CN107083680A - The method of modifying of carbon fiber surface in-situ polymerization pyrroles - Google Patents
The method of modifying of carbon fiber surface in-situ polymerization pyrroles Download PDFInfo
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- CN107083680A CN107083680A CN201710344637.6A CN201710344637A CN107083680A CN 107083680 A CN107083680 A CN 107083680A CN 201710344637 A CN201710344637 A CN 201710344637A CN 107083680 A CN107083680 A CN 107083680A
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- carbon fiber
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
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- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
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Abstract
The present invention discloses a kind of method of modifying of carbon fiber surface in-situ polymerization pyrroles, including：1) at 10~60 DEG C, carbon fiber is mixed with pyrroles's aqueous dispersions, wherein the mass ratio of carbon fiber and pyrroles is 2~2000：1, consumption and the carbon fiber mass values scope of water are 2~10；Being placed after mixing makes carbon fiber surface fully be contacted with pyrrole monomer and is adsorbed in carbon fiber surface；2) solution of oxidant is added to realize chemical oxidising polymerisation, and the mol ratio of oxidant and pyrrole monomer is 1：0.05~3, and the sustained response under 10~30 DEG C of temperature conditionss；3) after reaction terminates, reacting liquid pH value is adjusted to neutrality；4) carbon fiber is taken out from reaction solution, rinsed with clear water, drained away the water, and be dried to obtain carbon fiber/Pt/Polypyrrole composite material.Polypyrrole has a good biocompatibility, and due to doping dedoping characteristic after research finds that it is combined with carrier, therefore there is very strong characterization of adsorption, there is wide spectrum adsorptivity to the pollutant in sewage.
Description
Technical field
The invention belongs to chemistry and water treatment field, it is related to a kind of method of use chemical polymerization in situ in carbon fiber surface
The preparation method of carbon fiber/Pt/Polypyrrole composite material of polymerization one strata pyrroles of generation.
Background technology
The carbon fiber that the present invention relates to refers to that a kind of phosphorus content is up to more than 90% inorfil.Polyacrylonitrile is fine
Tie up, viscose filament rayon fiber, current widely used carbon can be made in pitch fibers etc. after different degrees of carbonization treatment process
Fibrous material.Under normal circumstances, carbon fiber surface is coated with one layer 1~3 μm of epoxy resin layer, and this is to improve carbon fiber
The cohesive force of synnema, forms smooth diaphragm in monofilament surface, prevents fiber attrition, produces lousiness；Protect carbon fiber
The active surface obtained after surface treated, it is to avoid moisture and dust in fiber surface absorption air；Improve the wetting of fiber
Property and adhesive force, improve the compatibility of fiber and matrix resin, improve the interface shear strength of composite.
Carbon fiber wire has less diameter (~7 μm) and higher specific surface area (~1000m2/ g), therefore have
Good characterization of adsorption, simultaneously because carbon fiber has a preferable biocompatibility, therefore can as excellent bio-carrier, and
With good chemical inertness and environmental stability.These good characteristics based on carbon fiber, Japanese Scientists Ojima Zhao professor
Take the lead in being applied to water treatment field.But the hydrophily of epoxy resin layer and carbon fiber in itself is poor, and this causes carbon fiber wire to exist
Expanding performance in water is poor, and microorganism adhesion property is poor.To solve this problem, scientists utilize sizing agent in epoxy
The outer layer of resin overlay applies last layer again has good water solubility, the good sizing agent of carbon fiber adhesion property
(ZL2012101957783) so that it has good aqueous phase developing power so that it has excellent microbe carrier
Energy.But this kind of sizing agent is also only the dispersive property for improving carbon fiber in aqueous phase, it is not lifted further in water
Other performances in processing, such as characterization of adsorption.
For waste water control in situ, the water body purification engineering in such as river, pond and lake natural water, in these water bodys
Pollutant concentration is far below the pollutant concentration of sewage treatment plant, therefore carbon fiber has stronger absorption property, will be more favourable
In the purification process of reinforcing natural water.
The content of the invention
It is an object of the invention to provide a kind of method of modifying of carbon fiber surface in-situ polymerization pyrroles, to solve above-mentioned skill
Art problem.The present invention can assign carbon fiber surface good water-wet behavior and biocompatibility characteristics, and with hydrophily sizing agent
Difference, the method for modifying will also assign carbon fiber stronger surface adsorption property, can quickly by concentration in natural water relatively
Low organic matter and heavy metal ion enrichment to carbon fiber surface, and by the microorganism of carbon fiber surface appendix carry out mineralising or
Solidification is removed, and strengthens the removal rate of pollutant.The inventive method is simple to operate, and building-up process is environment-friendly, prepared carbon
Fiber/Pt/Polypyrrole composite material good biocompatibility, absorption property is good, with good natural water in-situ treatment performance, has
Good application prospect.
To achieve these goals, the present invention is adopted the following technical scheme that：
The method of modifying of carbon fiber surface in-situ polymerization pyrroles, including：Carbon fiber is immersed in polypyrrole aqueous dispersions,
Make pyrroles in carbon fiber surface in-situ polymerization by adding oxidant, generate carbon fiber/polypyrrole compound.
Further, in compound, the mass ratio of carbon fiber and polypyrrole is 2~2000：1.
Further, following steps are specifically included：
1) at -10~60 DEG C, carbon fiber is mixed with pyrroles's aqueous dispersions, the mass ratio of wherein carbon fiber and pyrroles is
2~2000：1, consumption and the carbon fiber mass values scope of water are 2~10；Being placed after mixing makes carbon fiber surface single with pyrroles
Body fully contacts and is adsorbed in carbon fiber surface；
2) solution of oxidant is added to realize chemical oxidising polymerisation, and the mol ratio of oxidant and pyrrole monomer is 1：
0.05~3, and the sustained response under -10~30 DEG C of temperature conditionss；
3) after reaction terminates, reacting liquid pH value is adjusted to neutrality；
4) carbon fiber is taken out from reaction solution, rinsed with clear water, drained away the water, and be dried to obtain carbon fiber/polypyrrole
Composite.
Further, step 1) in standing time be 0.5~2h.
Further, step 2) in the sustained response time be 1~48h.
Further, step 3) in add NaOH reacting liquid pH value is adjusted to neutrality.
Further, oxidant is FeCl3Or ammonium persulfate.
Further, step 2) in oxidant solution concentration be 0.1~1mol/L.
Further, the numbering of carbon fiber is：3K, 12K or 24K.
Compared with the existing sizing agent technology using coating, the present invention has following beneficial technique effect：
The present invention is with carbon fiber, and pyrroles is raw material, and water is solvent, FeCl3Or ammonium persulfate is oxidant, due to reaction temperature
Spend relatively low (- 10~30 DEG C), and the boiling point of pyrroles is higher (~130 DEG C), and no coupling product is produced pyrroles in the course of the polymerization process, because
This is discharged without pernicious gas during the course of the reaction；Contain a small amount of Fe after reaction in solution2+, Cl-, NH4 +And SO4 2-Ion, these
Material is minimum to environmental hazard, and ammonia radical ion can be handled and removed by sewage treatment plant, it is to avoid cause water body richness battalion
Fosterization.Therefore whole building-up process is environment-friendly chemical synthesis process.Polypyrrole has good biocompatibility, and warp
Cross research and find that it due to doping-dedoping characteristic, therefore has very strong characterization of adsorption after being combined with carrier, to sewage
In pollutant there is wide spectrum adsorptivity.
Brief description of the drawings
Expanded schematic diagrams of the Fig. 1 for the present invention with contrast carbon fiber in water；Wherein, Fig. 1 (A) is actual sewage and used
Starch the apparent figure of carbon fiber of agent processing；Fig. 1 (B) is actual sewage and the apparent figure of sewage with carbon fiber/polypyrrole processing；
Fig. 2 is the prepared carbon fiber/Pt/Polypyrrole composite material Treating Municipal Sewage design sketch of the present invention；Wherein, Fig. 2 (A)
For purification schematic diagram at initial stage；Fig. 2 (B) is schematic diagram after purifying 3 hours.
Embodiment
With reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
The embodiment of the present invention is using 12K polyacrylonitrile-based carbon fibres and commercially available chemical pure pyrroles as synthesis material, first, profit
With the characteristic of carbon fiber high-specific surface area and its surface epoxy coating oleophylic, pyrrole monomer is fully adsorbed in carbon fiber
Surface, recycles oxidant to be aoxidized to realize the in-situ polymerization of pyrroles to pyrroles.The reactional equation related generally to is as follows：
(1)
(2)
After reaction equation, reaction in addition to generating water insoluble polypyrrole, accessory substance is water solubility
FeCl2,HCl,(NH4)2SO4And H2SO4.Therefore water-soluble substances can be removed by neutralizing, and after simple rinsing.
Embodiment 1
Deionized water 3L is added in 5L glass containers, pyrrole monomer 10g is added, is disperseed by stirring, and use water
Woven carbon fiber 1000.0g is positioned in glass container by bath by temperature control at 4 DEG C, afterwards stands 2h.Add afterwards
1mol/L FeCl3Solution 348mL, is sufficiently stirred for and is incubated 24h, so that reaction is complete.5M NaOH are used afterwards by reaction solution
PH value is adjusted to 7.0, and reaction solution is removed, and adds clear water rinsing once；Then fiber is taken out, at 105 DEG C after draining away the water
Baking is overnight until constant weight, the gross weight that fiber is restored with balance weighing apparatus is 1008.6g, and this shows most pyrroles in baking oven
It polymerize in fiber surface.
Embodiment 2
Deionized water 3L is added in 5L glass containers, pyrrole monomer 20g is added, is disperseed by stirring, and use water
Woven carbon fiber 1000.0g is positioned in glass container by bath by temperature control at 4 DEG C, afterwards stands 2h.Add afterwards
0.5mol/L (NH4)2S2O8Solution 348mL, is sufficiently stirred for and is incubated 24h, so that reaction is complete.Afterwards will be anti-with 5M NaOH
Answer the pH value of liquid to be adjusted to 7.0, and reaction solution is removed, add clear water rinsing once；Then fiber is taken out, after draining away the water
Baking is overnight until constant weight, the gross weight that fiber is restored with balance weighing apparatus is 1018.6g, and this shows major part in 105 DEG C of baking ovens
Pyrroles polymerize in fiber surface, the success of the home position polymerization reaction of pyrroles.
Embodiment 3
Deionized water 0.2L is added in 5L glass containers, pyrrole monomer 10g is added, is disperseed by stirring, be used in combination
Woven carbon fiber 20.0g is positioned in glass container and stands 0.5h by water-bath by temperature control at 60 DEG C, afterwards.Afterwards plus
Enter 1mol/L FeCl3Solution, FeCl3FeCl in solution3Mol ratio with pyrrole monomer is 1：1；It is sufficiently stirred for and is incubated 48h,
So that reaction is complete.The pH value of reaction solution is adjusted to 7.0 with 5M NaOH afterwards, and reaction solution is removed, clear water rinsing one is added
It is secondary；Then fiber is taken out, baking, overnight up to constant weight, fiber is restored with balance weighing apparatus in 105 DEG C of baking ovens after draining away the water
Gross weight be 28.8g, this show most pyrroles fiber surface polymerize.
Embodiment 4
Deionized water 10L is added in 5L glass containers, pyrrole monomer 10g is added, is disperseed by stirring, and use water
Woven carbon fiber 5000.0g is positioned in glass container by bath by temperature control at 25 DEG C, afterwards stands 1h.Add afterwards
1mol/L FeCl3Solution, FeCl3FeCl in solution3Mol ratio with pyrrole monomer is 1：3；It is sufficiently stirred for and is incubated 36h, with
Make reaction complete.The pH value of reaction solution is adjusted to 7.0 with 5M NaOH afterwards, and reaction solution is removed, clear water rinsing one is added
It is secondary；Then fiber is taken out, baking, overnight up to constant weight, fiber is restored with balance weighing apparatus in 105 DEG C of baking ovens after draining away the water
Gross weight be 5009.2g, this show most pyrroles fiber surface polymerize.
Embodiment 5
Deionized water 50L is added in 5L glass containers, pyrrole monomer 10g is added, is disperseed by stirring, and use water
Woven carbon fiber 20000.0g is positioned in glass container by bath by temperature control at -10 DEG C, afterwards stands 2h.Afterwards plus
The mol ratio for entering ammonium persulfate and pyrrole monomer in 1mol/L ammonium persulfate solution, ammonium persulfate solution is 1：0.05；Fully
Stir and be incubated 10h, so that reaction is complete.The pH value of reaction solution is adjusted to 7.0 with 5M NaOH afterwards, and reaction solution is removed,
Add clear water rinsing once；Then fiber is taken out, baking is overnight up to constant weight in 105 DEG C of baking ovens after draining away the water, with day
The gross weight that flat weighing obtains fiber is 2008.2g, and this shows that most pyrroles polymerize in fiber surface.
Actual sewage handles case：
Treatment effect of the carbon fiber/Pt/Polypyrrole composite material in actual sewage prepared for checking this method, we with
The carbon fibre material that certain company is treated with sizing agent is contrast, to take sewage to deal with objects from river, has been carried out pair
According to research, its result is as shown in Figure 1.It can be seen that expanding performance of the composite of the present invention in water is more preferably, this shows
The carbon fiber that using carbon fiber/Pt/Polypyrrole composite material prepared by the inventive method there is Billy to be handled with sizing agent is more preferable
Water-wet behavior, and with more preferable absorption property.
Fig. 2 is the effect contrast figure after carbon fiber/Pt/Polypyrrole composite material Treating Municipal Sewage 3h, it can be seen that through
Cross after 3h processing, composite material surface has adsorbed one layer of particulate pollutant, and the sewage after adsorption treatment then becomes more
Clarification, this shows that carbon fiber/Pt/Polypyrrole composite material prepared by the present invention has good characterization of adsorption, with it is higher into
Membrane property.
Claims (9)
1. the method for modifying of carbon fiber surface in-situ polymerization pyrroles, it is characterised in that including：Carbon fiber is immersed in polypyrrole water
In dispersion liquid, make pyrroles in carbon fiber surface in-situ polymerization by adding oxidant, generate carbon fiber/polypyrrole compound.
2. the method for modifying of carbon fiber surface in-situ polymerization pyrroles according to claim 1, it is characterised in that compound
In, the mass ratio of carbon fiber and polypyrrole is 2~2000：1.
3. the method for modifying of carbon fiber surface in-situ polymerization pyrroles according to claim 1, it is characterised in that specifically include
Following steps：
1) at -10~60 DEG C, carbon fiber is mixed with pyrroles's aqueous dispersions, wherein the mass ratio of carbon fiber and pyrroles be 2~
2000：1, consumption and the carbon fiber mass values scope of water are 2~10:1；Being placed after mixing makes carbon fiber surface and pyrrole monomer
Fully contact and be adsorbed in carbon fiber surface；
2) solution of oxidant is added to realize chemical oxidising polymerisation, and the mol ratio of oxidant and pyrrole monomer is 1：0.05~
3, and the sustained response under -10~30 DEG C of temperature conditionss；
3) after reaction terminates, reacting liquid pH value is adjusted to neutrality；
4) carbon fiber is taken out from reaction solution, rinsed with clear water, drained away the water, and be dried to obtain carbon fiber/polypyrrole and be combined
Material.
4. the method for modifying of carbon fiber surface in-situ polymerization pyrroles according to claim 3, it is characterised in that step 1) in
Standing time is 0.5~2h.
5. the method for modifying of carbon fiber surface in-situ polymerization pyrroles according to claim 3, it is characterised in that step 2) in
The sustained response time is 1~48h.
6. the method for modifying of carbon fiber surface in-situ polymerization pyrroles according to claim 3, it is characterised in that step 3) in
Add NaOH and reacting liquid pH value is adjusted to neutrality.
7. the method for modifying of carbon fiber surface in-situ polymerization pyrroles according to claim 3, it is characterised in that oxidant is
FeCl3Or ammonium persulfate.
8. the method for modifying of carbon fiber surface in-situ polymerization pyrroles according to claim 7, it is characterised in that step 2) in
The concentration of the solution of oxidant is 0.1~1mol/L.
9. the method for modifying of carbon fiber surface in-situ polymerization pyrroles according to claim 3, it is characterised in that carbon fiber
Numbering is：3K, 12K, 24K or other commercially available specification products.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112657474A (en) * | 2021-01-11 | 2021-04-16 | 西北师范大学 | Preparation of polypyrrole-polyacrylonitrile nanofiber membrane and application of polypyrrole-polyacrylonitrile nanofiber membrane in adsorption of chromium ions |
| CN113999489A (en) * | 2021-11-09 | 2022-02-01 | 齐盛时代(广州)科技有限公司 | High-power microwave resistant shielding film and preparation method thereof |
| CN114575157A (en) * | 2022-02-23 | 2022-06-03 | 中国科学院宁波材料技术与工程研究所 | Strong-water-absorption porous conductive carbon fiber rod and preparation method and application thereof |
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| CN102350317A (en) * | 2011-07-04 | 2012-02-15 | 西安交通大学苏州研究院 | Polypyrrole/titanium dioxide composite adsorbent, its preparation, application and regeneration methods |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112657474A (en) * | 2021-01-11 | 2021-04-16 | 西北师范大学 | Preparation of polypyrrole-polyacrylonitrile nanofiber membrane and application of polypyrrole-polyacrylonitrile nanofiber membrane in adsorption of chromium ions |
| CN113999489A (en) * | 2021-11-09 | 2022-02-01 | 齐盛时代(广州)科技有限公司 | High-power microwave resistant shielding film and preparation method thereof |
| CN114575157A (en) * | 2022-02-23 | 2022-06-03 | 中国科学院宁波材料技术与工程研究所 | Strong-water-absorption porous conductive carbon fiber rod and preparation method and application thereof |
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Application publication date: 20170822 |