CN110656397A - Preparation method of photochromic modified polyester fiber - Google Patents
Preparation method of photochromic modified polyester fiber Download PDFInfo
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- CN110656397A CN110656397A CN201911156140.7A CN201911156140A CN110656397A CN 110656397 A CN110656397 A CN 110656397A CN 201911156140 A CN201911156140 A CN 201911156140A CN 110656397 A CN110656397 A CN 110656397A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention provides a preparation method of a photochromic modified polyester fiber, which comprises the steps of firstly encapsulating nano photochromic powder in cellular inorganic substance or organic polymer micropores to prepare photochromic powder microcapsules, mixing and granulating the photochromic powder microcapsules with low-melting-point modified polyester chips, polyester toughening agent, antioxidant and coupling agent to obtain photochromic powder microcapsule solid master batches, then pre-crystallizing the prepared photochromic powder microcapsule solid master batches, uniformly mixing the obtained mixture with the modified polyester chips, extruding and melting the obtained mixture to obtain a melt, filtering, homopolymerizing and pressurizing the melt, finally sending the melt into a spinning assembly, oiling, balancing, winding and drafting the obtained product after spinning cooling and blowing to obtain the photochromic modified polyester fiber. The invention adopts microporous inorganic polymer or microporous organic polymer as packaging material, selects low-melting-point modified polyester to improve the fluidity of the melt, increases the toughness of the fiber, and solves the defects of instability of light fastness, washing fastness and the like.
Description
Technical Field
The invention relates to the technical field of photochromic modified polyester fibers, in particular to a preparation method of a photochromic modified polyester fiber.
Technical Field
The photochromic material is a novel functional material which is newly appeared internationally in recent years, is tasteless and nontoxic, cannot cause harm to human bodies, and cannot cause pollution to the environment. The new material is firstly used in high and new technical fields such as optical information storage and the like, and the application of the new material in the field of textile and clothing is gradually concerned at home and abroad in recent years. Photochromic textiles refer to fibers that exhibit different colors as a function of external environmental conditions (e.g., light, heat, pressure, moisture, etc.), such as photochromic fibers, thermochromic fibers, electrochromic fibers, and the like.
The photochromic fiber has photochromic property, i.e. the fiber changes color under the irradiation of light with certain wavelength, and the light reversibly changes back to the original color after disappearing. The advent of photochromic fibers has satisfied the consumer's quest for apparel color novelty, diversity, and variability. The preparation of the photochromic fiber is divided into a stock solution spinning method and a chemical modification method at present.
The dope spinning method is a method of uniformly dispersing a photochromic substance in a spinning solution of various chemical fibers to prepare a photochromic fiber. The method has the advantages of simple preparation method, no special requirements on the chemical structure of the photochromic dye and the like. Research on photochromic polypropylene fibers [ J ] synthetic fibers, 1998, 27 (5): 20-23. the photochromic material and polypropylene slice (PP) are blended to prepare slices, two photochromic polypropylene fibers with good performance are prepared by a melt spinning method, and after being irradiated by sunlight, one is changed from white to blue, and the other is changed from yellow (adding yellow master batch) to green. Experiments show that the mechanical property of the polypropylene fiber is not greatly influenced by adding a proper amount of photochromic dye. The photochromic polypropylene fiber has the color change effect which is not influenced by soap washing, but the color change durability is not ideal enough and needs to be improved.
The photochromic fiber prepared by chemically modifying raw materials is prepared by chemically modifying a fiber matrix by using a photochromic dye before fiber forming, so that the formed photochromic fiber has the advantages of common chemical methods, and compared with the formed fiber chemical modification, the photochromic fiber has the advantages of uniform dispersion of the photochromic dye in the fiber matrix by using a mechanical method, and the like.
Therefore, researchers are paying more attention to the solution of the problems that the photochromic material is poor in stability and oxidation resistance, low in fatigue resistance, slow in color development and color reduction due to environmental influences, large in particle size and the like.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a photochromic fiber production process, overcomes the defects that in the production process of the prior preparation process, photochromic materials are decomposed and lose efficacy when being heated, and chemical additives such as acidity and alkalinity can make the photochromic materials lose part or all of photochromic performance, and also solves the unstable factors such as light fastness, washing fastness and the like of photochromic fiber textiles in the later period.
The invention also aims to provide a photochromic modified polyester fiber product prepared by the preparation method of the photochromic modified polyester fiber.
The preparation method of the photochromic modified polyester fiber is characterized by comprising the following steps:
step 1: preparing photochromic powder microcapsule solid master batch: uniformly mixing nano photochromic powder with a high-molecular cross-linking agent and a dispersing agent, and then encapsulating the mixture in cellular inorganic matter or organic polymer micropores to prepare photochromic powder microcapsules, and then mixing and granulating the high-concentration photochromic powder microcapsules with low-melting-point modified polyester chips, a polyester toughening agent, an antioxidant and a coupling agent to obtain photochromic powder microcapsule solid master batches;
step 2: pre-crystallization: placing the prepared photochromic powder microcapsule solid master batch in a dry environment with ventilation for pre-crystallization;
and step 3: screw extrusion: uniformly mixing the pre-crystallized photochromic powder microcapsule solid master batch with modified polyester chips, a catalyst, an antioxidant and a stabilizer, and then sending the mixture into a screw extruder for extrusion and melting to obtain a melt;
and 4, step 4: and (3) filtering: filtering, homopolymerizing and pressurizing a melt after being extruded and melted by a screw extruder to ensure continuous production of spinning and constant melt pressure;
and 5: melt spinning: and (3) delivering the melt from the filter into a spinning assembly, spraying the melt from a spinneret plate through the spinning assembly, cooling and blowing the melt, and oiling, balancing, winding and drafting the cooled and blown melt to obtain the photochromic modified polyester fiber.
Preferably, the photochromic powder is a mixture of rare earth ore powder and original photosensitive powder OP powder, the cellular inorganic substance is one of ceramic powder, silicon dioxide, silicate rock and carbon powder, the polyester toughening agent is a polyolefin copolymer and/or graft copolymer with a reaction functional group, and the coupling agent is a zirconium coupling agent, a magnesium coupling agent and a tin coupling agent.
Preferably, the preparation method of the modified polyester chip in the step 1 comprises the following steps: selecting one or more of polyester fibers PBT, PTT and PET, mixing uniformly, then carrying out esterification reaction and prepolymerization reaction in sequence, and simultaneously adding a third or fourth component of dibasic acid and a dihydric alcohol monomer in the polyester polymerization process for copolymerization to obtain copolyester chips with the melting point range of 140-190 ℃; wherein:
the esterification reaction is carried out in two stages, wherein the esterification reaction temperature of the first stage is 170 ~ 200 ℃, the reaction time is 1 ~ 3h, the esterification reaction temperature of the second stage is 200 ~ 270 ℃, the reaction time is 1 ~ 2h, and the reaction pressure is normal pressure, the prepolymerization reaction is carried out in two stages, the reaction temperature of the first stage is 240 ~ 260 ℃, the reaction time is 0.5 ~ 1h, the reaction pressure is 1kpa ~ 10kpa absolute, the reaction temperature of the second stage is 250 ~ 270 ℃, the reaction time is 0.5 ~ 1h, and the reaction pressure is 500 ~ 1000pa absolute.
Preferably, the third component is aliphatic dibasic acid or aromatic dibasic acid, and the fourth component is butanediol, neopentyl glycol, hexanediol, cyclohexanedimethanol or polyethylene glycol.
Preferably, the high-concentration photosensitive color-changing powder microcapsules in the step 1 account for 99-99.9 Wt% of the total mass, and the balance is low-melting-point modified polyester chips, a polyester toughening agent, an antioxidant and a coupling agent.
Preferably, in the step 2, the pre-crystallization temperature is 120-125 ℃, the temperature of the hot air for drying is 110-140 ℃, the dew point of the air is less than or equal to 60 ℃, the water content of the material is 30ppm, and the drying time is 4-10 hours.
Preferably, the catalyst in step 3 is a metal oxide catalyst, a complex catalyst and/or a rare earth catalyst, the antioxidant is phosphate, catechol phosphate and/or terpene phenol, and the stabilizer is phosphoric acid, phosphorous acid or their ester derivatives.
Preferably, in the step 3, the photochromic powder microcapsule solid master batch occupies 2-10 Wt% of the total mass, the modified polyester occupies 89-97.9 Wt% of the total mass, and the balance is a catalyst, an antioxidant and a stabilizer.
Preferably, the pressure before filtration in the step 4 is less than or equal to 16Mpa, the pressure in the filtration process is constant at 8.5Mpa, and the filtration precision is 20-60 microns.
Preferably, the spinneret plate in the step 5 is a circular or special-shaped spinneret hole, the spinning assembly is a filter screen of 30/120/150/400/250/400 meshes, the spinning temperature is 180-220 ℃, the spinning speed is 1000-2000 m/min, the wind speed of cooling air blowing is 0.4-0.6 m/s, the wind temperature is 23-25 ℃, and the relative humidity is 70-80%.
A photochromic modified polyester fiber product prepared by the preparation method of the photochromic modified polyester fiber.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts the honeycomb-shaped porous and microporous inorganic polymer or organic polymer micropores as the packaging material, has convenient addition and good compatibility, and overcomes the difficulties of addition, quantification, dispersion and the like in the plastic modification processing process.
2. Mixing the high-concentration photosensitive color-changing powder microcapsule with low-melting-point modified polyester chips, a polyester toughening agent, an antioxidant, a coupling agent and the like for granulation. The addition is convenient, the quantification is accurate, and the dispersion is uniform. High stability and holding power.
3. One or more of modified polyester PBT, PTT or PET with low melting point is selected for mixing, so that the melting point is reduced, the fluidity of a melt is improved, the toughness of the fiber is improved, the crystallization speed is improved, and the crystallinity is high, which means excellent processing performance, thereby solving the problems that in the prior art, the photochromic material is decomposed and loses efficacy by heating in the production process, and chemical additives such as acidity and alkalinity can ensure that the photochromic material loses part or all of photochromic performance, and also solving the unstable factors such as light fastness, washing fastness and the like of the photochromic fiber textile in the later period.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, the present invention will be further described in detail with reference to the following detailed description.
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, the raw materials used are commercially available, and the percentage symbol "%" referred to in the present invention means mass percent unless otherwise specified.
Example 1:
the embodiment provides a preparation method of a modified polyester chip, which comprises the following steps:
selecting polyester fiber PBT, stirring uniformly, then carrying out esterification reaction and prepolymerization reaction in sequence, and simultaneously adding aliphatic dibasic acid, butanediol and neopentyl glycol to copolymerize with the polyester fiber PBT in the polyester polymerization process to obtain copolyester chips with the melting point range of 140-190 ℃, wherein:
the esterification reaction is carried out in two stages: the first stage esterification reaction temperature is 170 ℃, the reaction time is 1h, the second stage esterification reaction temperature is 200 ℃, the reaction time is 1h, and the reaction pressure is normal pressure;
the prepolymerization reaction is carried out in two stages: the reaction temperature of the first stage is 240 ℃, the reaction time is 0.5 h, and the reaction pressure is 1kpa absolute; the reaction temperature in the second stage is 250 ℃, the reaction time is 0.5 h, and the reaction pressure is 500pa absolute.
Example 2:
the embodiment provides a preparation method of a modified polyester chip, which comprises the following steps:
uniformly mixing polyester fibers PBT, PTT and PET, then carrying out esterification reaction and prepolymerization reaction in sequence, and simultaneously adding aromatic dibasic acid, hexanediol, cyclohexanedimethanol and polyethylene glycol to copolymerize with the polyester fibers in the polyester polymerization process to obtain copolyester chips with the melting point range of 140-190 ℃, wherein:
the esterification reaction is carried out in two stages: the first stage esterification reaction temperature is 200 ℃, the reaction time is 3 hours, the second stage esterification reaction temperature is 270 ℃, the reaction time is 2 hours, and the reaction pressure is normal pressure;
the prepolymerization reaction is carried out in two stages: the reaction temperature of the first stage is 260 ℃, the reaction time is 1h, and the reaction pressure is 10kpa absolute; the reaction temperature in the second stage is 270 ℃, the reaction time is 1h, and the reaction pressure is 1000pa absolute pressure.
Example 3
The embodiment provides a preparation method of a photochromic modified polyester fiber, which comprises the following steps:
step 1, uniformly mixing a mixture of rare earth ore powder and original photosensitive powder OP powder with a high-molecular cross-linking agent and a dispersing agent, and then encapsulating the mixture in micropores of a mixture of honeycomb ceramic powder and silicon dioxide to prepare a photochromic powder microcapsule, and then mixing and granulating the photochromic powder microcapsule with the low-melting-point modified polyester chips prepared in the embodiment 1, a polyester toughening agent, an antioxidant polyethylene and a zirconium coupling agent to obtain photochromic powder microcapsule solid master batch;
step 2, pre-crystallizing the prepared photochromic powder microcapsule solid master batch by adopting dry air; during pre-crystallization, the pre-crystallization temperature is 120 ℃, the temperature of hot drying air is 110 ℃, the dew point of the air is 40 ℃, the water content of the material is 30ppm, and the drying time is 4 hours.
Step 3, uniformly mixing the pre-crystallized photochromic powder microcapsule solid master batch with the low-melting-point modified polyester chip, the metal oxide catalyst, the antioxidant polyethylene, the phosphoric acid and the phosphorous acid, and feeding the mixture into a screw extruder through a special master batch feeder capable of metering the master batches;
wherein, the photochromic powder microcapsule solid master batch in the mixture accounts for 2Wt% of the total mass, the modified polyester accounts for 97.9Wt% of the total mass, and the balance is metal oxide catalyst, antioxidant polyethylene, phosphoric acid and phosphorous acid;
step 4, filtering the mixture extruded by the extruder, and ensuring the continuous production of spinning and the constant pressure of the screw extruder during the filtering; the pressure before filtration is less than or equal to 16Mpa, the constant pressure in the filtration process is 8.5Mpa, and the filtration precision of the filter used in the filtration is 20 microns.
And 5, feeding the mixture discharged from the filter into a spinning assembly, carrying out melt spinning at the temperature of 180 ℃ and spraying the mixture from a spinneret plate through the spinning assembly at the spinning speed of 1000m/min, cooling, oiling, balancing, winding and drafting to obtain the photochromic modified polyester fiber, wherein:
the spinneret orifices of the spinneret plate are round spinneret orifices, the spinning component is a filter screen of 30/120/150/400/250/400 meshes, the wind speed of cooling air blowing is 0.4 m/s, the wind temperature is 23 ℃, and the relative humidity is 70%.
Example 4:
the embodiment provides a preparation method of a photochromic modified polyester fiber, which comprises the following steps:
step 1, uniformly mixing a mixture of rare earth ore powder and original photosensitive powder OP powder with a high-molecular cross-linking agent and a dispersing agent, and then encapsulating the mixture in micropores of a mixture of honeycomb ceramic powder and silicon dioxide to prepare a photochromic powder microcapsule, and mixing and granulating the photochromic powder microcapsule with the low-melting-point modified polyester chips prepared in the embodiment 1, a polyester toughening agent, an antioxidant and a zirconium coupling agent to obtain photochromic powder microcapsule solid master batches;
step 2, pre-crystallizing the prepared photochromic powder microcapsule solid master batch by adopting dry air; during pre-crystallization, the pre-crystallization temperature is 125 ℃, the temperature of hot drying air is 140 ℃, the dew point of the air is 60 ℃, the water content of the material is 30ppm, and the drying time is 10 hours.
Step 3, uniformly mixing the pre-crystallized photochromic powder microcapsule solid master batch with the low-melting-point modified polyester chip, the metal oxide catalyst, the phosphate, the catechol phosphate, the phosphoric acid and the phosphorous acid, and feeding the mixture into a screw extruder through a special master batch feeder capable of metering the master batches;
wherein, the photochromic powder microcapsule solid master batch in the mixture accounts for 10Wt% of the total mass, the modified polyester accounts for 89 Wt% of the total mass, and the balance is metal oxide catalyst, phosphate, catechol phosphate, phosphoric acid and phosphorous acid;
step 4, filtering the mixture extruded by the extruder, and ensuring the continuous production of spinning and the constant pressure of the screw extruder during the filtering; the pressure before filtration is less than or equal to 16Mpa, the constant pressure in the filtration process is 8.5Mpa, and the filtration precision of the filter used in the filtration is 20 microns.
And 4, enabling the mixture discharged from the filter to enter a spinning assembly for melt spinning, wherein the temperature during spinning is 180 ℃, the mixture is sprayed out from a spinneret plate through the spinning assembly, the spinning speed is 1000m/min, and the mixture is cooled and then subjected to oiling, balancing, winding and drafting post-treatment to obtain the photochromic modified polyester fiber, wherein:
the spinneret orifices of the spinneret plate are round spinneret orifices, the spinning component is a filter screen with 30/120/150/400/250/400 meshes, the wind speed of cooling air blowing is 0.6m/s, the wind temperature is 25 ℃, and the relative humidity is 80%.
Example 5:
the embodiment provides a preparation method of a photochromic modified polyester fiber, which comprises the following steps:
step 1, uniformly mixing a mixture of rare earth ore powder and original photosensitive powder OP powder with a high-molecular cross-linking agent and a dispersing agent, and then encapsulating the mixture in micropores of a mixture of honeycomb-shaped silicate rock and carbon powder to prepare a photochromic powder microcapsule, and mixing and granulating the photochromic powder microcapsule with the low-melting-point modified polyester chips prepared in the embodiment 2, a polyester toughening agent, an antioxidant and a zirconium coupling agent to obtain photochromic powder microcapsule solid master batches;
step 2, pre-crystallizing the prepared photochromic powder microcapsule solid master batch by adopting dry air; during pre-crystallization, the pre-crystallization temperature is 122 ℃, the temperature of hot drying air is 120 ℃, the dew point of the air is 55 ℃, the water content of the material is 30ppm, and the drying time is 6 hours.
Step 3, uniformly mixing the pre-crystallized photochromic powder microcapsule solid master batch with low-melting-point modified polyester chips, rare earth catalyst, catechol phosphate, phosphoric acid, phosphorous acid and the like, and feeding the mixture into a screw extruder through a special master batch feeder capable of metering the master batches;
wherein, the photochromic powder microcapsule solid master batch in the mixture accounts for 5Wt% of the total mass, the modified polyester accounts for 92Wt% of the total mass, and the balance is rare earth catalyst, catechol phosphate, phosphoric acid and phosphorous acid;
step 4, filtering the mixture extruded by the extruder, and ensuring the continuous production of spinning and the constant pressure of the screw extruder during the filtering; the pressure before filtration was 10 MPa, the constant pressure during filtration was 8.5MPa, and the filtration precision of the filter used during filtration was 60 μm.
And 5, feeding the mixture discharged from the filter into a spinning assembly, carrying out melt spinning at the temperature of 180 ℃ and spraying the mixture from a spinneret plate through the spinning assembly at the spinning speed of 1000m/min, cooling, oiling, balancing, winding and drafting to obtain the photochromic modified polyester fiber, wherein:
the spinneret orifices of the spinneret plate are round spinneret orifices, the spinning component is a filter screen with 30/120/150/400/250/400 meshes, the wind speed of cooling air blowing is 0.5 m/s, the wind temperature is 24 ℃, and the relative humidity is 75%.
Example 6:
the embodiment provides a preparation method of a photochromic modified polyester fiber, which comprises the following steps:
step 1, uniformly mixing a mixture of rare earth ore powder and original photosensitive powder OP powder with a high-molecular cross-linking agent and a dispersing agent, and then encapsulating the mixture in micropores of a honeycomb ceramic powder mixture to prepare a photochromic powder microcapsule, and mixing and granulating the photochromic powder microcapsule with the low-melting-point modified polyester chips prepared in the embodiment 1, a polyester toughening agent, phosphate and a zirconium coupling agent to obtain photochromic powder microcapsule solid master batch;
step 2, pre-crystallizing the prepared photochromic powder microcapsule solid master batch by adopting dry air; and during pre-crystallization, the pre-crystallization temperature is 120-125 ℃, the temperature of hot drying air is 110-140 ℃, the dew point of the air is less than or equal to 60 ℃, the water content of the material is 30ppm, and the drying time is 4-10 hours.
Step 3, uniformly mixing the pre-crystallized photochromic powder microcapsule solid master batch with the low-melting-point modified polyester chip, a catalyst, phosphate, a stabilizer and the like, and feeding the mixture into a screw extruder through a special master batch feeder capable of metering the master batch;
wherein, the photochromic powder microcapsule solid master batch in the mixture accounts for 5Wt% of the total mass, the modified polyester accounts for 93 Wt% of the total mass, and the balance is a complex catalyst, a rare earth catalyst, phosphate, catechol phosphate and phosphorous acid;
step 4, filtering the mixture extruded by the extruder, and ensuring the continuous production of spinning and the constant pressure of the screw extruder during the filtering; the pressure before filtration is 16MPa, the constant pressure during filtration is 8.5MPa, and the filtration precision of the filter used during filtration is 40 microns.
And 5, feeding the mixture discharged from the filter into a spinning assembly, carrying out melt spinning at the temperature of 180 ℃ and spraying the mixture from a spinneret plate through the spinning assembly at the spinning speed of 1000m/min, cooling, oiling, balancing, winding and drafting to obtain the photochromic modified polyester fiber, wherein:
the spinneret orifices of the spinneret plate are round spinneret orifices, the spinning component is a filter screen of 30/120/150/400/250/400 meshes, the wind speed of cooling air blowing is 0.6m/s, the wind temperature is 25 ℃, and the relative humidity is 70%.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. The preparation method of the photochromic modified polyester fiber is characterized by comprising the following steps:
step 1, preparing photochromic powder microcapsule solid master batch: uniformly mixing nano photochromic powder with a high-molecular cross-linking agent and a dispersing agent, encapsulating the mixture in a honeycomb inorganic substance or a Microporous Organic Polymer (MOPs) to prepare photochromic powder microcapsules, and mixing and granulating the photochromic powder microcapsules with low-melting-point modified polyester chips, a polyester toughening agent, an antioxidant, a coupling agent and the like to obtain photochromic powder microcapsule solid master batches;
step 2, pre-crystallization: placing the prepared photochromic powder microcapsule solid master batch in a dry environment with ventilation for pre-crystallization;
step 3, screw extrusion: uniformly mixing the pre-crystallized photochromic powder microcapsule solid master batch with modified polyester chips, a catalyst, an antioxidant and a stabilizer, and then sending the mixture into a screw extruder for extrusion and melting to obtain a melt;
and 4, filtering: filtering, homopolymerizing and pressurizing a melt after being extruded and melted by a screw extruder to ensure continuous production of spinning and constant melt pressure;
step 5, melt spinning: and (3) delivering the melt from the filter into a spinning assembly, spraying the melt from a spinneret plate through the spinning assembly, cooling and blowing the melt, and oiling, balancing, winding and drafting the cooled and blown melt to obtain the photochromic modified polyester fiber.
2. The method for preparing the photochromic modified polyester fiber according to claim 1, wherein the method comprises the following steps: the photochromic powder is a mixture of rare earth ore powder and original photosensitive powder OP powder, the cellular inorganic substance is one or more of ceramic powder, silicon dioxide, silicate rock and carbon powder, the microporous organic polymer is one of microporous polymer, super-crosslinked microporous polymer, covalent organic framework polymer or conjugated microporous polymer, the polyester toughening agent is polyolefin copolymer and/or graft copolymer with reaction functional groups, and the coupling agent is zirconium coupling agent, magnesium coupling agent and tin coupling agent.
3. The method for preparing the photochromic modified polyester fiber according to claim 1, wherein the method for preparing the modified polyester chip in the step 1 comprises the following steps: selecting one or more of polyester fibers PBT, PTT and PET, mixing uniformly, then carrying out esterification reaction and prepolymerization reaction in sequence, and simultaneously adding a third or fourth component of dibasic acid and a dihydric alcohol monomer in the polyester polymerization process for copolymerization to obtain copolyester chips with the melting point range of 140-190 ℃; wherein the content of the first and second substances,
the esterification reaction is carried out in two stages, wherein the esterification reaction temperature of the first stage is 170 ~ 200 ℃, the reaction time is 1 ~ 3h, the esterification reaction temperature of the second stage is 200 ~ 270 ℃, the reaction time is 1 ~ 2h, and the reaction pressure is normal pressure;
the prepolymerization reaction is carried out in two stages, wherein the reaction temperature of the first stage is 240 ~ 260 ℃, the reaction time is 0.5 ~ 1h, the reaction pressure is 1kpa ~ 10kpa absolute, the reaction temperature of the second stage is 250 ~ 270 ℃, the reaction time is 0.5 ~ 1h, and the reaction pressure is 500 ~ 1000pa absolute.
4. The method for preparing the photochromic modified polyester fiber according to claim 3, wherein the method comprises the following steps: the third component is aliphatic dibasic acid and aromatic dibasic acid, and the fourth component is one or more of butanediol, neopentyl glycol, hexanediol, cyclohexanedimethanol and polyethylene glycol.
5. The method for preparing the photochromic modified polyester fiber according to claim 1, wherein the method comprises the following steps: in the step 1, the high-concentration photosensitive color-changing powder microcapsule accounts for 99-99.9 Wt% of the total mass, and the balance is low-melting-point modified polyester chips, a polyester toughening agent, an antioxidant and a coupling agent.
6. The method for preparing the photochromic modified polyester fiber according to claim 1, wherein the method comprises the following steps: in the step 2, the pre-crystallization temperature is 120-125 ℃, the temperature of the hot drying air is 110-140 ℃, the dew point of the air is less than or equal to 60 ℃, the water content of the material is 30ppm, and the drying time is 4-10 hours.
7. The method for preparing the photochromic modified polyester fiber according to claim 1, wherein the method comprises the following steps: in the step 3, the catalyst is a metal oxide catalyst, a complex catalyst and/or a rare earth catalyst, the antioxidant is phosphate, catechol phosphate and/or terpene phenol, and the stabilizer is phosphoric acid, phosphorous acid or ester derivatives thereof.
8. The method for preparing the photochromic modified polyester fiber according to claim 1, wherein the method comprises the following steps: in the step 3, the photochromic powder microcapsule solid master batch occupies 2-10 Wt% of the total mass, the modified polyester occupies 89-97.9 Wt% of the total mass, and the balance is a catalyst, an antioxidant and a stabilizer.
9. The method for preparing the photochromic modified polyester fiber according to claim 1, wherein the method comprises the following steps: and 4, filtering under the condition that the pressure before filtering is less than or equal to 16Mpa, and the pressure is constant to be 8.5Mpa in the filtering process, wherein the filtering precision is 20-60 micrometers.
10. The method for preparing the photochromic modified polyester fiber according to claim 1, wherein the method comprises the following steps: in the step 5, the spinneret plate is a circular or special-shaped spinneret hole, the spinning assembly is a filter screen of 30/120/150/400/250/400 meshes, the temperature during spinning is 180-220 ℃, the spinning speed is 1000-2000 m/min, the wind speed of cooling air blowing is 0.4-0.6 m/s, the wind temperature is 23-25 ℃, and the relative humidity is 70-80%.
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|---|---|---|---|---|
| CN112323168A (en) * | 2020-11-25 | 2021-02-05 | 江苏杜为新材料科技有限公司 | Photochromic fiber and preparation method thereof |
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