CN103752277B - A kind of oil suction aeroge and preparation method thereof - Google Patents
A kind of oil suction aeroge and preparation method thereof Download PDFInfo
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- CN103752277B CN103752277B CN201410064676.7A CN201410064676A CN103752277B CN 103752277 B CN103752277 B CN 103752277B CN 201410064676 A CN201410064676 A CN 201410064676A CN 103752277 B CN103752277 B CN 103752277B
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Abstract
The invention provides a kind of preparation method of oil suction aeroge, comprise the following steps: phenol-formaldehyde reaction is carried out in the mixing of resorcinol, formaldehyde, CNT, sodium carbonate and water, obtains hydrogel; Carry out the first Separation of Solid and Liquid after being mixed with surfactant by described hydrogel, 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 take CNT as skeleton, and the existence of CNT makes the hole of the oil suction aeroge obtained larger, improves oil absorbency.Experimental result shows: the oil absorbency of oil suction aeroge prepared by the present invention is 50g/g ~ 2000g/g.
Description
Technical field
The invention belongs to technical field of organic synthesis, particularly relate to a kind of oil suction aeroge and preparation method thereof.
Background technology
Along with industrial expansion, the pollution that waste water, offshore oil leakage etc. containing greasy dirt cause damages to the life condition of tellurian, forces the mankind to need exploitation oil absorption material excellent in a large number 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 the adsorbance of oil; Organic natural oil absorption material comprises straw, wood fiber, bark and mestha etc., and also absorb water while these organic natural oil absorption material oil suctions, buoyant properties 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, often by the material as process greasy dirt.
Aeroge in organic synthesis oil absorption material is a kind of nanoscopic network structure having nano level superfine particle and mutually assemble formation, and is full of lightweight, porous, amorphous solid-state material of air in the network architecture.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 Specific surface area of aeroge uniqueness, makes it have broad application prospects in absorption.
In prior art, with resorcinol and formaldehyde for raw material, under the effect of catalyst and surfactant, synthesize carbon aerogels through processes such as sol-gel, solvent displacement, supercritical drying, charings.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 obtains is higher.
The invention provides a kind of preparation method of oil suction aeroge, comprise the following steps:
A) phenol-formaldehyde reaction is carried out in the mixing of resorcinol, formaldehyde, sodium carbonate, CNT and water, obtain hydrogel;
B) carry out the first Separation of Solid and Liquid after being mixed with surfactant by the hydrogel that described step a) obtains, obtain solid hydrogel;
C) organic solvent is adopted to described step b) solid hydrogel that obtains soaks, then carries out the second Separation of Solid and Liquid, obtain 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, described step a) in the mol ratio of resorcinol, formaldehyde, CNT, sodium carbonate and water be 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 DEG C ~ 50 DEG C;
Described step a) in time of phenol-formaldehyde reaction be 2h ~ 200h.
Preferably, described step b) in surfactant comprise in sorbitan ester, APES, AEO, polyoxyethylene carboxylate, fatty acid methyl ester ethoxylate, the ethylene oxide adduct of polypropylene glycol and alkylolamides one or more;
Described step b) in surfactant and the mass ratio of described hydrogel be 0.0001 ~ 0.01:1.
Preferably, described step c) in organic solvent comprise in acetone, methyl alcohol, ethanol and oxolane one or more;
Described step c) in organic solvent and the volume ratio of solid hydrogel be 0.5 ~ 10:1.
Preferably, described step c) in soak time be 2h ~ 200h.
Preferably, described step c) in drying be supercritical drying.
Preferably, described steps d) in charing temperature be 500 DEG C ~ 2000 DEG C;
Described steps d) in charing time be 0.5h ~ 10h.
The invention provides a kind of oil suction aeroge, obtained by the preparation method described in technique scheme, the oil absorbency of described oil suction aeroge is 50g/g ~ 2000g/g.
The invention provides a kind of preparation method of oil suction aeroge, comprise the following steps: phenol-formaldehyde reaction is carried out in the mixing of resorcinol, formaldehyde, CNT, sodium carbonate and water, obtains hydrogel; Carry out the first Separation of Solid and Liquid after being mixed with surfactant by described hydrogel, 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 take CNT as skeleton, and the existence of described CNT makes the hole of the oil suction aeroge obtained larger, improves oil absorbency.Experimental result shows: the oil absorbency of oil suction aeroge prepared by the present invention can up to 2000g/g.
Detailed description of the invention
The invention provides a kind of preparation method of oil suction aeroge, comprise the following steps:
A) phenol-formaldehyde reaction is carried out in the mixing of resorcinol, formaldehyde, sodium carbonate, CNT and water, obtain hydrogel;
B) carry out the first Separation of Solid and Liquid after being mixed with surfactant by the hydrogel that described step a) obtains, obtain solid hydrogel;
C) organic solvent is adopted to described step b) solid hydrogel that obtains soaks, then carries out the second Separation of Solid and Liquid, obtain 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 take CNT as skeleton, and the existence of CNT makes the hole of oil suction aeroge larger, improves oil absorbency.
The mixing of resorcinol, formaldehyde, sodium carbonate, CNT and water is carried out phenol-formaldehyde reaction by the present invention, 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 by described resorcinol and formaldehyde mixing, add sodium carbonate, CNT and water wherein successively again, carry out phenol-formaldehyde reaction after mixing, obtain hydrogel.
The source of the present invention to described resorcinol, formaldehyde, CNT and sodium carbonate does not have special restriction, 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, and can be SWCN, the present invention have special restriction to this yet; The diameter of described CNT is preferably 1nm ~ 300nm, is 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 be preferably in running water, distilled water and deionized water one or more, be 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), be more preferably 1:(2 ~ 4): (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 DEG C ~ 50 DEG C, is more preferably 10 DEG C ~ 45 DEG C, most preferably is 15 DEG C ~ 25 DEG C; The time of described phenol-formaldehyde reaction is preferably 2h ~ 200h, is more preferably 10h ~ 150h, most preferably is 20h ~ 100h, is the most preferably 40h ~ 80h.
After obtaining hydrogel, the present invention carries out the first Separation of Solid and Liquid after being mixed with surfactant by described hydrogel, obtains solid hydrogel.The order of the present invention to described hydrogel and surfactant mixing does not have special restriction, is preferably joined by described surfactant in the hydrogel that technique scheme obtains.The present invention does not have special restriction to the mode that described hydrogel mixes with surfactant, preferably under the condition stirred, is mixed by described hydrogel with surfactant.In the present invention, the time that described hydrogel mixes with described surfactant is preferably 2h ~ 200h, is more preferably 70h ~ 100h, most preferably is 80h ~ 90h; The time of concrete described mixing is the time of stirring described hydrogel and surfactant.
In the present invention, described surfactant preferably include in sorbitan ester, APES, AEO, polyoxyethylene carboxylate, fatty acid methyl ester ethoxylate, the ethylene oxide adduct of polypropylene glycol and alkylolamides one or more, more preferably comprise in nonyl phenol polyethenoxy ether, octyl phenol APEO-10,4-hydroxy ethoxy methyl benzoate and 6501 diglycollic amides one or more.In the present invention, the mass ratio of described surfactant and described hydrogel is 0.0001 ~ 0.01:1, is more preferably 0.001 ~ 0.1:1, most preferably is 0.003 ~ 0.05:1.
The method of the present invention to described first Separation of Solid and Liquid does not have special restriction, 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, is more preferably 1000r/min ~ 5000r/min, most preferably is 1500r/min ~ 2000r/min.
After obtaining 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.When the present invention is to described immersion, the addition sequence of solid hydrogel and organic solvent does not have special restriction, preferably joins in described solid hydrogel by described organic solvent, soaks described solid hydrogel.
In the present invention, described organic solvent preferably include in acetone, methyl alcohol, ethanol and oxolane one or more, more preferably comprise in acetone and ethanol one or both; The volume ratio of described organic solvent and described solid hydrogel is preferably 0.5 ~ 10:1, is more preferably 1 ~ 5:1, most preferably is 1.5 ~ 3:1.In the present invention, the volume of described solid hydrogel preferably with the centrifuge tube tolerance that centrifugation described in technique scheme adopts, and then mixes with the organic solvent of different volumes according to actual needs, carries out the immersion of solid hydrogel.
In the present invention, the time of described immersion is preferably 2h ~ 200h, is more preferably 30h ~ 150h, most preferably is 7h ~ 100h.
The method of the present invention to the second Separation of Solid and Liquid does not have special restriction, 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, is more preferably 1000r/min ~ 5000r/min, most preferably is 1500r/min ~ 2000r/min.
After obtaining organogel, described organogel is carried out drying and charing by the present invention, obtains oil suction aeroge.In the present invention, described drying is preferably supercritical drying; The temperature of described supercritical drying is preferably-10 DEG C ~ 80 DEG C, is more preferably 0 DEG C ~ 50 DEG C, most preferably is 10 DEG C ~ 25 DEG C; The time of described supercritical drying is preferably 0.5h ~ 48h, is more preferably 1h ~ 4h, most preferably is 1h ~ 3h; The medium of described supercritical drying is preferably methyl alcohol and CO2, is more preferably methyl alcohol.
In the present invention, the temperature of described charing is preferably 500 DEG C ~ 2000 DEG C, is more preferably 700 DEG C ~ 1800 DEG C, most preferably is 720 DEG C ~ 1300 DEG C, is the most preferably 750 DEG C ~ 1100 DEG C; The time of described charing is preferably 0.5h ~ 10h, is 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, obtained by the preparation method described in technique scheme, 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 obtained, and 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 invention provides a kind of preparation method of oil suction aeroge, comprise the following steps: phenol-formaldehyde reaction is carried out in the mixing of resorcinol, formaldehyde, CNT, sodium carbonate and water, obtains hydrogel; Carry out the first Separation of Solid and Liquid after being mixed with surfactant by described hydrogel, 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 take CNT as skeleton, and the existence of CNT makes the hole of oil suction aeroge larger, improves 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 being described in detail, but they can not being interpreted as limiting the scope of the present invention.
Embodiment 1
Be the resorcinol of 1:2:0.1:0.01:1000 by mol ratio, formaldehyde, diameter be the mixing of the CNT of 50nm, natrium carbonicum calcinatum and deionized water, at 20 DEG C, carry out phenol-formaldehyde reaction 48h, obtain hydrogel;
Nonyl phenol polyethenoxy ether is added in the hydrogel obtained, the addition of nonyl phenol polyethenoxy ether is the quality of the hydrogel of 0.1%, after stirring 72h, the mixture obtained is placed in centrifuge and carries out the first Separation of Solid and Liquid with the rotating speed of 2000r/min, obtain solid hydrogel;
Again the solid hydrogel equal-volume acetone that obtains is soaked 90h, centrifugally obtain organogel;
By the organogel supercritical drying 2h at 0 DEG C obtained, then carbonize 3h at 800 DEG C, 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
Be the resorcinol of 1:2:0.1:0.01:500 by mol ratio, formaldehyde, diameter be the mixing of the CNT of 100nm, natrium carbonicum calcinatum and deionized water, at 15 DEG C, carry out phenol-formaldehyde reaction 48h, obtain hydrogel;
Octyl phenol APEO-10 is added in the hydrogel obtained, the addition of octyl phenol APEO-10 is the quality of the hydrogel of 0.3%, after stirring 72h, the mixture obtained is placed in centrifuge and carries out the first Separation of Solid and Liquid with the rotating speed of 2000r/min, obtain solid hydrogel;
The solid hydrogel equal-volume acetone that obtains is soaked 72h, centrifugally obtains organogel;
By the organogel supercritical drying 1.5h at 10 DEG C obtained, then carbonize 2h at 1000 DEG C, 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
Be the resorcinol of 1:2:0.1:0.01:800 by mol ratio, formaldehyde, diameter be the mixing of the CNT of 80nm, natrium carbonicum calcinatum and deionized water, at 25 DEG C, carry out phenol-formaldehyde reaction 48h, obtain hydrogel;
Octyl phenol APEO-10 is added in the hydrogel obtained, the addition of octyl phenol APEO-10 is the quality of the hydrogel of 0.2%, after stirring 100h, the mixture obtained is placed in centrifuge and carries out the first Separation of Solid and Liquid with the rotating speed of 1500r/min, obtain solid hydrogel;
By the solid hydrogel equal-volume alcohol immersion 81h obtained, centrifugally obtain organogel;
By the organogel supercritical drying 1h at 10 DEG C obtained, then carbonize 2h at 1200 DEG C, 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
Be the resorcinol of 1:2:0.01:0.001:100 by mol ratio, formaldehyde, diameter be the mixing of the CNT of 1nm, natrium carbonicum calcinatum and deionized water, at 5 DEG C, carry out phenol-formaldehyde reaction 200h, obtain hydrogel;
6501 diglycollic amides are added in the hydrogel obtained, the addition of 6501 diglycollic amides is the quality of the hydrogel of 0.01%, after stirring 100h, the mixture obtained is placed in centrifuge and carries out the first Separation of Solid and Liquid with the rotating speed of 500r/min, obtain solid hydrogel;
The solid hydrogel that obtains 0.5 volume ethanol is soaked 200h, centrifugally obtains organogel;
By the organogel supercritical drying 0.5h at 80 DEG C obtained, then carbonize 10h at 500 DEG C, 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
Be the resorcinol of 1:5:0.5:0.1:10000 by mol ratio, formaldehyde, diameter be the mixing of the CNT of 300nm, natrium carbonicum calcinatum and deionized water, at 50 DEG C, carry out phenol-formaldehyde reaction 2h, obtain hydrogel;
4-hydroxy ethoxy methyl benzoate is added in the hydrogel obtained, the addition of 4-hydroxy ethoxy methyl benzoate is the quality of the hydrogel of 1.0%, after stirring 100h, the mixture obtained is placed in centrifuge and carries out the first Separation of Solid and Liquid with the rotating speed of 50000r/min, obtain solid hydrogel;
The solid hydrogel that obtains 10 volume ethanol are soaked 2h, centrifugally obtains organogel;
By the organogel supercritical drying 48h at-10 DEG C obtained, then carbonize 0.5h at 2000 DEG C, 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: phenol-formaldehyde reaction is carried out in the mixing of resorcinol, formaldehyde, CNT, sodium carbonate and water, obtains hydrogel; Carry out the first Separation of Solid and Liquid after being mixed with surfactant by described hydrogel, 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.Be skeleton with CNT in oil suction aeroge prepared by method provided by the invention, the existence of CNT makes the hole of oil suction aeroge larger, improves 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 (9)
1. a preparation method for oil suction aeroge, comprises the following steps:
A) phenol-formaldehyde reaction is carried out in raw material mixing, obtain hydrogel; Described raw material is made up of resorcinol, formaldehyde, sodium carbonate, CNT and water;
B) carry out the first Separation of Solid and Liquid after being mixed with surfactant by the hydrogel that described step a) obtains, obtain solid hydrogel;
C) organic solvent is adopted to described step b) solid hydrogel that obtains soaks, then carries out the second Separation of Solid and Liquid, obtain organogel;
D) by described step c) the dry and charing of the organogel that obtains, obtain oil suction aeroge;
Described step a) in the mol ratio of resorcinol, formaldehyde, CNT, sodium carbonate and water be 1:(2 ~ 4): (0.1 ~ 0.4): (0.01 ~ 0.08): (500 ~ 1000); Described step a) in the temperature of phenol-formaldehyde reaction be 5 DEG C ~ 50 DEG C.
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, is characterized in that, described step a) in the temperature of phenol-formaldehyde reaction be 5 DEG C ~ 50 DEG C;
Described step a) in time of phenol-formaldehyde reaction be 2h ~ 200h.
4. preparation method according to claim 1, it is characterized in that, described step b) in surfactant comprise in sorbitan ester, APES, AEO, polyoxyethylene carboxylate, fatty acid methyl ester ethoxylate, the ethylene oxide adduct of polypropylene glycol and alkylolamides one or more;
Described step b) in surfactant and the mass ratio of described hydrogel be 0.0001 ~ 0.01:1.
5. preparation method according to claim 1, is characterized in that, described step c) in organic solvent comprise in acetone, methyl alcohol, ethanol and oxolane one or more;
Described step c) in organic solvent and the volume ratio of solid hydrogel be 0.5 ~ 10:1.
6. preparation method according to claim 1, is characterized in that, described step c) in soak time be 2h ~ 200h.
7. preparation method according to claim 1, is characterized in that, described steps d) in drying be supercritical drying.
8. preparation method according to claim 1, is characterized in that, described steps d) in charing temperature be 500 DEG C ~ 2000 DEG C;
Described steps d) in charing time be 0.5h ~ 10h.
9. an oil suction aeroge, is obtained by the preparation method described in claim 1 ~ 8 any one, and the oil absorbency of described oil suction aeroge is 50g/g ~ 2000g/g.
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| CN107398274A (en) * | 2016-05-20 | 2017-11-28 | 香港纺织及成衣研发中心有限公司 | The catalyst and preparation method of organic pollution in a kind of degraded dyeing waste water |
| CN107020071B (en) * | 2017-04-21 | 2019-09-06 | 山东省科学院新材料研究所 | Super-hydrophobic compound carbon aerogels oil absorption material of one kind and preparation method thereof |
| CN113387344B (en) * | 2021-06-28 | 2022-11-25 | 中国科学院合肥物质科学研究院 | Method for preparing carbon aerogel with assistance of epichlorohydrin |
| 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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