CN105671676A - Graphene reinforced luminescent polyester fiber and preparation method thereof - Google Patents
Graphene reinforced luminescent polyester fiber and preparation method thereof Download PDFInfo
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- CN105671676A CN105671676A CN201610071935.8A CN201610071935A CN105671676A CN 105671676 A CN105671676 A CN 105671676A CN 201610071935 A CN201610071935 A CN 201610071935A CN 105671676 A CN105671676 A CN 105671676A
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- graphene
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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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention belongs to the technical field of textile fibers and particularly relates to a graphene reinforced luminescent polyester fiber and a preparation method thereof. The fiber is prepared from 50wt%-75wt% of polyester chips and 25wt%-50wt% of graphene-containing luminescent master batch; the graphene-containing luminescent master batch is prepared from raw materials in parts by weight as follows: 100 parts of polyester chips, 0.05-0.1 parts of graphene, 25-50 parts of a luminescent material, 0.05-0.2 parts of a dispersing agent, 0.01-0.1 parts of a coupling agent, 0.01-0.1 parts of a heat stabilizer, 0.01-0.1 parts of a light stabilizer, 0.01-0.1 parts of an antioxidant and 0.1-1 part of an organic solvent. The prepared luminescent polyester fiber has the characteristics of high strength, good toughness and high comprehensive applicability. The preparation method is simple, easy to implement and prone to industrial production.
Description
Technical field
The invention belongs to textile fiber technology field, be specifically related to luminous polyester fiber of a kind of Graphene enhancing and preparation method thereof.
Background technology
Luminescent fibre is the new type functional fibrous material utilizing rare earth luminescent material to make. This fiber is with spinning material for matrix, and adopting long afterglow rare earth aluminate is luminous body, makes through extraordinary spinning processing. As long as luminescent fibre absorbs any visible ray 10 minutes, just luminous energy can be stored and store among fiber, continuous illumination more than 10 hours in the dark state, and can recycle. Can be widely applied to the fields such as building decoration, transportation, aviation and navigation, night work, fire-fighting emergent, daily life and amusement clothing, there is good development prospect.
But, it is low to there is intensity in luminescent fibre prepared at present, as luminous polyester fibre strength is about 1.72cN/dtex, is less than the half of conventional polyester fibre strength, and fiber rigidity is big, pliability is poor, and this seriously constrains the application of luminescent fibre. How to improve the intensity of luminescent fibre, become the technical bottleneck hindering luminescent fibre popularization and application. Academia is just finding the method improving luminescent fibre performance, and such as ZL201410099683.0 " a kind of compound luminous fiber with skin-core structure and manufacture method thereof ", employing skin-core structure, cortex is luminescent material, vector resin; Sandwich layer is vistanex, improves spinning properties and the luminosity of fiber, improves the combination property of fiber, wherein spinning technique is promoted and protection luminosity effect is obvious, but to intensity with flexible to improve insufficient amplitude big. Graphene as the nano material of a kind of excellent performance, more taller than best steel 200 times of its fracture strength, there is good elasticity simultaneously, stretch range can reach the 20% of own dimensions. Therefore, Graphene is improve luminescent fibre intensity to provide a new approach, it addition, Graphene is nearly transparent, above-mentioned advantage can be greatly improved the intensity of luminescent fibre, pliability and not affect the brightness of luminescent fibre, thus improving the integrated application performance of luminescent fibre. Therefore, in the urgent need to the method that research and development adopt Graphene enhancing luminescent fibre, the integrated application performance of luminescent fibre is improved.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that luminous polyester fiber that a kind of Graphene strengthens and preparation method thereof.Luminous polyester fiber prepared by the present invention has intensity height, good toughness, feature that integrated application performance is strong. And the manufacture method of the present invention is simple, it is simple to industrialized production.
For achieving the above object, the present invention adopts the following technical scheme that
The luminous polyester fiber that a kind of Graphene strengthens, it is made up of 50 ~ 75wt% polyester slice and 25 ~ 50wt% graphene-containing luminescence master batch;
Described graphene-containing luminescence master batch is made up of the raw material of following weight portion: polyester slice 100 parts, Graphene 0.05 ~ 0.1 part, luminescent material 25 ~ 50 parts, dispersant 0.05 ~ 0.2 part, coupling agent 0.01 ~ 0.1 part, heat stabilizer 0.01 ~ 0.1 part, light stabilizer 0.01 ~ 0.1 part, antioxidant 0.01 ~ 0.1 part, organic solvent 0.1 ~ 1 part;
Described polyester slice is spinning filament grade polyester chip.
Described Graphene is single-layer graphene or multi-layer graphene nanometer sheet.
Described Graphene can be prepared by methods such as mechanical stripping method, chemical vapour deposition technique (CVD), graphite oxide method, graphite intercalation compound methods (GICs).
Described Graphene includes graphene oxide (GrapheneOxide), namely with the Graphene of the oxy radicals such as part of hydroxyl, carboxyl, epoxy radicals in lamellar structure.
Described luminescent material is the one in rare earth aluminate luminescent powder, rare earth silicate luminescent powder, and mean diameter is 1-5 μm.
A kind of method preparing the luminous polyester fiber that Graphene as above strengthens, comprises the following steps:
(1) prepared by mixed powder: added by graphene powder in organic solvent, sonic oscillation, obtains finely dispersed graphene suspension; Luminescent material is mixed with dispersant, coupling agent, heat stabilizer, light stabilizer and antioxidant, in the process of mixing, will, in graphene suspension atomizing spray to luminescent material, be sufficiently mixed uniformly standby;
(2) prepared by graphene-containing luminescence master batch: by dry polyester slice, feeding double screw extruder, the mixed powder simultaneously step (1) obtained adopts side to feed method feeding double screw extruder, prepares the luminous master batch of graphene-containing through melted, casting and pelletizing, and vacuum drying is standby;
(3) prepared by luminous filament: by the luminous master batch of the graphene-containing that dry polyester slice and step (2) prepare, feeds spinning-drawing machine by corresponding quality proportioning, through Screw Extrusion, melt spinning, drawing-off and winding, obtains enhancement mode luminous filament.
In step (2), the drying means of the luminous master batch of polyester slice and graphene-containing is: 160 ~ 180 DEG C, the pre-crystallized 10 ~ 20min of air blast, then at 160 ~ 180 DEG C, and vacuum drying 4 ~ 6h.
The spin manifold temperature of the spinning-drawing machine described in step (3) is 260 ~ 300 DEG C, and the temperature of draw roll is 70 ~ 110 DEG C, drafting multiple is 1.5 ~ 5, winding speed is 300 ~ 1500m/min.
The beneficial effects of the present invention is:
1) present invention adopts Graphene effectively to breach the technical bottleneck that luminescent fibre is powerful low; Prepare luminous master batch by being mixed with luminescent material etc. by Graphene, be effectively increased grapheme material dispersibility in matrix resin, and enhance the boundary strength between matrix resin and Graphene;
2) luminous polyester fibrous fracture intensity and the pliability that prepared by the present invention are remarkably reinforced, and fiber integrated application performance is substantially improved, and preparation technology of the present invention is simple, it is simple to industrialized production.
Detailed description of the invention
Further illustrate the present invention with specific embodiment below, but protection scope of the present invention is not limited to the following example.
The luminescent material that following embodiment uses adopts commercially available prod, the LM serial emission powder that luminous Science and Technology Ltd. as bright in Dalian Road produces.
The grapheme material that following embodiment uses adopts commercially available prod, such as the graphene powder that Shanghai Ka Jite Chemical Industry Science Co., Ltd produces.
The vector resin that following embodiment uses is for being spinning filament grade polyester chip, for instance the SB500 fiber type grade polyester chip that Yizheng Chemical Fiber Co., Ltd., SINOPEC produces.
All the other auxiliary agents are conventional commercial product.
Embodiment 1
The luminous polyester fiber that a kind of Graphene strengthens, it is made up of polyester slice and graphene-containing luminescence master batch 70:30 by weight percentage;
Described graphene-containing luminescence master batch is made up of the raw material of following weight portion: polyester slice 100 parts, Graphene 0.05 part, luminescent material 35 parts, dispersant 0.1 part, coupling agent 0.05 part, heat stabilizer 0.05 part, light stabilizer 0.05 part, antioxidant 0.05 part, N, N '-dimethyl Methanamide 0.25 part;
A kind of concrete preparation method adopting Graphene to strengthen luminous polyester fiber:
(1) taking graphene powder addition bath raio is the N of 1:5, in N '-dimethyl formamide solvent, disperses 1h with ultrasonic washing unit, obtains finely dispersed graphene suspension; Add dispersant in luminescent material, coupling agent, heat stabilizer, light stabilizer and antioxidant mix, and in the process of mixing, by graphene suspension atomizing spray to luminescent material, and are sufficiently mixed uniformly standby;
(2) by polyester slice, by the pre-crystallized 20min of the air blast of 180 DEG C, then dry 5h in the vacuum of 180 DEG C; Taking the mixed powder feeding double screw extruder that dry polyester slice obtains with step (1), prepare the luminous master batch of graphene-containing through melted, casting and pelletizing, vacuum drying is standby;
(3) learn from else's experience dry polyester slice, the luminous master batch of the graphene-containing of gained in step (2), mixing feeding spinning-drawing machine, by screw extruder, melt spinning, screw rod is from Ith district to V district's heating-up temperature respectively 280 DEG C, 285 DEG C, 288 DEG C, 290 DEG C, 290 DEG C, condition of spinning manifold temperature is 290 DEG C, draw roll temperature is 85 DEG C, two sections of drafting multiples respectively 2.0 and 1.6, and total drafting multiple is 3.2, winding speed is 1000m/min, obtains strengthening luminous polyester fiber.
Enhancing luminous polyester fibre strength obtained by the present embodiment reaches 3.35cN/dtex, and pliability is good.
Embodiment 2
The luminous polyester fiber that a kind of Graphene strengthens, it is made up of polyester slice and graphene-containing luminescence master batch 70:30 by weight percentage;
Described graphene-containing luminescence master batch is made up of the raw material of following weight portion: 100 parts of polyester fiber, Graphene 0.1 part, luminescent material 35 parts, dispersant 0.1 part, coupling agent 0.05 part, heat stabilizer 0.05 part, light stabilizer 0.05 part, antioxidant 0.05 part, N, N '-dimethyl Methanamide 0.5 part;
A kind of concrete preparation method adopting Graphene to strengthen luminous polyester fiber:
(1) taking graphene powder addition bath raio is the N of 1:5, in N '-dimethyl formamide solvent, disperses 1h with ultrasonic washing unit, obtains finely dispersed graphene suspension; Add dispersant in luminescent material, coupling agent, heat stabilizer, light stabilizer and antioxidant mix, and in the process of mixing, by graphene suspension atomizing spray to luminescent material, and are sufficiently mixed uniformly standby;
(2) by polyester slice, by the pre-crystallized 20min of the air blast of 180 DEG C, then dry 5h in the vacuum of 180 DEG C;Taking the feeding double screw extruder of the luminescent material containing Graphene that dry polyester slice obtains with step (1), prepare the luminous master batch of graphene-containing through melted, casting and pelletizing, vacuum drying is standby;
(3) learn from else's experience dry polyester slice, the luminous master batch of gained in step (2), mixing feeding spinning-drawing machine, by screw extruder, melt spinning, screw rod is from Ith district to V district's heating-up temperature respectively 280 DEG C, 285 DEG C, 288 DEG C, 290 DEG C, 290 DEG C, condition of spinning manifold temperature is 290 DEG C, draw roll temperature is 85 DEG C, two sections of drafting multiples respectively 2.0 and 1.6, and total drafting multiple is 3.2, winding speed is 1000m/min, obtains strengthening luminous polyester fiber.
Enhancing luminous polyester fibre strength obtained by the present embodiment reaches 3.20cN/dtex, and pliability is good.
Embodiment 3
The luminous polyester fiber that a kind of Graphene strengthens, it is made up of polyester slice and graphene-containing luminescence master batch 70:30 by weight percentage;
Described graphene-containing luminescence master batch is made up of the raw material of following weight portion: 100 parts of polyester fiber, Graphene 0.01 part, luminescent material 35 parts, dispersant 0.1 part, coupling agent 0.05 part, heat stabilizer 0.05 part, light stabilizer 0.05 part, antioxidant 0.05 part, N, N '-dimethyl Methanamide 0.05 part;
A kind of concrete preparation method adopting Graphene to strengthen luminous polyester fiber:
(1) taking graphene powder addition bath raio is the N of 1:5, in N '-dimethyl formamide solvent, disperses 1h with ultrasonic washing unit, obtains finely dispersed graphene suspension; Add dispersant in luminescent material, coupling agent, heat stabilizer, light stabilizer and antioxidant mix, and in the process of mixing, by graphene suspension atomizing spray to luminescent material, and are sufficiently mixed uniformly standby;
(2) by polyester slice, by the pre-crystallized 20min of the air blast of 180 DEG C, then dry 5h in the vacuum of 180 DEG C; Taking the feeding double screw extruder of the luminescent material containing Graphene that dry polyester slice obtains with step (1), prepare the luminous master batch of graphene-containing through melted, casting and pelletizing, vacuum drying is standby;
(3) learn from else's experience dry polyester slice, the luminous master batch of gained in step (2), mixing feeding spinning-drawing machine, by screw extruder, melt spinning, screw rod is from Ith district to V district's heating-up temperature respectively 280 DEG C, 285 DEG C, 288 DEG C, 290 DEG C, 290 DEG C, condition of spinning manifold temperature is 290 DEG C, draw roll temperature is 85 DEG C, two sections of drafting multiples respectively 2.0 and 1.6, and total drafting multiple is 3.2, winding speed is 1000m/min, obtains strengthening luminous polyester fiber.
Enhancing luminous polyester fibre strength obtained by the present embodiment reaches 2.95cN/dtex, and pliability is good.
The foregoing is only presently preferred embodiments of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to the covering scope of the present invention.
Claims (9)
1. the luminous polyester fiber that a Graphene strengthens, it is characterised in that: it is made up of 50 ~ 75wt% polyester slice and 25 ~ 50wt% graphene-containing luminescence master batch;
Described graphene-containing luminescence master batch is made up of the raw material of following weight portion: polyester slice 100 parts, Graphene 0.05 ~ 0.1 part, luminescent material 25 ~ 50 parts, dispersant 0.05 ~ 0.2 part, coupling agent 0.01 ~ 0.1 part, heat stabilizer 0.01 ~ 0.1 part, light stabilizer 0.01 ~ 0.1 part, antioxidant 0.01 ~ 0.1 part, organic solvent 0.1 ~ 1 part.
2. the luminous polyester fiber that Graphene according to claim 1 strengthens, it is characterised in that: described polyester slice is spinning filament grade polyester chip.
3. the luminous polyester fiber that Graphene according to claim 1 strengthens, it is characterised in that: described Graphene is single-layer graphene or multi-layer graphene nanometer sheet.
4. the luminous polyester fiber that Graphene according to claim 1 strengthens, it is characterised in that: described Graphene includes with the Graphene containing oxide group.
5. the luminous polyester fiber that Graphene according to claim 1 strengthens, it is characterised in that: described luminescent material is the one in rare earth aluminate luminescent powder, rare earth silicate luminescent powder, and mean diameter is 1-5 μm.
6. the luminous polyester fiber that Graphene according to claim 1 strengthens, it is characterized in that: described organic solvent includes N, N '-dimethyl Methanamide, N, one or both in N '-dimethyl acetamide, N-Methyl pyrrolidone, dimethyl sulfoxide, dehydrated alcohol.
7. the method for the luminous polyester fiber that the Graphene that a kind is prepared as described in any one of claim 1-6 strengthens, it is characterised in that: comprise the following steps:
(1) prepared by mixed powder: added by graphene powder in organic solvent, sonic oscillation, obtains finely dispersed graphene suspension; Luminescent material is mixed with dispersant, coupling agent, heat stabilizer, light stabilizer and antioxidant, in the process of mixing, will, in graphene suspension atomizing spray to luminescent material, be sufficiently mixed uniformly standby;
(2) prepared by graphene-containing luminescence master batch: by dry polyester slice, feeding double screw extruder, the mixed powder simultaneously step (1) obtained adopts side to feed method feeding double screw extruder, prepares the luminous master batch of graphene-containing through melted, casting and pelletizing, and vacuum drying is standby;
(3) prepared by luminous filament: by the luminous master batch of the graphene-containing that dry polyester slice and step (2) prepare, feeds spinning-drawing machine by corresponding quality proportioning, through Screw Extrusion, melt spinning, drawing-off and winding, obtains enhancement mode luminous filament.
8. the preparation method of the luminous polyester fiber that Graphene according to claim 7 strengthens, it is characterized in that: in step (2), the drying means of the luminous master batch of polyester slice and graphene-containing is: 160 ~ 180 DEG C, pre-crystallized 10 ~ the 20min of air blast, then at 160 ~ 180 DEG C, vacuum drying 4 ~ 6h.
9. the preparation method of the luminous polyester fiber that Graphene according to claim 7 strengthens, it is characterized in that: the spin manifold temperature of the spinning-drawing machine described in step (3) is 260 ~ 300 DEG C, the temperature of draw roll is 70 ~ 110 DEG C, drafting multiple is 1.5 ~ 5, winding speed is 300 ~ 1500m/min.
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Cited By (4)
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| CN107475845A (en) * | 2017-08-07 | 2017-12-15 | 东华大学 | The elastic fasciated yarn of a kind of anti-electromagnetic radiation and by its obtained fabric |
| CN111155196A (en) * | 2020-01-03 | 2020-05-15 | 浙江颖诺泰材料科技有限公司 | Luminescent fiber based on recycled polyester material and preparation method thereof |
| CN112011849A (en) * | 2020-09-14 | 2020-12-01 | 揭东巴黎万株纱华纺织有限公司 | Preparation process of graphene super-imitation cotton fiber |
| CN113024949A (en) * | 2021-03-10 | 2021-06-25 | 南通强生石墨烯科技有限公司 | Graphene luminescent plastic master batch and preparation method thereof |
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