CN109267166A - The preparation method of functional high strength and modulus polyethylene fibre based on graphene - Google Patents
The preparation method of functional high strength and modulus polyethylene fibre based on graphene Download PDFInfo
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- CN109267166A CN109267166A CN201811147548.3A CN201811147548A CN109267166A CN 109267166 A CN109267166 A CN 109267166A CN 201811147548 A CN201811147548 A CN 201811147548A CN 109267166 A CN109267166 A CN 109267166A
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- graphene oxide
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- white oil
- graphene
- spinning solution
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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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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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
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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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
- D01F1/103—Agents inhibiting growth of microorganisms
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Fibers (AREA)
Abstract
The preparation method of the invention discloses a kind of functional high strength and modulus polyethylene fibre based on graphene, including the following steps: (1) prepare reductive modification graphene oxide-white oil mixed liquor；(2) the high-strength and high-modulus weight polyethylene composite material based on graphene is prepared.The present invention can obviously improve product cutting resistance, and product is made to have excellent antistatic property, anti-microbial property.
Description
Technical field
The preparation method of the present invention relates to a kind of functional high strength and modulus polyethylene fibre based on graphene.
Background technique
It is poly- that ultra high molecular weight polyethylene fiber (UHMWPE fiber) is also known as high strength and modulus polyethylene fibre, high-orientation
Vinyl fiber, high-performance polyethylene fibres have high intensity, high-modulus, characteristics and the carbon fiber, aramid fiber such as corrosion-resistant, density is low
And claim three big high-performance fibers.And UHMWPE fiber is the highest commercialization high-performance fiber of specific strength.But due to its tool
There is the molecular structure close to theoretical limit intensity, the conformational structure of planar zigzag form, less side-chain radical, crystallinity is high and divides
Without stronger associative key in subchain.Cause it that creep easily occurs under stress, deformation occurs under the effect of lasting stress, and
Structure has chemical inertness, and surface polarity is lower, it is difficult to form composite material, greatly limit the application of the fiber.
Although UHMWPE fiber is in security protection, aerospace navigation, electronics, weapons, shipbuilding, building materials, sport, medical treatment etc.
Numerous areas, but the application field of product and range need to be extended, developmental difference and high value-added product, it can be achieved that
China's chemical fibre industry is changed from " scalar type " to " technology kind profit evaluation model ", and is continued to develop and grown in market competition.
Graphene and its oxide have excellent electricity, calorifics, mechanics and optical property.Graphene is most thin in the world
Material, it only has the thickness of single layer atom, about 0.335nm.Resistivity is 10-6 Ω/cm, for current resistivity in the world
The smallest material.Thermal coefficient is up to 5300W/mK, and electron mobility is more than 15000cm2/Vs under room temperature, than carbon nanometer
Pipe and monocrystalline silicon are high.Young's modulus is 1.1TPa, and breaking strength is up to 130Gpa.
Summary of the invention
That the purpose of the present invention is to provide a kind of product cutting indexes is high, have excellent performance, easy-operating based on graphene
The preparation method of functional high strength and modulus polyethylene fibre.
The technical solution of the invention is as follows:
A kind of preparation method of the functional high strength and modulus polyethylene fibre based on graphene, it is characterized in that: including
The following steps:
(1) reductive modification graphene oxide-white oil mixed liquor is prepared:
A) silane coupling agent for being equivalent to graphene oxide quality 0.5-3% is taken, is prepared with ethyl alcohol by the volume ratio of 1:20
At mixed liquor；
B) it adds graphene oxide into the mixed solution of step a), 30-90 minutes ultrasonic at a temperature of 60-90 DEG C, 120-
150 DEG C of drying, obtain modified graphene oxide；
C) by modified graphene oxide obtained by step b), within the scope of 150-200 DEG C, in ptfe autoclave
In, hydrothermal reduction 5-8h, 60-80 DEG C of drying obtains reductive modification graphene oxide；
D) by the obtained reductive modification graphene oxide of step c), dispersion is added in ultrasonic disperse 30 minutes in white oil
Agent continues ultrasound 3-8 hours, obtains reductive modification graphene oxide-white oil mixed liquor of stably dispersing；
(2) the high-strength and high-modulus weight polyethylene composite material based on graphene is prepared:
A) ultra-high molecular weight polyethylene is added to reductive modification graphene oxide-white oil mixed liquor under ultrasonic wave state
In, wherein the quality of reductive modification graphene oxide is the 0.6~2% of ultra-high molecular weight polyethylene quality；Through mulser high speed
Shear agitation, the speed of high shear agitation are 1000-3000r/min, and mixing time is 2~4 hours, are uniformly mixed and obtain the
One spinning solution (spinning solution shared by the total weight of redox graphene and ultra-high molecular weight polyethylene in the first spinning solution
Mass percent be 10~20%)；
B) the first spinning solution for obtaining step a) is placed 6~18 hours at 0~5 DEG C, obtains the second spinning solution；
C) after the second spinning solution in step b) being placed 24 hours at room temperature, dissolvant white oil is continuously added, obtains matter
Measure third spinning solution (redox graphene and the superhigh molecular weight polyethylene in third spinning solution that concentration is 6%~10%
The mass percent of spinning solution shared by the total weight of alkene is 6~10%)；
D) the third spinning solution in step c) is used into gel spinning method, spinning temperature is 220~280 DEG C, after spinning
Composite fibre is obtained through extraction and hot gas spring.
The dispersing agent is AT-80 or lW.
The present invention can obviously improve product cutting resistance, and product is made to have excellent antistatic property, anti-microbial property.
Properties of product table
The additive amount of graphene described in upper table/% refers to step (2) a) in reductive modification graphene oxide quality it is opposite
In the percentage of ultra-high molecular weight polyethylene quality.
Below with reference to embodiment, the invention will be further described.
Specific embodiment
Embodiment 1:
A kind of preparation method of the functional high strength and modulus polyethylene fibre based on graphene, including the following steps:
(1) reductive modification graphene oxide-white oil mixed liquor is prepared:
A) silane coupling agent for being equivalent to graphene oxide quality 1.5% is taken, is configured to ethyl alcohol by the volume ratio of 1:20
Mixed liquor；
B) it adds graphene oxide into the mixed solution of step a), at a temperature of 80 DEG C, ultrasound 50 minutes, 135 DEG C of drying,
Obtain modified graphene oxide；
C) by modified graphene oxide obtained by step b), at 180 DEG C, in ptfe autoclave, hydro-thermal is also
Former 6h, 70 DEG C of drying, obtains reductive modification graphene oxide；
D) by the obtained reductive modification graphene oxide of step c), dispersion is added in ultrasonic disperse 30 minutes in white oil
Agent AT-80, continues ultrasound 5 hours, obtains reductive modification graphene oxide-white oil mixed liquor of stably dispersing；
(2) the high-strength and high-modulus weight polyethylene composite material based on graphene is prepared:
A) ultra-high molecular weight polyethylene is added to reductive modification graphene oxide-white oil mixed liquor under ultrasonic wave state
In, wherein the quality of reductive modification graphene oxide is the 1% of ultra-high molecular weight polyethylene quality；It is stirred through mulser high speed shear
It mixes, the speed of high shear agitation is 2000r/min, and mixing time is 3 hours, is uniformly mixed and obtains the first spinning solution (the
The mass percent of spinning solution shared by the total weight of redox graphene and ultra-high molecular weight polyethylene in one spinning solution
For 15%)；
B) the first spinning solution for obtaining step a) is placed 10 hours at 3 DEG C, obtains the second spinning solution；
C) after the second spinning solution in step b) being placed 24 hours at room temperature, dissolvant white oil is continuously added, obtains
Three spinning solutions (spinning solution shared by the total weight of redox graphene and ultra-high molecular weight polyethylene in third spinning solution
Mass percent be 8%)；
D) the third spinning solution in step c) is used into gel spinning method, spinning temperature is 250 DEG C, through extracting after spinning
Composite fibre is obtained with hot gas spring.The dispersing agent is AT-80 or lW.
Embodiment 2:
A kind of preparation method of the functional high strength and modulus polyethylene fibre based on graphene, it is characterized in that: including
The following steps:
(1) reductive modification graphene oxide-white oil mixed liquor is prepared:
A) silane coupling agent for being equivalent to graphene oxide quality 0.6% is taken, is configured to ethyl alcohol by the volume ratio of 1:20
Mixed liquor；
B) it adds graphene oxide into the mixed solution of step a), at a temperature of 70 DEG C, ultrasound 40 minutes, 150 DEG C of drying,
Obtain modified graphene oxide；
C) by modified graphene oxide obtained by step b), within the scope of 160 DEG C, in ptfe autoclave,
Hydrothermal reduction 7h, 65 DEG C of drying obtain reductive modification graphene oxide；
D) by the obtained reductive modification graphene oxide of step c), dispersion is added in ultrasonic disperse 30 minutes in white oil
Agent lW, continues ultrasound 7 hours, obtains reductive modification graphene oxide-white oil mixed liquor of stably dispersing；
(2) the high-strength and high-modulus weight polyethylene composite material based on graphene is prepared:
A) ultra-high molecular weight polyethylene is added to reductive modification graphene oxide-white oil mixed liquor under ultrasonic wave state
In, wherein the quality of reductive modification graphene oxide is the 0.8% of ultra-high molecular weight polyethylene quality；Through mulser high speed shear
Stirring, the speed of high shear agitation are 2500r/min, and mixing time is 4 hours, are uniformly mixed and obtain the first spinning solution
(the quality percentage of spinning solution shared by the total weight of redox graphene and ultra-high molecular weight polyethylene in the first spinning solution
12%) number is；
B) the first spinning solution for obtaining step a) is placed 7 hours at 1 DEG C, obtains the second spinning solution；
C) after the second spinning solution in step b) being placed 24 hours at room temperature, dissolvant white oil is continuously added, obtains
Three spinning solutions (spinning solution shared by the total weight of redox graphene and ultra-high molecular weight polyethylene in third spinning solution
Mass percent be 7%)；
D) the third spinning solution in step c) is used into gel spinning method, spinning temperature is 220~280 DEG C, after spinning
Composite fibre is obtained through extraction and hot gas spring.
Claims (2)
1. a kind of preparation method of the functional high strength and modulus polyethylene fibre based on graphene, it is characterized in that: under including
Column step:
(1) reductive modification graphene oxide-white oil mixed liquor is prepared:
A) silane coupling agent for being equivalent to graphene oxide quality 0.5-3% is taken, is configured to mix by the volume ratio of 1:20 with ethyl alcohol
Liquid；
B) it adds graphene oxide into the mixed solution of step a), 30-90 minutes ultrasonic at a temperature of 60-90 DEG C, 120-150
DEG C drying, obtain modified graphene oxide；
C) by modified graphene oxide obtained by step b), within the scope of 150-200 DEG C, in ptfe autoclave,
Hydrothermal reduction 5-8h, 60-80 DEG C of drying obtain reductive modification graphene oxide；
D) by the obtained reductive modification graphene oxide of step c), dispersing agent is added in ultrasonic disperse 30 minutes in white oil, after
Continuous ultrasound 3-8 hours, obtain reductive modification graphene oxide-white oil mixed liquor of stably dispersing；
(2) the high-strength and high-modulus weight polyethylene composite material based on graphene is prepared:
A) ultra-high molecular weight polyethylene is added in reductive modification graphene oxide-white oil mixed liquor under ultrasonic wave state,
The quality of middle reductive modification graphene oxide is the 0.6 ~ 2% of ultra-high molecular weight polyethylene quality；It is stirred through mulser high speed shear
It mixes, the speed of high shear agitation is 1000-3000r/min, and mixing time is 2~4 hours, is uniformly mixed and obtains the first spinning
Solution；
B) the first spinning solution for obtaining step a) is placed 6~18 hours at 0~5 DEG C, obtains the second spinning solution；
C) after the second spinning solution in step b) being placed 24 hours at room temperature, dissolvant white oil is continuously added, obtains third spinning
Silk solution；
D) the third spinning solution in step c) is used into gel spinning method, spinning temperature is 220~280 DEG C, through extracting after spinning
It takes and obtains composite fibre with hot gas spring.
2. the preparation method of the functional high strength and modulus polyethylene fibre according to claim 1 based on graphene,
It is characterized in that: the dispersing agent is AT-80 or lW.
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| CN201811147548.3A CN109267166A (en) | 2018-09-29 | 2018-09-29 | The preparation method of functional high strength and modulus polyethylene fibre based on graphene |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109912873A (en) * | 2019-02-28 | 2019-06-21 | 常州兴烯石墨烯科技有限公司 | Anti- cutting graphite alkene ultra-high molecular weight polyethylene laminated film and preparation method thereof |
| CN112359435A (en) * | 2020-08-28 | 2021-02-12 | 青岛信泰科技有限公司 | Antibacterial and antistatic ultra-high molecular weight polyethylene fiber and preparation method thereof |
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| CN104762683A (en) * | 2015-04-09 | 2015-07-08 | 江苏九九久科技股份有限公司 | Graphene composite modified high-strength polyethylene fiber and preparation method thereof |
| CN106149085A (en) * | 2016-06-30 | 2016-11-23 | 常州第六元素材料科技股份有限公司 | A kind of cut resistant superhigh molecular weight polyethylene fibers and preparation technology thereof |
| CN106222780A (en) * | 2016-06-23 | 2016-12-14 | 常州第六元素材料科技股份有限公司 | A kind of Graphene/UHMWPE composite fibre and its preparation method and application |
| CN107099868A (en) * | 2017-06-05 | 2017-08-29 | 江苏锵尼玛新材料有限公司 | A kind of preparation method of the smooth high cut resistant UHMWPE filament fibers in surface |
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2018
- 2018-09-29 CN CN201811147548.3A patent/CN109267166A/en active Pending
Patent Citations (4)
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| CN104762683A (en) * | 2015-04-09 | 2015-07-08 | 江苏九九久科技股份有限公司 | Graphene composite modified high-strength polyethylene fiber and preparation method thereof |
| CN106222780A (en) * | 2016-06-23 | 2016-12-14 | 常州第六元素材料科技股份有限公司 | A kind of Graphene/UHMWPE composite fibre and its preparation method and application |
| CN106149085A (en) * | 2016-06-30 | 2016-11-23 | 常州第六元素材料科技股份有限公司 | A kind of cut resistant superhigh molecular weight polyethylene fibers and preparation technology thereof |
| CN107099868A (en) * | 2017-06-05 | 2017-08-29 | 江苏锵尼玛新材料有限公司 | A kind of preparation method of the smooth high cut resistant UHMWPE filament fibers in surface |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109912873A (en) * | 2019-02-28 | 2019-06-21 | 常州兴烯石墨烯科技有限公司 | Anti- cutting graphite alkene ultra-high molecular weight polyethylene laminated film and preparation method thereof |
| CN112359435A (en) * | 2020-08-28 | 2021-02-12 | 青岛信泰科技有限公司 | Antibacterial and antistatic ultra-high molecular weight polyethylene fiber and preparation method thereof |
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