CN105586646A - Wet spinning method - Google Patents
Wet spinning method Download PDFInfo
- Publication number
- CN105586646A CN105586646A CN201510991314.7A CN201510991314A CN105586646A CN 105586646 A CN105586646 A CN 105586646A CN 201510991314 A CN201510991314 A CN 201510991314A CN 105586646 A CN105586646 A CN 105586646A
- Authority
- CN
- China
- Prior art keywords
- graphene oxide
- wet spinning
- ionic liquid
- spinning process
- fiber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000002166 wet spinning Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 37
- 239000000835 fiber Substances 0.000 claims abstract description 23
- 239000002608 ionic liquid Substances 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 238000007711 solidification Methods 0.000 claims abstract description 11
- 230000008023 solidification Effects 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000005516 engineering process Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- KAIPKTYOBMEXRR-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole Chemical compound CCCCN1CN(C)C=C1 KAIPKTYOBMEXRR-UHFFFAOYSA-N 0.000 claims description 4
- 238000005660 chlorination reaction Methods 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M Lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000008719 thickening Effects 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 6
- 238000009987 spinning Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 239000005416 organic matter Substances 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 10
- 239000011229 interlayer Substances 0.000 description 2
- 241000446313 Lamella Species 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
Classifications
-
- 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
- D01D5/06—Wet 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/12—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with inorganic substances ; Intercalation
-
- 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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/02—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fibres, slivers or rovings
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention relates to a wet spinning method and belongs to the technical field of graphene composite material preparation. According to the method, thick and sticky graphene oxide is used as a spinning solution, an ionic liquid aqueous solution is adopted as a solidification solution, and the performance of spun fiber is obviously improved after water washing. Graphene oxide fiber is prepared in the mode that ionic liquid of organic matter produces ionic bond connection between graphene oxide slice layers, the ionic liquid in the graphene oxide fiber can be sufficiently arranged between the graphene oxide slice layers through water washing, and therefore the performance of the graphene oxide fiber is improved. The wet spinning method is easy to operate, free of pollution, environmentally friendly, low in cost and capable of achieving rapid and mass production, and the performance of the washed graphene oxide fiber is significantly improved. The method can be widely applied to the field of modification and the like of graphene oxide materials.
Description
Technical field
The present invention relates to a kind of wet spinning process, belong to technology prepared by graphene oxide composite materialField.
Background technology
At present, what graphene oxide fiber mainly adopted is the technology preparation of wet spinning, and it tests stepRapid relatively immobilization. As its step 1, be all first graphite to be become to thick graphite oxide through oxidizing processAlkene, then selects suitable solidification liquid to prepare fiber with liquid graphene oxide as spinning solution. ButBe this process not focus be placed on wet spinning process the follow-up place of spun graphene oxide fiberIn reason. We draw by experiment and utilize the spun fiber of wet spinning institute its graphite oxide after washingBetween alkene lamella, active force increases, and causes its performance to increase significantly.
Summary of the invention
The technical problem that the present invention solves is: propose a kind of wet spinning process, prepare through wet spinningAfter the graphene oxide fiber going out dries through washing 5～100 seconds. Can make like this graphene oxide sheetIt is large that the active force of interlayer becomes, thereby promote the performance of graphene oxide fiber.
In order to solve the problems of the technologies described above, the technical scheme that the present invention proposes is: a kind of wet spinning sideMethod, comprises the following steps:
Step 1: prepare graphene oxide as raw material through oxidizing process taking graphite, be placed in oil bath panUnder uniform temperature, stirring is concentrated to thick.
Step 2: the ionic liquid aqueous solution that configuration concentration is suitable
Step 3: utilize wet spinning technology, prepare graphene fiber taking the ionic liquid aqueous solution as solidification liquid.
Step 4: put into and fill distillation after spun graphene oxide fiber dries in air atmosphereAfter soaking in the tank of water, take out and dry.
Preferably, the graphene oxide thickening temperature described in step 1 is 50 DEG C～60 DEG C, concentrated oxidationGraphene viscosity is 985MPa.S left and right.
Preferably, the ionic liquid concentration of aqueous solution described in step 2 is respectively: 1-butyl-3-methylimidazole LLactate 0.00477mol/L; Chlorination 1-amine propyl group-3-methylimidazole 0.00067mol/L.
Preferably, in the wet spinning process described in step 3, the extrusion capacity of graphene oxide is0.4mL/min; The pin mouth internal diameter of wet spinning syringe needle used is 0.50mm.
Preferably, the graphene oxide fiber drying described in step 4 is immersed in distilled water 10 seconds
Beneficial effect of the present invention: prepare graphene oxide taking graphite as raw material through oxidizing process, with thicknessThe graphene oxide of shape is as spinning solution, and what solidification liquid adopted is the aqueous solution of ionic liquid. Utilize wet methodAfter the spun fiber of spinning process dries, be placed in distilled water and wash 5～100 seconds. Fiber surface after washingSoluble in water the getting rid of of ionic liquid, the ionic liquid of fibrous inside can fully enter graphene oxide sheetInterlayer, increases the active force of sheet interlayer, thereby increases the performance of graphene oxide fiber.
Brief description of the drawings
Fig. 1 is the side SEM figure of the silk in embodiment 1～2.
Fig. 2 is the XRD collection of illustrative plates of the silk in embodiment 1～2.
Fig. 3 is the mechanical property figure in embodiment 1～2.
Detailed description of the invention
Embodiment 1:
The present embodiment is taking the Lactated aqueous solution of 1-butyl-3-methylimidazole L as solidification liquid wet spinning systemStandby fiber:
Step 1: get appropriate graphene oxide in beaker, this beaker is placed in to oil bath pan and is stirringConcentrated one day of lower 50 DEG C～60 DEG C of situation, make its viscosity reach 985MPa.S left and right;
Step 2: get 1-butyl-3-methylimidazole L lactate 50uL and be configured to concentration in 50mL waterFor the solution of 0.00477mol/L, as solidification liquid;
Step 3: utilize wet spinning technology to prepare fiber taking the ionic liquid aqueous solution as solidification liquid
Step 4: put into and fill distilled water after spun graphene oxide fiber dries in air atmosphereTank in soak 10 seconds afterwards take out dry.
Embodiment 2
The present embodiment is preparation taking the aqueous solution of chlorination 1-amine propyl group-3-methylimidazole as solidification liquid wet spinningFiber:
Step 1: get appropriate graphene oxide in beaker, this beaker is placed in to oil bath pan and is stirringConcentrated one day of lower 50 DEG C～60 DEG C of situation, make its viscosity reach 985MPa.S left and right;
Step 2: get chlorination 1-amine propyl group-3-methylimidazole 5uL and be configured to concentration be in 50mL waterThe solution of 0.00067mol/L, as solidification liquid;
Step 3: utilize wet spinning technology to prepare fiber taking the ionic liquid aqueous solution as solidification liquid
Step 4: put into and fill distilled water after spun graphene oxide fiber dries in air atmosphereTank in soak 10 seconds afterwards take out dry.
The concrete technical scheme being not limited to described in above-described embodiment of the present invention, all employings are equal to replacementThe technical scheme forming is the protection domain that the present invention requires.
Claims (5)
1. a wet spinning process, is characterized in that: comprise the following steps:
Step 1: make graphene oxide taking graphite as raw material through oxidizing process, be placed in oil bath panUnder uniform temperature, stirring is concentrated to thick.
Step 2: the ionic liquid aqueous solution that configuration concentration is suitable
Step 3: utilize wet spinning technology, prepare graphene oxide taking the ionic liquid aqueous solution as solidification liquidFiber.
Step 4: put into and fill distilled water after spun graphene oxide fiber dries in air atmosphereTank in soak after take out dry.
2. according to a kind of wet spinning process described in claims 1, it is characterized in that: step 1Described graphene oxide thickening temperature is 40 DEG C～80 DEG C, and concentrated graphene oxide viscosity is985MPa.S left and right.
3. according to a kind of wet spinning process described in claims 1, it is characterized in that: step 2Described ionic liquid concentration of aqueous solution is respectively: 1-butyl-3-methylimidazole L lactate 0.001～0.010Mol/L; Chlorination 1-amine propyl group-3-methylimidazole 0.0001～0.0010mol/L.
4. according to a kind of wet spinning process described in claims 1, it is characterized in that: step 3In described wet spinning process, the extrusion capacity of graphene oxide is 0.1～1.0mL/min; Wet spinning instituteWith the pin mouth internal diameter of syringe needle be 0.10～0.80mm.
5. according to a kind of wet spinning process described in claims 1, it is characterized in that: step 4The described graphene oxide fiber drying is immersed in distilled water 5～100 seconds.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510991314.7A CN105586646A (en) | 2015-12-27 | 2015-12-27 | Wet spinning method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510991314.7A CN105586646A (en) | 2015-12-27 | 2015-12-27 | Wet spinning method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105586646A true CN105586646A (en) | 2016-05-18 |
Family
ID=55926539
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510991314.7A Pending CN105586646A (en) | 2015-12-27 | 2015-12-27 | Wet spinning method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105586646A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106087114A (en) * | 2016-06-27 | 2016-11-09 | 南京邮电大学 | A kind of graphene oxide fiber and preparation method thereof |
| CN106948165A (en) * | 2017-04-28 | 2017-07-14 | 浙江大学 | A kind of graphene fiber of fusion certainly and preparation method thereof |
| CN110629325A (en) * | 2019-09-30 | 2019-12-31 | 华中科技大学 | Multi-element doped graphene fiber, and preparation and application thereof |
| JP2022531167A (en) * | 2019-04-30 | 2022-07-06 | 青島大学 | Method for producing graphene oxide fiber and obtained fiber |
-
2015
- 2015-12-27 CN CN201510991314.7A patent/CN105586646A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106087114A (en) * | 2016-06-27 | 2016-11-09 | 南京邮电大学 | A kind of graphene oxide fiber and preparation method thereof |
| CN106948165A (en) * | 2017-04-28 | 2017-07-14 | 浙江大学 | A kind of graphene fiber of fusion certainly and preparation method thereof |
| WO2018196475A1 (en) * | 2017-04-28 | 2018-11-01 | 浙江大学 | Self-fusion graphene fiber and preparation method therefor |
| CN106948165B (en) * | 2017-04-28 | 2019-06-21 | 浙江大学 | It is a kind of to merge graphene fiber and preparation method thereof certainly |
| US11486086B2 (en) | 2017-04-28 | 2022-11-01 | Zhejiang University | Self-fused graphene fiber and method of preparing the same |
| JP2022531167A (en) * | 2019-04-30 | 2022-07-06 | 青島大学 | Method for producing graphene oxide fiber and obtained fiber |
| JP7377564B2 (en) | 2019-04-30 | 2023-11-10 | 青島大学 | Method for producing graphene oxide fiber and obtained fiber |
| CN110629325A (en) * | 2019-09-30 | 2019-12-31 | 华中科技大学 | Multi-element doped graphene fiber, and preparation and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105586646A (en) | Wet spinning method | |
| CN106884210B (en) | A kind of graphene tencel composite fibre and preparation method thereof | |
| CN102704027B (en) | Preparation method for graphene oxide-modified PAN carbon fiber precursor | |
| CN107338642A (en) | A kind of functionalization non-woven cloth desalinization material and its preparation method and application | |
| CN104264263B (en) | A kind of silk-fibroin/carbon nano-tube hybridization fiber and preparation method thereof | |
| WO2012124934A3 (en) | Graphene fiber and method for manufacturing same | |
| CN105603582A (en) | High-strength continuous graphene fiber and preparing method thereof | |
| CN103397391B (en) | A kind of biological enzyme degumming method of linen fibre | |
| CN103572390B (en) | A kind of dry spray-wet-spinning method manufacturing aramid IIII fiber | |
| CN103334180B (en) | A kind of preparation method of Triangular-cross-secpolyacrylonitrile polyacrylonitrile carbon fiber | |
| CN102011202B (en) | Fiber beam spinning washes with water and hot gas spring device | |
| CN103696224A (en) | Method for improving degreasing efficiency of down feather | |
| CN105038996A (en) | Nanofiber composite membrane reactor | |
| CN104313876A (en) | Method for modifying natural fibers for anion polymer nylon 6 reaction | |
| CN109167007A (en) | Heat-resisting lithium ion battery coated separator and preparation method thereof | |
| CN105603580A (en) | Preparing method for oriented graphene oxide fibers | |
| CN105937066A (en) | Preparation method of highly oriented graphene oxide fiber | |
| CN106422779A (en) | Structural design and preparation method of chitosan and nanofiber composite forward osmosis membrane | |
| CN104964541A (en) | Fast drying method for adhesive base felt | |
| CN103820882B (en) | Hollow inorganic oxide fibre and preparation method thereof | |
| CN202482509U (en) | Washing machine | |
| CN107871614A (en) | A kind of DSSC using eggshell film preparation is to electrode material and method | |
| CN204282119U (en) | A kind of three pressure roller press-dehydrating structures of paper machine | |
| CN110938897A (en) | Technology for rapidly preparing fibrous porous material | |
| CN202761210U (en) | Wiping cloth absorbing oil and water rapidly |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160518 |
|
| WD01 | Invention patent application deemed withdrawn after publication |