CN103752277A - Oil-absorbing aerogel and preparation method thereof - Google Patents
Oil-absorbing aerogel and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of an oil-absorbing aerogel. The preparation method comprises the following steps of mixing resorcinol, formaldehyde, a carbon nano-tube, sodium carbonate, and water to conduct a phenolic aldehyde reaction to obtain a hydrogel, and carrying out first solid liquid separation after blending the hydrogel and a surfactant to obtain a solid hydrogel; using an organic solvent to soak the solid hydrogel, then carrying out second solid liquid separation to obtain an organogel, and drying and carbonizing the organogel to obtain the oil-absorbing aerogel. The oil-absorbing aerogel prepared through the method provided by the invention takes the carbon nano-tube as a skeleton, the existence of the carbon nano-tube leads to larger pore of the oil-absorbing aerogel, and the oil absorption rate is increased. The experiment result shows that the oil absorption rate of the oil-absorbing aerogel prepared through the method provided by the invention is 50g/g-2,000g/g.
Description
Technical field
The invention belongs to technical field of organic synthesis, relate in particular to a kind of oil suction aeroge and preparation method thereof.
Background technology
Along with industrial expansion, the pollution causing containing the waste water of greasy dirt, offshore oil leakage etc. damages to the life condition of tellurian, forces the mankind to need a large amount of good oil absorption materials of exploitation badly.At present, oil absorption material is mainly divided into three major types: inorganic oil absorption material, organic natural oil absorption material and organic synthesis oil absorption material.Inorganic oil absorption material comprises zeolite, diatomite, clay and silica etc., and they are less to oily adsorbance; Organic natural oil absorption material comprises straw, wood fiber, bark and mestha etc., in the time of these organic natural oil absorption material oil suctions, also absorbs water, and buoyancy character is poor; Organic synthesis oil absorption material comprises polyurethane foam oil-absorbing resin, expanded polystyrene (EPS), fusion-jetting polypropylene, aeroge etc.Compare with organic natural oil absorption material with inorganic oil absorption material, organic synthesis oil absorption material has lipophile and hydrophobicity, has better oil absorbency, and easily prepares and reuse, and is often used as the material of processing greasy dirt.
Aeroge in organic synthesis oil absorption material is a kind ofly to have the nanoscale network structure that nano level superfine particle is assembled formation mutually, and in network structure, is full of lightweight, porous, amorphous solid-state material of air.The particle size of aeroge is between 1nm～100nm, and porosity is up to 99%, and density is 0.03g/m
3～0.80g/m
3.The nanometer network structure of aeroge uniqueness has broad application prospects it aspect absorption.
In prior art, take resorcinol and formaldehyde as raw material, under the effect of catalyst and surfactant, through processes such as sol-gel, solvent exchange, supercritical drying, charings, synthesized carbon aerogels.Experimental result shows: the oil absorbency of this carbon aerogels is 27g/g, and oil absorbency is lower.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of oil suction aeroge and preparation method thereof, the oil absorbency of the oil suction aeroge that method provided by the invention makes is higher.
The preparation method who the invention provides a kind of oil suction aeroge, comprises the following steps:
A) resorcinol, formaldehyde, sodium carbonate, CNT and water are mixed and carries out phenol-formaldehyde reaction, obtain hydrogel;
B) after the hydrogel described step a) being obtained mixes with surfactant, carry out the first Separation of Solid and Liquid, obtain solid hydrogel;
C) adopting organic solvent to described step b) solid hydrogel that obtains soaks, and then carries out the second Separation of Solid and Liquid, obtains organogel;
D) by described step c) the dry and charing of the organogel that obtains, obtain oil suction aeroge.
Preferably, the diameter of described CNT is 1nm～300nm.
Preferably, the mol ratio of resorcinol, formaldehyde, CNT, sodium carbonate and the water of described step in a) is 1:(1.5～5): (0.01～0.5): (0.001～0.1): (100～10000).
Preferably, described step a) in the temperature of phenol-formaldehyde reaction be 5 ℃～50 ℃;
A) time of middle phenol-formaldehyde reaction is 2h～200h to described step.
Preferably, the surfactant described step b) comprises the ethylene oxide adduct of sorbitan ester, APES, AEO, polyoxyethylene carboxylate, fatty acid methyl ester ethoxylate, polypropylene glycol and one or more in alkylolamides;
Described step b) surfactant in and the mass ratio of described hydrogel are 0.0001～0.01:1.
Preferably, the organic solvent described step c) comprises one or more in acetone, methyl alcohol, ethanol and oxolane;
Described step c) organic solvent in and the volume ratio of solid hydrogel are 0.5～10:1.
The time of soaking preferably, described step c) is 2h～200h.
Preferably, described step c), be dried as supercritical drying.
Preferably, described steps d), the temperature of charing is 500 ℃～2000 ℃;
Described steps d) in, the time of charing is 0.5h～10h.
The invention provides a kind of oil suction aeroge, by the preparation method described in technique scheme, made, the oil absorbency of described oil suction aeroge is 50g/g～2000g/g.
The preparation method who the invention provides a kind of oil suction aeroge, comprises the following steps: resorcinol, formaldehyde, CNT, sodium carbonate and water are mixed and carries out phenol-formaldehyde reaction, obtain hydrogel; After described hydrogel is mixed with surfactant, carry out the first Separation of Solid and Liquid, obtain solid hydrogel; Adopt organic solvent to soak described solid hydrogel, then carry out the second Separation of Solid and Liquid, obtain organogel; By described organogel, dry and charing, obtains oil suction aeroge.The oil suction aeroge that method provided by the invention prepares be take CNT as skeleton, and the existence of described CNT makes the hole of the oil suction aeroge that obtains larger, has improved oil absorbency.Experimental result shows: the oil absorbency of oil suction aeroge prepared by the present invention can be up to 2000g/g.
The specific embodiment
The preparation method who the invention provides a kind of oil suction aeroge, comprises the following steps:
A) resorcinol, formaldehyde, sodium carbonate, CNT and water are mixed and carries out phenol-formaldehyde reaction, obtain hydrogel;
B) after the hydrogel described step a) being obtained mixes with surfactant, carry out the first Separation of Solid and Liquid, obtain solid hydrogel;
C) adopting organic solvent to described step b) solid hydrogel that obtains soaks, and then carries out the second Separation of Solid and Liquid, obtains organogel;
D) by described step c) the dry and charing of the organogel that obtains, obtain oil suction aeroge.
Oil suction aeroge prepared by method provided by the invention be take CNT as skeleton, and the existence of CNT makes the hole of oil suction aeroge larger, has improved oil absorbency.
The present invention mixes resorcinol, formaldehyde, sodium carbonate, CNT and water to carry out phenol-formaldehyde reaction, obtains hydrogel.Order by merging when the present invention carries out phenol-formaldehyde reaction to described resorcinol, formaldehyde, sodium carbonate, CNT and water does not have special restriction, preferably described resorcinol and formaldehyde are mixed, add wherein successively again sodium carbonate, CNT and water, after mixing, carry out phenol-formaldehyde reaction, obtain hydrogel.
The present invention does not have special restriction to the source of described resorcinol, formaldehyde, CNT and sodium carbonate, adopts resorcinol well known to those skilled in the art, formaldehyde, CNT and sodium carbonate.In the present invention, described CNT can be multi-walled carbon nano-tubes, can be also SWCN, and the present invention does not have special restriction to this; The diameter of described CNT is preferably 1nm～300nm, and more preferably 10nm～250nm, most preferably is 50nm～200nm, is the most preferably 80nm～150nm.In the present invention, described sodium carbonate is preferably natrium carbonicum calcinatum; Described water is preferably one or more in running water, distilled water and deionized water, more preferably deionized water.In the present invention, the mol ratio of described resorcinol, formaldehyde, CNT, sodium carbonate and water is preferably 1:(1.5～5): (0.01～0.5): (0.001～0.1): (100～10000), 1:(2～4 more preferably): (0.1～0.4): (0.01～0.08): (500～1000), most preferably are 1:(2.5～3): (0.2～0.3): (0.02～0.06): (600～800).
In the present invention, the temperature of described phenol-formaldehyde reaction is preferably 5 ℃～50 ℃, more preferably 10 ℃～45 ℃, most preferably is 15 ℃～25 ℃; The time of described phenol-formaldehyde reaction is preferably 2h～200h, and more preferably 10h～150h, most preferably is 20h～100h, is the most preferably 40h～80h.
Obtain after hydrogel, the present invention carries out the first Separation of Solid and Liquid after described hydrogel is mixed with surfactant, obtains solid hydrogel.The order that the present invention mixes described hydrogel and surfactant does not have special restriction, preferably described surfactant is joined in the hydrogel that technique scheme obtains.The mode that the present invention mixes with surfactant described hydrogel does not have special restriction, preferably, under the condition stirring, described hydrogel is mixed with surfactant.In the present invention, described hydrogel is preferably 2h～200h with the time that described surfactant mixes, and more preferably 70h～100h, most preferably is 80h～90h; The time of concrete described mixing is the time to described hydrogel and surfactant stirring.
In the present invention, described surfactant preferably includes the ethylene oxide adduct of sorbitan ester, APES, AEO, polyoxyethylene carboxylate, fatty acid methyl ester ethoxylate, polypropylene glycol and one or more in alkylolamides, more preferably comprises one or more in nonyl phenol polyethenoxy ether, octyl phenol APEO-10,4-hydroxy ethoxy methyl benzoate and 6501 diglycollic amides.In the present invention, the mass ratio of described surfactant and described hydrogel is 0.0001～0.01:1, and more preferably 0.001～0.1:1, most preferably is 0.003～0.05:1.
The present invention does not have special restriction to the method for described the first Separation of Solid and Liquid, adopts solid-liquid separation technique scheme well known to those skilled in the art, as adopted centrifugation well known to those skilled in the art.In the present invention, the rotating speed of described centrifugation is preferably 500r/min～50000r/min, and more preferably 1000r/min～5000r/min, most preferably is 1500r/min～2000r/min.
Obtain after solid hydrogel, the present invention adopts organic solvent to soak described solid hydrogel, then carries out the second Separation of Solid and Liquid, obtains organogel.The present invention is during to described immersion, and the addition sequence of solid hydrogel and organic solvent does not have special restriction, preferably described organic solvent is joined in described solid hydrogel, and described solid hydrogel is soaked.
In the present invention, described organic solvent preferably includes one or more in acetone, methyl alcohol, ethanol and oxolane, more preferably comprises one or both in acetone and ethanol; The volume ratio of described organic solvent and described solid hydrogel is preferably 0.5～10:1, and more preferably 1～5:1, most preferably is 1.5～3:1.In the present invention, the centrifuge tube tolerance that the volume of described solid hydrogel preferably adopts with centrifugation described in technique scheme, and then mix with the organic solvent of different volumes according to actual needs, carry out the immersion of solid hydrogel.
In the present invention, the time of described immersion is preferably 2h～200h, and more preferably 30h～150h, most preferably is 7h～100h.
The present invention does not have special restriction to the method for the second Separation of Solid and Liquid, adopts solid-liquid separation technique scheme well known to those skilled in the art, as adopted centrifugation well known to those skilled in the art.In the present invention, the rotating speed of described centrifugation is preferably 500r/min～50000r/min, and more preferably 1000r/min～5000r/min, most preferably is 1500r/min～2000r/min.
Obtain after organogel, the present invention is dried described organogel and charing, obtains oil suction aeroge.In the present invention, the described dry supercritical drying that is preferably; The temperature of described supercritical drying is preferably-10 ℃～80 ℃, more preferably 0 ℃～50 ℃, most preferably is 10 ℃～25 ℃; The time of described supercritical drying is preferably 0.5h～48h, and more preferably 1h～4h, most preferably is 1h～3h; The medium of described supercritical drying is preferably methyl alcohol and CO2, more preferably methyl alcohol.
In the present invention, the temperature of described charing is preferably 500 ℃～2000 ℃, and more preferably 700 ℃～1800 ℃, most preferably be 720 ℃～1300 ℃, be the most preferably 750 ℃～1100 ℃; The time of described charing is preferably 0.5h～10h, and more preferably 1h～8h, most preferably is 2h～5h, and in an embodiment of the present invention, the time of described charing can be specially 2 hours, 3 hours or 5 hours.
The invention provides a kind of oil suction aeroge, by the preparation method described in technique scheme, made, the oil absorbency of described oil suction aeroge is 50g/g～2000g/g.
The present invention carries out the test of oil absorbency to the oil suction aeroge obtaining, method of testing is with reference to national standard (GB/T3780.2-2007): carbon black part 2: the mensuration of oil factor.
Test result shows, the oil absorbency of the oil suction aeroge that method provided by the invention prepares is 50g/g～2000g/g.
The preparation method who the invention provides a kind of oil suction aeroge, comprises the following steps: resorcinol, formaldehyde, CNT, sodium carbonate and water are mixed and carries out phenol-formaldehyde reaction, obtain hydrogel; After described hydrogel is mixed with surfactant, carry out the first Separation of Solid and Liquid, obtain solid hydrogel; Adopt organic solvent to soak described solid hydrogel, then carry out the second Separation of Solid and Liquid, obtain organogel; By described organogel, dry and charing, obtains oil suction aeroge.Oil suction aeroge prepared by method provided by the invention be take CNT as skeleton, and the existence of CNT makes the hole of oil suction aeroge larger, has improved oil absorbency.
In order to further illustrate the present invention, below in conjunction with embodiment, a kind of oil suction aeroge provided by the invention and preparation method thereof is described in detail, but they can not be interpreted as to limiting the scope of the present invention.
Embodiment 1
The CNT that the resorcinol that is 1:2:0.1:0.01:1000 by mol ratio, formaldehyde, diameter are 50nm, natrium carbonicum calcinatum and deionized water are mixed, and carry out phenol-formaldehyde reaction 48h at 20 ℃, obtain hydrogel;
In the hydrogel obtaining, add nonyl phenol polyethenoxy ether, the addition of nonyl phenol polyethenoxy ether is the quality of 0.1% hydrogel, after stirring 72h, the mixture obtaining is placed in to centrifuge and with the rotating speed of 2000r/min, carries out the first Separation of Solid and Liquid, obtain solid hydrogel;
Again the solid hydrogel obtaining is soaked to 90h, the centrifugal organogel that obtains with equal-volume acetone;
By the organogel obtaining supercritical drying 2h at 0 ℃, then at 800 ℃ charing 3h, obtain oil suction aeroge.
The present invention tests oil suction aeroge according to the method for testing of oil absorbency described in technique scheme, and test result shows: the oil absorbency of the oil suction aeroge that the embodiment of the present invention 1 obtains is 192g/g.
Embodiment 2
The CNT that the resorcinol that is 1:2:0.1:0.01:500 by mol ratio, formaldehyde, diameter are 100nm, natrium carbonicum calcinatum and deionized water are mixed, and carry out phenol-formaldehyde reaction 48h at 15 ℃, obtain hydrogel;
In the hydrogel obtaining, add octyl phenol APEO-10, the quality of the hydrogel that the addition of octyl phenol APEO-10 is 0.3%, after stirring 72h, the mixture obtaining is placed in to centrifuge and with the rotating speed of 2000r/min, carries out the first Separation of Solid and Liquid, obtain solid hydrogel;
The solid hydrogel obtaining is soaked to 72h, the centrifugal organogel that obtains with equal-volume acetone;
By the organogel obtaining supercritical drying 1.5h at 10 ℃, then at 1000 ℃ charing 2h, obtain oil suction aeroge.
The present invention tests oil suction aeroge according to the method for testing of oil absorbency described in technique scheme, and test result shows: the oil absorbency of the oil suction aeroge that the embodiment of the present invention 2 obtains is 258g/g.
Embodiment 3
The CNT that the resorcinol that is 1:2:0.1:0.01:800 by mol ratio, formaldehyde, diameter are 80nm, natrium carbonicum calcinatum and deionized water are mixed, and carry out phenol-formaldehyde reaction 48h at 25 ℃, obtain hydrogel;
In the hydrogel obtaining, add octyl phenol APEO-10, the quality of the hydrogel that the addition of octyl phenol APEO-10 is 0.2%, after stirring 100h, the mixture obtaining is placed in to centrifuge and with the rotating speed of 1500r/min, carries out the first Separation of Solid and Liquid, obtain solid hydrogel;
By equal-volume alcohol immersion 81h for the solid hydrogel obtaining, the centrifugal organogel that obtains;
By the organogel obtaining supercritical drying 1h at 10 ℃, then at 1200 ℃ charing 2h, obtain oil suction aeroge.
The present invention tests oil suction aeroge according to the method for testing of oil absorbency described in technique scheme, and test result shows: the oil absorbency of the oil suction aeroge that the embodiment of the present invention 3 obtains is 210g/g.
Embodiment 4
The CNT that the resorcinol that is 1:2:0.01:0.001:100 by mol ratio, formaldehyde, diameter are 1nm, natrium carbonicum calcinatum and deionized water are mixed, and carry out phenol-formaldehyde reaction 200h at 5 ℃, obtain hydrogel;
In the hydrogel obtaining, add 6501 diglycollic amides, the addition of 6501 diglycollic amides is the quality of 0.01% hydrogel, after stirring 100h, the mixture obtaining is placed in to centrifuge and with the rotating speed of 500r/min, carries out the first Separation of Solid and Liquid, obtain solid hydrogel;
The solid hydrogel obtaining is soaked to 200h, the centrifugal organogel that obtains by 0.5 volume ethanol;
By the organogel obtaining supercritical drying 0.5h at 80 ℃, then at 500 ℃ charing 10h, obtain oil suction aeroge.
The present invention tests oil suction aeroge according to the method for testing of oil absorbency described in technique scheme, and test result shows: the oil absorbency of the oil suction aeroge that the embodiment of the present invention 4 obtains is 50g/g.
Embodiment 5
The CNT that the resorcinol that is 1:5:0.5:0.1:10000 by mol ratio, formaldehyde, diameter are 300nm, natrium carbonicum calcinatum and deionized water are mixed, and carry out phenol-formaldehyde reaction 2h at 50 ℃, obtain hydrogel;
In the hydrogel obtaining, add 4-hydroxy ethoxy methyl benzoate, the quality of the hydrogel that the addition of 4-hydroxy ethoxy methyl benzoate is 1.0%, after stirring 100h, the mixture obtaining is placed in to centrifuge and with the rotating speed of 50000r/min, carries out the first Separation of Solid and Liquid, obtain solid hydrogel;
The solid hydrogel obtaining is soaked to 2h, the centrifugal organogel that obtains by 10 volume ethanol;
By the organogel obtaining supercritical drying 48h at-10 ℃, then at 2000 ℃ charing 0.5h, obtain oil suction aeroge.
The present invention tests oil suction aeroge according to the method for testing of oil absorbency described in technique scheme, and test result shows: the oil absorbency of the oil suction aeroge that the embodiment of the present invention 5 obtains is 2000g/g.
As seen from the above embodiment, the invention provides a kind of preparation method of oil suction aeroge, comprise the following steps: resorcinol, formaldehyde, CNT, sodium carbonate and water are mixed and carries out phenol-formaldehyde reaction, obtain hydrogel; After described hydrogel is mixed with surfactant, carry out the first Separation of Solid and Liquid, obtain solid hydrogel; Adopt organic solvent to soak described solid hydrogel, then carry out the second Separation of Solid and Liquid, obtain organogel; By described organogel, dry and charing, obtains oil suction aeroge.In oil suction aeroge prepared by method provided by the invention, take CNT as skeleton, the existence of CNT makes the hole of oil suction aeroge larger, has improved oil absorbency.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a preparation method for oil suction aeroge, comprises the following steps:
A) resorcinol, formaldehyde, sodium carbonate, CNT and water are mixed and carries out phenol-formaldehyde reaction, obtain hydrogel;
B) after the hydrogel described step a) being obtained mixes with surfactant, carry out the first Separation of Solid and Liquid, obtain solid hydrogel;
C) adopting organic solvent to described step b) solid hydrogel that obtains soaks, and then carries out the second Separation of Solid and Liquid, obtains organogel;
D) by described step c) the dry and charing of the organogel that obtains, obtain oil suction aeroge.
2. preparation method according to claim 1, is characterized in that, the diameter of described CNT is 1nm～300nm.
3. preparation method according to claim 1, it is characterized in that, the mol ratio of resorcinol, formaldehyde, CNT, sodium carbonate and the water of described step in a) is 1:(1.5～5): (0.01～0.5): (0.001～0.1): (100～10000).
4. preparation method according to claim 1, is characterized in that, the described step a) temperature of middle phenol-formaldehyde reaction is 5 ℃～50 ℃;
A) time of middle phenol-formaldehyde reaction is 2h～200h to described step.
5. preparation method according to claim 1, it is characterized in that described step b) in surfactant comprise the ethylene oxide adduct of sorbitan ester, APES, AEO, polyoxyethylene carboxylate, fatty acid methyl ester ethoxylate, polypropylene glycol and one or more in alkylolamides;
Described step b) surfactant in and the mass ratio of described hydrogel are 0.0001～0.01:1.
6. preparation method according to claim 1, is characterized in that, described step c) in organic solvent comprise one or more in acetone, methyl alcohol, ethanol and oxolane;
Described step c) organic solvent in and the volume ratio of solid hydrogel are 0.5～10:1.
7. preparation method according to claim 1, is characterized in that, described step c) in time of soaking be 2h～200h.
8. preparation method according to claim 1, is characterized in that, described steps d) in be dried as supercritical drying.
9. preparation method according to claim 1, is characterized in that, described steps d) in the temperature of charing be 500 ℃～2000 ℃;
Described steps d) in, the time of charing is 0.5h～10h.
10. an oil suction aeroge, is made by the preparation method described in claim 1～9 any one, and the oil absorbency of described oil suction aeroge is 50g/g～2000g/g.
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| CN114455564A (en) * | 2022-01-11 | 2022-05-10 | 西安理工大学 | Carbon aerogel for regulating and controlling density by space limited-area centrifugal force field and method |
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| CN114455564A (en) * | 2022-01-11 | 2022-05-10 | 西安理工大学 | Carbon aerogel for regulating and controlling density by space limited-area centrifugal force field and method |
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