CN109173344A - A kind of preparation method of hydrophobicity three-dimensional porous material - Google Patents
A kind of preparation method of hydrophobicity three-dimensional porous material Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of hydrophobicity three-dimensional porous material, belong to porous material technical field.Hydrophobicity three-dimensional porous material prepared by the present invention, elasticity is good, and density is small, and porosity is high, has three-dimensional structure, high to the adsorption efficiency of oil product, and water will not be absorbed while adsorbing oil leak, more conducively recycling of the later period to oil product；When the adsorbance of this material reaches maximum, this material can be pulled out from water, by Oil Recovery by way of squeezing or wringing out, then this material can be continued to put into progress oil suction operation, reusable rate in water very high；The hardness of carbon nanotube is worked as with diamond phase, but but have outstanding toughness, it can stretch, carbon nanotube sponge is to overlap the macroscopic body with three-dimensional porous structure formed by carbon nanotube is unordered, property with carbon nanotube and traditional sponge body, have the characteristics that elasticity is good, low-density, high porosity, high-specific surface area, still can be restored under arbitrary torsional deformation.
Description
Technical field
The present invention relates to a kind of preparation methods of hydrophobicity three-dimensional porous material, belong to porous material technical field.
Background technique
Offshore oil leakage accident causes catastrophic destruction to marine environment, and the noxious material leaked out passes through food
Object chain threatens various species, including from rudimentary seaweed to advanced mammal even the mankind.The harm of Oil spills is anxious
It need to be dealt carefully with.Compare previous directly burning across the sea, and artificially separating the oil in water will be one more preferably
Mode while not will lead to other environmental pollutions because such processing can recycle the oil of these leakages again.Tradition
Oily water separation technique include electrochemistry, flotation, centrifugation, filtering and Gravity Separation method.But most conventional method is all
It takes a long time and cumbersome manual operation.Moreover, the separation process of these oil water mixtures is largely to rely on
Experience, it is easy to cause in oil there are also part water or water in there are also part oil be not completely separated from phenomenon appearance.
It is underwater super thin with colloid and interface science and bionic fast development, especially super hydrophobic surface and later period
The appearance of oil meter face mentions to develop effective, from driving, circulating and without other driving external force water-oil separating materials
Many wide and novel ideas are supplied.It is compared with traditional isolation technics, this water-oil separating driven by special wetability
Technology has shown the advantage that separating rate is fast and separative efficiency is high.As a kind of typical wetability, super-hydrophobic/super-oleophilic is
A kind of water contact angle is greater than 150 ° and a kind of surface characteristic of the slide angle less than 10 °.This super-hydrophobic surface has various each
The application of sample, including self-cleaning window, resistance to fogging application, the drag reduction application of micro runner device and water-oil separating material.Make
For a kind of most wide application, the oily water separation technique of gravity drive is further developed, and is prolonged from original oily penetration material
Reach later water penetration material.In past ten years, there are various water-oil separating materials to be developed.For
It makes good use of this special wetability and carrys out oil-water separation mixture, most of water-oil separating material all possesses on the contrary water and oil
Wetability.Generally speaking, water-oil separating material can be prepared according to two thinkings, one is super-hydrophobic/super-oleophilic material,
Another be superoleophobic/super hydrophilic material in certain circumstances.Existing water-oil separating material be usually by the former come
Preparation.And the latter due to that will obtain superoleophobic/super hydrophilic property there is very big challenge, just until 2011 years in air
It is used by successfully exploitation.Therefore, scientists advisably devise it is a kind of simply pre-wet membrane technology obtain it is underwater it is superoleophobic/
Water-oil separating is realized on super hydrophilic surface.
The material with different wetting performance surface is designed by a variety of different methods, is that a kind of current hot topic is ground
Study carefully field, has critically important application value to the leakage of processing offshore oil and industrial oily waste water.
Summary of the invention
The technical problems to be solved by the invention: it is reused for the hydrophobicity three-dimensional porous material that developed now
The problem of inefficiency, provides a kind of preparation method of hydrophobicity three-dimensional porous material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) ferrocene is taken to be put into 1g/L o-dichlorobenzene solution, ultrasound arrives carbon source solution to being completely dissolved；
(2) horizontal electric resistance furnace is preheated, after conversion zone temperature is stablized, carbon source is imported in furnace and is reacted；
(3) to the end of reacting, feed pump is closed, stops heating, closes hydrogen, and argon flow is adjusted to 300~400mL/
Min is down to room temperature to furnace temperature, closes argon gas, obtain carbon nanotube sponge；
(4) 18.4mol/L sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide and graphite are taken, is warming up to 80 DEG C, reacts 4~6 hours,
Reactant is obtained, then reactant is washed with a large amount of deionized waters to neutrality, then by the reactant after flushing in 60 DEG C of vacuum
It is 12 hours dry in baking oven, obtain pre-oxidation graphite；
(5) 18.4mol/L sulfuric acid and pre-oxidation graphite are taken, cooling in ice-water bath is put into after mixing evenly, permanganic acid is then added
Potassium is warming up to 35 DEG C, and reaction is taken out after 2 hours, obtains reaction solution, and deionized water is added dropwise in reaction solution, controls reaction temperature
At 98 DEG C or so, the reaction was continued 15 minutes；
(6) 10mol/L hydrogenperoxide steam generator is added in reaction solution, until reaction solution color becomes golden yellow, by reaction solution from
The heart, and obtained solid is washed 5~8 times respectively with 0.01mol/L hydrochloric acid and deionized water, then the solid after washing is put into
It is 10~14 hours dry in 60 DEG C of vacuum drying ovens, obtain graphene oxide；
(7) it takes graphene oxide and puts it into deionized water, ultrasonic vibration obtains graphene oxide solution, then by carbon nanometer
Pipe sponge is immersed in graphene oxide solution, and taking-up is dried, and obtains hydrophobic porous fibrous material.
The mass ratio of step (1) ferrocene and o-dichlorobenzene solution is 3:50.
When step (2) the preheating horizontal electric resistance furnace, setting reaction temperature is 800~900 DEG C, and preheating temperature is at feeding
200~300 DEG C, the air-tightness of check device is passed through high-purity argon gas, and throughput is 300~400mL/min, begins to warm up straight
Reach 800~900 DEG C to reaction temperature, after preheating reaches 200~300 DEG C, argon flow is adjusted to 2000~2500mL/
Min, while it being passed through high-purity hydrogen, hydrogen flowing quantity is 300~400mL/min.
Step (4) sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide and graphite mass fraction be 10:1:1:1.
The mass ratio of step (5) concentrated sulfuric acid, pre-oxidation graphite and potassium permanganate is 10:1:4.
Step (7) graphene oxide, deionized water and the mass ratio of carbon nanotube sponge are 1:500:400.
The present invention is compared with other methods, and advantageous effects are:
(1) hardness of carbon nanotube is worked as with diamond phase, but but have outstanding toughness, can stretch, carbon nanotube sponge
It is to overlap the macroscopic body with three-dimensional porous structure that is formed by carbon nanotube is unordered, there is carbon nanotube and traditional sponge body
Property has the characteristics that elasticity is good, low-density, high porosity, high-specific surface area, and appointing under arbitrary torsional deformation can so answer
It is former；
(2) graphene oxide after restoring has super-hydrophobicity and super-oleophilic, after being adhered to carbon nanotube sponge surface, due to
Carbon nanotube sponge has the characteristics that high porosity and elastomeric, can adsorb a large amount of oil leaks while not absorbing water；
(3) the hydrophobicity three-dimensional porous material prepared by the present invention, elasticity is good, and density is small, and porosity is high, has 3 D stereo knot
Structure, it is high to the adsorption efficiency of oil product, and water will not be absorbed while adsorbing oil leak, the more conducively later period is sharp to the recycling of oil product
With；When the adsorbance of this material reaches maximum, this material can be pulled out from water, it will be oily by way of squeezing or wringing out
Then it is very high can be continued to put into progress oil suction operation, reusable rate in water by product recycling for this material.
Specific embodiment
3~6g ferrocene is taken to be put into the 1g/L o-dichlorobenzene solution of 50~100g, ultrasound obtains carbon source to being completely dissolved
Solution；It is 800~900 DEG C that reaction temperature, which is arranged, and preheating temperature is 200~300 DEG C at feeding, is passed through high-purity argon gas, air-flow
Amount is 300~400mL/min, preheats horizontal electric resistance furnace, after preheating reaches 200~300 DEG C, argon flow is adjusted to 2000~
2500mL/min, while it being passed through high-purity hydrogen, hydrogen flowing quantity is 300~400mL/min, will after conversion zone temperature is stablized
Carbon source solution, which imports in furnace, to be reacted；To the end of reacting, feed pump is closed, stops heating, closes hydrogen, and by argon flow
It is adjusted to 300~400mL/min；It is down to room temperature to furnace temperature, argon gas is closed, obtains carbon nanotube sponge；Take 10~
20g18.4mol/L sulfuric acid, 1~2g potassium peroxydisulfate, 1~2g phosphorus pentoxide and 1~2g graphite are warming up to 80 DEG C, reaction 4
~6 hours obtain reactant, then reactant are washed with a large amount of deionized waters to neutrality, then by the reactant after flushing
It is 12 hours dry in 60 DEG C of vacuum drying ovens；It takes 40~80g18.4mol/L concentrated sulfuric acid and 1~2g to pre-oxidize graphite, stirs evenly
After be put into ice-water bath cooling, 4~8g potassium permanganate is then added, is warming up to 35 DEG C, reaction is taken out after 2~3 hours, is obtained anti-
Liquid is answered, deionized water is added dropwise in reaction solution, controls reaction temperature at 98 DEG C or so, the reaction was continued 15 minutes；In reaction solution
10mol/L hydrogenperoxide steam generator is added until reaction solution color becomes golden yellow；Reaction solution is centrifuged, and with 0.01mol/L salt
Acid and deionized water respectively wash obtained solid 5~8 times, then the solid after washing is put into drying in 60 DEG C of vacuum drying ovens
12 hours, obtain graphene oxide；It takes 1~2g graphene oxide and puts it into 500~1000g deionized water, ultrasound shake
It swings to obtain graphene oxide solution, then 400~800g carbon nanotube sponge is immersed in graphene oxide solution, taking-up is dried in the air
It is dry, obtain hydrophobic porous fibrous material.
3g ferrocene is taken to be put into the 1g/L o-dichlorobenzene solution of 50g, ultrasound obtains carbon source solution to being completely dissolved；If
Setting reaction temperature is 800 DEG C, and preheating temperature is 200 DEG C at feeding, is passed through high-purity argon gas, throughput 300mL/min, preheating
Argon flow is adjusted to 2000mL/min, while being passed through high-purity hydrogen, hydrogen stream after preheating reaches 200 DEG C by horizontal electric resistance furnace
Amount is 300mL/min, after conversion zone temperature is stablized, carbon source solution is imported in furnace and is reacted；To the end of reacting, close
Feed pump stops heating, closes hydrogen, and argon flow is adjusted to 300mL/min；It is down to room temperature to furnace temperature, closes argon gas,
Obtain carbon nanotube sponge；10g18.4mol/L sulfuric acid, 1g potassium peroxydisulfate, 1g phosphorus pentoxide and 1g graphite are taken, is warming up to
80 DEG C, 4 hours are reacted, obtain reactant, then reactant is washed with a large amount of deionized waters to neutrality, it then will be after flushing
Reactant is 12 hours dry in 60 DEG C of vacuum drying ovens；It takes the 40g18.4mol/L concentrated sulfuric acid and 1g to pre-oxidize graphite, stirs evenly
After be put into ice-water bath cooling, 4g potassium permanganate is then added, is warming up to 35 DEG C, reaction is taken out after 2 hours, obtain reaction solution,
Deionized water is added dropwise in reaction solution, controls reaction temperature at 98 DEG C or so, the reaction was continued 15 minutes；It is added in reaction solution
10mol/L hydrogenperoxide steam generator becomes golden yellow until reaction solution color；Reaction solution is centrifuged, and with 0.01mol/L hydrochloric acid and
Deionized water respectively washs obtained solid 5 times, then the solid after washing is put into drying 12 hours in 60 DEG C of vacuum drying ovens,
Obtain graphene oxide；It takes 1g graphene oxide and puts it into 500g deionized water, ultrasonic vibration obtains graphene oxide
Solution, then 400g carbon nanotube sponge is immersed in graphene oxide solution, taking-up is dried, and hydrophobic porous undulation degree is obtained
Material.
5g ferrocene is taken to be put into the 1g/L o-dichlorobenzene solution of 80g, ultrasound obtains carbon source solution to being completely dissolved；If
Setting reaction temperature is 850 DEG C, and preheating temperature is 250 DEG C at feeding, is passed through high-purity argon gas, throughput 350mL/min, preheating
Argon flow is adjusted to 2250mL/min, while being passed through high-purity hydrogen, hydrogen stream after preheating reaches 250 DEG C by horizontal electric resistance furnace
Amount is 350mL/min, after conversion zone temperature is stablized, carbon source solution is imported in furnace and is reacted；To the end of reacting, close
Feed pump stops heating, closes hydrogen, and argon flow is adjusted to 350mL/min；It is down to room temperature to furnace temperature, closes argon gas,
Obtain carbon nanotube sponge；15g18.4mol/L sulfuric acid, 1g potassium peroxydisulfate, 1g phosphorus pentoxide and 1g graphite are taken, is warming up to
80 DEG C, 5 hours are reacted, obtain reactant, then reactant is washed with a large amount of deionized waters to neutrality, it then will be after flushing
Reactant is 12 hours dry in 60 DEG C of vacuum drying ovens；60g18.4mol/L sulfuric acid and 1g is taken to pre-oxidize graphite, after mixing evenly
It is put into cooling in ice-water bath, 6g potassium permanganate is then added, is warming up to 35 DEG C, reaction is taken out after 2 hours, reaction solution is obtained,
Deionized water is added dropwise in reaction solution, controls reaction temperature at 98 DEG C or so, the reaction was continued 15 minutes；It is added in reaction solution
10mol/L hydrogenperoxide steam generator becomes golden yellow until reaction solution color；Reaction solution is centrifuged, and with 0.01mol/L hydrochloric acid and
Deionized water respectively washs obtained solid 7 times, then the solid after washing is put into drying 12 hours in 60 DEG C of vacuum drying ovens,
Obtain graphene oxide；It takes 1g graphene oxide and puts it into 750g deionized water, ultrasonic vibration obtains graphene oxide
Solution, then 600g carbon nanotube sponge is immersed in graphene oxide solution, taking-up is dried, and hydrophobic porous undulation degree is obtained
Material.
6g ferrocene is taken to be put into the 1g/L o-dichlorobenzene solution of 100g, ultrasound obtains carbon source solution to being completely dissolved；If
Setting reaction temperature is 900 DEG C, and preheating temperature is 300 DEG C at feeding, is passed through high-purity argon gas, throughput 400mL/min, preheating
Argon flow is adjusted to 2500mL/min, while being passed through high-purity hydrogen, hydrogen stream after preheating reaches 300 DEG C by horizontal electric resistance furnace
Amount is 400mL/min, after conversion zone temperature is stablized, carbon source solution is imported in furnace and is reacted；To the end of reacting, close
Feed pump stops heating, closes hydrogen, and argon flow is adjusted to 400mL/min；It is down to room temperature to furnace temperature, closes argon gas,
Obtain carbon nanotube sponge；20g18.4mol/L sulfuric acid, 2g potassium peroxydisulfate, 2g phosphorus pentoxide and 2g graphite are taken, is warming up to
80 DEG C, 6 hours are reacted, obtain reactant, then reactant is washed with a large amount of deionized waters to neutrality, it then will be after flushing
Reactant is 12 hours dry in 60 DEG C of vacuum drying ovens；80g18.4mol/L sulfuric acid and 2g is taken to pre-oxidize graphite, after mixing evenly
It is put into cooling in ice-water bath, 8g potassium permanganate is then added, is warming up to 35 DEG C, reaction is taken out after 3 hours, reaction solution is obtained,
Deionized water is added dropwise in reaction solution, controls reaction temperature at 98 DEG C or so, the reaction was continued 15 minutes；It is added in reaction solution
10mol/L hydrogenperoxide steam generator becomes golden yellow until reaction solution color；Reaction solution is centrifuged, and with 0.01mol/L hydrochloric acid and
Deionized water respectively washs obtained solid 8 times, then the solid after washing is put into drying 12 hours in 60 DEG C of vacuum drying ovens,
Obtain graphene oxide；It takes 2g graphene oxide and puts it into 1000g deionized water, ultrasonic vibration obtains graphene oxide
Solution, then 800g carbon nanotube sponge is immersed in graphene oxide solution, taking-up is dried, and hydrophobic porous undulation degree is obtained
Material.
Reference examples: the hydrophobic porous fibrous material of Jiangsu Materials Co., Ltd production.
The hydrophobic porous fibrous material of example and reference examples is detected, specific detection is as follows:
Surface wettability test: it is tested by contact angle tester, the model OCA20LHT-TEC700- of instrument
HTFC1500。
Thermogravimetric analysis: it is completed with NETZSCHTG209 instrument.Wherein heating rate is 10 DEG C of min-1, the temperature range of test
It is 30 to 800 DEG C.
Specific testing result such as table 1.
1 performance characterization contrast table of table
| Detection project | Example 1 | Example 2 | Example 3 | Reference examples |
| Water contact angle/° | 142.5 | 149 | 143 | 127.2 |
| Thermogravimetric analysis/mgcm﹣ 3 | 92 | 93 | 95 | 25 |
As shown in Table 1, hydrophobic porous fibrous material prepared by the present invention has good hydrophobicity and self-cleaning function, has
The saturated absorption capacity of higher volumes absorbs the oil property of can choose in oil water mixture, realizes water-oil separating.
Claims (6)
1. a kind of preparation method of hydrophobicity three-dimensional porous material, which is characterized in that specific production step are as follows:
(1) ferrocene is taken to be put into 1g/L o-dichlorobenzene solution, ultrasound arrives carbon source solution to being completely dissolved；
(2) horizontal electric resistance furnace is preheated, after conversion zone temperature is stablized, carbon source is imported in furnace and is reacted；
(3) to the end of reacting, feed pump is closed, stops heating, closes hydrogen, and argon flow is adjusted to 300~400mL/
Min is down to room temperature to furnace temperature, closes argon gas, obtain carbon nanotube sponge；
(4) 18.4mol/L sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide and graphite are taken, is warming up to 80 DEG C, reacts 4~6 hours,
Reactant is obtained, then reactant is washed with a large amount of deionized waters to neutrality, then by the reactant after flushing in 60 DEG C of vacuum
It is 12 hours dry in baking oven, obtain pre-oxidation graphite；
(5) 18.4mol/L sulfuric acid and pre-oxidation graphite are taken, cooling in ice-water bath is put into after mixing evenly, permanganic acid is then added
Potassium is warming up to 35 DEG C, and reaction is taken out after 2 hours, obtains reaction solution, and deionized water is added dropwise in reaction solution, controls reaction temperature
At 98 DEG C or so, the reaction was continued 15 minutes；
(6) 10mol/L hydrogenperoxide steam generator is added in reaction solution, until reaction solution color becomes golden yellow, by reaction solution from
The heart, and obtained solid is washed 5~8 times respectively with 0.01mol/L hydrochloric acid and deionized water, then the solid after washing is put into
It is 10~14 hours dry in 60 DEG C of vacuum drying ovens, obtain graphene oxide；
(7) it takes graphene oxide and puts it into deionized water, ultrasonic vibration obtains graphene oxide solution, then by carbon nanometer
Pipe sponge is immersed in graphene oxide solution, and taking-up is dried, and obtains hydrophobic porous fibrous material.
2. a kind of preparation method of hydrophobicity three-dimensional porous material as described in claim 1, which is characterized in that step (1) institute
The mass ratio for stating ferrocene and o-dichlorobenzene solution is 3:50.
3. a kind of preparation method of hydrophobicity three-dimensional porous material as described in claim 1, which is characterized in that step (2) institute
When stating preheating horizontal electric resistance furnace, setting reaction temperature is 800~900 DEG C, and preheating temperature is 200~300 DEG C at feeding, checks dress
The air-tightness set is passed through high-purity argon gas, and throughput is 300~400mL/min, begins to warm up until reaction temperature reaches 800
~900 DEG C, after preheating reaches 200~300 DEG C, argon flow is adjusted to 2000~2500mL/min, while being passed through High Purity Hydrogen
Gas, hydrogen flowing quantity are 300~400mL/min.
4. a kind of preparation method of hydrophobicity three-dimensional porous material as described in claim 1, which is characterized in that step (4) institute
The mass fraction for stating sulfuric acid, potassium peroxydisulfate, phosphorus pentoxide and graphite is 10:1:1:1.
5. a kind of preparation method of hydrophobicity three-dimensional porous material as described in claim 1, which is characterized in that step (5) institute
The mass ratio for stating the concentrated sulfuric acid, pre-oxidation graphite and potassium permanganate is 10:1:4.
6. a kind of preparation method of hydrophobicity three-dimensional porous material as described in claim 1, which is characterized in that step (7) institute
The mass ratio for stating graphene oxide, deionized water and carbon nanotube sponge is 1:500:400.
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| CN114960190A (en) * | 2022-05-13 | 2022-08-30 | 西南交通大学 | Preparation method of basalt fiber in-situ growth carbon nanotube sponge for solar water evaporation |
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