Patent
US 10,793,974Method for Preparing Graphene-Polyamide Nanocomposite Fiber
Yongxiao Bai
US
Copyright © 2026 Matter42. All rights reserved.
Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a preparation process fl o w diagram of graphene-PA masterbatch;
Figure 2 is a preparation process fl o w diagram of grap h ene-p o lyamide nan ocompo site fiber.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
In the preparation of graphene-PA m asterbatch, A rotational speed of the high-speed mixing is 15000 rad/m in, and a mixing time thereof is 5 m in. A mass ratio of the modified graphene to the PA₆ chips is 1%:1 and the modified graphene is a mixture of the graphene oxide modified by CTAB (Cetyltrimethyl Ammonium Bromide) and the graphene oxide modified by polyethe rim ide (PE I) with a mass ratio of 1:2. The method for modifying the graphene by CTAB comprises steps o f: (1) sonicating the graphene oxide to be evenly dispersed in a deionized water; (2) and then adding the CTAB, wherein a ratio of the CTAB to the graphene oxide is 2:1; and (3) heating a solution obtained by the step (2) with stirring in a water bath at 50 ° C for two hours t o prepare the desired modified graphene. The method f o r modifying the graphene by p o lyetherimide (PEI) comprises steps o f: (1) ultrasonically dispersing the graphene oxide in a deionized water; (2) sonicating the PE I to be evenly dispersed, wherein a ratio of the PEI to the graphene oxide is 2:1-1:20; (3) mixing a product obtained by the step (1) with a product obtained by the step (2), adding a certain amount of EDC and sonicating f o r 60 m in, and then continui ng to add a c ertain am ou nt of EDC f or c atalyt ic r eact io n by stirr ing; and (4) obtaining the product after washed by cent rifigat ion. The PA₆ chips are dried until the water content thereof reaches 40 ppm.
In t h e preparation of graphene-PA c ompo site fiber, Th e graphene-PA masterbatch is dried at a temperature of 70-1 80° C f o r a peri od of 2 5 ho urs. A water c o ntent of the dried graphene-PA masterbatch is 40 pp m. Embodiment 4 The present embodiment relates to a method for preparing graphene-polya m ide nanoco m posi t e fiber; the specific operational steps are basically the same as those in Embodiment 1, except that:
Canceled
p A method fo r preparing grap h ene-pol y ami de nanocomposite fiber, wherein the method compri s es steps of: (S₁) mixing polyamide chips and graphene or modified graphene, and then extruding and palletizing, and obtaining graphene-polya m ide m asterbatch; and (S 2) melt-spinning after drying the graphene-po ly amide masterbatch, and finally obtaining the graph en e-po lyami de nanocompo s ite fiber, wherei n: the graphene i s graphene oxide or graphene; the modified g r aphene i s one or more members selected from a gro u p consisting of a graphene oxide modified by coupling agent, a g r aphene oxide modified by cation surfactant, a grap hene modified by alkyl bromide, a graphene modified by amin o compound and a graphene modified by pol y vin y l pyrrolidone and by pol y vinyl alcohol; the gr a phene modified by alkyl bromide is one o r more members selected f r om a group con s isting of a graphene oxide modified by br om odod ecane, a graphene oxide modified by bromohexadecane and a graphene oxide modified by bromooctadecane. Currently amended
(current ly amended): The method for preparing the graphene-polya m ide nanocomposite fiber according to claim 4, wherein a type of graphene in the modified grap h ene is one or more membe r s selected f rom a group consisting of a reduced graphene oxide obtained by thermal exp a nsion at elevated te m perature, a reduced graphene oxide obtained by thermal expansion at low temperature, a graphene exfoliated electro ch emica lly, a modified electrochemi cal ly-exfol i ated graph en e, a ball-milling mechanically exfoliated graphene, a three-roll milling mechanically e xfoliated graphene, a CVD gro wt h graphene, a graphene prepared by C 0 2-supercritical expansion and exfoliation, a graphene oxide exfoliated by c h emical oxidation, a gra phene p r epared by Hummers, and a graphene prepared by Modified Hummers. Currently amended
The method for preparing the graphene-polyamide nanocomposite fiber according to claim 4, wh erein in the step (S I), a mass ratio of the pol yam ide chips to the graphene or the modified graphene is 1: 0.01%-15 %. Currently amended
The method for preparing the grap h ene- polyamide nanocomposite fiber according to claim 4, wherein in the step (S₂), the graphene-p ol yamide masterbatch is dried and then melt-spun; the graphene-p oly amide masterbatch is d r ied at a temperature r ange from 50 to 220 0 C an d d ryin g time from 4 to 40 hours, and a water content of the dried graphene-polyamid e masterbatch is below 100 ppm. Currently amended
C laim 11: The method fo r preparing the graphene-p o lyamide nanocomposite fiber according to claim 4, wherein the polyamide comprises polyamide 6 and po l yamide 66. New
The method for preparing the graphene-polyamide nan oco m posite fibe r ac cording to cla im 4, wherein the graphene modified b y amino compound is one or more members selected from a group consisting of a graphene modified by capr o lactam, a graphene oxide modified by amino-terminated polyethylene glycol, a g raph ene modified by poly dial lyldim ethy lammn oniu mn chloride, a gr a phene modified by polyetherimide, a graphene modified by polyether amine, a graphene modified by hexade c yl trimethyl a m moni u m bromide, a gr aphene modified by N,N- dimeth ylac etamide, a graphene modified by N-(-A cetamido)iminodia cetic acid, a graphene oxide modified by pol y eth y lene imine and a graphene modified by N,N- dinethylami no- 2-c hloropropa n e hydrochloride. Currently amended
The method for preparing the graphene-polyamide nanocomposite fiber according to c laim 4, wherein in the step (S i), the p oly amide c hips an d the graphene or the modified graphene are separ ately dried and then mixed; the polyamide chips are dried until a water content thereof is controlled to be below 60 ppm. Currently amended
The method for preparing the graphene-polyamide nanocomposite fiber acco r ding to cla im 4, wh erein in the step (S I), the mixing is an intermittent mixing in a high-speed mixer; a rotational speed corresponding to the mixing is 5000-15000 rad/min a n d a mixing time is 1-30 minutes. Currently amended
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials2 process steps
Preparation of graphene-PA₆ nanocomposite fiber. PA₆ chips and modified graphene (electrochemically exfoliated graphene modified by caprolactam) are dried and mixed at high speed (15000 rad/min, 5 min), then fed into a twin-screw extruder (zone temperatures 220-235°C). The resulting masterbatch is dried and melt-spun by one-step FDY spin-drawing. PA₆ chips are dried to 30 ppm water content. Masterbatch is dried at 70-150°C for 30 hours to 30 ppm water content.
3 materials2 process steps
Preparation of graphene-PA₆ nanocomposite fiber. Modified graphene is a 1:1 mixture of CVD graphene modified by polydiallyldimethylammonium chloride and reduced graphene oxide (thermal expansion at elevated temperature) modified by polyetheramine. High-speed mixing at 14000 rad/min for 5 min. PA₆ chips dried to 60 ppm. Masterbatch dried at 60-150°C for 28 hours, water content below 60 ppm.
Layer stacks claimed or described, ordered top of device to substrate.
graphene-polyamide nanocomposite fiber
Materials described outside the worked examples.
graphene oxide modified by CTAB
graphene oxide modified by polyetherimide (PEI)
CTAB (Cetyltrimethyl Ammonium Bromide)
EDC
graphene-PA masterbatch
graphene oxide
graphene
graphene oxide modified by coupling agent
graphene oxide modified by cation surfactant
graphene modified by alkyl bromide
graphene modified by amino compound
graphene modified by polyvinyl pyrrolidone
graphene modified by polyvinyl alcohol
graphene oxide modified by bromododecane
graphene oxide modified by bromohexadecane
graphene oxide modified by bromooctadecane
graphene modified by caprolactam
graphene oxide modified by amino-terminated polyethylene glycol
graphene modified by polydiallyldimethylammonium chloride
graphene modified by polyetherimide
graphene modified by polyetheramine
graphene modified by hexadecyl trimethyl ammonium bromide
graphene modified by N,N-dimethylacetamide
graphene modified by N-(-Acetamido)iminodiacetic acid
graphene oxide modified by polyethylene imine
graphene modified by N,N-dimethylamino-2-chloropropane hydrochloride
reduced graphene oxide obtained by thermal expansion at elevated temperature
reduced graphene oxide obtained by thermal expansion at low temperature
graphene exfoliated electrochemically
modified electrochemically-exfoliated graphene
ball-milling mechanically exfoliated graphene
three-roll milling mechanically exfoliated graphene
CVD growth graphene
graphene prepared by CO₂-supercritical expansion and exfoliation
graphene oxide exfoliated by chemical oxidation
graphene prepared by Hummers method
graphene prepared by Modified Hummers method
polyamide 6 (PA₆)
polyamide 66 (PA₆₆)
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | 0–150 °C | — |
Temperature | 60–150 °C | — |
Duration | 4–40 hours | — |
Temperature | 70–150 °C | — |
Temperature | 70–140 °C | — |
Duration | 1–30 minutes | — |
Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a preparation process fl o w diagram of graphene-PA masterbatch;
Figure 2 is a preparation process fl o w diagram of grap h ene-p o lyamide nan ocompo site fiber.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
In the preparation of graphene-PA m asterbatch, A rotational speed of the high-speed mixing is 15000 rad/m in, and a mixing time thereof is 5 m in. A mass ratio of the modified graphene to the PA₆ chips is 1%:1 and the modified graphene is a mixture of the graphene oxide modified by CTAB (Cetyltrimethyl Ammonium Bromide) and the graphene oxide modified by polyethe rim ide (PE I) with a mass ratio of 1:2. The method for modifying the graphene by CTAB comprises steps o f: (1) sonicating the graphene oxide to be evenly dispersed in a deionized water; (2) and then adding the CTAB, wherein a ratio of the CTAB to the graphene oxide is 2:1; and (3) heating a solution obtained by the step (2) with stirring in a water bath at 50 ° C for two hours t o prepare the desired modified graphene. The method f o r modifying the graphene by p o lyetherimide (PEI) comprises steps o f: (1) ultrasonically dispersing the graphene oxide in a deionized water; (2) sonicating the PE I to be evenly dispersed, wherein a ratio of the PEI to the graphene oxide is 2:1-1:20; (3) mixing a product obtained by the step (1) with a product obtained by the step (2), adding a certain amount of EDC and sonicating f o r 60 m in, and then continui ng to add a c ertain am ou nt of EDC f or c atalyt ic r eact io n by stirr ing; and (4) obtaining the product after washed by cent rifigat ion. The PA₆ chips are dried until the water content thereof reaches 40 ppm.
In t h e preparation of graphene-PA c ompo site fiber, Th e graphene-PA masterbatch is dried at a temperature of 70-1 80° C f o r a peri od of 2 5 ho urs. A water c o ntent of the dried graphene-PA masterbatch is 40 pp m. Embodiment 4 The present embodiment relates to a method for preparing graphene-polya m ide nanoco m posi t e fiber; the specific operational steps are basically the same as those in Embodiment 1, except that:
Canceled
p A method fo r preparing grap h ene-pol y ami de nanocomposite fiber, wherein the method compri s es steps of: (S₁) mixing polyamide chips and graphene or modified graphene, and then extruding and palletizing, and obtaining graphene-polya m ide m asterbatch; and (S 2) melt-spinning after drying the graphene-po ly amide masterbatch, and finally obtaining the graph en e-po lyami de nanocompo s ite fiber, wherei n: the graphene i s graphene oxide or graphene; the modified g r aphene i s one or more members selected from a gro u p consisting of a graphene oxide modified by coupling agent, a g r aphene oxide modified by cation surfactant, a grap hene modified by alkyl bromide, a graphene modified by amin o compound and a graphene modified by pol y vin y l pyrrolidone and by pol y vinyl alcohol; the gr a phene modified by alkyl bromide is one o r more members selected f r om a group con s isting of a graphene oxide modified by br om odod ecane, a graphene oxide modified by bromohexadecane and a graphene oxide modified by bromooctadecane. Currently amended
(current ly amended): The method for preparing the graphene-polya m ide nanocomposite fiber according to claim 4, wherein a type of graphene in the modified grap h ene is one or more membe r s selected f rom a group consisting of a reduced graphene oxide obtained by thermal exp a nsion at elevated te m perature, a reduced graphene oxide obtained by thermal expansion at low temperature, a graphene exfoliated electro ch emica lly, a modified electrochemi cal ly-exfol i ated graph en e, a ball-milling mechanically exfoliated graphene, a three-roll milling mechanically e xfoliated graphene, a CVD gro wt h graphene, a graphene prepared by C 0 2-supercritical expansion and exfoliation, a graphene oxide exfoliated by c h emical oxidation, a gra phene p r epared by Hummers, and a graphene prepared by Modified Hummers. Currently amended
The method for preparing the graphene-polyamide nanocomposite fiber according to claim 4, wh erein in the step (S I), a mass ratio of the pol yam ide chips to the graphene or the modified graphene is 1: 0.01%-15 %. Currently amended
The method for preparing the grap h ene- polyamide nanocomposite fiber according to claim 4, wherein in the step (S₂), the graphene-p ol yamide masterbatch is dried and then melt-spun; the graphene-p oly amide masterbatch is d r ied at a temperature r ange from 50 to 220 0 C an d d ryin g time from 4 to 40 hours, and a water content of the dried graphene-polyamid e masterbatch is below 100 ppm. Currently amended
C laim 11: The method fo r preparing the graphene-p o lyamide nanocomposite fiber according to claim 4, wherein the polyamide comprises polyamide 6 and po l yamide 66. New
The method for preparing the graphene-polyamide nan oco m posite fibe r ac cording to cla im 4, wherein the graphene modified b y amino compound is one or more members selected from a group consisting of a graphene modified by capr o lactam, a graphene oxide modified by amino-terminated polyethylene glycol, a g raph ene modified by poly dial lyldim ethy lammn oniu mn chloride, a gr a phene modified by polyetherimide, a graphene modified by polyether amine, a graphene modified by hexade c yl trimethyl a m moni u m bromide, a gr aphene modified by N,N- dimeth ylac etamide, a graphene modified by N-(-A cetamido)iminodia cetic acid, a graphene oxide modified by pol y eth y lene imine and a graphene modified by N,N- dinethylami no- 2-c hloropropa n e hydrochloride. Currently amended
The method for preparing the graphene-polyamide nanocomposite fiber according to c laim 4, wherein in the step (S i), the p oly amide c hips an d the graphene or the modified graphene are separ ately dried and then mixed; the polyamide chips are dried until a water content thereof is controlled to be below 60 ppm. Currently amended
The method for preparing the graphene-polyamide nanocomposite fiber acco r ding to cla im 4, wh erein in the step (S I), the mixing is an intermittent mixing in a high-speed mixer; a rotational speed corresponding to the mixing is 5000-15000 rad/min a n d a mixing time is 1-30 minutes. Currently amended
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials2 process steps
Preparation of graphene-PA₆ nanocomposite fiber. PA₆ chips and modified graphene (electrochemically exfoliated graphene modified by caprolactam) are dried and mixed at high speed (15000 rad/min, 5 min), then fed into a twin-screw extruder (zone temperatures 220-235°C). The resulting masterbatch is dried and melt-spun by one-step FDY spin-drawing. PA₆ chips are dried to 30 ppm water content. Masterbatch is dried at 70-150°C for 30 hours to 30 ppm water content.
3 materials2 process steps
Preparation of graphene-PA₆ nanocomposite fiber. Modified graphene is a 1:1 mixture of CVD graphene modified by polydiallyldimethylammonium chloride and reduced graphene oxide (thermal expansion at elevated temperature) modified by polyetheramine. High-speed mixing at 14000 rad/min for 5 min. PA₆ chips dried to 60 ppm. Masterbatch dried at 60-150°C for 28 hours, water content below 60 ppm.
Layer stacks claimed or described, ordered top of device to substrate.
graphene-polyamide nanocomposite fiber
Materials described outside the worked examples.
graphene oxide modified by CTAB
graphene oxide modified by polyetherimide (PEI)
CTAB (Cetyltrimethyl Ammonium Bromide)
EDC
graphene-PA masterbatch
graphene oxide
graphene
graphene oxide modified by coupling agent
graphene oxide modified by cation surfactant
graphene modified by alkyl bromide
graphene modified by amino compound
graphene modified by polyvinyl pyrrolidone
graphene modified by polyvinyl alcohol
graphene oxide modified by bromododecane
graphene oxide modified by bromohexadecane
graphene oxide modified by bromooctadecane
graphene modified by caprolactam
graphene oxide modified by amino-terminated polyethylene glycol
graphene modified by polydiallyldimethylammonium chloride
graphene modified by polyetherimide
graphene modified by polyetheramine
graphene modified by hexadecyl trimethyl ammonium bromide
graphene modified by N,N-dimethylacetamide
graphene modified by N-(-Acetamido)iminodiacetic acid
graphene oxide modified by polyethylene imine
graphene modified by N,N-dimethylamino-2-chloropropane hydrochloride
reduced graphene oxide obtained by thermal expansion at elevated temperature
reduced graphene oxide obtained by thermal expansion at low temperature
graphene exfoliated electrochemically
modified electrochemically-exfoliated graphene
ball-milling mechanically exfoliated graphene
three-roll milling mechanically exfoliated graphene
CVD growth graphene
graphene prepared by CO₂-supercritical expansion and exfoliation
graphene oxide exfoliated by chemical oxidation
graphene prepared by Hummers method
graphene prepared by Modified Hummers method
polyamide 6 (PA₆)
polyamide 66 (PA₆₆)
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | 0–150 °C | — |
Temperature | 60–150 °C | — |
Duration | 4–40 hours | — |
Temperature | 70–150 °C | — |
Temperature | 70–140 °C | — |
Duration | 1–30 minutes | — |
Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a preparation process fl o w diagram of graphene-PA masterbatch;
Figure 2 is a preparation process fl o w diagram of grap h ene-p o lyamide nan ocompo site fiber.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
In the preparation of graphene-PA m asterbatch, A rotational speed of the high-speed mixing is 15000 rad/m in, and a mixing time thereof is 5 m in. A mass ratio of the modified graphene to the PA₆ chips is 1%:1 and the modified graphene is a mixture of the graphene oxide modified by CTAB (Cetyltrimethyl Ammonium Bromide) and the graphene oxide modified by polyethe rim ide (PE I) with a mass ratio of 1:2. The method for modifying the graphene by CTAB comprises steps o f: (1) sonicating the graphene oxide to be evenly dispersed in a deionized water; (2) and then adding the CTAB, wherein a ratio of the CTAB to the graphene oxide is 2:1; and (3) heating a solution obtained by the step (2) with stirring in a water bath at 50 ° C for two hours t o prepare the desired modified graphene. The method f o r modifying the graphene by p o lyetherimide (PEI) comprises steps o f: (1) ultrasonically dispersing the graphene oxide in a deionized water; (2) sonicating the PE I to be evenly dispersed, wherein a ratio of the PEI to the graphene oxide is 2:1-1:20; (3) mixing a product obtained by the step (1) with a product obtained by the step (2), adding a certain amount of EDC and sonicating f o r 60 m in, and then continui ng to add a c ertain am ou nt of EDC f or c atalyt ic r eact io n by stirr ing; and (4) obtaining the product after washed by cent rifigat ion. The PA₆ chips are dried until the water content thereof reaches 40 ppm.
In t h e preparation of graphene-PA c ompo site fiber, Th e graphene-PA masterbatch is dried at a temperature of 70-1 80° C f o r a peri od of 2 5 ho urs. A water c o ntent of the dried graphene-PA masterbatch is 40 pp m. Embodiment 4 The present embodiment relates to a method for preparing graphene-polya m ide nanoco m posi t e fiber; the specific operational steps are basically the same as those in Embodiment 1, except that:
Canceled
p A method fo r preparing grap h ene-pol y ami de nanocomposite fiber, wherein the method compri s es steps of: (S₁) mixing polyamide chips and graphene or modified graphene, and then extruding and palletizing, and obtaining graphene-polya m ide m asterbatch; and (S 2) melt-spinning after drying the graphene-po ly amide masterbatch, and finally obtaining the graph en e-po lyami de nanocompo s ite fiber, wherei n: the graphene i s graphene oxide or graphene; the modified g r aphene i s one or more members selected from a gro u p consisting of a graphene oxide modified by coupling agent, a g r aphene oxide modified by cation surfactant, a grap hene modified by alkyl bromide, a graphene modified by amin o compound and a graphene modified by pol y vin y l pyrrolidone and by pol y vinyl alcohol; the gr a phene modified by alkyl bromide is one o r more members selected f r om a group con s isting of a graphene oxide modified by br om odod ecane, a graphene oxide modified by bromohexadecane and a graphene oxide modified by bromooctadecane. Currently amended
(current ly amended): The method for preparing the graphene-polya m ide nanocomposite fiber according to claim 4, wherein a type of graphene in the modified grap h ene is one or more membe r s selected f rom a group consisting of a reduced graphene oxide obtained by thermal exp a nsion at elevated te m perature, a reduced graphene oxide obtained by thermal expansion at low temperature, a graphene exfoliated electro ch emica lly, a modified electrochemi cal ly-exfol i ated graph en e, a ball-milling mechanically exfoliated graphene, a three-roll milling mechanically e xfoliated graphene, a CVD gro wt h graphene, a graphene prepared by C 0 2-supercritical expansion and exfoliation, a graphene oxide exfoliated by c h emical oxidation, a gra phene p r epared by Hummers, and a graphene prepared by Modified Hummers. Currently amended
The method for preparing the graphene-polyamide nanocomposite fiber according to claim 4, wh erein in the step (S I), a mass ratio of the pol yam ide chips to the graphene or the modified graphene is 1: 0.01%-15 %. Currently amended
The method for preparing the grap h ene- polyamide nanocomposite fiber according to claim 4, wherein in the step (S₂), the graphene-p ol yamide masterbatch is dried and then melt-spun; the graphene-p oly amide masterbatch is d r ied at a temperature r ange from 50 to 220 0 C an d d ryin g time from 4 to 40 hours, and a water content of the dried graphene-polyamid e masterbatch is below 100 ppm. Currently amended
C laim 11: The method fo r preparing the graphene-p o lyamide nanocomposite fiber according to claim 4, wherein the polyamide comprises polyamide 6 and po l yamide 66. New
The method for preparing the graphene-polyamide nan oco m posite fibe r ac cording to cla im 4, wherein the graphene modified b y amino compound is one or more members selected from a group consisting of a graphene modified by capr o lactam, a graphene oxide modified by amino-terminated polyethylene glycol, a g raph ene modified by poly dial lyldim ethy lammn oniu mn chloride, a gr a phene modified by polyetherimide, a graphene modified by polyether amine, a graphene modified by hexade c yl trimethyl a m moni u m bromide, a gr aphene modified by N,N- dimeth ylac etamide, a graphene modified by N-(-A cetamido)iminodia cetic acid, a graphene oxide modified by pol y eth y lene imine and a graphene modified by N,N- dinethylami no- 2-c hloropropa n e hydrochloride. Currently amended
The method for preparing the graphene-polyamide nanocomposite fiber according to c laim 4, wherein in the step (S i), the p oly amide c hips an d the graphene or the modified graphene are separ ately dried and then mixed; the polyamide chips are dried until a water content thereof is controlled to be below 60 ppm. Currently amended
The method for preparing the graphene-polyamide nanocomposite fiber acco r ding to cla im 4, wh erein in the step (S I), the mixing is an intermittent mixing in a high-speed mixer; a rotational speed corresponding to the mixing is 5000-15000 rad/min a n d a mixing time is 1-30 minutes. Currently amended
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials2 process steps
Preparation of graphene-PA₆ nanocomposite fiber. PA₆ chips and modified graphene (electrochemically exfoliated graphene modified by caprolactam) are dried and mixed at high speed (15000 rad/min, 5 min), then fed into a twin-screw extruder (zone temperatures 220-235°C). The resulting masterbatch is dried and melt-spun by one-step FDY spin-drawing. PA₆ chips are dried to 30 ppm water content. Masterbatch is dried at 70-150°C for 30 hours to 30 ppm water content.
3 materials2 process steps
Preparation of graphene-PA₆ nanocomposite fiber. Modified graphene is a 1:1 mixture of CVD graphene modified by polydiallyldimethylammonium chloride and reduced graphene oxide (thermal expansion at elevated temperature) modified by polyetheramine. High-speed mixing at 14000 rad/min for 5 min. PA₆ chips dried to 60 ppm. Masterbatch dried at 60-150°C for 28 hours, water content below 60 ppm.
Layer stacks claimed or described, ordered top of device to substrate.
graphene-polyamide nanocomposite fiber
Materials described outside the worked examples.
graphene oxide modified by CTAB
graphene oxide modified by polyetherimide (PEI)
CTAB (Cetyltrimethyl Ammonium Bromide)
EDC
graphene-PA masterbatch
graphene oxide
graphene
graphene oxide modified by coupling agent
graphene oxide modified by cation surfactant
graphene modified by alkyl bromide
graphene modified by amino compound
graphene modified by polyvinyl pyrrolidone
graphene modified by polyvinyl alcohol
graphene oxide modified by bromododecane
graphene oxide modified by bromohexadecane
graphene oxide modified by bromooctadecane
graphene modified by caprolactam
graphene oxide modified by amino-terminated polyethylene glycol
graphene modified by polydiallyldimethylammonium chloride
graphene modified by polyetherimide
graphene modified by polyetheramine
graphene modified by hexadecyl trimethyl ammonium bromide
graphene modified by N,N-dimethylacetamide
graphene modified by N-(-Acetamido)iminodiacetic acid
graphene oxide modified by polyethylene imine
graphene modified by N,N-dimethylamino-2-chloropropane hydrochloride
reduced graphene oxide obtained by thermal expansion at elevated temperature
reduced graphene oxide obtained by thermal expansion at low temperature
graphene exfoliated electrochemically
modified electrochemically-exfoliated graphene
ball-milling mechanically exfoliated graphene
three-roll milling mechanically exfoliated graphene
CVD growth graphene
graphene prepared by CO₂-supercritical expansion and exfoliation
graphene oxide exfoliated by chemical oxidation
graphene prepared by Hummers method
graphene prepared by Modified Hummers method
polyamide 6 (PA₆)
polyamide 66 (PA₆₆)
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | 0–150 °C | — |
Temperature | 60–150 °C | — |
Duration | 4–40 hours | — |
Temperature | 70–150 °C | — |
Temperature | 70–140 °C | — |
Duration | 1–30 minutes | — |
Patent drawings and their descriptions. Click a drawing to enlarge it.
Figure 1 is a preparation process fl o w diagram of graphene-PA masterbatch;
Figure 2 is a preparation process fl o w diagram of grap h ene-p o lyamide nan ocompo site fiber.
Claims define the patent's legal scope. Independent claims stand alone; dependent claims (nested) narrow them. Click a claim to expand its dependents.
In the preparation of graphene-PA m asterbatch, A rotational speed of the high-speed mixing is 15000 rad/m in, and a mixing time thereof is 5 m in. A mass ratio of the modified graphene to the PA₆ chips is 1%:1 and the modified graphene is a mixture of the graphene oxide modified by CTAB (Cetyltrimethyl Ammonium Bromide) and the graphene oxide modified by polyethe rim ide (PE I) with a mass ratio of 1:2. The method for modifying the graphene by CTAB comprises steps o f: (1) sonicating the graphene oxide to be evenly dispersed in a deionized water; (2) and then adding the CTAB, wherein a ratio of the CTAB to the graphene oxide is 2:1; and (3) heating a solution obtained by the step (2) with stirring in a water bath at 50 ° C for two hours t o prepare the desired modified graphene. The method f o r modifying the graphene by p o lyetherimide (PEI) comprises steps o f: (1) ultrasonically dispersing the graphene oxide in a deionized water; (2) sonicating the PE I to be evenly dispersed, wherein a ratio of the PEI to the graphene oxide is 2:1-1:20; (3) mixing a product obtained by the step (1) with a product obtained by the step (2), adding a certain amount of EDC and sonicating f o r 60 m in, and then continui ng to add a c ertain am ou nt of EDC f or c atalyt ic r eact io n by stirr ing; and (4) obtaining the product after washed by cent rifigat ion. The PA₆ chips are dried until the water content thereof reaches 40 ppm.
In t h e preparation of graphene-PA c ompo site fiber, Th e graphene-PA masterbatch is dried at a temperature of 70-1 80° C f o r a peri od of 2 5 ho urs. A water c o ntent of the dried graphene-PA masterbatch is 40 pp m. Embodiment 4 The present embodiment relates to a method for preparing graphene-polya m ide nanoco m posi t e fiber; the specific operational steps are basically the same as those in Embodiment 1, except that:
Canceled
p A method fo r preparing grap h ene-pol y ami de nanocomposite fiber, wherein the method compri s es steps of: (S₁) mixing polyamide chips and graphene or modified graphene, and then extruding and palletizing, and obtaining graphene-polya m ide m asterbatch; and (S 2) melt-spinning after drying the graphene-po ly amide masterbatch, and finally obtaining the graph en e-po lyami de nanocompo s ite fiber, wherei n: the graphene i s graphene oxide or graphene; the modified g r aphene i s one or more members selected from a gro u p consisting of a graphene oxide modified by coupling agent, a g r aphene oxide modified by cation surfactant, a grap hene modified by alkyl bromide, a graphene modified by amin o compound and a graphene modified by pol y vin y l pyrrolidone and by pol y vinyl alcohol; the gr a phene modified by alkyl bromide is one o r more members selected f r om a group con s isting of a graphene oxide modified by br om odod ecane, a graphene oxide modified by bromohexadecane and a graphene oxide modified by bromooctadecane. Currently amended
(current ly amended): The method for preparing the graphene-polya m ide nanocomposite fiber according to claim 4, wherein a type of graphene in the modified grap h ene is one or more membe r s selected f rom a group consisting of a reduced graphene oxide obtained by thermal exp a nsion at elevated te m perature, a reduced graphene oxide obtained by thermal expansion at low temperature, a graphene exfoliated electro ch emica lly, a modified electrochemi cal ly-exfol i ated graph en e, a ball-milling mechanically exfoliated graphene, a three-roll milling mechanically e xfoliated graphene, a CVD gro wt h graphene, a graphene prepared by C 0 2-supercritical expansion and exfoliation, a graphene oxide exfoliated by c h emical oxidation, a gra phene p r epared by Hummers, and a graphene prepared by Modified Hummers. Currently amended
The method for preparing the graphene-polyamide nanocomposite fiber according to claim 4, wh erein in the step (S I), a mass ratio of the pol yam ide chips to the graphene or the modified graphene is 1: 0.01%-15 %. Currently amended
The method for preparing the grap h ene- polyamide nanocomposite fiber according to claim 4, wherein in the step (S₂), the graphene-p ol yamide masterbatch is dried and then melt-spun; the graphene-p oly amide masterbatch is d r ied at a temperature r ange from 50 to 220 0 C an d d ryin g time from 4 to 40 hours, and a water content of the dried graphene-polyamid e masterbatch is below 100 ppm. Currently amended
C laim 11: The method fo r preparing the graphene-p o lyamide nanocomposite fiber according to claim 4, wherein the polyamide comprises polyamide 6 and po l yamide 66. New
The method for preparing the graphene-polyamide nan oco m posite fibe r ac cording to cla im 4, wherein the graphene modified b y amino compound is one or more members selected from a group consisting of a graphene modified by capr o lactam, a graphene oxide modified by amino-terminated polyethylene glycol, a g raph ene modified by poly dial lyldim ethy lammn oniu mn chloride, a gr a phene modified by polyetherimide, a graphene modified by polyether amine, a graphene modified by hexade c yl trimethyl a m moni u m bromide, a gr aphene modified by N,N- dimeth ylac etamide, a graphene modified by N-(-A cetamido)iminodia cetic acid, a graphene oxide modified by pol y eth y lene imine and a graphene modified by N,N- dinethylami no- 2-c hloropropa n e hydrochloride. Currently amended
The method for preparing the graphene-polyamide nanocomposite fiber according to c laim 4, wherein in the step (S i), the p oly amide c hips an d the graphene or the modified graphene are separ ately dried and then mixed; the polyamide chips are dried until a water content thereof is controlled to be below 60 ppm. Currently amended
The method for preparing the graphene-polyamide nanocomposite fiber acco r ding to cla im 4, wh erein in the step (S I), the mixing is an intermittent mixing in a high-speed mixer; a rotational speed corresponding to the mixing is 5000-15000 rad/min a n d a mixing time is 1-30 minutes. Currently amended
Embodiments described in the patent, grouped by the materials and process steps they use.
3 materials2 process steps
Preparation of graphene-PA₆ nanocomposite fiber. PA₆ chips and modified graphene (electrochemically exfoliated graphene modified by caprolactam) are dried and mixed at high speed (15000 rad/min, 5 min), then fed into a twin-screw extruder (zone temperatures 220-235°C). The resulting masterbatch is dried and melt-spun by one-step FDY spin-drawing. PA₆ chips are dried to 30 ppm water content. Masterbatch is dried at 70-150°C for 30 hours to 30 ppm water content.
3 materials2 process steps
Preparation of graphene-PA₆ nanocomposite fiber. Modified graphene is a 1:1 mixture of CVD graphene modified by polydiallyldimethylammonium chloride and reduced graphene oxide (thermal expansion at elevated temperature) modified by polyetheramine. High-speed mixing at 14000 rad/min for 5 min. PA₆ chips dried to 60 ppm. Masterbatch dried at 60-150°C for 28 hours, water content below 60 ppm.
Layer stacks claimed or described, ordered top of device to substrate.
graphene-polyamide nanocomposite fiber
Materials described outside the worked examples.
graphene oxide modified by CTAB
graphene oxide modified by polyetherimide (PEI)
CTAB (Cetyltrimethyl Ammonium Bromide)
EDC
graphene-PA masterbatch
graphene oxide
graphene
graphene oxide modified by coupling agent
graphene oxide modified by cation surfactant
graphene modified by alkyl bromide
graphene modified by amino compound
graphene modified by polyvinyl pyrrolidone
graphene modified by polyvinyl alcohol
graphene oxide modified by bromododecane
graphene oxide modified by bromohexadecane
graphene oxide modified by bromooctadecane
graphene modified by caprolactam
graphene oxide modified by amino-terminated polyethylene glycol
graphene modified by polydiallyldimethylammonium chloride
graphene modified by polyetherimide
graphene modified by polyetheramine
graphene modified by hexadecyl trimethyl ammonium bromide
graphene modified by N,N-dimethylacetamide
graphene modified by N-(-Acetamido)iminodiacetic acid
graphene oxide modified by polyethylene imine
graphene modified by N,N-dimethylamino-2-chloropropane hydrochloride
reduced graphene oxide obtained by thermal expansion at elevated temperature
reduced graphene oxide obtained by thermal expansion at low temperature
graphene exfoliated electrochemically
modified electrochemically-exfoliated graphene
ball-milling mechanically exfoliated graphene
three-roll milling mechanically exfoliated graphene
CVD growth graphene
graphene prepared by CO₂-supercritical expansion and exfoliation
graphene oxide exfoliated by chemical oxidation
graphene prepared by Hummers method
graphene prepared by Modified Hummers method
polyamide 6 (PA₆)
polyamide 66 (PA₆₆)
Performance values and ranges asserted in the specification or claims.
| Property | Value | Material |
|---|---|---|
Temperature | 0–150 °C | — |
Temperature | 60–150 °C | — |
Duration | 4–40 hours | — |
Temperature | 70–150 °C | — |
Temperature | 70–140 °C | — |
Duration | 1–30 minutes | — |