CN107983303A - A kind of preparation method of organic wastewater absorption degradation modified carbon fiber - Google Patents
A kind of preparation method of organic wastewater absorption degradation modified carbon fiber Download PDFInfo
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- CN107983303A CN107983303A CN201711095009.5A CN201711095009A CN107983303A CN 107983303 A CN107983303 A CN 107983303A CN 201711095009 A CN201711095009 A CN 201711095009A CN 107983303 A CN107983303 A CN 107983303A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28023—Fibres or filaments
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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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- Hydrology & Water Resources (AREA)
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Abstract
The invention discloses a kind of preparation method of organic wastewater absorption degradation modified carbon fiber, by waterglass, surfactant, ferrous sulfate, sodium borohydride, coconut husk, phenol, the raw materials such as polyvinyl alcohol are made, the present invention prepares porous carbon fiber with coconut husk, handled through multiple modified technique, obtain high mechanical properties, the porous carbon fiber of high adsorption, Zero-valent Iron is carried on carbon fiber finally by impregnation, Organic Pollutants In Water is enriched with using the adsorptivity of carbon fiber, organic degradation is carried out by Zero-valent Iron, realize the purpose for thoroughly removing removal organic polluter, its preparation method is simple, reaction condition is gentle, products obtained therefrom is reusable, secondary pollution will not be produced in environment, it can be widely applied to organic sewage process field.
Description
Technical field
The present invention relates to technical field of sewage, more particularly to a kind of organic wastewater absorption degradation modified carbon fiber
Preparation method.
Background technology
With horizontal growing of China's industrial or agricultural, the demand of water resource is gradually increased.And Chinese population is numerous,
Per capita resources relative shortage.How to save the recycling of water resource and water resource becomes problem of concern, and
In the recycling of water resource, treatment of Organic Wastewater is the most important thing.Relied primarily on currently for the governing measure of organic water body
Municipal works means, that is, cut dirt, revetment, dredging and change water, these methods have the following disadvantages：1st, revetment and the quantities of dredging
Greatly, of high cost, the Treatment of Sludge that cleans out is improper easily to cause secondary pollution；2nd, can not accomplish to cut dirt completely, due to water such as river, lakes
Body is open system, and pollution sources as similar atmospheric sedimentation can not be accomplished to amputate completely；3rd, changed after dredging the water quality of water without
Method is kept, and since microecosystem is destroyed with the removing of bed mud in water body, river, the self-purification capacity in lake decline, once
Eutrophication will be continued by running into xenobiotic pollutants, form vicious circle.
To in the processing of pollutant, absorption method is got over because of the features such as its is easy, efficient, economic, renewable, non-secondary pollution
To be more valued by people.And the sorbing material such as traditional activated carbon, metal oxide, chitosan, humic acid because of price, make
Have been unable to meet treatment of Organic Wastewater demand at this stage with the problems such as mode, treatment effeciency, be badly in need of research and development efficiently, cheap, environmental protection,
Good new organic wastewater sorbing material.
Porous carbon fiber is a kind of new porous fibrous sorbing material, is had because of its unique pore structure and form
There are the specific surface area of more general porous charcoal bigger, the pore volume of higher, the faster rate of adsorption and stronger power of regeneration.Since upper
Since century the seventies appearance, air purification, exhaust gas wastewater treatment, military protection, metal recovery, electricity just it have been widely used in
Sub- equipment etc..At present, the porous carbon fiber of in the market mainly has polyacrylonitrile-radical porous carbon fiber, asphaltic base porous carbon fibre
Dimension, viscose glue base porous carbon fiber and phenolic aldehyde base porous carbon fiber etc., different carbon fibers carbonization speed, production carbon rate, porosity with
And the toughness after carbonization is different.Therefore, it is necessary to combine traditional carbon fibres preparation method, pass through Optimal improvements technique, there is provided
Aperture is small, porosity is high, fiber homogeneity is good and combines the strong porous carbon fiber of power.
At the same time, since the preparation process of carbon fiber includes carbonization or graphitization so that the carbon atom of carbon fiber surface
Stack orientation is more consistent, atom interlamellar spacing smaller, so fiber surface shows as nonpolar and chemical inertness, other carbon fiber surface
There are the shortcomings such as hydrophobic, smooth, absorption property is low in face, and the storeroom interface adhesion for causing carbon fiber compound with it is poor.Therefore, need
Carbon fiber surface is modified, improve its interface binding intensity with composite material.
The content of the invention
A kind of the defects of the object of the invention is exactly to make up prior art, there is provided organic wastewater absorption degradation carbon modified
The preparation method of fiber.
The present invention is achieved by the following technical solutions：
A kind of preparation method of organic wastewater absorption degradation modified carbon fiber, comprises the following steps：
（1）By waterglass and water by volume 1：（4-6）Stirred evenly after mixing, mixed liquor is exchanged by highly acidic cation
Resin removes sodium ion, then the surfactant of 1-2.5% mass is added into resulting solution, stirs complete to surfactant
Dissolving, it is spare to obtain silicate solution；
（2）Spinning solution is placed in electrostatic spinning machine, receiver is wrapped up using aluminium-foil paper, as-spun fibre is collected in aluminium-foil paper
On, spinning process technological parameter is positive pressure 15-16kV, negative pressure 1.5-2kV, promotes speed 0.04-0.05mm/min, receiving velocity
30-32r/min, distance is 15-18cm between syringe needle and receiver, and 30-40 DEG C of environment temperature is quiet at room temperature after the completion of spinning
Put one day, obtain as-spun fibre, then be placed in baking oven, be warming up to 160-170 DEG C and cure 60-70 minutes, sent again after taking-up
Enter in tube furnace, rise to 750-850 DEG C, when insulation 1-2 is small from room temperature in a nitrogen atmosphere with the heating rate of 5-10 DEG C/min,
It is spare that carbon fiber is obtained after natural cooling；
（3）Using step 2 gained carbon fiber as anode, graphite is cathode, in the ammonium phosphate electrolyte that mass fraction is 8-10%
In, it is 0.3-0.35A/m to control current density2, anodized 1.5-2 minutes, collects carbon fiber and is rinsed only with clear water, obtained
It is spare to modified carbon fiber；
（4）Step 3 gained modified carbon fiber is added in step 1 gained silicate solution, the dosage of wherein modified carbon fiber is
The 14-16% of silicate solution quality, ultrasonic disperse is uniform afterwards, drying for standby after filtering；
（5）By the carbon fiber handled through step 4 and ferrous sulfate in mass ratio（1-3）：Solid-to-liquid ratio 1 is pressed after 1 mixing：50-100g/
ML is added in 10% ethanol solution, and stirring adds sodium borohydride thereto again after 90-120 minutes, and adjusts pH with sodium hydroxide
To 11-12, stirring reaction 20-30 minutes under nitrogen protection, after the completion of product is rinsed to neutrality and is dried in vacuo with clear water,
Up to modified carbon fiber of the present invention.
The surfactant is neopelex, any one in lauryl sodium sulfate, methylcellulose
Kind.
The preparation method of spinning solution is that coconut husk crushed 100-120 mesh sieves in the step 2, after drying with phenol, dense
Sulfuric acid is in mass ratio（5-7）：（20-25）：（0.6-0.9）It is mixed and stirred for uniformly, being placed in 140-160 DEG C of oil bath pan and reacting
100-120 minutes, room temperature is down to afterwards, adds in sodium hydroxide and pH is to neutrality, product and 80% dioxanes aqueous solution are pressed into body
Product ratio 1：（9-11）It is mixed 60-80 minutes, centrifuges and filter, by the rotated evaporimeter of filtrate in 60-70 after removing residue
Concentrated at DEG C, remove dioxanes, obtain pure liquefied substance, then with polyvinyl alcohol in mass ratio（45-46）：（4-5）Hydrogen-oxygen is used after mixing
Change sodium and adjust pH to 10-11, add formalin afterwards, be warming up to 80-85 DEG C, postcooling is obtained to room temperature when reaction 2-3 is small
Spinning solution.
Ultrasound condition is ultrasonic disperse 10-30 minutes under 25-30kHz in the step 4.
The ratio between amount of material of sodium borohydride and ferrous sulfate is 1 in the step 5：（2-2.5）.
The preparation method of the spinning solution, the ratio between the formaldehyde of addition and the amount of phenol material are n（Formaldehyde）：n（Phenol）=
（1.4-1.5）：1.
It is an advantage of the invention that：
The method that the present invention uses Liquefaction Products in Phenol, is more active small moleculars by coconut husk liquefaction, avoids conventional wooden procatarxis structure from answering
It is miscellaneous and contain a large amount of impurity, the defects of spinning effect is undesirable is directly used in, then high polymer is connected as by unit of phenolic aldehyde, have more
The production carbon rate and porosity of fast carbonization speed, higher, and phenolic resin due to formed cross-linked structure, so carbonization after still may be used
Certain toughness is kept, is handled in conjunction with the technological parameter of electrostatic spinning optimization, more traditional melt spinning, makes fibre diameter more
Carefully, nanoscale is reached, so that the specific surface area with bigger, thus obtained carbon fiber is further tied with silicate solution through ultrasound
Close, silica is fitted together in the carbon fibers effectively to prevent the entanglement of carbon fiber and reunion, finally by impregnation by zeroth order
Iron is carried on carbon fiber, is enriched with Organic Pollutants In Water using the adsorptivity of carbon fiber, by Zero-valent Iron into
Row organic degradation, realizes the purpose for thoroughly removing removal organic polluter, carbon fiber production method of the present invention is simple, reaction condition temperature
With products obtained therefrom is reusable, will not produce secondary pollution in environment, can be widely applied to organic sewage process field.
Embodiment
A kind of preparation method of organic wastewater absorption degradation modified carbon fiber, comprises the following steps：
（1）By waterglass and water by volume 1：Stirred evenly after 5 mixing, mixed liquor is passed through into storng-acid cation exchange resin
Sodium ion is removed, then the lauryl sodium sulfate of 1% mass is added into resulting solution, is stirred complete to lauryl sodium sulfate
Dissolving, it is spare to obtain silicate solution；
（2）Spinning solution is placed in electrostatic spinning machine, receiver is wrapped up using aluminium-foil paper, as-spun fibre is collected in aluminium-foil paper
On, spinning process technological parameter is positive pressure 15kV, negative pressure 1.5kV, promotes speed 0.04mm/min, receiving velocity 30r/min, pin
Distance is 15cm between head and receiver, and 30 DEG C of environment temperature, stands one day at room temperature after the completion of spinning, obtains just spinning fine
Dimension, then is placed in baking oven, is warming up to 160 DEG C and cures 60 minutes, is re-fed into after taking-up in tube furnace, in a nitrogen atmosphere with
The heating rate of 5 DEG C/min rises to 750 DEG C, when insulation 1 is small from room temperature, and it is spare to obtain carbon fiber after natural cooling；
（3）Using step 2 gained carbon fiber as anode, graphite is cathode, in the ammonium phosphate electrolyte that mass fraction is 8%, control
Current density processed is 0.3A/m2, anodized 1.5 minutes, collects carbon fiber and is rinsed only with clear water, obtain modified carbon fiber
It is spare；
（4）Step 3 gained modified carbon fiber is added in step 1 gained silicate solution, the dosage of wherein modified carbon fiber is
The 14% of silicate solution quality, afterwards ultrasonic disperse 10 minutes under 25kHz, drying for standby after filtering；
（5）By the carbon fiber handled through step 4 and ferrous sulfate in mass ratio 2：Solid-to-liquid ratio 1 is pressed after 1 mixing：50g/mL is added to
In 10% ethanol solution, stirring adds sodium borohydride thereto again after 90 minutes, the amount of the material of sodium borohydride and ferrous sulfate it
Than for 1：2.5, and pH to 11 is adjusted with sodium hydroxide, stirring reaction 20 minutes under nitrogen protection, after the completion of by product with clear
Water is rinsed to neutrality and is dried in vacuo, up to modified carbon fiber of the present invention.
The preparation method of the spinning solution is that coconut husk crushed 100 mesh sieves, after drying with phenol, the concentrated sulfuric acid in mass ratio
6：22：0.8 is mixed and stirred for uniformly, being placed in 140 DEG C of oil bath pans and reacting 100 minutes, is down to room temperature afterwards, adds sodium hydroxide
PH is neutralized to neutrality, by product and 80% dioxanes aqueous solution by volume 1：10 are mixed 60 minutes, centrifuge and filter, remove
The rotated evaporimeter of filtrate is concentrated at 60 DEG C after removing residue, dioxanes is removed, obtains pure liquefied substance, then matter is pressed with polyvinyl alcohol
Measure ratio 45：PH to 10 is adjusted with sodium hydroxide after 4 mixing, adds formalin, the formaldehyde of addition and the amount of phenol material afterwards
The ratio between be n（Formaldehyde）：n（Phenol）=1.5：1,80 DEG C are warming up to, postcooling obtains spinning solution to room temperature when reaction 2 is small.
Claims (6)
1. a kind of preparation method of organic wastewater absorption degradation modified carbon fiber, it is characterised in that comprise the following steps：
（1）By waterglass and water by volume 1：（4-6）Stirred evenly after mixing, mixed liquor is exchanged by highly acidic cation
Resin removes sodium ion, then the surfactant of 1-2.5% mass is added into resulting solution, stirs complete to surfactant
Dissolving, it is spare to obtain silicate solution；
（2）Spinning solution is placed in electrostatic spinning machine, receiver is wrapped up using aluminium-foil paper, as-spun fibre is collected in aluminium-foil paper
On, spinning process technological parameter is positive pressure 15-16kV, negative pressure 1.5-2kV, promotes speed 0.04-0.05mm/min, receiving velocity
30-32r/min, distance is 15-18cm between syringe needle and receiver, and 30-40 DEG C of environment temperature is quiet at room temperature after the completion of spinning
Put one day, obtain as-spun fibre, then be placed in baking oven, be warming up to 160-170 DEG C and cure 60-70 minutes, sent again after taking-up
Enter in tube furnace, rise to 750-850 DEG C, when insulation 1-2 is small from room temperature in a nitrogen atmosphere with the heating rate of 5-10 DEG C/min,
It is spare that carbon fiber is obtained after natural cooling；
（3）Using step 2 gained carbon fiber as anode, graphite is cathode, in the ammonium phosphate electrolyte that mass fraction is 8-10%
In, it is 0.3-0.35A/m to control current density2, anodized 1.5-2 minutes, collects carbon fiber and is rinsed only with clear water, obtained
It is spare to modified carbon fiber；
（4）Step 3 gained modified carbon fiber is added in step 1 gained silicate solution, the dosage of wherein modified carbon fiber is
The 14-16% of silicate solution quality, ultrasonic disperse is uniform afterwards, drying for standby after filtering；
（5）By the carbon fiber handled through step 4 and ferrous sulfate in mass ratio（1-3）：Solid-to-liquid ratio 1 is pressed after 1 mixing：50-100g/
ML is added in 10% ethanol solution, and stirring adds sodium borohydride thereto again after 90-120 minutes, and adjusts pH with sodium hydroxide
To 11-12, stirring reaction 20-30 minutes under nitrogen protection, after the completion of product is rinsed to neutrality and is dried in vacuo with clear water,
Up to modified carbon fiber of the present invention.
2. the preparation method of organic wastewater absorption degradation modified carbon fiber according to claim 1, it is characterised in that institute
Surfactant is stated as any one in neopelex, lauryl sodium sulfate, methylcellulose.
3. the preparation method of organic wastewater absorption degradation modified carbon fiber according to claim 1, it is characterised in that institute
The preparation method for stating spinning solution in step 2 is that coconut husk crushed 100-120 mesh sieves, and quality is pressed with phenol, the concentrated sulfuric acid after drying
Than（5-7）：（20-25）：（0.6-0.9）It is mixed and stirred for uniformly, being placed in 140-160 DEG C of oil bath pan and reacting 100-120 minutes,
It is down to room temperature afterwards, adds in sodium hydroxide and pH is to neutrality, by product and 80% dioxanes aqueous solution by volume 1：（9-11）
It is mixed 60-80 minutes, centrifuges and filter, concentrate the rotated evaporimeter of filtrate at 60-70 DEG C after removing residue, removes
Dioxanes, obtains pure liquefied substance, then with polyvinyl alcohol in mass ratio（45-46）：（4-5）After mixing with sodium hydroxide adjust pH to
10-11, adds formalin afterwards, is warming up to 80-85 DEG C, postcooling obtains spinning solution to room temperature when reaction 2-3 is small.
4. the preparation method of organic wastewater absorption degradation modified carbon fiber according to claim 1, it is characterised in that institute
It is ultrasonic disperse 10-30 minutes under 25-30kHz to state ultrasound condition in step 4.
5. the preparation method of organic wastewater absorption degradation modified carbon fiber according to claim 1, it is characterised in that institute
It is 1 to state the ratio between amount of material of sodium borohydride and ferrous sulfate in step 5：（2-2.5）.
6. the preparation method of spinning solution according to claim 3, it is characterised in that the formaldehyde of addition and the amount of phenol material
The ratio between be n（Formaldehyde）：n（Phenol）=（1.4-1.5）：1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110652978A (en) * | 2019-08-27 | 2020-01-07 | 浙江理工大学 | Preparation method and application of nonmetal modified carbon fiber |
| CN109881368B (en) * | 2019-02-01 | 2021-07-06 | 武汉理工大学 | Preparation method of composite nanofiber membrane with coaxial structure and containing zero-valent iron nanoparticles |
| CN113083372A (en) * | 2021-05-17 | 2021-07-09 | 天津工业大学 | Preparation method of heterogeneous oxidation reaction catalytic fiber |
| CN113877637A (en) * | 2021-09-29 | 2022-01-04 | 南京恒丰医疗器械有限公司 | Preparation method and application of nano zero-valent iron modified aerogel-coated carbon fiber heterogeneous Fenton catalyst |
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| CN109881368B (en) * | 2019-02-01 | 2021-07-06 | 武汉理工大学 | Preparation method of composite nanofiber membrane with coaxial structure and containing zero-valent iron nanoparticles |
| CN110652978A (en) * | 2019-08-27 | 2020-01-07 | 浙江理工大学 | Preparation method and application of nonmetal modified carbon fiber |
| CN113083372A (en) * | 2021-05-17 | 2021-07-09 | 天津工业大学 | Preparation method of heterogeneous oxidation reaction catalytic fiber |
| CN113877637A (en) * | 2021-09-29 | 2022-01-04 | 南京恒丰医疗器械有限公司 | Preparation method and application of nano zero-valent iron modified aerogel-coated carbon fiber heterogeneous Fenton catalyst |
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