CN111607839A - Method for preparing modified white graphene polyester composite fiber and fiber prepared by method - Google Patents
Method for preparing modified white graphene polyester composite fiber and fiber prepared by method Download PDFInfo
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- CN111607839A CN111607839A CN202010581278.8A CN202010581278A CN111607839A CN 111607839 A CN111607839 A CN 111607839A CN 202010581278 A CN202010581278 A CN 202010581278A CN 111607839 A CN111607839 A CN 111607839A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 209
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 208
- 229920000728 polyester Polymers 0.000 title claims abstract description 169
- 239000000835 fiber Substances 0.000 title claims abstract description 95
- 239000002131 composite material Substances 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 60
- 239000000843 powder Substances 0.000 claims abstract description 73
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 43
- 238000001035 drying Methods 0.000 claims abstract description 41
- 238000009987 spinning Methods 0.000 claims abstract description 38
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 239000011812 mixed powder Substances 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000002844 melting Methods 0.000 claims abstract description 16
- 230000008018 melting Effects 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 38
- 239000003607 modifier Substances 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 24
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 229920004933 Terylene® Polymers 0.000 claims description 14
- 229960003638 dopamine Drugs 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 8
- 238000001125 extrusion Methods 0.000 claims description 8
- 238000005469 granulation Methods 0.000 claims description 8
- 230000003179 granulation Effects 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 238000005229 chemical vapour deposition Methods 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 229920004934 Dacron® Polymers 0.000 claims 1
- 230000006750 UV protection Effects 0.000 abstract description 6
- 230000003115 biocidal effect Effects 0.000 abstract description 5
- 239000004627 regenerated cellulose Substances 0.000 abstract description 4
- 229910052582 BN Inorganic materials 0.000 description 6
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 6
- 230000008901 benefit Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000002265 prevention Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002074 melt spinning Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 241000222122 Candida albicans Species 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229940095731 candida albicans Drugs 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
-
- 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
-
- 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
- D01F1/103—Agents inhibiting growth of microorganisms
-
- 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
- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Artificial Filaments (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a method for preparing modified white graphene polyester composite fibers and fibers prepared by the method, wherein the method comprises the following steps: step 1, preparing modified white graphene powder; step 2, preparing white graphene polyester mixed powder; step 3, preparing modified white graphene polyester master batches; and 4, drying the modified white graphene polyester master batch, adding the dried modified white graphene polyester master batch into a screw extruder for heating and melting, filtering the mixture by a spinning manifold, and spinning the mixture into bundles. The invention also provides the modified white graphene polyester composite fiber prepared by the method. According to the invention, the white graphene is preferentially modified so as to improve the dispersibility of the white graphene in the regenerated cellulose pulp and better exert the functionality of the regenerated cellulose composite fiber, the white graphene polyester composite fiber prepared by the method has the characteristics of antibiosis, far infrared and ultraviolet resistance, and the white graphene in the white graphene polyester composite fiber is uniformly dispersed and is not easy to fall off, so that the functionality has durability.
Description
Technical Field
The invention relates to a preparation method of composite fibers and fibers prepared by the composite fibers, in particular to a method for preparing modified white graphene polyester composite fibers and fibers prepared by the method.
Background
"white graphene" is a name given to a nanosheet obtained after exfoliation of Hexagonal boron nitride (english name: Hexagonal boronnide, abbreviated as h-BN) with crystal grains in a lamellar structure. Since the structure of hexagonal boron nitride is very similar to that of graphite, it has a hexagonal layered structure, is soft in texture, is highly processable, and is white in color. Corresponding to graphene, hexagonal boron nitride is therefore referred to as "white graphene".
Hexagonal boron nitride and graphene are both layered two-dimensional materials of only one atom thickness, except that graphene is bonded purely by covalent bonds between carbon atoms, whereas the bonds in a hexagonal boron nitride crystal are covalent bonds between boron and nitrogen heterogeneous atoms.
The highly similar crystal structure gives white graphene and graphene some common characteristics, such as extremely high in-plane elastic modulus, high temperature stability, and atomically smooth surface. The white graphene has high transparency and chemical inertness, and has the properties of high mechanical strength, high melting point, high thermal conductivity, extremely low friction coefficient and the like. A monolayer of atomic thick boron nitride can withstand high temperatures of 800 c in air. The white graphene has excellent impermeability, and is very suitable for corrosion prevention of metal under high temperature and corrosive liquid environment. Meanwhile, the latest research of my company discovers that the white graphene also has excellent antibacterial, far infrared, ultraviolet-resistant and other performances, and has great development potential in fiber application.
The polyester fiber is a chemical fiber with low cost, good performance and extremely wide application, but the traditional polyester fiber does not have functionality, along with social development, the traditional polyester fiber cannot meet the requirements of people on functional textiles, the white graphene polyester fiber has good antibacterial property, far infrared, ultraviolet resistance and other functions, the melting method white graphene polyester composite fiber is permanent in functionality, the condition that the functionality is weakened along with the increase of washing times is avoided, the application range of the traditional polyester fiber is expanded, the product added value is improved, and the requirements of people on healthy and environment-friendly functional textiles are well met.
Disclosure of Invention
The invention aims to provide a preparation method of composite fiber and the prepared fiber, which are used for preferentially modifying white graphene so as to improve the dispersibility of the white graphene, better exert the functionality of the composite fiber, prepare the modified white graphene polyester composite fiber with the functions of antibiosis, mite prevention, ultraviolet resistance, far infrared resistance and the like, improve the additional value of polyester and expand the application range of the polyester fiber.
In order to achieve the above object, the present invention provides a method for preparing a modified white graphene polyester composite fiber, wherein the method comprises: step 1, preparing an ethanol solution, adding dopamine, uniformly stirring, adding white graphene into the solution, performing ultrasonic dispersion, filtering and drying to obtain modified white graphene powder; step 2, respectively drying the modified white graphene powder obtained in the step 1 and common polyester slices, then grinding the polyester slices to obtain polyester slice powder, adding the dried modified white graphene powder and a modifier into the polyester slice powder, and mixing and stirring to obtain white graphene and polyester mixed powder; step 3, adding the white graphene polyester mixed powder obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain modified white graphene polyester master batches; and 4, drying the modified white graphene polyester master batch obtained in the step 3, adding the dried modified white graphene polyester master batch into a screw extruder for heating and melting, filtering the mixture through a spinning box, and then spinning the mixture into bundles to obtain the modified white graphene polyester composite fiber.
The preparation method of the modified white graphene polyester composite fiber comprises the following steps of: 84-99% of polyester chips, 0.1-15% of white graphene and 0.1-1% of modifier.
The preparation method of the modified white graphene polyester composite fiber comprises the step of preparing the white graphene by any one of a borax-ammonium chloride method, a chemical vapor deposition method, a borax-urea method, a high-frequency plasma method, a hydrothermal method and a precursor method.
The preparation method of the modified white graphene polyester composite fiber comprises the following steps of mixing the modifying agent with polyvinyl alcohol, polyvinylpyrrolidone and sodium dodecyl benzene sulfonate in a mass ratio of 1: (2-4): (3-5).
In the step 1, deionized water and ethanol are used for preparing an ethanol solution with the mass concentration of 10% -50% at room temperature, the mass concentration of dopamine in the solution is 0.1% -5%, then the white graphene is added into the solution, ultrasonic dispersion is carried out for 10-30 min, the mass concentration of the white graphene in the solution is 0.1% -10%, and the modified white graphene polyester composite fiber is obtained by filtering and drying.
In the step 2, the modified white graphene polyester composite fiber and the common polyester chips are respectively dried, and the water content after drying is controlled below 100 ppm.
In the step 2, the polyester slices are ground to obtain polyester slice powder, the mesh number of the powder is larger than 100 meshes, then the white graphene powder and the modifier are added into the polyester slice powder, the mixture is placed into a high-speed mixer to be mixed and stirred, the rotating speed is 3000-10000 r/min, and the stirring time is 10-30 min, so that the white graphene polyester mixed powder is obtained.
In the step 3, the temperatures from the first zone to the fifth zone of the twin-screw extruder are respectively controlled at 270 ℃ and 265 ℃ in the range of 260-.
In the step 4, the modified white graphene polyester master batch is dried, the drying temperature is controlled to be 80-200 ℃, the water content of the master batch is controlled to be less than 100ppm, the master batch is added into a screw extruder for heating and melting, the master batch is filtered by a spinning box and then spun into bundles, the spinning temperature is 270-290 ℃, the spinning speed is 500-1500m/min, and the obtained nascent fiber is subjected to processes of stretching, curling and the like to obtain the modified white graphene polyester composite fiber used under different conditions.
The invention also provides the modified white graphene polyester composite fiber prepared by the method.
The method for preparing the modified white graphene polyester composite fiber and the prepared fiber have the following advantages:
according to the method, the white graphene is preferentially modified, so that the dispersity of the white graphene is improved, the functionality of the composite fiber is better exerted, and the method is used for modifying the white graphene so that the edge of the white graphene is grafted with hydroxyl and carboxyl, and the white graphene has good dispersity in the subsequent production process.
According to the invention, the modified white graphene polyester composite fiber is prepared by preparing the white graphene polyester master batch and then carrying out melt spinning on the white graphene polyester master batch. The modified white graphene polyester composite fiber with the functions of antibiosis, mite prevention, ultraviolet resistance, far infrared and the like, prepared by the invention, can improve the polyester additional value and expand the application range of polyester fiber.
The melting method white graphene polyester fiber has excellent performances of antibiosis, mite prevention, far infrared, ultraviolet resistance and the like, wherein the bacteriostasis rate of escherichia coli, staphylococcus aureus and candida albicans reaches 99.9%, the mite inhibition rate is greater than 90%, the far infrared temperature rise reaches 0.88, the UPF is greater than 100, and the functionality is good.
The fusion-method modified white graphene polyester composite fiber prepared by the method has the advantages of simple process, easy operation, low cost and high economic benefit, and is suitable for large-scale industrial production.
Detailed Description
The following further describes embodiments of the present invention.
The invention provides a method for preparing modified white graphene polyester composite fibers, which comprises the following steps: step 1, preparing an ethanol solution, adding dopamine, uniformly stirring, adding white graphene into the solution, performing ultrasonic dispersion, filtering and drying to obtain modified white graphene powder; step 2, respectively drying the modified white graphene powder obtained in the step 1 and common polyester slices, then grinding the polyester slices to obtain polyester slice powder, adding the dried modified white graphene powder and a modifier into the polyester slice powder, and mixing and stirring to obtain white graphene and polyester mixed powder; step 3, adding the white graphene polyester mixed powder obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain modified white graphene polyester master batches; and 4, drying the modified white graphene polyester master batch obtained in the step 3, adding the dried modified white graphene polyester master batch into a screw extruder for heating and melting, filtering the mixture through a spinning box, and then spinning the mixture into bundles to obtain the modified white graphene polyester composite fiber.
Preferably, the modified white graphene polyester composite fiber comprises the following raw materials in percentage by mass: 84-99% of polyester chips, 0.1-15% of white graphene and 0.1-1% of modifier.
The white graphene is prepared by any one of a borax-ammonium chloride method, a chemical vapor deposition method, a borax-urea method, a high-frequency plasma method, a hydrothermal method and a precursor method.
The modifier is a mixture of polyvinyl alcohol, polyvinylpyrrolidone and sodium dodecyl benzene sulfonate, and the mass ratio of the modifier is 1: (2-4): (3-5).
In the step 1, deionized water and ethanol are used for preparing an ethanol solution with the mass concentration of 10% -50% at room temperature, the mass concentration of dopamine in the solution is 0.1% -5%, then white graphene is added into the solution, ultrasonic dispersion is carried out for 10-30 min, the mass concentration of the white graphene in the solution is 0.1% -10%, and filtering and drying are carried out to obtain the modified white graphene powder.
And 2, respectively drying the modified white graphene powder and the common polyester chips, wherein the water content after drying is controlled below 100 ppm.
And 2, grinding the polyester chips to obtain polyester chip powder, wherein the mesh number of the powder is more than 100 meshes, adding the white graphene powder and the modifier into the polyester chip powder, putting the polyester chip powder into a high-speed mixer, and mixing and stirring the mixture at the rotating speed of 3000-10000 r/min for 10-30 min to obtain the white graphene polyester mixed powder.
In step 3, the temperatures of the first zone to the fifth zone of the double-screw extruder are respectively controlled at 270 ℃ of 260-.
And 4, drying the modified white graphene terylene master batch at the drying temperature of 80-200 ℃ and the water content of the master batch below 100ppm, adding the dried modified white graphene terylene master batch into a screw extruder for heating and melting, filtering the mixture by a spinning box, spinning into bundles at the spinning temperature of 270-290 ℃ and the spinning speed of 500-1500m/min, and stretching and curling the obtained nascent fiber to obtain the modified white graphene terylene composite fiber used under different conditions.
The invention also provides the modified white graphene polyester composite fiber prepared by the method.
The method for preparing the modified white graphene polyester composite fiber and the fiber prepared by the method provided by the invention are further described with reference to the following examples.
Example 1
A method of preparing a modified white graphene polyester composite fiber, comprising:
step 1, preparing an ethanol solution with the mass concentration of 10% -50% by using deionized water and ethanol at room temperature, wherein the mass concentration of dopamine in the solution is 0.1% -5%, adding white graphene into the solution, performing ultrasonic dispersion for 10-30 min, wherein the mass concentration of the white graphene in the solution is 0.1% -10%, filtering and drying to obtain modified white graphene powder;
and 2, respectively drying the modified white graphene powder obtained in the step 1 and common polyester slices, controlling the water content of the dried white graphene powder and the water content of the common polyester slices to be below 100ppm, then grinding the polyester slices to obtain polyester slice powder, wherein the mesh number of the powder is more than 100 meshes, adding the dried modified white graphene powder and a modifier into the polyester slice powder, putting the polyester slice powder into a high-speed mixer, mixing and stirring at the rotating speed of 3000-10000 r/min for 10-30 min to obtain the white graphene polyester mixed powder.
Step 3, adding the white graphene polyester mixed powder obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain modified white graphene polyester master batches; the temperatures of the first zone to the fifth zone of the double-screw extruder are respectively controlled at 270 ℃, 265 ℃, 275 ℃, 270 ℃, 280 ℃, 265 ℃, 275 ℃ and 260 ℃.
And 4, drying the modified white graphene terylene master batch obtained in the step 3, controlling the drying temperature to be 80-200 ℃, controlling the water content of the master batch to be below 100ppm, adding the master batch into a screw extruder for heating and melting, filtering the master batch through a spinning box, spinning into bundles at the spinning temperature of 270-290 ℃ and the spinning speed of 500-1500m/min, and stretching and curling the obtained nascent fiber to obtain the modified white graphene terylene composite fiber used under different conditions.
Preferably, the modified white graphene polyester composite fiber comprises the following raw materials in percentage by mass: 99% of polyester chips, 0.1% of white graphene and 0.9% of modifier.
The white graphene is prepared by adopting a borax-ammonium chloride method.
The modifier is a mixture of polyvinyl alcohol, polyvinylpyrrolidone and sodium dodecyl benzene sulfonate, and the mass ratio of the modifier is 1: 2: 3.
example 2
A method of preparing a modified white graphene polyester composite fiber, comprising:
step 1, preparing an ethanol solution with the mass concentration of 10% -50% by using deionized water and ethanol at room temperature, wherein the mass concentration of dopamine in the solution is 0.1% -5%, adding white graphene into the solution, performing ultrasonic dispersion for 10-30 min, wherein the mass concentration of the white graphene in the solution is 0.1% -10%, filtering and drying to obtain modified white graphene powder;
and 2, respectively drying the modified white graphene powder obtained in the step 1 and common polyester slices, controlling the water content of the dried white graphene powder and the water content of the common polyester slices to be below 100ppm, then grinding the polyester slices to obtain polyester slice powder, wherein the mesh number of the powder is more than 100 meshes, adding the dried modified white graphene powder and a modifier into the polyester slice powder, putting the polyester slice powder into a high-speed mixer, mixing and stirring at the rotating speed of 3000-10000 r/min for 10-30 min to obtain the white graphene polyester mixed powder.
Step 3, adding the white graphene polyester mixed powder obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain modified white graphene polyester master batches; the temperatures of the first zone to the fifth zone of the double-screw extruder are respectively controlled at 270 ℃, 265 ℃, 275 ℃, 270 ℃, 280 ℃, 265 ℃, 275 ℃ and 260 ℃.
And 4, drying the modified white graphene terylene master batch obtained in the step 3, controlling the drying temperature to be 80-200 ℃, controlling the water content of the master batch to be below 100ppm, adding the master batch into a screw extruder for heating and melting, filtering the master batch through a spinning box, spinning into bundles at the spinning temperature of 270-290 ℃ and the spinning speed of 500-1500m/min, and stretching and curling the obtained nascent fiber to obtain the modified white graphene terylene composite fiber used under different conditions.
Preferably, the modified white graphene polyester composite fiber comprises the following raw materials in percentage by mass: 97.7% of polyester chips, 2% of white graphene and 0.3% of modifier.
The white graphene is prepared by adopting a chemical vapor deposition method.
The modifier is a mixture of polyvinyl alcohol, polyvinylpyrrolidone and sodium dodecyl benzene sulfonate, and the mass ratio of the modifier is 1: 2.5: 3.5.
example 3
A method of preparing a modified white graphene polyester composite fiber, comprising:
step 1, preparing an ethanol solution with the mass concentration of 10% -50% by using deionized water and ethanol at room temperature, wherein the mass concentration of dopamine in the solution is 0.1% -5%, adding white graphene into the solution, performing ultrasonic dispersion for 10-30 min, wherein the mass concentration of the white graphene in the solution is 0.1% -10%, filtering and drying to obtain modified white graphene powder;
and 2, respectively drying the modified white graphene powder obtained in the step 1 and common polyester slices, controlling the water content of the dried white graphene powder and the water content of the common polyester slices to be below 100ppm, then grinding the polyester slices to obtain polyester slice powder, wherein the mesh number of the powder is more than 100 meshes, adding the dried modified white graphene powder and a modifier into the polyester slice powder, putting the polyester slice powder into a high-speed mixer, mixing and stirring at the rotating speed of 3000-10000 r/min for 10-30 min to obtain the white graphene polyester mixed powder.
Step 3, adding the white graphene polyester mixed powder obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain modified white graphene polyester master batches; the temperatures of the first zone to the fifth zone of the double-screw extruder are respectively controlled at 270 ℃, 265 ℃, 275 ℃, 270 ℃, 280 ℃, 265 ℃, 275 ℃ and 260 ℃.
And 4, drying the modified white graphene terylene master batch obtained in the step 3, controlling the drying temperature to be 80-200 ℃, controlling the water content of the master batch to be below 100ppm, adding the master batch into a screw extruder for heating and melting, filtering the master batch through a spinning box, spinning into bundles at the spinning temperature of 270-290 ℃ and the spinning speed of 500-1500m/min, and stretching and curling the obtained nascent fiber to obtain the modified white graphene terylene composite fiber used under different conditions.
Preferably, the modified white graphene polyester composite fiber comprises the following raw materials in percentage by mass: 91.5% of polyester chips, 8% of white graphene and 0.5% of modifier.
The white graphene is prepared by adopting a borax-urea method.
The modifier is a mixture of polyvinyl alcohol, polyvinylpyrrolidone and sodium dodecyl benzene sulfonate, and the mass ratio of the modifier is 1: 3: 4.
example 4
A method of preparing a modified white graphene polyester composite fiber, comprising:
step 1, preparing an ethanol solution with the mass concentration of 10% -50% by using deionized water and ethanol at room temperature, wherein the mass concentration of dopamine in the solution is 0.1% -5%, adding white graphene into the solution, performing ultrasonic dispersion for 10-30 min, wherein the mass concentration of the white graphene in the solution is 0.1% -10%, filtering and drying to obtain modified white graphene powder;
and 2, respectively drying the modified white graphene powder obtained in the step 1 and common polyester slices, controlling the water content of the dried white graphene powder and the water content of the common polyester slices to be below 100ppm, then grinding the polyester slices to obtain polyester slice powder, wherein the mesh number of the powder is more than 100 meshes, adding the dried modified white graphene powder and a modifier into the polyester slice powder, putting the polyester slice powder into a high-speed mixer, mixing and stirring at the rotating speed of 3000-10000 r/min for 10-30 min to obtain the white graphene polyester mixed powder.
Step 3, adding the white graphene polyester mixed powder obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain modified white graphene polyester master batches; the temperatures of the first zone to the fifth zone of the double-screw extruder are respectively controlled at 270 ℃, 265 ℃, 275 ℃, 270 ℃, 280 ℃, 265 ℃, 275 ℃ and 260 ℃.
And 4, drying the modified white graphene terylene master batch obtained in the step 3, controlling the drying temperature to be 80-200 ℃, controlling the water content of the master batch to be below 100ppm, adding the master batch into a screw extruder for heating and melting, filtering the master batch through a spinning box, spinning into bundles at the spinning temperature of 270-290 ℃ and the spinning speed of 500-1500m/min, and stretching and curling the obtained nascent fiber to obtain the modified white graphene terylene composite fiber used under different conditions.
Preferably, the modified white graphene polyester composite fiber comprises the following raw materials in percentage by mass: 87.2% of polyester chips, 12% of white graphene and 0.8% of modifier.
The white graphene is prepared by adopting a high-frequency plasma method.
The modifier is a mixture of polyvinyl alcohol, polyvinylpyrrolidone and sodium dodecyl benzene sulfonate, and the mass ratio of the modifier is 1: 3.5: 4.5.
example 5
A method of preparing a modified white graphene polyester composite fiber, comprising:
step 1, preparing an ethanol solution with the mass concentration of 10% -50% by using deionized water and ethanol at room temperature, wherein the mass concentration of dopamine in the solution is 0.1% -5%, adding white graphene into the solution, performing ultrasonic dispersion for 10-30 min, wherein the mass concentration of the white graphene in the solution is 0.1% -10%, filtering and drying to obtain modified white graphene powder;
and 2, respectively drying the modified white graphene powder obtained in the step 1 and common polyester slices, controlling the water content of the dried white graphene powder and the water content of the common polyester slices to be below 100ppm, then grinding the polyester slices to obtain polyester slice powder, wherein the mesh number of the powder is more than 100 meshes, adding the dried modified white graphene powder and a modifier into the polyester slice powder, putting the polyester slice powder into a high-speed mixer, mixing and stirring at the rotating speed of 3000-10000 r/min for 10-30 min to obtain the white graphene polyester mixed powder.
Step 3, adding the white graphene polyester mixed powder obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain modified white graphene polyester master batches; the temperatures of the first zone to the fifth zone of the double-screw extruder are respectively controlled at 270 ℃, 265 ℃, 275 ℃, 270 ℃, 280 ℃, 265 ℃, 275 ℃ and 260 ℃.
And 4, drying the modified white graphene terylene master batch obtained in the step 3, controlling the drying temperature to be 80-200 ℃, controlling the water content of the master batch to be below 100ppm, adding the master batch into a screw extruder for heating and melting, filtering the master batch through a spinning box, spinning into bundles at the spinning temperature of 270-290 ℃ and the spinning speed of 500-1500m/min, and stretching and curling the obtained nascent fiber to obtain the modified white graphene terylene composite fiber used under different conditions.
Preferably, the modified white graphene polyester composite fiber comprises the following raw materials in percentage by mass: 84% of polyester chips, 15% of white graphene and 1% of modifier.
The white graphene is prepared by adopting any one of a hydrothermal method and a precursor method.
The modifier is a mixture of polyvinyl alcohol, polyvinylpyrrolidone and sodium dodecyl benzene sulfonate, and the mass ratio of the modifier is 1: 4: 5.
according to the method for preparing the modified white graphene polyester composite fiber and the prepared fiber, the white graphene is preferentially modified so as to improve the dispersibility of the white graphene in the regenerated cellulose pulp and better exert the functionality of the regenerated cellulose composite fiber, and the method enables the edge of the white graphene to be grafted with hydroxyl and carboxyl, so that the white graphene polyester composite fiber has good dispersibility in the subsequent production process. The modified white graphene polyester composite fiber is prepared by using a modified white graphene dispersion system and a polyester melting method technology. Specifically, the modified white graphene polyester master batch is prepared preferentially, and then melt spinning is carried out on the dried master batch to prepare the white graphene polyester composite fiber. The composite fiber has the characteristics of antibiosis, far infrared and ultraviolet resistance, and the white graphene in the white graphene polyester composite fiber is uniformly dispersed and not easy to fall off, and the functionality has durability.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims.
Claims (10)
1. A method for preparing modified white graphene polyester composite fibers is characterized by comprising the following steps:
step 1, preparing an ethanol solution, adding dopamine, uniformly stirring, adding white graphene into the solution, performing ultrasonic dispersion, filtering and drying to obtain modified white graphene powder;
step 2, respectively drying the modified white graphene powder obtained in the step 1 and common polyester slices, then grinding the polyester slices to obtain polyester slice powder, adding the dried modified white graphene powder and a modifier into the polyester slice powder, and mixing and stirring to obtain white graphene and polyester mixed powder;
step 3, adding the white graphene polyester mixed powder obtained in the step 2 into a double-screw extruder for extrusion granulation to obtain modified white graphene polyester master batches;
and 4, drying the modified white graphene polyester master batch obtained in the step 3, adding the dried modified white graphene polyester master batch into a screw extruder for heating and melting, filtering the mixture through a spinning box, and then spinning the mixture into bundles to obtain the modified white graphene polyester composite fiber.
2. The preparation method of the modified white graphene polyester composite fiber according to claim 1, wherein the modified white graphene polyester composite fiber comprises the following raw materials in percentage by mass: 84-99% of polyester chips, 0.1-15% of white graphene and 0.1-1% of modifier.
3. The modified white graphene-dacron composite fiber according to claim 2, wherein the white graphene is prepared by any one of a borax-ammonium chloride method, a chemical vapor deposition method, a borax-urea method, a high-frequency plasma method, a hydrothermal method and a precursor method.
4. The modified white graphene polyester composite fiber according to claim 2, wherein the modifier is a mixture of polyvinyl alcohol, polyvinylpyrrolidone and sodium dodecyl benzene sulfonate, and the mass ratio of the modifier is 1: (2-4): (3-5).
5. The preparation method of the modified white graphene polyester composite fiber according to claim 1, wherein in the step 1, an ethanol solution with a mass concentration of 10% -50% is prepared from deionized water and ethanol at room temperature, dopamine is added and uniformly stirred, the mass concentration of the dopamine in the solution is 0.1% -5%, then the white graphene is added into the solution, ultrasonic dispersion is carried out for 10-30 min,
the mass concentration of the white graphene in the solution is 0.1-10%, and the modified white graphene powder is obtained by filtering and drying.
6. The method for preparing the modified white graphene polyester composite fiber according to claim 1, wherein in the step 2, the modified white graphene powder and the common polyester chips are respectively dried, and the water content after drying is controlled below 100 ppm.
7. The preparation method of the modified white graphene polyester composite fiber according to claim 6, wherein in the step 2, the polyester chips are ground to obtain polyester chip powder, the mesh number of the powder is more than 100 meshes, and then the white graphene powder and the modifier are added into the polyester chip powder and put into a high-speed mixer for mixing and stirring, wherein the rotating speed is 3000-10000 r/min, and the stirring time is 10-30 min, so as to obtain the white graphene polyester mixed powder.
8. The method for preparing the modified white graphene terylene composite fiber according to claim 1, wherein in the step 3, the temperatures from the first zone to the fifth zone of the double-screw extruder are respectively controlled at 270 ℃ of 260-.
9. The method for preparing the modified white graphene polyester composite fiber according to claim 1, wherein in the step 4, the modified white graphene polyester master batch is dried, the drying temperature is controlled to be 80-200 ℃, the water content of the master batch is controlled to be less than 100ppm, the dried master batch is added into a screw extruder for heating and melting, the master batch is filtered by a spinning box and then spun into bundles, the spinning temperature is 270-290 ℃, the spinning speed is 500-1500m/min, and the obtained primary yarns are subjected to processes of stretching, curling and the like to obtain the modified white graphene polyester composite fiber used under different conditions.
10. The modified white graphene polyester composite fiber prepared by the method of any one of claims 1 to 9.
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