscopic scale, which seriously affects the uniformity and stability of the product, and limits the wide use of mass production and customers.
Disclosure of Invention
Technical problems: in order to solve the problems in the prior art, the invention aims to provide the composite spandex, which has excellent uniformity and stability, has no spiral phenomenon, has no skin-core interface in the cross section and presents a single area when observed under an optical microscope.
The technical scheme is as follows: the preparation method of the composite spandex comprises the following steps:
1) Uniformly mixing 10-50% of polyurethane urea, 45-85% of thermoplastic polyurethane and 0.5-5.0% of dipropylene glycol dibenzoate in dimethylacetamide to obtain a polyurethane solution A;
2) Uniformly mixing 65-85% of polyurethane urea, 10-30% of thermoplastic polyurethane and 0.5-5.0% of dipropylene glycol dibenzoate in dimethylacetamide to obtain a polyurethane solution B;
3) And respectively passing the polyurethane solution A and the polyurethane solution B through a sheath feeding port and a core feeding port of the sheath-core composite component, and preparing the composite spandex by a dry spinning technology.
Wherein, the liquid crystal display device comprises a liquid crystal display device,
the end capping rate of diethylamine of the polyurethane urea is 2.5% -5.5%, and free-NH in the solution of diethylamine and polyurethane urea 2 The molar ratio of (2) is 1:1-8:1.
The diethylamine end capping rate is calculated according to formula (1),
diethylamine end-capping = C/D100% (1)
Wherein C is the molar amount of diethylamine and D is the molar amount of-NCO in the diisocyanate.
The polyurethane solution A and the polyurethane solution B have the same solid content and dynamic viscosity.
The solid content is 20-40%, and the dynamic viscosity is 1000-4000 poise at 40 ℃.
The weight ratio of the polyurethane solution A to the polyurethane solution B fed through the sheath-core composite component is 1:1-1:9.
The length-diameter ratio of the cylindrical guide hole in the spinneret plate of the sheath-core composite component is 4:1-8:1, and the length-diameter ratio of the micropore is 2:1-5:1.
The cross section of the composite spandex is observed to have a skin-core-free interface under an optical microscope, and shows a single area, and the uniformity is less than or equal to 2.5%.
The melt index of the thermoplastic polyurethane is 10cm under the conditions of 180 ℃ and 5kg pressure 3 /10min～50cm 3 The melt index test standard is referred to ASTM D1238, which is established by the American society for testing and materials (American Society for Testing and Materials, ASTM).
The melt index of the thermoplastic polyurethane is 10cm under the conditions of 180 ℃ and 5kg pressure 3 /10min～50cm 3 The melt index test standard is referred to ASTM D1238, which is established by the American society for testing and materials (American Society for Testing and Materials, ASTM).
The beneficial effects are that: compared with the prior art, the preparation method of the composite spandex has excellent compatibility by the aid of the post-polymerization capability and the mass and heat transfer process of the sheath solution and the core solution. Therefore, the composite spandex provided by the invention has the advantages that the cross section of the composite spandex is observed under an optical microscope, a skin-core-free interface is displayed, a single area is formed, the product has no spiral yarn phenomenon, and the composite spandex has excellent uniformity and is widely applied to the fields of silk stockings, seamless underwear and the like.
Drawings
Fig. 1 is a schematic view of the pilot hole and micropore cross section of a spinneret. The method comprises the following steps: spinneret plate guide holes 1 and micropores 2.
Detailed Description
The preparation method of the composite spandex comprises the following steps:
1) Uniformly mixing 10-50% of polyurethane urea, 45-85% of thermoplastic polyurethane and 0.5-5.0% of dipropylene glycol dibenzoate in dimethylacetamide to obtain a polyurethane solution A;
2) Uniformly mixing 65-85% of polyurethane urea, 10-30% of thermoplastic polyurethane and 0.5-5.0% of dipropylene glycol dibenzoate in dimethylacetamide to obtain a polyurethane solution B;
3) And respectively passing the polyurethane solution A and the polyurethane solution B through a sheath feeding port and a core feeding port of the sheath-core composite assembly, and preparing the composite spandex by a dry spinning technology.
The polyurethane urea is polymerized by diisocyanate, oligomer polyol and mixed amine, wherein the mixed amine consists of a chain extender and a chain terminator, and the chain terminator at least contains diethylamine.
The diethylamine end capping rate of the polyurethane urea is 2.5% -5.5%, and the molar ratio of diethylamine to excessive-NH 2 in the polyurethane urea solution is 1:1-8:1.
The melt index of the thermoplastic polyurethane is 10cm under the conditions of 180 ℃ and 5kg pressure 3 /10min～50cm 3 The melt index test standard is referred to ASTM D1238, which is established by the American society for testing and materials (American Society for Testing and Materials, ASTM).
The polyurethane solution A and the polyurethane solution B have the same solid content and dynamic viscosity, the solid content is 20% -40%, and the dynamic viscosity is 1000 poise-4000 poise at 40 ℃.
The weight ratio of the polyurethane solution A to the polyurethane solution B fed through the sheath-core composite component is 1:1-1:9.
The length-diameter ratio of the cylindrical guide hole in the spinneret plate of the sheath-core composite component is 4:1-8:1, and the length-diameter ratio of the micropore is 2:1-5:1.
The dry spinning technology is that polyurethane solution is extruded by a spinneret plate, and polyurethane solution is subjected to high Wen Yongdao, solvent volatilization, strand solidification and forming, drafting, false twisting, oiling and winding to prepare spandex.
For further explanation of the present invention, specific operation of the present invention will be described in detail with reference to specific examples, but these examples should not be construed as limiting the present invention in any sense. It is also to be understood that various modifications of the invention may be made by those skilled in the art after reading the disclosure herein, and that such equivalents are intended to fall within the scope of the claims appended hereto.
In the following examples and comparative examples, the cross-sectional morphology, spiral, uniformity, and the like of the composite spandex were evaluated as follows.
(1) Cross-sectional morphology: the cross-sectional morphology of the composite spandex was observed by an XSP-9CE microscope.
(2) Spiral wire: one end of the 30mm long composite spandex is fixed, the other end of the composite spandex naturally sags, and obvious bending phenomenon of the silk thread can be observed.
(3) Uniformity: the composite spandex is unwound with 3 times of drafting, the tension (gf) change in the unwinding process of 1000 meters of spandex is tested by a tension device system, the coefficient of variation of the tension value reflects the uniformity, and the smaller the numerical value, the better the uniformity.
Example 1:
preparation of a polyurethaneurea solution: 10kg of PTMEG having a molecular weight of 1810 and 2.52kg of 4,4' -MDI were reacted at 70℃for 120min to give an isocyanate-terminated prepolymer, which was then completely dissolved by adding DMAC, cooled to 12℃and then slowly added to a mixed amine solution containing 203.0g of ethylenediamine, 62.6g of propylenediamine, 45.0g of diethylamine and 5902.0g of DMAC for chain extension, and finally 35.7g of 2-methylpentanediamine was added.
Preparation of polyurethane solution a (skin stock solution): the components with the weight percentage of 23 percent of polyurethane urea, 75 percent of thermoplastic polyurethane and 2 percent of dipropylene glycol dibenzoate are uniformly mixed in DMAC solution to form a cortical stock solution with the solid content of 35 percent and the dynamic viscosity of 3900 poise at 40 ℃.
Preparation of polyurethane solution B (core stock solution): the components with the weight percentage of 83 percent of polyurethane urea, 15 percent of thermoplastic polyurethane and 2 percent of dipropylene glycol dibenzoate are uniformly mixed in DMAC solution to form core layer stock solution with the solid content of 35 percent and the dynamic viscosity of 3900 poise at 40 ℃.
And (3) enabling the sheath stock solution and the core layer stock solution to pass through a sheath-core composite component according to the weight ratio of 3:7, wherein the length-diameter ratio of a cylindrical guide hole in a spinneret plate of the sheath-core composite component is 4:1, the length-diameter ratio of micropores is 3:1, forming a yarn through solvent evaporation and solidification by a dry spinning technology, and preparing the composite spandex through drafting, false twisting, oiling and winding.
The thermoplastic polyurethane described in this example has a melt index of 19.4cm 3 /10min。
In the embodiment, the composite spandex has no spiral filament phenomenon, the cross section has no skin-core interface, and the uniformity is 1.22%.
Example 2:
composite spandex was prepared in the same manner as in example 1, except that the aspect ratio of the cylindrical pilot holes in the spinneret of the sheath-core composite assembly was 8:1 and the aspect ratio of the micropores was 2:1.
In the embodiment, the composite spandex has no spiral filament phenomenon, the cross section has no skin-core interface, and the uniformity is 1.05%.
Example 3:
composite spandex was prepared in the same manner as in example 1 except that polyurethane solution a was obtained by uniformly mixing 20% polyurethaneurea, 79% thermoplastic polyurethane, 1% dipropylene glycol dibenzoate in DMAC solution; the core layer stock solution is prepared by uniformly mixing 79% of polyurethane urea, 20% of thermoplastic polyurethane and 1% of dipropylene glycol dibenzoate in DMAC solution.
In the embodiment, the composite spandex has no spiral filament phenomenon, the cross section has no skin-core interface, and the uniformity is 1.68%.
Example 4:
preparation of a polyurethaneurea solution: 10kg of PTMEG with molecular weight 1810 and 2.42kg of 4,4' -MDI are reacted for 120min at 70 ℃ to obtain isocyanate end-capped prepolymer, then DMAC is added to be completely dissolved, after cooling to 12 ℃, a mixed amine solution containing 172.5g of ethylenediamine, 70.9g of propylenediamine, 20.0g of diethylamine, 22.0g of monoethanolamine and 4951.3g of DMAC is slowly added to carry out chain extension reaction, and finally 14.3g of 2-methylpentanediamine is added to be uniformly stirred to obtain the polyurethane urea solution with solid content of 35%.
Preparation of polyurethane solution a (skin stock solution): the components with the weight percentage of 20 percent of polyurethane urea, 79 percent of thermoplastic polyurethane and 1 percent of dipropylene glycol dibenzoate are uniformly mixed in DMAC solution to form a cortical stock solution with the solid content of 35 percent and the dynamic viscosity of 3900 poise at 40 ℃.
Preparation of polyurethane solution B (core stock solution): the components with the weight percentage of 79 percent of polyurethane urea, 20 percent of thermoplastic polyurethane and 1 percent of dipropylene glycol dibenzoate are uniformly mixed in DMAC solution to form core layer stock solution with the solid content of 35 percent and the dynamic viscosity of 3900 poise at 40 ℃.
And (3) enabling the sheath stock solution and the core layer stock solution to pass through a sheath-core composite component according to the weight ratio of 3:7, wherein the length-diameter ratio of a cylindrical guide hole in a spinneret plate of the sheath-core composite component is 4:1, the length-diameter ratio of micropores is 5:1, forming a yarn through solvent evaporation and solidification by a dry spinning technology, and preparing the composite spandex through drafting, false twisting, oiling and winding.
The thermoplastic polyurethane described in this example has a melt index of 19.4cm 3 /10min。
In the embodiment, the composite spandex has no spiral filament phenomenon, the cross section has no skin-core interface, and the uniformity is 2.03%.
Comparative example 1:
preparation of a polyurethaneurea solution: 10kg of PTMEG with molecular weight 1810 and 2.32kg of 4,4' -MDI are reacted for 120min at 70 ℃ to obtain isocyanate end-capped prepolymer, then DMAC is added to be completely dissolved, after cooling to 12 ℃, a mixed amine solution containing 266.4g of ethylenediamine, 88.8g of propylenediamine, 30.0g of diethylamine and 4892.5g of DMAC is slowly added to carry out chain extension reaction, and finally 28.6g of 2-methylpentanediamine is added to be uniformly stirred to obtain the polyurethane urea solution with solid content of 33.5%.
Preparation of polyurethane solution a (skin stock solution): the polyurethane urea with the weight percentage of 25 percent and the thermoplastic polyurethane with the weight percentage of 75 percent are uniformly mixed in DMAC solution to form skin stock solution with the solid content of 33.5 percent and the dynamic viscosity of 3600 poise at 40 ℃.
Preparation of polyurethane solution B (core stock solution): uniformly mixing polyurethane urea with the weight percentage of 85% and thermoplastic polyurethane with the weight percentage of 15% in DMAC solution to form core layer stock solution with the solid content of 35% and the dynamic viscosity of 3900 poise at 40 ℃.
And (3) enabling the sheath stock solution and the core layer stock solution to pass through a sheath-core composite component according to the weight ratio of 3:7, wherein the length-diameter ratio of a cylindrical guide hole in a spinneret plate of the sheath-core composite component is 3:1, the length-diameter ratio of micropores is 8:1, forming a yarn through solvent evaporation and solidification by a dry spinning technology, and preparing the composite spandex through drafting, false twisting, oiling and winding.
The thermoplastic polyurethane described in this comparative example had a melt index of 19.4cm 3 /10min。
The composite spandex in the comparative example has a severe spiral yarn phenomenon, and the cross section has a clear skin-core interface, and the uniformity is 5.35%.
Fig. 1 shows a schematic diagram of a guide hole and a micropore section of a spinneret plate, wherein a polyurethane solution A and a polyurethane solution B respectively pass through a sheath feed port and a core feed port of a sheath-core composite assembly, are combined above the guide hole 1 of the spinneret plate, are extruded and cured through micropores 2, and finally form the composite spandex.
The invention has been described with reference to specific embodiments and examples. Various changes in form and details may be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (4)

1. The preparation method of the composite spandex is characterized by comprising the following steps of:
1) Uniformly mixing 10-50% of polyurethane urea, 45-85% of thermoplastic polyurethane and 0.5-5.0% of dipropylene glycol dibenzoate in dimethylacetamide to obtain a polyurethane solution A;
2) Uniformly mixing 65-85% of polyurethane urea, 10-30% of thermoplastic polyurethane and 0.5-5.0% of dipropylene glycol dibenzoate in dimethylacetamide to obtain a polyurethane solution B;
3) Respectively passing the polyurethane solution A and the polyurethane solution B through a sheath feed inlet and a core feed inlet of a sheath-core composite component, and preparing composite spandex by a dry spinning technology;
the end capping rate of diethylamine of the polyurethane urea is 2.5% -5.5%, and free-NH in the solution of diethylamine and polyurethane urea 2 The molar ratio of the (2) to the (1:1) to (8:1);
the length-diameter ratio of a cylindrical guide hole in a spinneret plate of the sheath-core composite component is 4:1-8:1, and the length-diameter ratio of a micropore is 2:1-5:1;
the diethylamine end capping rate is calculated according to formula (1),
diethylamine end capping = C/D100% (1) wherein C is the molar amount of diethylamine and D is the molar amount of-NCO in the diisocyanate;
the polyurethane solution A and the polyurethane solution B have the same solid content and dynamic viscosity.
2. The method for preparing composite spandex according to claim 1, wherein the solid content is 20-40% and the dynamic viscosity is 1000-4000 poise at 40 ℃.
3. The preparation method of the composite spandex according to claim 1, wherein the weight ratio of the polyurethane solution A to the polyurethane solution B fed through the sheath-core composite component is 1:1-1:9.
4. The composite spandex of claim 1, wherein the cross section of the composite spandex exhibits a single area with uniformity of 2.5% or less when viewed in an optical microscope without a sheath-core interface.
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US5969051A (en) * 1997-08-11 1999-10-19 The Goodyear Tire & Rubber Company Hydrophilic nitrile rubber
JP4860261B2 (en) * 2005-12-27 2012-01-25 旭化成せんい株式会社 Polyurethane elastic fiber
BRPI0915235B1 (en) * 2008-10-17 2018-10-09 Invista Tech Sarl fibers, fabric and process for the preparation of a multi-component, spun-solution, fusible, elastic fiber
JP5676456B2 (en) * 2009-03-11 2015-02-25 インヴィスタ テクノロジーズ エスアエルエル Fusion two-component spandex
CN108048952B (en) * 2017-12-15 2020-11-10 浙江华峰氨纶股份有限公司 Preparation method of high-elasticity and easy-adhesion polyurethane urea fiber
CN108085780B (en) * 2017-12-15 2020-04-24 浙江华峰氨纶股份有限公司 High-uniformity easy-adhesion spandex fiber and preparation method thereof

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