CN101033286A - Shape memory polyurethane yarn and fabric - Google Patents

Shape memory polyurethane yarn and fabric Download PDF

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Publication number
CN101033286A
CN101033286A CN200610058886.0A CN200610058886A CN101033286A CN 101033286 A CN101033286 A CN 101033286A CN 200610058886 A CN200610058886 A CN 200610058886A CN 101033286 A CN101033286 A CN 101033286A
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China
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shape memory
yarn
fabric
fiber
temperature
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CN200610058886.0A
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胡金莲
刘晓霞
刘岩
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Hong Kong Polytechnic University HKPU
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Hong Kong Polytechnic University HKPU
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Priority to CN200610058886.0A priority Critical patent/CN101033286A/en
Publication of CN101033286A publication Critical patent/CN101033286A/en
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Abstract

The invention relates to temperature sensor shape memory polyurethane yarn and fabric. In the invention, it uses the shape memory polyurethane fiber or with other fibers to spin into yarn with shape memory effect. It uses the shape memory yarn spin or spin with other yarns, or it uses the shape memory polyurethane in other forms, such as emulsion, film, powder to handle the ordinary fabric to achieve a shape memory effect fabric. The shape memory yarn includes monofilament yarn and yarn-silk yarn. The shape memory fabrics include woven, knitted fabric, nonwoven fabric, laminated fabric, coated fabrics and composite fabrics.

Description

Shape memory polyurethane yarn and fabric
Technical field
The present invention relates to have the yarn and the fabric of shape memory function, this yarn and fabric adopt the shape memory polyurethane with temperature sense to process.
Background technology
Shape-memory material is most promising, most important applications is mainly in fields such as biomedical, weaving dress ornament, toy, packing, defence and militaries.As necktie, abdominal belt, dress ornament lining, brassiere etc., dentistry orthopedic instrument, Osteological device, bandage, Sportswear, military fighting uniform, anorak, tent etc., these materials mostly use with the form of fiber, yarn or fabric.And application report and the patent in these fields mainly concentrates on the fabric that adopts the Ni-Ti alloy fiber and be made at present, and is mainly used in medical field.
Shape memory alloy fiber Boardy Feeling, restoring force is big.In weaving, can be used as yarn core and other various fibers spin the Fancy Yarns with shape memory effect, and be made into dynamic fabric.Britain implants the shape memory alloy fiber in the fabric, works out the insulation shape memory fabrics.Italy develops the clever shirt of turn-up cuff automatically in summer with shape memory alloy.Many patents and bibliographical information shape memory alloy be woven into therapeutic medical human organ.But up to the present, seldom to the report of shape-memory polymer yarn and fabric.
Compare with shape memory alloy, the application potential of shape-memory polymer in weaving is much bigger.Its feel is soft; Strain can reach 300% even bigger; The technology of easy shaping and higher shape stability are arranged; The mechanical properties adjustable extent is bigger, promptly only its chemical structure and composition is carried out little change, just can make its shape memory transition temperature and mechanical properties obtain bigger variation, thereby produces the product of multiple shape memory.
In recent years, because the shape-memory polymer fiber spinning performance of being developed can not meet the demands, limited directly and produced yarn and fabric thereof with shape memory fiber.U.S. Patent Publication a kind of preparation method of shape memory fabrics, this fabric is made up of the polymer powder that natural fiber/synthon and one deck have shape memory.Textile college of Britain Heriot-Watt university has delivered the article of relevant shape memory alloy and shape-memory polymer fabric, but does not see relevant patent.Therefore author Chan points out that in article the mechanical property such as the tensile strength of the shape-memory polymer fiber that is adopted are lower, and impurity is more, has added the intensity that the part trevira improves fiber when spinning.But this yarn is because the low raw material that still can only be used as blanket kind fabric and hand-Braided Fabrics of intensity.
Summary of the invention
The purpose of this invention is to provide yarn and fabric with temperature sense shape memory function, it adopts the shape memory polyurethane fiber to be spun into the yarn with shape memory effect separately or with other blending in of fibers; Adopt shape memory yarn of the present invention weave separately or with other yarns interwoven, or adopt shape memory polyurethane other forms such as emulsion, film, powder, resin is put in order common fabric and obtain to have the fabric of shape memory effect.Shape memory yarn comprises monofilament yarn and multifilament yarn.Shape memory fabrics comprises woven fabrics, knitted fabrics, supatex fabric, laminated fabric, coated fabric and compound fabric.
Other forms of above-mentioned shape memory polyurethane fiber or shape memory polyurethane such as emulsion, film, powder, resin all are to be prepared by shape memory polyurethane, but this shape memory polyurethane can be prepared into by component that forms anti-phase (A) and the component (B) that forms stationary phase, wherein component (A) and (B) be:
(A):
Catalyzer 0.01-0.20 weight part
Polyethers or polyester diol 30-100 weight part
Aromatic series or aliphatic diisocyanate 5-30 weight part
Solvent 0-500 weight part
(B):
Aromatic diisocyanate 5-100 weight part
Linking agent trihydroxy-polyvalent alcohol 0.10-2.00 weight part
The dibasic alcohol 2-30 of chainextender short-chain fat family weight part
The carboxylic short-chain fat dibasic alcohol 0-10 of family weight part
Solvent 0-200 weight part
The method for preparing shape memory polyurethane by component (A) and component (B):
(1) a, the reversible phase component that comprises 0.01-0.20 weight part catalyzer, 30-100 weight part polyethers or polyester diol, 5-30 weight part aromatic series or aliphatic diisocyanate, 0-500 parts by weight solvent is reacted in reactor, obtain containing the polyurethane prepolymer of reversible phase structure;
(1) b, add and comprise 5-100 weight part aromatic diisocyanate, 2-30 weight part chainextender short-chain fat family dibasic alcohol, the carboxylic short-chain fat of 0-10 weight part family's dibasic alcohol and 0.10-2.00 weight part linking agent trihydroxy-polyvalent alcohol, continue reaction, add the 0-200 parts by weight solvent and adjust viscosity and concentration, but obtain to comprise the urethane with shape memory characteristic of anti-phase and stationary phase.
Then, utilize the shape memory polyurethane make to make other forms of shape memory polyurethane fiber or shape memory polyurethane such as emulsion, film, powder, resin, foam etc. respectively.
The shape memory polyurethane fiber is to utilize the shape memory polyurethane for preparing to be prepared into by melt spinning or wet spinning process.
The emulsion of shape memory polyurethane is ionic or non-ionic type emulsion, and latex particle size is distributed in 50-1000nm, and solid content is 10-40%, and its glued membrane has shape memory function.
The preparation method of shape memory polyurethane film can adopt currently known methods, as referring to U.S. Pat 5,098, and the method in 776/1992 and US5,128,197/1992.
The preparation method of shape memory polyurethane resin can adopt currently known methods, as referring to the method in the Japanese Patent (publication number 252353/1986).
Shape memory polyurethane foamy preparation method also can adopt currently known methods.
Shape memory polyurethane of the present invention is a kind of block polyurethane of forming by stationary phase (also claim hard section phase) but with anti-phase (also claiming soft section mutually), and wherein stationary phase has good heat endurance, but anti-phase has-10 ℃~60 ℃ deformation recovery temperature (T s), stationary phase has the second-order transition temperature (T that is higher than 100 ℃ Gh) or crystalline melt temperature (T Mh), when envrionment temperature is higher than T sThe time, but anti-phase produces high elastic deformation under external force, and this moment is higher owing to the phase transition temperature of stationary phase, still is in vitreous state or crystal form, plays a part support, and required elastic restoring force is provided in the deformation recovery process.When envrionment temperature is reduced to T again sWhen following, but owing to be in the elastic restoring force height that the brute force of the anti-phase of vitreous state compares stationary phase this moment, deformation still " is freezed " after the external force unloading and is fixed up; When envrionment temperature rises to T sWhen above, the reversible flexible state that is in mutually, the factor that resists the stationary phase elastic restoring force is eliminated, and polymkeric substance is owing to the elastic recovery of stationary phase is returned to original state.Therefore the urethane of this block structure reaches and has good shape memory characteristic by its fiber that makes.
But the anti-phase of shape memory polyurethane provided by the invention and the ratio between the stationary phase can change in the scope of broad, do not have specific restriction.But in order to realize purpose of the present invention better, be benchmark in the solids content, the quality percentage composition of preferred stationary phase is 20%-80%, but the quality percentage composition of anti-phase is 80%-20%; More preferably the quality percentage composition of stationary phase is 20%-50%, but the quality percentage composition of anti-phase is 80%-50%.In another preferred embodiment of the present invention, in the block shape memory polyurethane-NCO is 1.0~1.5 with the mole number ratio of-OH.
Preferably, the used water base block shape memory polyurethane of the present invention is colourless to faint yellow viscous liquid, and its mass percent concentration is 15%-25%, and has tangible two phase structure, preferably deformation recovery temperature (T wherein s) between-10~60 ℃, the second-order transition temperature (T of stationary phase Gh) be higher than 100 ℃.The deformation fixed rate of film and deformation-recovery rate are all more than 90%.
Used catalyzer can be to promote the isocyanate group of reversible phase component and any material of the reaction between the alcoholic extract hydroxyl group in reversible being combined to of shape memory polyurethane of the present invention, preferred organotin, organic germanium, organic zinc compound or polynary tertiary amine, preferred especially dibutyl tin laurate, stannous octoate or triethylenediamine or its combination.
Polyethers or polyester diol are preferably the crystalline melt point temperature range at 10-60 ℃ glycol, as polyethylene glycol adipate glycol (PHEP), poly adipate succinic acid ester glycol (PHB), polycaprolactone glycol (PCL), at least a in polyoxyethylene glycol (PEG) and/or the polytetrahydrofuran diol (PTMG), preferred especially number average relative molecular mass are 1000~4000 polyethylene glycol adipate glycol (PHEP), the number average relative molecular mass is 1000~6000 poly adipate succinic acid ester glycol (PHB), the number average relative molecular mass is 1250~8000 polycaprolactone glycol (PCL), the number average relative molecular mass is 200~6000 polyoxyethylene glycol (PEG), the number average relative molecular mass is 200~4000 polytetrahydrofuran diol (PTMG), or its combination.
Aromatic series or aliphatic diisocyanate are preferably 2,4 toluene diisocyanate (TDI), 4, at least a in 4 '-'-diphenylmethane diisocyanate (MDI), hexamethylene diisocyanate (HDI) or the isophorone diisocyanate (IPDI).
Linking agent trihydroxy-polyvalent alcohol is preferably at least a in glycerol, Viscotrol C, TriMethylolPropane(TMP) or the polypropylene glycol (PPG-303, PPG-330, its number average relative molecular mass is respectively 300 and 3000).
Chainextender is preferably short-chain fat family dibasic alcohol, for example 1,4-butyleneglycol, 1,5-pentanediol, 1,6-hexylene glycol, 1,1, at least a in ammediol or the glycol ether, more preferably 1,4-butyleneglycol, 1,6-hexylene glycol, ethylene glycol or glycol ether or its combination.
Carboxylic short-chain fat family dibasic alcohol is preferably at least a in dimethylol propionic acid, dimethylolpropionic acid or the tartrate.
Organic solvent is preferably at least a in dimethyl formamide, N,N-DIMETHYLACETAMIDE, dimethyl sulfoxide (DMSO), acetone or the methylethylketone.
Preferably, the reaction of step (1) a under agitation, have in the reactor of reflux exchanger, under temperature 40-100 ℃, carry out under preferred 60-85 ℃.Reaction times is depended on temperature of reaction and concrete reaction process, is generally 30 minutes to 6 hours, most preferably is 2-3 hour.Preferably, under being temperature in room temperature to 85 ℃, the continuation of step (1) b reaction carries out.More preferably, continuing reaction is what to carry out under 50-70 ℃ temperature.A kind of preferred embodiment in, wherein in step (1) b, the stationary phase component is that gradation adds, and identical or different in the identical or different following reaction times of temperature.More preferably, in step (1) b, add 5-100 weight part aromatic diisocyanate, 5-30 weight part chainextender short-chain fat family's dibasic alcohol and the carboxylic short-chain fat of 0-10 weight part family dibasic alcohol, 0.10-2.00 weight part linking agent trihydroxy-polyvalent alcohol down at 50-60 ℃, temperature control 55-70 ℃ then, reacted 3-4 hour.Preferably, the solvent in the step (1) is a polar organic solvent, as dimethyl formamide, N,N-DIMETHYLACETAMIDE, dimethyl sulfoxide (DMSO), acetone or methylethylketone etc.
Preferably, the solvent in the step (1) is a polar organic solvent, as dimethyl formamide, N,N-DIMETHYLACETAMIDE, dimethyl sulfoxide (DMSO), acetone or methylethylketone etc.
The shape memory fiber that is prepared by shape memory polyurethane of the present invention has following characteristics: fiber number is higher than 300dtex, breaking tenacity 1~1.5CN/dtex, extension at break 100%~400%, its deformation fixed rate 〉=90%, deformation-recovery rate 〉=90%.
Compared with prior art, shape memory fiber of the present invention or other forms all have outstanding feature on structure and performance:
(1) constructional feature:
Introduced tangible two phase structure (block structure), but wherein the deformation recovery temperature range of anti-phase is-10 ℃≤T s≤ 60 ℃, the phase transition temperature of stationary phase is higher than 100 ℃.
(2) performance characteristics:
Intelligent characteristic with shape memory.
When envrionment temperature is higher than Ts, but anti-phase produces high elastic deformation under external force, reduces to Ts again when following when envrionment temperature, and deformation is in external force unloading back " being freezed " and be fixed up, and its deformation fixed rate is greater than 90%; When envrionment temperature rises to Ts when above again, polymkeric substance is returned to original state again; Its deformation-recovery rate also reaches and reaches more than 90%.
Yarn of the present invention comprises monofilament yarn and multifilament yarn, pure spinning and union yarn.Wherein union yarn finger-type shape memory fiber and any natural fiber or other man-made fiber mix spinnings.According to the different excitation temperatures of shape memory fiber, yarn can have difference in functionality.As, can be designed to shape when normal temperature keeps typing keeping the design outward appearance and to spin smoothly and weave, yarn returns to designed original-shape when being in excitation temperature, as is curled into the shape of spiral, high elongation etc.Because the structure difference of various yarns can produce a variety of variations when being stimulated as yarns such as fasciated yarn, knot yarn, spiral yarn, Chenille Yarns wreath yarns.Fiber species, morphological structure, physicals and the ratio difference of blending simultaneously also can produce the yarn of various different-styles and shape memory effect.
The yarn and the fabric that utilize above-mentioned shape memory fiber spinning to obtain have shape memory function, and its deformation-recovery temperature is at-10 ℃ to 100 ℃.Shape memory yarn and fabric show the better practicability energy at aspects such as elasticity, brute force and shape-memory properties.Its feature finds expression in yarn and fabric can change shape when being higher than the shape memory transition temperature, and this shape is finalized when being cooled to be lower than the shape memory transition temperature.When near the envrionment temperature shape memory transition temperature or when above, yarn and fabric can be returned to original shape.
Shape memory fabrics of the present invention comprises woven fabrics, knitted fabrics, supatex fabric, laminated fabric, coated fabric and compound fabric.Fabric obtains shape memory function by three kinds of forms: the one, and adopt shape memory fiber spinning of the present invention to weave; The 2nd, fabric is made by general fibre or yarn, carries out the back arrangement with shape memory emulsion, film or resin then; The 3rd, adopt shape memory polyurethane fiber, film, foam or resin and common material to be processed into matrix material, make shape memory fabrics then.Fabric of the present invention can the overall applicability shape memory yarn, also can topical application.In conjunction with different weave constructions, yarn types and processing parameter produce Protean fabric.The method of utilizing emulsion, film or resin to put in order all is an ordinary method, can be as the adjustment method of emulsion, will treat that finish fabric is immersed in the emulsion, and two soak two rolls, and mangle expression 100% 85 ℃ of preliminary dryings 3 minutes, was baked and banked up with earth 2 minutes at 150 ℃ then again; The adjustment method of resin can be and will treat that finish fabric pads the finishing composition of tape tree fat (soaks rolls) → dry → bake and bank up with earth; The adjustment method of film makes film and fabric compound under tackiness agent and heating condition for adopting lamination industry.
No matter institute's invention yarn and fabric produce fold or distortion when placing or wearing for a long time, as long as this yarn fabric is heated in air or hot water near the shape memory transition temperature or more than, yarn and fabric are easier to return to the virgin state that it remembers and eliminate distortion.This shape memory function can be widely used in non-ironing guarantor's type, deformation-recovery, warming vapour, water-proof air-permeable, insulation fire prevention etc. in the field of textiles function aspects; Can produce the dynamic fabric of multidimensional of multiple colored type, color in aesthetic.
Shape memory yarn can be separately or with other yarn weaving shape memory fabrics.The shape memory function of these linings can be used for: (1) typing keeps, non-ironing and arch camber recovery function; (2) produce various novelty fabric and three-dimensional dynamic fabric.
In weaving, can be used as purposes such as shirt, underwear, overcoat, decoration with the woven fabric of shape memory yarn and with the fabric that the shape memory emulsion is put in order.Especially can satisfy the neckline of (1) shirt, the higher shape maintenance requirement of cuff; (2) recovery of shape requirement after upper garment ancon and the position arch camber of trousers knee; (3) next to the shin, the elasticity of underwear and comfortableness requirement; (4) typing of denim and elasticity requirement; (5) waist of trousers or abdominal belt use after the anamorphic stretching through deformation recovery, can recover the original length again; (6) the dimensionally stable requirement of knitted fabrics.Knitting shape memory clothes have overcome the shortcoming of knitted fabrics model keeping character difference, after clothes use to be produced distortion, as long as envrionment temperature is increased to the shape that just can be returned to more than the deformation-recovery temperature when finalizing the design.The shape memory novelty fabric can be used for fashionable dress, Curtains Fabrics, the tablecloth etc.
Shape memory fabrics also can be applicable to medical gauze, bandage, solid shape etc.Lamination and coated fabric have warming vapour, water-proof air-permeable function, can be used for thermal cloth, Sportswear, fighting uniform, tent, raincoat etc.The shape memory supatex fabric can be used for clothes liner and industry.Composite material of shape memory can be applicable to engineering as building, Industry Control.
Embodiment
Below the yarn that is spun into to shape memory polyurethane fiber and preparation method thereof and by this shape memory polyurethane fiber and the fabric that further obtains and be described specifically by the shape memory fabrics that other forms of shape memory polyurethane obtain, by these descriptions, characteristics of the present invention and advantage will more clearly show.
Embodiment
Embodiment 1-embodiment 6 (preparation of shape memory polyurethane fiber)
Embodiment 1
But with 60 kilograms of 0.02 kilogram of anti-phase component dibutyl tin laurates, polycaprolactone glycol (number average relative molecular mass 3000), 2,6.96 kilograms of 4-tolylene diisocyanates, dimethyl formamide add 1000L for 400 kilograms and have in the reactor of agitator, thermometer and reflux exchanger, react 2 hours down in temperature 70-80 ℃.Be cooled to 50~55 ℃ then, add stationary phase component 1,0.1 kilogram of 5.4 kilograms of 4-butyleneglycol, TriMethylolPropane(TMP), 4,1.34 kilograms of 20 kilograms of 4 '-'-diphenylmethane diisocyanates and dihydroxymethyl third carboxylics, temperature control 55-60 ℃, react after 3-4 hour, add 131 kilograms in acetone, regulate viscosity, obtain colourless to faint yellow, thick urethane.
Through Theoretical Calculation, in the present embodiment gained urethane-NCO :-OH=1: 1.27; The quality percentage composition of stationary phase is 37.1%, but the quality percentage composition of anti-phase is 62.9%; Its quality percentage composition is 15%; But the crystalline melt point temperature of anti-phase and the second-order transition temperature of stationary phase adopt the DSC thermal analyzer test of PE company to be respectively 48 ℃ and 147 ℃; The shape memory characteristic of film adopts the test of INSTRON 4466 (Instron company) universal testing machine, and its deformation fixed rate is 96.4%, and deformation-recovery rate is 94.1%.
The nascent fibre of gained polyurethane solution preparation is at room temperature dried, but do not carry out back draft and typing processing, the fiber number 360dtex of gained fiber, intensity 1.36CN/dtex, extension at break 235%.The deformation fixed rate of fiber is 95.1%, and deformation-recovery rate is 95.4%.
Embodiment 2
With stannous octoate 0.01 gram, polycaprolactone glycol (number average relative molecular mass 4000) 24 grams, polyethylene glycol adipate glycol (number average relative molecular mass 1000) 6 grams, hexamethylene diisocyanate 5.0 grams, N,N-DIMETHYLACETAMIDE 100 grams add 250mL and have in the reaction flask of agitator, thermometer and reflux exchanger, react 2 hours down for 65~70 ℃ in temperature.Be cooled to 55-60 ℃ then, add 1,4-butyleneglycol 1.0 grams, glycol ether 1.0 grams, Viscotrol C 2.0 grams, 4,4 '-'-diphenylmethane diisocyanate, 11.96 grams and dihydroxymethyl fourth carboxylic 1.48 grams, 60~65 ℃ of temperature controls, react after 3 hours, add methylethylketone 57 grams and regulate viscosity, obtain faint yellow, thick urethane.
Through Theoretical Calculation, in the present embodiment gained urethane-NCO :-OH=1.5: 1.0; The quality percentage composition of stationary phase is 50.0%, but the quality percentage composition of anti-phase is 50.0%; Its quality percentage composition is 25%; But the crystalline melt point temperature of anti-phase and the second-order transition temperature of stationary phase adopt the DSC thermal analyzer test of PE company to be respectively 44 ℃ and 139 ℃; The shape memory characteristic of film adopts the test of INSTRON4466 (Instron company) universal testing machine, and its deformation fixed rate is 95.2%, and deformation-recovery rate is 94.3%.
With the polyurethane solution that obtains, adjusting polymer content with N,N-DIMETHYLACETAMIDE is 15%.Spinning condition is orifice diameter 0.15mm, hole count 40, volume pump 0.6cc/r.40-55 ℃ of spinning solution temperature, solidifying medium be water, coagulation bath temperature 30-40 ℃, spinning speed 10-15M/min, stretch 2.0 times in bathing.The gained fiber is removed in the fiber behind the contained solvent through extraction, dries under 20-25 ℃, and in 65-70 ℃ of 1.5 times of typings 6-8 minute that stretch down, obtains the polyurethane shape memory fiber.
The mechanical property of this fiber and extensibility etc. adopt the test of INSTRON 4466 (Instron company) universal testing machine, this fibre number of its fiber 369dtex, intensity 1.0CN/dtex, extension at break 228.3%.The shape memory characteristic of fiber adopts the method test of embodiment 1-4, and its deformation fixed rate is 95.2%, and deformation-recovery rate is 96.9%.
Embodiment 3
With 0.02 kilogram of trimethylene diamines, 85 kilograms of poly adipate succinic acid ester glycol (number average relative molecular mass 4000), 15 kilograms of polyoxyethylene glycol (number average relative molecular mass 600), 10.45 kilograms of isophorone diisocyanates, dimethyl sulfoxide (DMSO) adds 1000L for 375 kilograms and has in the reactor of agitator, thermometer and reflux exchanger, reacts 2~3 hours down in temperature 78-80 ℃.Be cooled to 55-60 ℃ then, add 1,1.125 kilograms of 6-hexylene glycol 2.36 grams, glycerol, 4,1.5 kilograms in 10.21 kilograms of 4 '-'-diphenylmethane diisocyanates and tartrate, 60~65 ℃ of temperature controls react after 3 hours, be cooled to 30-40 ℃, obtain colourless, thick urethane.
Through Theoretical Calculation, in the present embodiment gained urethane-NCO :-OH=1.0: 1.0; The quality percentage composition of stationary phase is 20.0%, but the quality percentage composition of anti-phase is 80.0%; Its quality percentage composition is 25%; But the crystalline melt point temperature of anti-phase and the second-order transition temperature of stationary phase adopt the DSC thermal analyzer test of PE company to be respectively 52 ℃ and 144 ℃; The shape memory characteristic of film adopts the test of INSTRON4466 (Instron company) universal testing machine, and its deformation fixed rate is 92.2%, and deformation-recovery rate is 94.3%.
With the urethane/dimethyl formamide solution of gained, reconciling polymer content with dimethyl formamide is 15%.Spinning condition is orifice diameter 0.15mm, hole count 25, volume pump 0.6cc/r.60 ℃ of spinning solution temperature, solidifying medium be water, coagulation bath temperature 30-40 ℃, spinning speed 8-12M/min, bathe in stretching 1.5-2.5 doubly.The gained fiber is removed in the fiber behind the contained solvent through extraction, at room temperature dries, and in 60 ℃ of 1.3 times of typings 8 minutes that stretch down, obtains the polyurethane shape memory fiber.
The mechanical property of this fiber and extensibility etc. adopt the test of INSTRON 4466 (Instron company) universal testing machine, and its fibre number is 315dtex, and intensity is 1.26CN/dtex, and extension at break is 190.1%.The shape memory characteristic of fiber adopts the method test of embodiment 1-3, and its deformation fixed rate is 94.2%, and deformation-recovery rate is 95.3%.
Embodiment 4
With 0.02 kilogram of dibutyl tin laurate, 15 kilograms of polyethylene glycol adipate glycol (number average relative molecular mass 6000), polytetrahydrofuran diol 20 kilograms (number average relative molecular mass 1000), 2,7.5 kilograms of 4-tolylene diisocyanates, dimethyl formamide adds 300L for 200 kilograms and has in the reactor of agitator, thermometer and reflux exchanger, reacts 2 hours down for 75~80 ℃ in temperature.Be cooled to 50~55 ℃ then, add 1,4.0 kilograms of 4-butyleneglycols, polypropylene glycol (PPG303, number average relative molecular mass 300) 0.6 kilogram of 3.0 kilogram, ethylene glycol, 4,2.5 kilograms of 19.1 kilograms of 4 '-'-diphenylmethane diisocyanates and dimethylol propionic acids, 65~70 ℃ of temperature controls, react 85 kilograms of adjustings of adding methylethylketone viscosity after 2.5 hours, obtain faint yellow, thick polyurethane solution.
Through Theoretical Calculation, in the present embodiment gained urethane-NCO :-OH=1: 1.15; The quality percentage composition of stationary phase is 40.7%, but the quality percentage composition of anti-phase is 59.3%; Its quality percentage composition is 20%; But the crystalline melt point temperature of anti-phase and the second-order transition temperature of stationary phase adopt the DSC thermal analyzer test of PE company to be respectively 47 ℃ and 154 ℃; The shape memory characteristic of film adopts the test of INSTRON4466 (Instron company) universal testing machine, and its deformation fixed rate is 96.2%, and deformation-recovery rate is 97.8%.
With the polyurethane solution that obtains, adjusting polymer content with dimethyl formamide solution is 17-20%.Spinning condition is orifice diameter 0.15mm, hole count 40, volume pump 0.6-0.8cc/r.55-60 ℃ of spinning solution temperature, solidifying medium be water, coagulation bath temperature 30-35 ℃, spinning speed 8-10m/min, bathe in stretching 1.5-2.0 doubly.The gained fiber is removed in the fiber behind the contained solvent through extraction, dries under 18-25 ℃, and in 65 ℃ of 1.5 times of typings 8-10 minute that stretch down, obtains the polyurethane shape memory fiber.
The mechanical property of this fiber and extensibility etc. adopt the test of INSTRON 4466 (Instron company) universal testing machine, this fibre number of its fiber 375dtex, intensity 1.29CN/dtex, extension at break 258.3%.The shape memory characteristic of fiber adopts the method test of embodiment 1-3, and its deformation fixed rate is 95.8%, and deformation-recovery rate is 96%.
Embodiment 5
But with 0.02 kilogram of anti-phase component dibutyl tin laurate, 60 kilograms of polycaprolactone glycols (number average relative molecular mass 3000), polytetrahydrofuran diol 20 kilograms (number average relative molecular mass 2000), 4,12.5 kilograms of 4 '-'-diphenylmethane diisocyanates, dimethyl sulfoxide (DMSO) add 1000L for 500 kilograms and have in the reactor of agitator, thermometer and reflux exchanger, react 2 hours down in temperature 75-80 ℃.Be cooled to 50~55 ℃ then, add stationary phase component 1,15 kilograms of 15.75 kilograms of 4-butyleneglycols, polypropylene glycol PPG 330 (number average relative molecular mass 3000), 4,2.01 kilograms of 48.12 kilograms of 4 '-'-diphenylmethane diisocyanates and dihydroxymethyl third carboxylics, temperature control 55-60 ℃, react after 3-4 hour, add 200.0 kilograms in acetone, regulate viscosity, obtain colourless to faint yellow, thick urethane.
Through Theoretical Calculation, in the present embodiment gained urethane-NCO :-OH=1.1: 1.0; The quality percentage composition of stationary phase is 54.3%, but anti-phase quality percentage composition is 45.7%; Its quality percentage composition is 16.27%; But the crystalline melt point temperature of anti-phase and the second-order transition temperature of stationary phase adopt the DSC thermal analyzer test of PE company to be respectively 47.2 ℃ and 168 ℃; The shape memory characteristic of film adopts the test of INSTRON 4466 (Instron company) universal testing machine, and its deformation fixed rate is 95.4%, and deformation-recovery rate is 94.8%.
With the polyurethane solution that obtains, adjusting polymer content with dimethyl formamide solution is 17-20%.Spinning condition is orifice diameter 0.15mm, hole count 40, volume pump 0.6-0.8cc/r.55-60 ℃ of spinning solution temperature, solidifying medium be water, coagulation bath temperature 30-35 ℃, spinning speed 8-10m/min, bathe in stretching 1.5-2.0 doubly.The gained fiber is removed in the fiber behind the contained solvent through extraction, dries under 18-25 ℃, and in 65 ℃ of 1.5 times of typings 8-10 minute that stretch down, obtains the polyurethane shape memory fiber.
The mechanical property of this fiber and extensibility etc. adopt the test of INSTRON 4466 (Instron company) universal testing machine, this fibre number of its fiber 323dtex, intensity 1.49CN/dtex, extension at break 128.1%.The shape memory characteristic of fiber adopts the method test of embodiment 1-4, and its deformation fixed rate is 94.6%, and deformation-recovery rate is 93.2%.
Embodiment 6
With 0.02 kilogram of dibutyl tin laurate, 10 kilograms of poly adipate succinic acid ester glycol (number average relative molecular mass 6000), polyoxyethylene glycol 20 kilograms (number average relative molecular mass 600), 4,30 kilograms of 4 '-'-diphenylmethane diisocyanates, dimethyl formamide adds 1000L for 400 kilograms and has in the reactor of agitator, thermometer and reflux exchanger, reacts 2 hours down for 75 ℃ in temperature.Be cooled to 50~55 ℃ then, add 1,30.0 kilograms of 4-butyleneglycols, polypropylene glycol (PPG303, number average relative molecular mass 300) 10.0 kilograms, 4,10.0 kilograms of 4 '-'-diphenylmethane diisocyanate double centner and dimethylol propionic acids, 65~70 ℃ of temperature controls, react 200 kilograms of adjustings of adding methylethylketone viscosity after 2.5 hours, obtain faint yellow, thick polyurethane solution.
Through Theoretical Calculation, in the present embodiment gained urethane-NCO :-OH=1.03: 1.0; The quality percentage composition of stationary phase is 80%, but the quality percentage composition of anti-phase is 20%; Its quality percentage composition is 20%; But the crystalline melt point temperature of anti-phase and the second-order transition temperature of stationary phase adopt the DSC thermal analyzer test of PE company to be respectively 12 ℃ and 198 ℃; The shape memory characteristic of film adopts the test of INSTRON 4466 (Instron company) universal testing machine, and its deformation fixed rate is 96.2%, and deformation-recovery rate is 90.0%.
With the polyurethane solution that obtains, adjusting polymer content with dimethyl formamide solution is 17-20%.Spinning condition is orifice diameter 0.15mm, hole count 40, volume pump 0.6-0.8cc/r.55-60 ℃ of spinning solution temperature, solidifying medium be water, coagulation bath temperature 30-35 ℃, spinning speed 8-10m/min, bathe in stretching 1.5-2.0 doubly.The gained fiber is removed in the fiber behind the contained solvent through extraction, dries under 18-25 ℃, and in 65 ℃ of 1.5 times of typings 8-10 minute that stretch down, obtains the polyurethane shape memory fiber.
The mechanical property of this fiber and extensibility etc. adopt the test of INSTRON 4466 (Instron company) universal testing machine, this fibre number of its fiber 335dtex, intensity 1.5CN/dtex, extension at break 100%.The shape memory characteristic of fiber adopts the method test of embodiment 1-3, and its deformation fixed rate is 95.8%, and deformation-recovery rate is 90.2%.
Embodiment 7-embodiment 26 (shape memory yarn and shape memory fabrics)
Embodiment 7
Adopt shape memory polyurethane fiber and cotton fibre blending, blending ratio is 10/90~90/10.Shape memory fiber deformation recovery temperature is between 20 ℃~70 ℃.Under the normal temperature, yarn keeps the primary flat shape, through stretch repeatedly and bend after Yarn texturing.Put near 40 ℃ yarn or above water, yarn is returned to original flat shape very soon.When yarn is not subjected to the external force effect, when dropping to normal temperature, temperature still keeps original flat shape.
Embodiment 8
Yarn adopts shape memory polyurethane long filament and cotton fibre to be spun into core yarn.Wherein single shape memory fiber is made heart yarn, and cotton fibre is a fasciated yarn.Shape memory fiber deformation recovery temperature is 20 ℃~70 ℃.Under the normal temperature, yarn keeps the primary flat shape, through stretch repeatedly and bend after Yarn texturing.Put near 50 ℃ yarn or above water, yarn is returned to original flat shape very soon.When yarn is not subjected to the external force effect, when dropping to normal temperature, temperature still keeps original flat shape.
Embodiment 9
Yarn adopts shape memory filament fiber and viscose staple fibre to spin and forms, and blending ratio is 10/90~90/10.Shape memory fiber deformation recovery temperature is 20 ℃~70 ℃.The normal temperature yarn under working is in the flat shape of typing state, makes Yarn texturing through alternating bending, bending.In the time of near then yarn being immersed 50 ℃ or in the above water, the very fast answer of yarn is original flat, and has snappiness.Do not apply external force, when temperature drops to deformation temperature when following, yarn still remains the straightened condition of typing.
Embodiment 10
Yarn adopts shape memory fiber and the blending of terylene textured filament to form, and blending ratio is 10/90~90/10.Shape memory fiber deformation recovery temperature is 20 ℃~70 ℃.The normal temperature yarn under working is straight, blows with hot blast to cause the yarn envrionment temperature near the deformation recovery temperature or when above, and yarn shrinks for the shape that curls with the deformation-recovery of shape memory fiber, and surperficial POLYESTER YARNS plays round, and it is plentiful luxurious that outward appearance becomes.This moment is stretching with yarn, removes drawing force when following when temperature drops to deformation temperature, and yarn then keeps stretching shape.
Embodiment 11
Yarn adopt shape memory fiber and wool fiber to be spun into and, blending ratio is 10/90~90/10.Shape memory fiber deformation recovery temperature is 20 ℃~70 ℃.Because deformation temperature is lower than normal temperature, normal temperature yarn under working profile is straight, and it is soft plentiful, good springiness.Apply external force and make it be deformed into waviness, put into temperature and be 0~5 ℃ thermostatted, remove external force then, the yarn shape is fixed to waviness.When yarn is fetched near about 15 ℃ from thermostatted or in the above environment time, yarn returns to original straightened condition again.
Embodiment 12
Yarn adopts shape memory fiber and PET Hollow fiber to be spun into fluffy yarn, and blending ratio is 10/90~90/10.Shape memory fiber deformation recovery temperature is 20 ℃~70 ℃.Yarn is fixed to linear before spinning.After yarn spins, immerse temperature near the deformation recovery temperature or in the above water, very fast the answer with the shape memory fiber of yarn is original waviness.Do not add the external force effect, taking-up is cooled to below the deformation temperature, and yarn promptly remains wave-like.Repeatedly yarn is stretched, waviness is stretched gradually.Yarn is immersed temperature near the deformation recovery temperature or in the above water, yarn is returned to original waviness again again.
Embodiment 13
Adopt the shape memory fiber monofilament to be made into cylindrical plain knit fabric, shape memory fiber deformation recovery temperature is 20 ℃~70 ℃.Feel is harder under the normal temperature, fabric is immersed 50 ℃ near or in the above water, fabric distortion is shunk, smaller volume has snappiness.When taking-up is cooled to deformation temperature when following, fabric returns to original state again.
Embodiment 14
Knitted fabrics is made into by embodiment 7 yarns.Fabric is stretched repeatedly, produce lax and diagonal distortion.The fabric of distortion is blown with hot blast, cause the fabric envrionment temperature to rise near the deformation recovery temperature or when above, fabric form is returned to original-shape.Cooling back fabric still keeps original-shape.The fabric that another piece is same is exerted pressure repeatedly with globe and is made it produce the distortion of projection, immerses temperature then near the deformation recovery temperature or in the above water, and the very fast deformation-recovery of fabric is to original-shape.This knitted fabrics is made the underwear snug fit, makees overcoat and has good conformality.
Embodiment 15
Weft yarn made by the yarn of employing embodiment 8 and textile warp thread is made into denim.Fabric has the advantage of denim, and certain elasticity is arranged simultaneously, is easy to typing.When fabric is subjected to external force effect generation distortion repeatedly, it is immersed temperature near the deformation recovery temperature or in the above water, the shape when original the typing arrived in the very fast deformation-recovery of fabric.
Embodiment 16
Woven fabrics makes weft yarn by the yarn of embodiment 9 and cotton was made at interval with 1: 1.Fabric is smooth during normal temperature, produces obvious fold through rubbing repeatedly.Blow with hot blast then, the fabric envrionment temperature is risen near the deformation recovery temperature or more than, the very fast answer of fabric is original formation state.When envrionment temperature drops to the deformation recovery temperature when following, the formation state of fabric keeps getting off.
Embodiment 17
Fabric adopts the yarn of embodiment 10 to make weft yarn, and polyester yarn is made into as warp thread.Thread count is rarer, can do the clothing fabric in summer.In the time of near fabric immerses the deformation recovery temperature or in the above warm water, fabric is replied original curling shape with shape memory yarn and is shunk.Do not apply the external force effect, reduce to the deformation recovery temperature when following when temperature, this shape keeps getting off.The lining of this moment is abundant plentiful and luxurious, can be used as the water clothes lining.To summer, lining can be immersed near the deformation recovery temperature again or in the above water, apply external force cloth cover is evened up whole, when temperature drop to the deformation recovery temperature when following this shape be fixed, lining thins out nice and cool again.
Embodiment 18
Adopt embodiment 12 yarns to be made into the overcoat lining.Be made into the back and immerse temperature near the deformation recovery temperature or in the above water, fabric becomes fluffy plentiful with the shape memory yarn answer for original waviness.Do not apply external force and drop to the deformation recovery temperature when following when temperature, fabric is fixed up at this state.The clothes that simulation is made by this fabric are in the suffered stretching repeatedly of wearing process, and the wave state of yarn stretches gradually, and fabric is relaxation of deformation gradually.At this moment, fabric is immersed temperature near the deformation recovery temperature or in the above water, fabric becomes fluffy plentiful because of the wave-like that yarn is returned to again in the memory.
Embodiment 19
The high-count pure cotton drills is after shape memory polyurethane emulsion arrangement typing.Fabric rubbed repeatedly make its fold, put into temperature then near the recovery of shape temperature or above environment, the fold Lock-out.Do not add any external force, after temperature descended, the formation state of cloth cover kept getting off.
Embodiment 20
Pure fine linen imitates ancon at normal temperatures and fabric is applied power repeatedly makes it arch camber after shape memory polyurethane emulsion arrangement.Immerse temperature then near the recovery of shape temperature or in the above water, fabric is replied formation state again.Take out from water, do not add any external force, after temperature descended, the cloth cover formation state kept getting off.
Embodiment 21
After common non-woven was put in order with the shape memory polyurethane emulsion, flatiron produced folding line.The folding line that stretches repeatedly under the normal temperature fades away and flattens, and immerses then near or the above water of recovery of shape temperature, and cloth cover is replied the folding line state again.Take out from water, do not add any external force, after temperature descended, the folding line state kept getting off.
Embodiment 22
Shape memory polyurethane is joined in the used tamanori of production non-woven.The fabric typing time is an arc, stretches repeatedly under the normal temperature and flattens gradually.When be warmed to the shape memory transition temperature with hot blast near or when above, the bowed state when fabric is replied typing naturally.
Embodiment 23
Water-proof air-permeable shape memory polyurethane film and looped fabric lamination is compound, and the gained laminated fabric has the windproof property of waterproof, has vapour permeability simultaneously.The shape memory transition temperature is the human body comfort temperature, and when envrionment temperature was higher than this temperature, the laminated fabric vapour permeability increased, and human body sensory is comfortable; When temperature was lower than this temperature, vapour permeability weakened, and had heat-preserving function.This lining can be used for cold-proof underwear, insulated cold wear etc.
Embodiment 24
Water-proof air-permeable shape memory polyurethane film and slim non-woven lamination is compound, and the gained fabric has temperature sense water-proof air-permeable heat-preserving function.When envrionment temperature was higher than the shape memory conversion temp, the laminated fabric vapour permeability increases permeable steam but moisture can not pass, and is waterproof and human body sensory is comfortable; When temperature was lower than this temperature, vapour permeability weakened, and had heat-preserving function.This kind fabric can be used for water-proof air-permeable, Thermal textile product such as insulated cold wear liner, footwear, tent etc.
Embodiment 25
With water-proof air-permeable shape memory polyurethane reagent fabric is carried out coating and handle, obtain to have the water-proof air-permeable fabric of temperature sense.Its deformation recovery temperature is 20 ℃~70 ℃.The fabric vapor-permeable, water-proof can be used for submarine armour, both waterproof, saturating again vapour, degree height comfortable and easy to wear; Also can make overcoat, wind coat, raincoat, have the function of comfortable vapour.
Embodiment 26
Shape memory polyurethane material and body material are made matrix material.Material has the temperature sense shape memory function.Its deformation recovery temperature is 20 ℃~70 ℃.Material structure is tight, waterproof vapour.When temperature is higher than conversion temp,, the shape-memory material material structure cause permeability to water vapour to increase because changing.When being lower than this temperature, material structure becomes again closely, waterproof vapour.This matrix material can be used for Industry Control.

Claims (17)

1. shape memory polyurethane, but this urethane is prepared into component (A) and (B) be by component that forms anti-phase (A) and the component (B) that forms stationary phase:
(A):
Catalyzer 0.01-0.20 weight part;
Polyethers or polyester diol 30-100 weight part;
Aromatic series or aliphatic diisocyanate 5-30 weight part;
Solvent 0-500 weight part;
(B):
Aromatic diisocyanate 5-100 weight part;
Linking agent trihydroxy-polyvalent alcohol 0.1-2.0 weight part;
The dibasic alcohol 2-30 of chainextender short-chain fat family weight part;
The carboxylic short-chain fat dibasic alcohol 0-10 of family weight part;
Solvent 0-200 weight part;
Wherein, the quality percentage composition of stationary phase is 20%-80%, but the quality percentage composition of anti-phase is 80%-20%.
2. shape memory fiber is characterized in that: this shape memory fiber is to utilize urethane that claim 1 obtains to make by the method for wet-spinning or melt spinning.
3. shape memory yarn, it is characterized in that: described yarn is to be made of the described shape memory fiber of claim 2, the shape memory transition temperature of this yarn is-10 ℃~100 ℃.
4. shape memory yarn according to claim 3 is characterized in that: described yarn is pure monofilament yarn and/or the multifilament yarn of spinning.
5. shape memory yarn according to claim 3 is characterized in that: described yarn is the union yarn that shape memory fiber and other fiber are spun into.
6. shape memory yarn according to claim 5 is characterized in that: described other fiber is selected from one or more in cotton fibre, hair fibre, flaxen fiber, silk and the man-made fiber.
7. according to claim 5 or 6 described shape memory yarn, it is characterized in that: described union yarn is various Fancy Yarnss.
8. shape memory fabrics, it is characterized in that: described fabric is to be made of any described shape memory yarn among the claim 3-7.
9. shape memory fabrics according to claim 8 is characterized in that: described shape memory fabrics comprises uni-material fabric, BLENDED FABRIC and intertexture.
10. shape memory fabrics according to claim 8 is characterized in that: the shape memory transition temperature of described shape memory fabrics is-10 ℃~100 ℃.
11. a shape memory emulsion is characterized in that: described shape memory emulsion is to be made by the described shape memory polyurethane of claim 1.
12. a thin film shape memory is characterized in that: described thin film shape memory is to be made by the described shape memory polyurethane of claim 1.
13. a shape memory resin is characterized in that: described shape memory resin is to be made by the described shape memory polyurethane of claim 1.
14. a shape memory foam is characterized in that: described shape memory foam is to be made by the described shape memory polyurethane of claim 1.
15. a shape memory fabrics is characterized in that: described shape memory fabrics is common fabric to be put in order obtained by the described shape memory emulsion of claim 11-13, film, resin.
16. a shape memory fabrics is characterized in that: described shape memory fabrics is to adopt the described shape memory polyurethane fiber of claim 2, the described film of claim 12, the described resin of claim 13 or the described foam of claim 14 and common material to be processed into matrix material and make.
17. according to Claim 8,15 or 16 described shape memory fabrics, it is characterized in that this shape memory fabrics comprises the form of woven fabrics, knitted fabrics, supatex fabric, laminated fabric, coated fabric and compound fabric.
CN200610058886.0A 2006-03-08 2006-03-08 Shape memory polyurethane yarn and fabric Pending CN101033286A (en)

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