CN107020068B - A kind of preparation method for the super-hydrophobic ethyl cellulose sponge that the carbon nanotube for water-oil separating enhances - Google Patents
A kind of preparation method for the super-hydrophobic ethyl cellulose sponge that the carbon nanotube for water-oil separating enhances Download PDFInfo
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- CN107020068B CN107020068B CN201710164573.1A CN201710164573A CN107020068B CN 107020068 B CN107020068 B CN 107020068B CN 201710164573 A CN201710164573 A CN 201710164573A CN 107020068 B CN107020068 B CN 107020068B
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- 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
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- 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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Abstract
The present invention relates to a kind of preparation methods of super-hydrophobic ethyl cellulose sponge that the carbon nanotube for water-oil separating enhances.Specific steps are as follows: the ethyl cellulose for preparing crosslinking first adds the modified carbon nanotube of Silanized hydrophobic and obtains a kind of super-hydrophobic three-dimensional porous material of water-oil separating of high intensity by pore former occupy-place method.The present invention innovatively uses ethyl cellulose as the material of water-oil separating for the first time, economical and efficient, preparation process are simple, raw material sources are extensive, environmentally protective, durable, enhancing sponge matrix is cooperateed with by being crosslinked and introducing carbon nanotube, obtained super hydrophobic porous sponge has many advantages, such as excellent oil absorption, stability, recuperability and biodegradability, and of the present invention preparation method is simple, raw material can industrialized production, have good application value.
Description
Technical field
The invention belongs to high molecular materials and functional material field, and in particular to a kind of carbon nanometer for water-oil separating
The preparation method of the super-hydrophobic ethyl cellulose sponge of pipe enhancing.
Background technique
In recent years, oil extraction position has begun from continent to ocean and shifts.The exploitation of offshore oil, which already becomes, to be obtained
One of the important channel of the energy is taken, however the accident of all kinds of crude oil leakages is also more commonplace.To local marine ecology
While environment causes significant damage, but also the processing work of Oil spills pollution becomes various circles of society's focus of attention.Such as
What, which effectively realizes water-oil separating, has a very important significance marine eco-environment protection.
The Physical Absorption method of hydrophobicity three-dimensional porous material is a kind of very effective oily water separation technique, three-dimensional porous material
Material possess high porosity, excellent chemical stability, biggish saturated extent of adsorption, can the porous microstructure of intercommunication to having
Practical application value.[Ramezani M, Vaezi M R, the Kazemzadeh A. such as Maedeh RamezaniApplied Surface Science, 2014,317 (2): 147-153.] and using ethyl triethoxysilane as presoma, ethyl alcohol is molten
Agent, ammonium hydroxide are that SiO has been made in catalyst2Substrate glasses piece is immersed in colloidal sol by colloidal sol, the sheet glass various concentration of drying
Iso- trimethoxy silane/ethanol solution carry out hydrophobic silanization modification, the water contact angle of obtained super hydrophobic surface is up to
160°.[Pham V H, the Dickerson J H. such as DickersonAcs Applied Materials & Interfaces,
2014,6 (16): 14181-14188.] by solution infusion method melamine foams are carried out with trichlorine octadecylsilane it is hydrophobic
It is modified, its surface tension is reduced to increase the hydrophobicity of material surface.The water contact angle of the modification foam finally obtained is
151 °, there is superhydrophobic characteristic.The experiment of its Oil & Water shows that the saturated absorption capacity of modified foam is distributed in 80 times or more certainly
Body weight, and repeatedly circulation water-oil separating can be realized by absorption/extrusion cycle, during 1000 circulation experiments always
Keep excellent saturated absorption rate.[Wang X, Xu S, Tan Y, the et al. such as WangCarbohydrate Polymers, 2016,140 (20): 188-194.] and utilize hexadecyl trimethoxy silane (HDTMS) by sol-gel
Method is prepared silanization microcrystalline cellulose (MCC), and the porous hydrophobic cellulose composite material of synthesis can be used for high efficiency oil-water separation,
And it recycles 10 uses and up to 99.77% water-oil separating efficiency can still be maintained later.
However the above hydrophobicity sponge can face many problems, such as complicated processing preparation in practical applications
Process, expensive experiment reagent and equipment, material reusability be poor, in preparation process with secondary pollution etc..Especially this
For a little modified sponge overwhelming majority using materials such as polyurethane and melamine resins as template, template preparation process can generation environment
Pollution.Although the reusing of sponge is good, its recyclable power of regeneration is poor, is especially difficult to drop in the natural environment
Solution, does not meet the concept of Green Chemistry and the trend of era development.This patent commodity in use ethyl cellulose, passes through a kind of warp
Ji efficiently, low cost, free of contamination preparation process hydrophobic ethyl cellulose sponge is made, by be crosslinked and introduce carbon nanotube come
Collaboration enhancing sponge matrix, obtained hydrophobic three-dimensional porous sponge have preferable stability, oil absorption, synthetic operation letter
Single, good industrialization production feasibility may be implemented to produce in enormous quantities, have good application in marine oil pollution treatment process
Prospect.
Summary of the invention
The purpose of the present invention is to provide a kind of super-hydrophobic ethyl celluloses that the carbon nanotube for water-oil separating enhances
The preparation method of sponge, this method economical and efficient, preparation process are simple, raw material sources are extensive, environmentally protective.
The system for the super-hydrophobic ethyl cellulose sponge that a kind of carbon nanotube for water-oil separating proposed by the present invention enhances
Preparation Method, the specific steps are as follows:
(1) it is crosslinked the preparation of ethyl cellulose: the ethyl cellulose powder of 1.0-2.0g is added to the dioxy of 5-15mL
In six rings, stirring dissolves it sufficiently；0.1-2mL epoxychloropropane is added, magnetic agitation 3-6 hours at 30-60 DEG C, is handed over
The ethyl cellulose of connection；
(2) 0.02-0.1g hydroxyl carbon nano tube the preparation of the carbon nanotube of silane hydrophobic modification: is added to 100-
In the deionized water of 200mL and ultrasonic disperse 45min, addition 6ml contain 2ml hexadecyl trimethoxy silane (HDTMS)
Aqueous solution, 75 DEG C of constant temperature oil baths, is heated to reflux 6h；Product filters, and with deionized water and ethanol washing, 80 DEG C of vacuum of filter cake are dry
It is dry to get arrive silane hydrophobic modification carbon nanotube；
(3) preparation of pore former；
(4) preparation of the super-hydrophobic ethyl cellulose sponge of carbon nanotube enhancing: 0.02-0.5g silane hydrophobic modification is taken
Carbon nanotube be added to step (1) crosslinking ethyl cellulose in, stirring so that it is uniformly dispersed；After sieving then is added portionwise
Anhydrous sodium sulfate pore former, be stirring evenly and then adding into mold；Mold and sample are put into -80 DEG C of refrigerator freezings to be aged 48 hours
Demoulding is taken out afterwards, is placed in deionized water and cleans pore former and solvent, and freeze-drying obtains the super of carbon nanotube enhancing for 24 hours
Hydrophobic ethyl cellulose sponge；
(5) contact angle experiments and water-oil separating experiment.
In the present invention, the preparation of the step (3) pore former: grinding pore former with mortar, then will grinding
Pore former afterwards is put into the mesh screen of 80-150 mesh, sieving；The pore former is sodium chloride, sodium bicarbonate, sodium carbonate or sodium sulphate
One of.
In the present invention, step (5) contact angle experiments and water-oil separating experiment: respectively using contact angle tester (OCA20)
Test contact angle of the sponge under water, 1M HCl solution, 1M NaOH solution and 10wt%NaCl solution environmental.Use tonyred 1
Number different oil products are dyed, be respectively placed in a beaker different oil water mixtures, the carbon nanotube of certain mass is increased
Strong super-hydrophobic ethyl cellulose sponge puts into beaker, time used in record saturation oil absorption and oil suction.Sample is taken out, is passed through
Absorption-distillation method is effectively recycled internal oil product；Different oil products are n-hexane, gasoline, diesel oil, dimethyl-silicon
Oil, petroleum ether and edible oil.
The good effect that the super-hydrophobic ethyl cellulose sponge of the enhancing of carbon nanotube prepared by the present invention has:
A. there is stronger oil and water separation capability and higher water-oil separating efficiency.Sponge can absorb own wt decades of times
Different types of oil product, separative efficiency is more than 99%.
B. the super-hydrophobic ethyl cellulose sponge of carbon nanotube enhancing and the contact angle of water reach 155.2 °, oily contact angle
Reach 0 °, roll angle is 5 °, has super-hydrophobic property, can be used for oil water separation process.
C. there is density and very high porosity very light.
D. the super-hydrophobic ethyl cellulose sponge of carbon nanotube enhancing has the property of acidproof alkali salt, can be used for varying environment
Under water-oil separating.
E. there is good recycling and mechanical strength, the water-oil separating still with higher after being recycled 50 times
Ability.
Detailed description of the invention
Fig. 1 is the flow diagram for preparing the super-hydrophobic ethyl cellulose sponge of carbon nanotube enhancing.
Fig. 2 is the synthesis schematic diagram of the carbon nanotube of silane hydrophobization.
Fig. 3 is the water contact angle image of the super-hydrophobic ethyl cellulose sponge of carbon nanotube enhancing.
Fig. 4 is the super-hydrophobic ethyl cellulose sponge pictorial diagram of carbon nanotube enhancing.
Specific embodiment
The present invention is further illustrated below by embodiment.
Embodiment 1:
A kind of preparation method for the super-hydrophobic ethyl cellulose sponge that the carbon nanotube for water-oil separating enhances, including such as
Lower processing step:
(1) it is crosslinked the preparation of ethyl cellulose:
The ethyl cellulose powder of 2.0g is added in the dioxane of 10mL, stirring dissolves it sufficiently.It is added
0.5mL epoxychloropropane, magnetic agitation 5 hours at 35 DEG C, the ethyl cellulose being crosslinked.
(2) preparation of the carbon nanotube of silane hydrophobic modification:
0.1g hydroxyl carbon nano tube is added in the deionized water of 150mL and ultrasonic disperse 45min, addition 6ml contain
There is the aqueous solution of 2ml hexadecyl trimethoxy silane (HDTMS), 75 DEG C of constant temperature oil baths are heated to reflux 6h.Product filters, and uses
Deionized water and ethanol washing, 80 DEG C of filter cake vacuum drying are to get the carbon nanotube for arriving silane hydrophobic modification.
(3) preparation of pore former:
Anhydrous sodium sulfate pore former is ground with mortar, the pore former after grinding is then put into the mesh screen of 100 mesh,
Sieving.
(4) preparation of the super-hydrophobic ethyl cellulose sponge of carbon nanotube enhancing:
The carbon nanotube of 0.25g silane hydrophobic modification is taken to be added in the ethyl cellulose of step (1) crosslinking, stirring makes
It is uniformly dispersed.Anhydrous sodium sulfate pore former after sieving is then added portionwise, is stirring evenly and then adding into mold.By mold and sample
Product are put into after -80 DEG C of refrigerator freezings are aged 48 hours and take out demoulding, are placed in deionized water and clean pore former and solvent, and freezing is dry
Obtain within dry 24 hours the super-hydrophobic ethyl cellulose sponge of carbon nanotube enhancing.
(5) contact angle experiments and water-oil separating experiment:
Sponge is tested respectively using contact angle tester (OCA20) in water, 1M HCl solution, 1M NaOH solution and 10wt%
Contact angle under NaCl solution environment.Using Sudan hong Ⅰ to a series of different oil product (n-hexane, gasoline, diesel oil, dimethyl
Silicone oil, petroleum ether and edible oil) it is dyed, different oil water mixtures is placed in a beaker respectively, by the carbon of certain mass
The super-hydrophobic ethyl cellulose sponge of nanotube enhancing puts into beaker, time used in record saturation oil absorption and oil suction.It takes out
Sample is effectively recycled internal oil product by absorption-distillation method.This cyclic absorption experiment repeatable at least 50
It is secondary.Embodiment 2:
A kind of preparation method for the super-hydrophobic ethyl cellulose sponge that the carbon nanotube for water-oil separating enhances, including such as
Lower processing step:
(1) it is crosslinked the preparation of ethyl cellulose:
The ethyl cellulose powder of 1.5g is added in the dioxane of 8mL, stirring dissolves it sufficiently.It is added
0.35mL epoxychloropropane, magnetic agitation 5 hours at 30 DEG C, the ethyl cellulose being crosslinked.
(2) preparation of the carbon nanotube of silane hydrophobic modification:
0.08g hydroxyl carbon nano tube is added in the deionized water of 120mL and ultrasonic disperse 45min, addition 6ml contain
There is the aqueous solution of 2ml hexadecyl trimethoxy silane (HDTMS), 75 DEG C of constant temperature oil baths are heated to reflux 6h.Product filters, and uses
Deionized water and ethanol washing, 80 DEG C of filter cake vacuum drying are to get the carbon nanotube for arriving silane hydrophobic modification.
(3) preparation of pore former:
Natrium carbonicum calcinatum pore former is ground with mortar, the pore former after grinding is then put into the mesh screen of 100 mesh,
Sieving.
(4) preparation of the super-hydrophobic ethyl cellulose sponge of carbon nanotube enhancing:
The carbon nanotube of 0.15g silane hydrophobic modification is taken to be added in the ethyl cellulose of step (1) crosslinking, stirring makes
It is uniformly dispersed.Anhydrous sodium sulfate pore former after sieving is then added portionwise, is stirring evenly and then adding into mold.By mold and sample
Product are put into after -80 DEG C of refrigerator freezings are aged 48 hours and take out demoulding, are placed in deionized water and clean pore former and solvent, and freezing is dry
Obtain within dry 24 hours the super-hydrophobic ethyl cellulose sponge of carbon nanotube enhancing.
(5) contact angle experiments and water-oil separating experiment:
Sponge is tested respectively using contact angle tester (OCA20) in water, 1M HCl solution, 1M NaOH solution and 10wt%
Contact angle under NaCl solution environment.Using Sudan hong Ⅰ to a series of different oil product (n-hexane, gasoline, diesel oil, dimethyl
Silicone oil, petroleum ether and edible oil) it is dyed, different oil water mixtures is placed in a beaker respectively, by the carbon of certain mass
The super-hydrophobic ethyl cellulose sponge of nanotube enhancing puts into beaker, time used in record saturation oil absorption and oil suction.It takes out
Sample is effectively recycled internal oil product by absorption-distillation method.This cyclic absorption experiment repeatable at least 50
It is secondary.
Embodiment 3:
A kind of preparation method for the super-hydrophobic ethyl cellulose sponge that the carbon nanotube for water-oil separating enhances, including such as
Lower processing step:
(1) it is crosslinked the preparation of ethyl cellulose:
The ethyl cellulose powder of 1.0g is added in the dioxane of 6mL, stirring dissolves it sufficiently.It is added
0.2mL epoxychloropropane, magnetic agitation 5 hours at 35 DEG C, the ethyl cellulose being crosslinked.
(2) preparation of the carbon nanotube of silane hydrophobic modification:
0.04g hydroxyl carbon nano tube is added in the deionized water of 100mL and ultrasonic disperse 45min, addition 6ml contain
There is the aqueous solution of 2ml hexadecyl trimethoxy silane (HDTMS), 75 DEG C of constant temperature oil baths are heated to reflux 6h.Product filters, and uses
Deionized water and ethanol washing, 80 DEG C of filter cake vacuum drying are to get the carbon nanotube for arriving silane hydrophobic modification.
(3) preparation of pore former:
Natrium carbonicum calcinatum pore former is ground with mortar, the pore former after grinding is then put into the mesh screen of 100 mesh,
Sieving.
(4) preparation of the super-hydrophobic ethyl cellulose sponge of carbon nanotube enhancing:
The carbon nanotube of 0.1g silane hydrophobic modification is taken to be added in the ethyl cellulose of step (1) crosslinking, stirring makes
It is uniformly dispersed.Anhydrous sodium sulfate pore former after sieving is then added portionwise, is stirring evenly and then adding into mold.By mold and sample
Product are put into after -80 DEG C of refrigerator freezings are aged 48 hours and take out demoulding, are placed in deionized water and clean pore former and solvent, and freezing is dry
Obtain within dry 24 hours the super-hydrophobic ethyl cellulose sponge of carbon nanotube enhancing.
(5) contact angle experiments and water-oil separating experiment:
Sponge is tested respectively using contact angle tester (OCA20) in water, 1M HCl solution, 1M NaOH solution and 10wt%
Contact angle under NaCl solution environment.Using Sudan hong Ⅰ to a series of different oil product (n-hexane, gasoline, diesel oil, dimethyl
Silicone oil, petroleum ether and edible oil) it is dyed, different oil water mixtures is placed in a beaker respectively, by the carbon of certain mass
The super-hydrophobic ethyl cellulose sponge of nanotube enhancing puts into beaker, time used in record saturation oil absorption and oil suction.It takes out
Sample is effectively recycled internal oil product by absorption-distillation method.This cyclic absorption experiment repeatable at least 50
It is secondary.
The super-hydrophobic ethyl cellulose sponge of the enhancing of carbon nanotube prepared by the present invention has stronger water-oil separating energy
Power and higher water-oil separating efficiency.Sponge can absorb different types of oil product of own wt decades of times, and separative efficiency is greater than
99%.Contact angle with water is 155.2 °, and oily contact angle reaches 0 °, and roll angle is 5 °, has super-hydrophobic property, can be used for
Oil water separation process.With density and very high porosity very light.The super-hydrophobic ethyl cellulose of carbon nanotube enhancing
Sponge has the property of acidproof alkali salt, the water-oil separating that can be used under varying environment.It is prolonged resistance to good recycling
With the oil and water separation capability still with higher after being recycled 50 times.
Claims (3)
1. a kind of preparation method for the super-hydrophobic ethyl cellulose sponge that the carbon nanotube for water-oil separating enhances, feature exist
In specific step is as follows:
(1) it is crosslinked the preparation of ethyl cellulose: the ethyl cellulose powder of 1.0-2.0g is added to the dioxane of 5-15mL
In, stirring dissolves it sufficiently；0.1-2mL epoxychloropropane is added, magnetic agitation 3-6 hours at 30-60 DEG C, is crosslinked
Ethyl cellulose；
(2) 0.02-0.1g hydroxyl carbon nano tube the preparation of the carbon nanotube of silane hydrophobic modification: is added to 100-
In the deionized water of 200mL and ultrasonic disperse 45min, addition 6ml contain 2ml hexadecyl trimethoxy silane (HDTMS)
Aqueous solution, 75 DEG C of constant temperature oil baths, is heated to reflux 6h；Product filters, and with deionized water and ethanol washing, 80 DEG C of vacuum of filter cake are dry
It is dry to get arrive silane hydrophobic modification carbon nanotube；
(3) preparation of pore former；
(4) preparation of the super-hydrophobic ethyl cellulose sponge of carbon nanotube enhancing: the carbon of 0.02-0.5g silane hydrophobic modification is taken
Nanotube is added in the ethyl cellulose of step (1) crosslinking, and stirring makes it be uniformly dispersed；Then be added portionwise sieving after at
Hole agent, is stirring evenly and then adding into mold；Mold and sample are put into after -80 DEG C of refrigerator freezings are aged 48 hours and take out demoulding, is set
Pore former and solvent are cleaned in deionized water, freeze-drying obtains the super-hydrophobic ethyl cellulose of carbon nanotube enhancing for 24 hours
Sponge；
(5) contact angle experiments and water-oil separating experiment.
2. the super-hydrophobic ethyl cellulose sponge that a kind of carbon nanotube for water-oil separating according to claim 1 enhances
Preparation method, it is characterized in that the preparation of described step (3) pore former: being ground with mortar to pore former, will then be ground
Pore former after mill is put into the mesh screen of 80-150 mesh, sieving；The pore former is sodium chloride, sodium bicarbonate, sodium carbonate or sulfuric acid
One of sodium.
3. the super-hydrophobic ethyl cellulose sponge that a kind of carbon nanotube for water-oil separating according to claim 1 enhances
Preparation method, it is characterized in that step (5) contact angle experiments and water-oil separating experiment: distinguished using contact angle tester
Contact angle of the sponge under water, 1M HCl solution, 1M NaOH solution and 10wt%NaCl solution environmental is tested, tonyred 1 is used
Number different oil products are dyed, be respectively placed in a beaker different oil water mixtures, the carbon nanotube of certain mass is increased
Strong super-hydrophobic ethyl cellulose sponge puts into beaker, the time used in record saturation oil absorption and oil suction, takes out sample, passes through
Absorption-distillation method is effectively recycled internal oil product；Different oil products are n-hexane, gasoline, diesel oil, dimethyl-silicon
Oil, petroleum ether and edible oil.
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| CN112409022A (en) * | 2020-11-20 | 2021-02-26 | 武汉科技大学 | Carbon nanotube/fiber modified self-heating porous hydrophobic/oleophylic ceramic and preparation method thereof |
| CN113176217A (en) * | 2021-03-29 | 2021-07-27 | 西安理工大学 | Carrot-based chemical and material analysis professional course experimental method |
| CN114733498B (en) * | 2022-05-17 | 2023-08-22 | 常州大学 | Preparation method of polydimethylsiloxane/ethylcellulose sponge body with organic solvent as template |
| CN118027606B (en) * | 2024-02-02 | 2024-07-09 | 重庆克那维环保科技有限公司 | Repair material for pipeline non-excavation and preparation method thereof |
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| CN101928996A (en) * | 2010-07-20 | 2010-12-29 | 东华大学 | Preparation method of fibrous membrane with super hydrophobic multi-stage nanometer structure |
| US9254466B2 (en) * | 2014-06-30 | 2016-02-09 | Pall Corporation | Crosslinked cellulosic membranes |
| CN106283161A (en) * | 2016-08-25 | 2017-01-04 | 山东清大银光金属海绵新材料有限责任公司 | The preparation method of sponge structure sections/SiC particulate base oil-water separation enhancement layer material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928996A (en) * | 2010-07-20 | 2010-12-29 | 东华大学 | Preparation method of fibrous membrane with super hydrophobic multi-stage nanometer structure |
| US9254466B2 (en) * | 2014-06-30 | 2016-02-09 | Pall Corporation | Crosslinked cellulosic membranes |
| CN106283161A (en) * | 2016-08-25 | 2017-01-04 | 山东清大银光金属海绵新材料有限责任公司 | The preparation method of sponge structure sections/SiC particulate base oil-water separation enhancement layer material |
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