CN104073916A - Preparation method of temperature responsive fiber for window curtain - Google Patents
Preparation method of temperature responsive fiber for window curtain Download PDFInfo
- Publication number
- CN104073916A CN104073916A CN201410283302.4A CN201410283302A CN104073916A CN 104073916 A CN104073916 A CN 104073916A CN 201410283302 A CN201410283302 A CN 201410283302A CN 104073916 A CN104073916 A CN 104073916A
- Authority
- CN
- China
- Prior art keywords
- pvdf
- temperature
- preparation
- spinning
- doughnut
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Artificial Filaments (AREA)
Abstract
The invention discloses a preparation method of a temperature responsive hollow fiber for a window curtain. The preparation method comprises the following steps: (1), adding PVDF (Polyvinylidene Fluoride) powder according to a proportion of 100g/L to 180g/L into an alkali solution, then adding anhydrous ethyl alcohol according to a proportion of 14ml/L to 45ml/L into the alkali solution and stirring the mixtureso as to enable the PVDF powder to be dispersed in the solution sufficiently, placing the mixed solution into a water bath with a constant temperature of 50 to 80 DEG C, carrying out suction filtration after the chemical substances react for 10-20 minutes, and putting the PVDF powder obtained after washing into an oven at a temperature of 60 DEG C for drying; (2), preparing thermosensitive copolymer: adding the PVDF powder treated into three flasks, then adding DMF(dimethylformamide) for mixing, then adding NIPAAm (N-isopropylacrylamide) and an initiating agent AIBN, continuously stirring the mixture to allow the chemical substances to react for 8 to 12 hours after dissolution, adding methanol for precipitation after cooling, carrying out suction filtration, and performing pumping and drying after repeated cleaning with distilled water, so as to obtain thermosensitive PVDF-g-PNIPAAm copolymer; and (3), dissolving the PVDF-g-PNIPAAm, PAN (peroxyacetyl nitrate) and PEG (polyethylene glycol) into the solvent DMF, and spinning according to a conventional method. The preparation method provided by the invention has the advantages that the processing is simple, the cost is low, special equipment is not required, the spinning performance of obtained products is excellent, the spinning cost is low, and industrialized implementation is easy.
Description
Technical field
The present invention relates to a kind of intelligent chemical fibre, particularly a kind of temperature-responsive curtain fiber preparation method with moisture absorption, ventilative, sound absorption function.
Background technology
Intellectual material is a large focus of recent domestic new material research field, conventionally matrix material, sensitive components, actuating unit and message handler etc., partly consists of.Wherein actuating unit is extremely important member, and its major function is after perception environmental stimulus, can carry out appropriateness response by the geometric shape or other character that change self.Macromolecular material has the most typical feature of soft material, be easy to outfield to make response, so macromolecular material has irreplaceable effect in the research of intellectual material.
Temperature sensitivity macromolecular material is a hot issue in intelligent macromolecule material research in recent years.So-called profile of thermo sensitive polymers, refers to that it can produce response to the variations in temperature of environment, and, when ambient temperature changes, the character of material self changes thereupon.At present, studying more is vary with temperature and the gel rubber material that volume changes mutually occurs, and when environment temperature changes, gel volume can change thereupon; When meeting and exceeding certain critical-temperature, even can there is discontinuous sudden change, so-called volume changes mutually.This gel has a certain proportion of hydrophobic and hydrophilic radical, and the variation of temperature can affect the hydrophobic effect of these groups and the hydrogen bond action between macromolecular chain, thereby gel structure is changed, and volume phase transition occurs, and conventionally this temperature is called to phase transition temperature.The critical conversion temperature that volume changes is called low temperature critical solution temperature (lower critical solution temperature, LCST).
In recent years, along with improving constantly of living standards of the people and quality of life, curtain product is no longer unalterable " soft decoration ", the functionalization demand of curtain highlights just increasingly, modern science and technology strength is incorporated to curtain industry development, and development functionality curtain product has become the important directions of curtain industry development.
Therefore,, if the performance requirement of the temp. sensitive characteristic of temperature sensitive macromolecular material and Curtains Fabrics fiber is combined, be expected to develop a class New temperature response curtain fibrous material.In recent years, about the research of temperature sensitive fibrous material and report a lot, but how to develop a kind of temperature sensitive fibrous material, make its fabric there is the functions such as moisture absorption, ventilative, sound absorption, and can make response by the temperature variations to environment of living in, intelligent moisture absorption, ventilative, the sound absorption function controlled, is still a difficult problem at present.
Summary of the invention
The technical problem that quasi-solution of the present invention is determined is to provide a kind of temperature-responsive curtain fiber preparation method with moisture absorption, ventilative, sound absorption function.
Described temperature-responsive curtain fiber is temperature response type polyacrylonitrile (PAN) doughnut.Described doughnut preparation method is as follows:
(1) Kynoar (PVDF) powder alkali treatment; (2) preparation of temperature sensitive copolymer: the PVDF powder after alkali treatment and temperature sensitive monomer NIPA (NIPAAm) are carried out to copolymerization, synthetic PVDF-g-
pnIPAAm copolymer; (3) temperature response type PAN doughnut preparation.Specific as follows:
(1) PVDF powder alkali treatment.The PVDF powder that additional proportion is 100g/L-180g/L in aqueous slkali.In above-mentioned aqueous slkali, add 14ml/L～45ml/L absolute ethyl alcohol and stir subsequently, PVDF is fully disperseed in solution.Above-mentioned mixed solution reaction system is placed in to 50～80 ℃ of waters bath with thermostatic control, reacts 10～20 minutes.Suction filtration products therefrom, it is dry that the rear gained PVDF pulverulent solids product of washing is put into 60 ℃ of baking ovens.
In suction filtration product process, with distilled water, constantly wash, to remove fluoride and the ethanol in product.
Described aqueous slkali refers to a kind of in potassium hydroxide, NaOH or lithium hydroxide solution, and described alkaline concentration is 2 ~ 3mol/L.
(2) preparation of temperature sensitive copolymer.The PVDF powder of getting after alkali treatment adds in there-necked flask, logical nitrogen, then add DMF (DMF), stirring and dissolving under heating condition under 50～80 ℃ of water-baths.The in the situation that of logical nitrogen, add refining NIPA (NIPAAm), initator azodiisobutyronitrile (AIBN) in there-necked flask, after dissolving completely, logical nitrogen is 10～20 minutes again, continues stirring reaction and within 8～12 hours, can obtain temperature sensitive type PVDF-g-PNIPAAm copolymer.Reactant liquor is poured into from there-necked flask in beaker, added methanol extraction after cooling, suction filtration, rinses repeatedly with distilled water, to remove unreacted little molecule, then drains, and it is stand-by that gained copolymer p VDF-g-PNIPAAm product is put into 60 ℃ of oven dryings.
PVDF powder after described alkali treatment and the mass ratio of NIPAAm are 1:0.5 ~ 1.25, and the addition of described DMF (DMF) is 6 ~ 12 times of PVDF powder quality.The addition of described initator azodiisobutyronitrile (AIBN) is 1% ~ 2.5% of PVDF powder quality.
Described methyl alcohol addition is 10 ~ 25 times of PVDF powder quality.
(3) temperature response type PAN doughnut preparation.Thermo-sensitive PVDF-g-PNIPAAm copolymer, PAN and polyethylene glycol (PEG) are dissolved in DMF solvent, at the temperature of 40 ° of C ~ 70 ° C, add thermal agitation, then by spinning liquid standing 30-60 minute at the temperature of 40 ° of C ~ 70 ° C, be made into consoluet co-blended spinning feed liquid.Spinning liquid is poured in spinning machine still, sealing spinning machine still, heating spinning machine still, makes spinning liquid temperature at 25 ° of C ~ 50 ° C, and vacuumizing and defoaming is processed 20 ~ 60 minutes.
spinning liquidafter deaeration is disposed, open still gate out switch, in still, pass into nitrogen pressurization, open measuring pump switch, adjust 8 ~ 20 revs/min of rotating speeds, start spinning.After coagulating bath by the doughnut of extruding from spinnerets by 20 ° of C ~ 30 ° C, be wound up on take up roll, control 10 ~ 25 revs/min of take up roll rotating speeds.Coiler device is shut down, and takes off fiber, and the doughnut spinning out is soaked one week in distilled water, refreshes the water periodically; Doughnut is soaked in glycerine water solution 1 ~ 2 day, and taking-up is dried, and obtains temperature sensitive type PAN doughnut.
The mass ratio of described Thermo-sensitive PVDF-g-PNIPAAm copolymer and PAN is 1:3 ~ 1:1;
The mass ratio of the mixture of described PVDF-g-PNIPAAm copolymer and PAN in DMF is 15% ~ 20%;
The mass ratio of described PEG in DMF is 5% ~ 10%.
In coagulating bath water tank and core flow container, inject distilled water, coagulating bath water tank plays the freezing action of doughnut outer wall, and the core liquid in core flow container leads in doughnut inner tube, and fiber inwall is played to freezing action.
In described glycerine water solution, glycerine and water ratio are 1:1.
Film dry-wet spinning machine and attached coagulating bath water tank thereof and core flow container, nitrogen pot, drafting system etc. are connected before spinning.
The method is by first designing a kind of temperature response type PVDF copolymer, and then utilizes this copolymer and PAN blend, adopts dry-wet spinning technique preparation temperature response type doughnut, comprises the steps:
In the present invention, spinning technique is the chemical fibre spinning method that the feature of dry spinning and wet spinning is combined.The spinning speed of dry-wet spinning is high more than wet spinning, and can use the larger spinning head in aperture.High when spinning solution concentration and viscosity can resemble dry-spinning, can also more effectively control the structure-forming process of fiber.
beneficial effect:
The present invention is on the previous patent of inventor [ZL200910228657.2] and [ZL200910228658.7] basis, and the requirement for Curtains Fabrics with fiber, carries out blend by the temperature sensitive copolymer of PVDF-g-PNIPAAm and PAN, spins temperature sensitive PAN doughnut.With early stage patent compare, the present invention has realized the good fibroblast after PVDF-g-PNIPAAm and PAN blend, solved the spinnability requirement of the two blend, and spun doughnut size is tiny, moderate strength, can meets the performance requirements such as curtain weaving and dyeing arrangement.
The present invention early stage, patent adopted alkali treatment technology to be prepared into line polymer, and method is simple, cost is low, do not need special installation, industrializing implementation is easy; The temperature sensitive copolymer of PVDF-g-PNIPAAm that the present invention is synthetic and PAN blend fibre-forming performance, good spinning property; Therefore temperature response type PAN doughnut tube wall prepared by the present invention has microcellular structure, has the functions such as ventilative, sound absorption; In temperature response type PAN doughnut prepared by the present invention, owing to containing PNIPAAm, so fiber has certain hygroscopicity; Near doughnut prepared by the present invention tube wall pore size critical-temperature of 27 ℃～32 ℃ changes, thereby the performances such as moisture absorption, ventilative, sound absorption are changed thereupon, shows obvious temperature response characteristics.
The specific embodiment
The following examples can make the present invention of those skilled in the art comprehend, but do not limit the present invention in any way.
Embodiment 1:
(1) preliminary treatment of PVDF powder.The sodium hydroxide solution that preparation mol ratio is 2mol/L, pours this alkali lye of 350ml in beaker into, adds in this aqueous slkali of PVDF powder of 40g white, adds 5ml absolute ethyl alcohol more subsequently in reaction system, stirs, and PVDF is fully disperseed in solution.Reaction system is placed in to 50 ℃ of waters bath with thermostatic control, reacts 10 minutes.By products therefrom suction filtration, and constantly wash with distilled water, to remove NaF and the ethanol in product, finally gained pulverulent solids product after washing is put into 60 ℃ of baking oven dried for standby.
(2) preparation of temperature sensitive copolymer.The PVDF powder of getting after 10g alkali treatment adds in there-necked flask, logical nitrogen, then add 120ml solvent DMF, stirring and dissolving under heating condition under 50 ℃ of water-baths.Get the refining NIPAAm of 10g, 0.2g initiator A IBN joins in there-necked flask in the situation that of logical nitrogen, after dissolving completely, then leads to nitrogen 10 minutes, continues stirring reaction and within 8 hours, can obtain temperature sensitive type PVDF-g-PNIPAAm copolymer.Reactant liquor is poured into from there-necked flask in clean beaker, added about 250ml methanol extraction after cooling, suction filtration, rinses repeatedly with distilled water, to remove unreacted little molecule, then drains, and puts into 60 ℃ of oven dryings stand-by.
(3) preparation temperature response type PAN doughnut.By PVDF-g-PNIPAAm and PAN mass ratio 1:3, be made into blend, the PEG that is 6% by the blend of mass ratio 15% and mass ratio is dissolved in the DMF solvent of 1000mL, is mixed with spinning liquid, in course of dissolution, at the temperature of 60 ° of C, adds thermal agitation.Then spinning liquid is descended standing 30 minutes at the temperature of 60 ° of C, fully dissolve and be made into consoluet spinning liquid.Spinning liquid is poured in spinning machine still, by after still good seal, utilized circulation constant temperature device to heat still, spinning liquid temperature is controlled to 30 ° of C left and right, then vacuumize and carry out deaeration processing 30 minutes with vavuum pump.
In coagulating bath water tank and core flow container, inject distilled water, film dry-wet spinning machine and attached coagulating bath water tank thereof and core flow container, nitrogen pot, drafting system etc. are connected.After spinning liquid deaeration is disposed, open still gate out switch, in still, pass into nitrogen pressurization, open measuring pump switch, adjust 12 revs/min of rotating speeds, start spinning.After coagulating bath by the doughnut of extruding from spinnerets by 25 ° of C, be wound up on take up roll, control 15 revs/min of take up roll rotating speeds.After spinning finishes, coiler device is shut down, take off fiber, the doughnut spinning out is soaked one week in distilled water, refresh the water periodically, guarantee PEG to be dissolved out.The aqueous solution of the glycerine of configuration 1:1, soaks doughnut wherein 2 days, then takes out and dries, and obtains temperature sensitive type PAN doughnut.
Embodiment 2:
(1) preliminary treatment of PVDF powder.The potassium hydroxide solution that preparation mol ratio is 2mol/L, pours this alkali lye of 350ml in beaker into, adds in this aqueous slkali of PVDF powder of 60g white, adds 15ml absolute ethyl alcohol more subsequently in reaction system, stirs, and PVDF is fully disperseed in solution.Reaction system is placed in to 80 ℃ of waters bath with thermostatic control, reacts 20 minutes.By products therefrom suction filtration, and constantly wash with distilled water, to remove KF and the ethanol in product, finally gained pulverulent solids product after washing is put into 60 ℃ of baking oven dried for standby.
(2) preparation of temperature sensitive copolymer.The PVDF powder of getting after 20g alkali treatment adds in there-necked flask, logical nitrogen, then add 120ml solvent DMF, stirring and dissolving under heating condition under 80 ℃ of water-baths.Get the refining NIPAAm of 20g, 0.5g initiator A IBN joins in there-necked flask in the situation that of logical nitrogen, after dissolving completely, then leads to nitrogen 20 minutes, continues stirring reaction and within 12 hours, can obtain temperature sensitive type PVDF-g-PNIPAAm copolymer.Reactant liquor is poured into from there-necked flask in clean beaker, added about 250ml methanol extraction after cooling, suction filtration, rinses repeatedly with distilled water, to remove unreacted little molecule, then drains, and puts into 60 ℃ of oven dryings stand-by.
(3) preparation temperature response type PAN doughnut.By PVDF-g-PNIPAAm and PAN mass ratio 1:2, be made into blend, the PEG that is 8% by the blend of mass ratio 16% and mass ratio is dissolved in the DMF solvent of 1000mL, is mixed with spinning liquid, in course of dissolution, at the temperature of 60 ° of C, adds thermal agitation.Then spinning liquid is descended standing 30 minutes at the temperature of 60 ° of C, fully dissolve and be made into consoluet spinning liquid.Spinning liquid is poured in spinning machine still, by after still good seal, utilized circulation constant temperature device to heat still, spinning liquid temperature is controlled to 30 ° of C left and right, then vacuumize and carry out deaeration processing 30 minutes with vavuum pump.
In coagulating bath water tank and core flow container, inject distilled water, film dry-wet spinning machine and attached coagulating bath water tank thereof and core flow container, nitrogen pot, drafting system etc. are connected.After spinning liquid deaeration is disposed, open still gate out switch, in still, pass into nitrogen pressurization, open measuring pump switch, adjust 12 revs/min of rotating speeds, start spinning.After coagulating bath by the doughnut of extruding from spinnerets by 25 ° of C, be wound up on take up roll, control 15 revs/min of take up roll rotating speeds.After spinning finishes, coiler device is shut down, take off fiber, the doughnut spinning out is soaked one week in distilled water, refresh the water periodically, guarantee PEG to be dissolved out.The aqueous solution of the glycerine of configuration 1:1, soaks doughnut wherein 2 days, then takes out and dries, and obtains temperature sensitive type PAN doughnut.
Embodiment 3:
(1) preliminary treatment of PVDF powder.The sodium hydroxide solution that preparation mol ratio is 2mol/L, pours this alkali lye of 350ml in beaker into, adds in this aqueous slkali of PVDF powder of 50g white, adds 10ml absolute ethyl alcohol more subsequently in reaction system, stirs, and PVDF is fully disperseed in solution.Reaction system is placed in to 60 ℃ of waters bath with thermostatic control, reacts 20 minutes.By products therefrom suction filtration, and constantly wash with distilled water, to remove NaF and the ethanol in product, finally gained pulverulent solids product after washing is put into 60 ℃ of baking oven dried for standby.
(2) preparation of temperature sensitive copolymer.The PVDF powder of getting after 15g alkali treatment adds in there-necked flask, logical nitrogen, then add 120ml solvent DMF, stirring and dissolving under heating condition under 60 ℃ of water-baths.Get the refining NIPAAm of 15g, 0.2g initiator A IBN joins in there-necked flask in the situation that of logical nitrogen, after dissolving completely, then leads to nitrogen 20 minutes, continues stirring reaction and within 12 hours, can obtain temperature sensitive type PVDF-g-PNIPAAm copolymer.Reactant liquor is poured into from there-necked flask in clean beaker, added about 250ml methanol extraction after cooling, suction filtration, rinses repeatedly with distilled water, to remove unreacted little molecule, then drains, and puts into 60 ℃ of oven dryings stand-by.
(3) preparation temperature response type PAN doughnut.By PVDF-g-PNIPAAm and PAN mass ratio 1:1, be made into blend, the PEG that is 8% by the blend of mass ratio 16% and mass ratio is dissolved in the DMF solvent of 1000mL, is mixed with spinning liquid, in course of dissolution, at the temperature of 60 ° of C, adds thermal agitation.Then spinning liquid is descended standing 30 minutes at the temperature of 60 ° of C, fully dissolve and be made into consoluet PVDF-g-PNIPAAm spinning liquid.Spinning liquid is poured in spinning machine still, by after still good seal, utilized circulation constant temperature device to heat still, spinning liquid temperature is controlled to 35 ° of C left and right, then vacuumize and carry out deaeration processing 40 minutes with vavuum pump.
In coagulating bath water tank and core flow container, inject distilled water, film dry-wet spinning machine and attached coagulating bath water tank thereof and core flow container, nitrogen pot, drafting system etc. are connected.After spinning liquid deaeration is disposed, open still gate out switch, in still, pass into nitrogen pressurization, open measuring pump switch, adjust 13 revs/min of rotating speeds, start spinning.After coagulating bath by the doughnut of extruding from spinnerets by 30 ° of C, be wound up on take up roll, control 15 revs/min of take up roll rotating speeds.After spinning finishes, coiler device is shut down, take off fiber, the doughnut spinning out is soaked one week in distilled water, refresh the water periodically, guarantee PEG to be dissolved out.The aqueous solution of the glycerine of configuration 1:1, soaks doughnut wherein 2 days, then takes out and dries, and obtains temperature sensitive type PAN doughnut.
Embodiment 4:
(1) preliminary treatment of PVDF powder.The sodium hydroxide solution that preparation mol ratio is 3mol/L, pours this alkali lye of 350ml in beaker into, adds in this aqueous slkali of PVDF powder of 40g white, adds 5ml absolute ethyl alcohol more subsequently in reaction system, stirs, and PVDF is fully disperseed in solution.Reaction system is placed in to 50 ℃ of waters bath with thermostatic control, reacts 20 minutes.By products therefrom suction filtration, and constantly wash with distilled water, to remove NaF and the ethanol in product, finally gained pulverulent solids product after washing is put into 60 ℃ of baking oven dried for standby.
(2) preparation of temperature sensitive copolymer.The PVDF powder of getting after 20g alkali treatment adds in there-necked flask, logical nitrogen, then add 120ml solvent DMF, stirring and dissolving under heating condition under 60 ℃ of water-baths.Get the refining NIPAAm of 10g, 0.2g initiator A IBN joins in there-necked flask in the situation that of logical nitrogen, after dissolving completely, then leads to nitrogen 20 minutes, continues stirring reaction and within 12 hours, can obtain temperature sensitive type PVDF-g-PNIPAAm copolymer.Reactant liquor is poured into from there-necked flask in clean beaker, added about 250ml methanol extraction after cooling, suction filtration, rinses repeatedly with distilled water, to remove unreacted little molecule, then drains, and puts into 60 ℃ of oven dryings stand-by.
(3) preparation temperature response type PAN doughnut.By PVDF-g-PNIPAAm and PAN mass ratio 1:2.5, be made into blend, the PEG that is 10% by the blend of mass ratio 18% and mass ratio is dissolved in the DMF solvent of 1000mL, is mixed with spinning liquid, in course of dissolution, at the temperature of 60 ° of C, adds thermal agitation.Then spinning liquid is descended standing 30 minutes at the temperature of 60 ° of C, fully dissolve and be made into consoluet PVDF-g-PNIPAAm spinning liquid.Spinning liquid is poured in spinning machine still, by after still good seal, utilized circulation constant temperature device to heat still, spinning liquid temperature is controlled to 35 ° of C left and right, then vacuumize and carry out deaeration processing 40 minutes with vavuum pump.
In coagulating bath water tank and core flow container, inject distilled water, film dry-wet spinning machine and attached coagulating bath water tank thereof and core flow container, nitrogen pot, drafting system etc. are connected.After spinning liquid deaeration is disposed, open still gate out switch, in still, pass into nitrogen pressurization, open measuring pump switch, adjust 12 revs/min of rotating speeds, start spinning.After coagulating bath by the doughnut of extruding from spinnerets by 25 ° of C, be wound up on take up roll, control 15 revs/min of take up roll rotating speeds.After spinning finishes, coiler device is shut down, take off fiber, the doughnut spinning out is soaked one week in distilled water, refresh the water periodically, guarantee PEG to be dissolved out.The aqueous solution of the glycerine of configuration 1:1, soaks doughnut wherein 2 days, then takes out and dries, and obtains temperature sensitive type PAN doughnut.
Embodiment 5:
(1) preliminary treatment of PVDF powder.The sodium hydroxide solution that preparation mol ratio is 2.5mol/L, pours this alkali lye of 350ml in beaker into, adds in this aqueous slkali of PVDF powder of 40g white, adds 12ml absolute ethyl alcohol more subsequently in reaction system, stirs, and PVDF is fully disperseed in solution.Reaction system is placed in to 60 ℃ of waters bath with thermostatic control, reacts 20 minutes.By products therefrom suction filtration, and constantly wash with distilled water, to remove NaF and the ethanol in product, finally gained pulverulent solids product after washing is put into 60 ℃ of baking oven dried for standby.
(2) preparation of temperature sensitive copolymer.The PVDF powder of getting after 12g alkali treatment adds in there-necked flask, logical nitrogen, then add 120ml solvent DMF, stirring and dissolving under heating condition under 60 ℃ of water-baths.Get the refining NIPAAm of 10～20g, 0.3g initiator A IBN joins in there-necked flask in the situation that of logical nitrogen, after dissolving completely, then leads to nitrogen 20 minutes, continues stirring reaction and within 12 hours, can obtain temperature sensitive type PVDF-g-PNIPAAm copolymer.Reactant liquor is poured into from there-necked flask in clean beaker, added about 250ml methanol extraction after cooling, suction filtration, rinses repeatedly with distilled water, to remove unreacted little molecule, then drains, and puts into 60 ℃ of oven dryings stand-by.
(3) preparation temperature response type PAN doughnut.By PVDF-g-PNIPAAm and PAN mass ratio 1:2.5, be made into blend, the PEG that is 8% by the blend of mass ratio 16% and mass ratio is dissolved in the DMF solvent of 1000mL, is mixed with spinning liquid, in course of dissolution, at the temperature of 60 ° of C, adds thermal agitation.Then spinning liquid is descended standing 30 minutes at the temperature of 60 ° of C, fully dissolve and be made into consoluet PVDF-g-PNIPAAm spinning liquid.Spinning liquid is poured in spinning machine still, by after still good seal, utilized circulation constant temperature device to heat still, spinning liquid temperature is controlled to 35 ° of C left and right, then vacuumize and carry out deaeration processing 60 minutes with vavuum pump.
In coagulating bath water tank and core flow container, inject distilled water, film dry-wet spinning machine and attached coagulating bath water tank thereof and core flow container, nitrogen pot, drafting system etc. are connected.After spinning liquid deaeration is disposed, open still gate out switch, in still, pass into nitrogen pressurization, open measuring pump switch, adjust 15 revs/min of rotating speeds, start spinning.After coagulating bath by the doughnut of extruding from spinnerets by 28 ° of C, be wound up on take up roll, control 18 revs/min of take up roll rotating speeds.After spinning finishes, coiler device is shut down, take off fiber, the doughnut spinning out is soaked one week in distilled water, refresh the water periodically, guarantee PEG to be dissolved out.The aqueous solution of the glycerine of configuration 1:1, soaks doughnut wherein 2 days, then takes out and dries, and obtains temperature sensitive type PAN doughnut.
Claims (5)
1. the preparation method of temperature response type doughnut for curtain, is characterized in that comprising the steps:
(1) PVDF powder alkali treatment, the PVDF powder that additional proportion is 100g/L-180g/L in aqueous slkali, in above-mentioned aqueous slkali, add 14ml/L～45ml/L absolute ethyl alcohol and stir subsequently, PVDF is fully disperseed in solution, above-mentioned mixed solution reaction system is placed in to 50～80 ℃ of waters bath with thermostatic control, react 10～20 minutes, suction filtration products therefrom, it is dry that the rear gained PVDF pulverulent solids product of washing is put into 60 ℃ of baking ovens;
(2) preparation of temperature sensitive copolymer, the PVDF powder of getting after alkali treatment adds in there-necked flask, logical nitrogen, add again N, dinethylformamide (DMF), stirring and dissolving under heating condition under 50～80 ℃ of water-baths, the in the situation that of logical nitrogen, add refining NIPA (NIPAAm), initator azodiisobutyronitrile (AIBN) in there-necked flask, after dissolving completely, logical nitrogen is 10～20 minutes again, continues stirring reaction and within 8～12 hours, can obtain temperature sensitive type PVDF-g-PNIPAAm copolymer;
Reactant liquor is poured into from there-necked flask in beaker, added methanol extraction after cooling, suction filtration, rinses repeatedly with distilled water, to remove unreacted little molecule, then drains, and it is stand-by that gained copolymer p VDF-g-PNIPAAm product is put into 60 ℃ of oven dryings;
(3) temperature response type PAN doughnut preparation, Thermo-sensitive PVDF-g-PNIPAAm copolymer, PAN and polyethylene glycol (PEG) are dissolved in DMF solvent, at the temperature of 40 ° of C ~ 70 ° C, add thermal agitation, then by spinning liquid standing 30-60 minute at the temperature of 40 ° of C ~ 70 ° C, be made into consoluet co-blended spinning feed liquid; Spinning liquid is poured in spinning machine still, sealing spinning machine still, heating spinning machine still, makes spinning liquid temperature at 25 ° of C ~ 50 ° C, and vacuumizing and defoaming is processed spinning after 20 ~ 60 minutes.
2. the preparation method of temperature response type doughnut for curtain as claimed in claim 1, is characterized in that: described aqueous slkali refers to a kind of in potassium hydroxide, NaOH or lithium hydroxide solution, and described alkaline concentration is 2 ~ 3mol/L.
3. the preparation method of temperature response type doughnut for curtain as claimed in claim 1, it is characterized in that: the PVDF powder after described alkali treatment and the mass ratio of NIPAAm are 1:0.5 ~ 1.25, described N, the addition of dinethylformamide (DMF) is 6 ~ 12 times of PVDF powder quality, and the addition of described initator azodiisobutyronitrile (AIBN) is 1% ~ 2.5% of PVDF powder quality; Described methyl alcohol addition is 10 ~ 25 times of PVDF powder quality.
4. the preparation method of temperature response type doughnut for curtain as claimed in claim 1, is characterized in that: the mass ratio of described Thermo-sensitive PVDF-g-PNIPAAm copolymer and PAN is 1:3 ~ 1:1;
The mass ratio of the mixture of described PVDF-g-PNIPAAm copolymer and PAN in DMF is 15% ~ 20%;
The mass ratio of described PEG in DMF is 5% ~ 10%.
5. the preparation method of temperature response type doughnut for curtain as claimed in claim 1, is characterized in that: described sweet
In oil solution, glycerine and water ratio are 1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410283302.4A CN104073916A (en) | 2014-06-24 | 2014-06-24 | Preparation method of temperature responsive fiber for window curtain |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410283302.4A CN104073916A (en) | 2014-06-24 | 2014-06-24 | Preparation method of temperature responsive fiber for window curtain |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104073916A true CN104073916A (en) | 2014-10-01 |
Family
ID=51595507
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410283302.4A Pending CN104073916A (en) | 2014-06-24 | 2014-06-24 | Preparation method of temperature responsive fiber for window curtain |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104073916A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088767A (en) * | 2015-08-05 | 2015-11-25 | 贵州大学 | Temperature-sensitive cotton fiber preparation method |
| CN108374223A (en) * | 2018-03-14 | 2018-08-07 | 江苏圣澜服饰创意有限公司 | Renewable temperature sensitive textile fabric of one kind and preparation method thereof |
| CN116657289A (en) * | 2023-08-01 | 2023-08-29 | 江苏恒力化纤股份有限公司 | Preparation method of thermosensitive polyester yarns |
-
2014
- 2014-06-24 CN CN201410283302.4A patent/CN104073916A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088767A (en) * | 2015-08-05 | 2015-11-25 | 贵州大学 | Temperature-sensitive cotton fiber preparation method |
| CN108374223A (en) * | 2018-03-14 | 2018-08-07 | 江苏圣澜服饰创意有限公司 | Renewable temperature sensitive textile fabric of one kind and preparation method thereof |
| CN116657289A (en) * | 2023-08-01 | 2023-08-29 | 江苏恒力化纤股份有限公司 | Preparation method of thermosensitive polyester yarns |
| CN116657289B (en) * | 2023-08-01 | 2023-11-24 | 江苏恒力化纤股份有限公司 | Preparation method of thermosensitive polyester yarns |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100381621C (en) | Method of in situ encapsulation preparing phase-change energy-storage fibre | |
| CN106555248B (en) | The preparation method of moisture absorption acrylic fibers | |
| CN103243588B (en) | A kind of method of Polyester Textiles high-temperature pressure dyeing | |
| CN103409837B (en) | The method of water-soluble polyvinyl alcohol fibers prepared by a kind of melt spinning | |
| CN108221081B (en) | High-strength carboxymethyl cellulose/sodium alginate blend fiber and preparation method thereof | |
| SE544547C2 (en) | A process for wet spinning of cellulose fibers from an alkaline spin bath | |
| CN103055724B (en) | Method for preparing polysulfones polymer microporous membrane by counter-current thermally induced phase separation method | |
| CN101429682A (en) | Method for producing regenerated cellulose fiber by dual-bath coagulation | |
| CN104073916A (en) | Preparation method of temperature responsive fiber for window curtain | |
| CN101942705B (en) | Preparation method of regenerated bacterial cellulose fiber | |
| CN101240468A (en) | Polyacrylonitrile-chitin composite fiber and its production process | |
| CN104047067B (en) | A kind of cellulose dissolution agent and application thereof | |
| CN104073907A (en) | Polyester fiber and preparation method thereof | |
| CN104060346A (en) | Hollow fiber for temperature response type curtain | |
| CN101696517B (en) | Method for manufacturing adsorption transfer fiber | |
| CN102877288A (en) | Preparation method of halamine-containing antibacterial polyacrylonitrile fiber | |
| CN101711951B (en) | Method for preparing fiber separation film | |
| TW201816211A (en) | Modified acrylonitrile-based fiber, method for manufacturing fiber of the same, and fiber structure containing fiber thereof | |
| CN103741249B (en) | large-diameter polyvinyl alcohol monofilament and production method thereof | |
| CN105463607A (en) | Manufacturing method for 48K polyacrylonitrile-based carbon fiber precursor | |
| CN102912474B (en) | Composite fiber and preparation method thereof | |
| CN107325303B (en) | Degumming-free silk fiber solution, preparation method and application thereof | |
| CN110541304A (en) | preparation method of single-sided hydrophilic modified polyester fabric | |
| CN101985086A (en) | Temperature response hollow fiber separation membrane | |
| CN105544193B (en) | The hydrophilic modification method of a kind of bromoethane and PVA to polyester fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141001 |
|
| WD01 | Invention patent application deemed withdrawn after publication |