CN103495397A - Method for preparing carbon foams capable of adsorbing grease and organic solvents from waste paper - Google Patents
Method for preparing carbon foams capable of adsorbing grease and organic solvents from waste paper Download PDFInfo
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- CN103495397A CN103495397A CN201310472616.4A CN201310472616A CN103495397A CN 103495397 A CN103495397 A CN 103495397A CN 201310472616 A CN201310472616 A CN 201310472616A CN 103495397 A CN103495397 A CN 103495397A
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Abstract
The invention discloses a method for preparing carbon foams capable of adsorbing grease and organic solvents from waste paper. The method comprises the following steps: carrying out pulping, freeze drying, high temperature decomposition and annealing treatment on the waste paper so as to obtain the water-repellent carbon foams. The method provided by the invention is simple, low in cost and suitable for large scale production, the prepared carbon foams have good mechanical properties and the strong adsorption capacity of organic solvents or grease, and thus, the carbon foams can be applied to the field of sewage treatment or liquid-liquid separation; by a fractionation and extruding method, the reutilization of the carbon foams and adsorbates are realized.
Description
Technical field
The present invention relates to a kind of method of utilizing waste paper to prepare the carbon foam of adsorbed oil and organic solvent.
Background technology
Chief component-waste paper (D.H.Vynios, D.A.Papaioannou, G.Filos as municipal pollution, G.Karigiannis, T.Tziala, G.Lagios, BioResources2009,4,509), caused serious environmental problem (A.A.Zorpas, D.Arapoglou, K.Panagiotis, Waste Manage.2003,23,27).
Traditional waste paper is recycled, mainly to be translated into again new paper product (http://en.wikipedia.org/wiki/Paper_recycling), but along with the increase that recycles number of times, increasing waste paper has been not suitable for making paper product again, therefore can cause a large amount of waste paper to pollute.
In order to recycle these waste paper and to reduce the pollution that it brings to environment, people start to utilize waste paper ethanol (M.Wayman processed, S.Chen, K.Doan, Process Biochem.1992, 27, 239), biodegradable foamed (S.H.Lee, Y.Teramoto, N.Shiraishi, J.Appl.Polym.Sci.2002, 83, 1482), methane (H.W.Yen, D.E.Brune, Bioresource Technol.2007, 98, the product such as 130), but along with the sharply increase of paper product quantity and the enhancing of people's environmental consciousness, need in a hurry to find other and utilize the approach of waste paper.
In addition, the leakage of crude oil and organic solvent has caused very large pollution to environment, and in order to remove these pollutants, solid adsorbent has obtained people's broad research.Traditional adsorbent comprises: natural product (wool, zeolite etc.) (H.M.Choi, R.M.Cloud, Environ.Sci.Technol.1992,26,772; D.Bastani, A.A.Safekordi, A.Alihosseini, V.Taghikhani, Sep.Purif.Technol.2006,52,295), expanded graphite (X.P.Yan, Y.Y.Zhou, S.W.Wang, K.N.Kim, J.H.Li, Talanta2006,69,970; M.F.Zhao, P.Liu, Desalination2009,249,331), active carbon (S.D.Li, S.H.Tian, Y.F.Feng, J.J.Lei, P.P.Wang, Y.Xiong, J.Hazard.Mater.2010,183,506), polymer (A.M.Atta, R.A.M.El-Ghazawy, R.K.Farag, A.-A.A.Abdel-Azim, React.Funct.Polym.2006,66,931; A.M.Atta, S.H.El-Hamouly, A.M.AlSabagh, M.M.Gabr, J.Appl.Polym.Sci.2007,105,2113) etc.Although they have the advantage of oneself separately, generally, can not meet practical needs, although such as natural product cost is low, but they do not have adsorptive selectivity, and adsorption rate is very low; Owing to being graininess, use quite inconvenience although the expanded graphite adsorption rate is higher; In use may there be secondary pollution in porous polymer.
Along with the appearance of new material CNT and Graphene, the solid adsorbent based on these two also is developed rapidly (X.C.Gui, J.Q.Wei, K.L.Wang, A.Y.Cao, H.W.Zhu, Y.Jia, Q.K.Shu, D.H.Wu, Adv.Mater.2010,22,617; Y.Zhao, C.Hu, Y.Hu, H.Cheng, G.Shi, L.Qu, Angew.Chem.Int.Ed.2012,51,11371), the adsorbent consisted of them not only has good adsorptive selectivity, also has very high adsorption rate simultaneously, but this class adsorbent still also has problems: the process of preparation can produce to pollute as prepare graphite oxide and can produce acid pollution liquid; The higher chemical gaseous phase depositing process that particularly adopts of cost is produced porous adsorbent.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art, the invention provides a kind of method of utilizing waste paper to prepare the carbon foam of adsorbed oil and organic solvent, take and originate waste paper abundant, with low cost as raw material, it is carried out to freeze drying, high annealing etc. and process to obtain adsorptive selectivity carbon foam preferably, implementation method is simple, pollute little and can be mass-produced, and takes full advantage of waste paper and effectively reduces the environmental problem that waste paper brings.
Technical scheme: for achieving the above object, the technical solution used in the present invention is:
A kind of method of utilizing waste paper to prepare the carbon foam of adsorbed oil and organic solvent, be specially waste paper after making beating, freeze drying, pyrolytic, annealing in process, obtains the carbon foam of hydrophobic.
In the method, making beating is about to waste paper and makes paper pulp, belongs to prior art; Freeze drying first is frozen into paper pulp freezing, then under vacuum environment, allows the process of cryosublimation, belongs to prior art.Inventive point of the present invention is to use waste paper to carry out the preparation of carbon foam, and the carbon foam of preparing can be used in adsorbed oil and organic solvent.
Described waste paper is the waste paper that three major polymers: cellulose is made, and comprises paper for daily use, paper in the office, printing and carton etc.
Preferably, the temperature of described pyrolytic is 400～1500 ℃.
Preferably, described pyrolytic carries out in vacuum or inert gas (such as nitrogen or argon gas) environment.
The carbon foam that utilizes the inventive method to obtain, have extraordinary machinery and newly can and organic solvent or grease be had to very strong adsorption capacity, can be used for the field that sewage disposal or liquid liquid separate.The waste paper used comprises carton, newspaper, paper in the office, house paper using etc.Described organic solvent or grease comprise vegetable oil, crude oil, pump oil, dodecane, decane, octane, hexane, phenol, nitrobenzene, chloroform, dichloro-benzenes, ethylo benzene, toluene, benzene, dimethyl sulfoxide (DMSO), oxolane, dimethyl formamide, acetone, ethanol, methyl alcohol, kerosene, castor oil, heptane, diesel oil, gasoline, rape seed oil, olive oil, carbon tetrachloride, octadecylene, cyclohexane, isopropyl alcohol, phenmethylol etc.In addition, the methods such as fractionation, extruding of can utilizing the carbon foam that utilizes the inventive method to obtain realize recycling.
Beneficial effect: the method for utilizing waste paper to prepare the carbon foam of adsorbed oil and organic solvent provided by the invention, the prior art of comparing has following advantage: 1, take waste paper as raw material, the preparation method is simple and pollution that produce is few, therefore with low cost and can effectively eliminate the environmental pollution that waste paper causes; 2, the carbon foam obtained has good mechanical performance, organic solvent and grease are had to high adsorption capacity, the fast characteristics of adsorption rate, so by the carbon foam for adsorbing organic solvent and grease has the advantage on performance, can be used for that liquid liquid separates and sewage disposal in organic solvent and the absorption of grease; 3, the carbon foam obtained has extraordinary heat endurance and mechanical property, can adopt recycling and the recycling of pollutant of accomplished in many ways carbon foam.
The accompanying drawing explanation
The ESEM picture that Fig. 1 is the paper pulp gel;
The ESEM picture that Fig. 2 is the carbon foam;
Fig. 3 is the adsorption rate figure of carbon foam to various organic liquids;
Fig. 4 utilizes the method for fractionation to carry out adsorption and desorption circulation experiment figure to the carbon foam;
Fig. 5 carries out adsorption and desorption circulation experiment figure for the method for utilizing extruding to the carbon foam.
The specific embodiment
Below in conjunction with accompanying drawing, the present invention is further described.
Be illustrated in figure 1 a kind of method of utilizing waste paper to prepare the carbon foam of adsorbed oil and organic solvent, be specially useless printing paper (paper in the office) after making beating, freeze drying, pyrolytic, annealing in process, obtain the carbon foam of hydrophobic.In general, the temperature of described pyrolytic is 400～1500 ℃, and described pyrolytic carries out in vacuum or inert gas environment.
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
The first step: the waste paper of retrieving is ground into to paper scrap, as for soaking 24 hours in water, then adds watery hydrochloric acid and continue and soak 12 hours, then wash, then be poured into water again also strong stirring and obtain paper pulp, then utilize freeze drying to obtain the paper pulp gel.The ESEM picture that Fig. 1 is the paper pulp gel, can see a large amount of fibers.
Second step: the paper pulp gel is placed in to heating tube, and the good seal heating tube, then by the air emptying in heating tube, make the paper pulp gel in vacuum state.
The 3rd step: heating tube is heated to 850 ℃ and maintain 2h, then naturally cools to room temperature, can obtain required carbon foam.The ESEM picture that Fig. 2 is the carbon foam, can find out, with respect to the fiber in Fig. 1, in this figure, fiber has obviously attenuated, and illustrates that high temperature has caused the decomposition of some materials of pulp fiber surface.
The 4th step: the absorption property to the carbon foam carries out a series of signs.The carbon foam is used as adsorbent, separate or the sewage separation field for liquid liquid, for adsorbing organic solvent or grease, the adsorption rate of test carbon foam to various organic solvents or grease; The test mode of described adsorption rate is: the carbon foam is cut into to fritter, and take the quality of every fritter, be designated as W
dry, then the carbon foam of fritter is put into to solvent upon adsorption, allow the carbon foam fully adsorb, then take the quality of the fritter carbon foam after abundant absorption, be designated as W
wet, the adsorption rate of carbon foam is calculated by following formula:
Utilize said method, calculate the carbon foam adsorption rate of pump oil, olive oil, rape seed oil, heptane, hexane, chloroform, toluene, dimethyl formamide, acetone, ethanol, phenmethylol, isopropyl alcohol, octadecylene, cyclohexane is carried out to Measurement and Computation, result as shown in Figure 3, abscissa means the adsorption rate of carbon foam, and ordinate means organic solvent upon adsorption or grease; For example the carbon foam is 18800% to the adsorption rate of pump oil, and the carbon foam is 8500% to the adsorption rate of ethanol, and the carbon foam is 7000% to the adsorption rate of hexane, and the carbon foam is 15100% to the adsorption rate of chloroform.
The 5th step: the circulation experiment that the carbon foam is carried out to adsorption/desorption.Because the carbon foam made has extraordinary heat endurance and mechanical stability, therefore can recycle, in this example, used the method for fractionation and extruding to be tested respectively, below be introduced respectively.
Because the carbon foam has heat endurance preferably, therefore can use fractionating process to recycle the carbon foam; Use the carbon foam to carry out corresponding experiment to heptane, detailed process is: the carbon foam that will adsorb heptane is placed in flask, then be heated near heptane boiling point (98.5 ℃), or by reducing the air pressure in flask, to reduce the boiling point of heptane, at this moment heptane will be by the mode of evaporation, from the carbon foam, escape out, to be distilled completing, then this carbon foam is placed in to heptane, re-start absorption, so circulation is gone down.Experiment has repeated 5 times altogether continuously, and Fig. 4 has shown adsorbance and the desorption rate of carbon foam in each experiment, and abscissa means the cycle-index (totally 5 times) of experiment, and ordinate means the weight of the heptane that the carbon foam adsorbs, the mg of unit; The point that is positioned at top means the weight of adsorbed heptane, and the curve that is arranged in below means the heptane weight that the carbon foam is residual.
Because the carbon foam has mechanical stability preferably, so the method for extruding also can be used for reclaiming the carbon foam, for higher boiling and more expensive solvent, the method has larger advantage; Use extrusion to carry out corresponding experiment to octadecylene, detailed process is: with clip, the carbon foam that has adsorbed octadecylene is pushed, so just the octadecylene in foam can be extruded, then the foam pushed through is placed in to octadecylene, re-start absorption, so circulation is gone down.Experiment has repeated 5 times altogether continuously, and Fig. 5 has shown adsorbance and the desorption rate of carbon foam in each experiment, and abscissa means the cycle-index (totally 5 times) of experiment, and ordinate means the weight of the octadecylene that the carbon foam adsorbs, the mg of unit; The point that is positioned at top means the weight of adsorbed octadecylene, and the curve that is arranged in below means the octadecylene weight that the carbon foam is residual.
Method is substantially with embodiment 1, and difference is, the temperature of pyrolytic is 400 ℃, and gained carbon foam is similar to shown in Fig. 2, adsorption rate and recycle result and be similar to situation about implementing in 1.
Method is substantially with embodiment 1, and difference is, the temperature of pyrolytic is 1500 ℃, and gained carbon foam is similar to shown in Fig. 2, adsorption rate and recycle result and be similar to situation about implementing in 1.
Embodiment 4
Method is substantially with embodiment 2, and difference is, the temperature of pyrolytic is 1000 ℃, and protective gas is nitrogen, and gained carbon foam is similar to shown in Fig. 2, adsorption rate and recycle result and be similar to situation about implementing in 1.
Embodiment 5
Method is substantially with embodiment 3, and difference is, protective gas is argon gas, and gained carbon foam is similar to shown in Fig. 2, adsorption rate and recycle result and be similar to situation about implementing in 1.
Embodiment 6
Method is substantially with embodiment 1, difference is: the printing paper that will give up changes useless books (printing) or waste paper towel (paper for daily use) into, the carbon foam of gained is similar to shown in Fig. 2, it is pattern thickness difference, main component or carbon fiber, therefore this carbon foam has the characteristic of hydrophobic oleophylic equally, and adsorption capacity, recycling rate of waterused are similar to Fig. 3, Fig. 4.
The above is only the preferred embodiment of the present invention; be noted 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 (4)
1. a method of utilizing waste paper to prepare the carbon foam of adsorbed oil and organic solvent, is characterized in that: waste paper, after making beating, freeze drying, pyrolytic, annealing in process, is obtained to the carbon foam of hydrophobic.
2. the method for utilizing waste paper to prepare the carbon foam of adsorbed oil and organic solvent according to claim 1, it is characterized in that: described waste paper is the waste paper that three major polymers: cellulose is made, and comprises paper for daily use, paper in the office, printing and carton.
3. the method for utilizing waste paper to prepare the carbon foam of adsorbed oil and organic solvent according to claim 1, it is characterized in that: the temperature of described pyrolytic is 400～1500 ℃.
4. the method for utilizing waste paper to prepare the carbon foam of adsorbed oil and organic solvent according to claim 1, it is characterized in that: described pyrolytic carries out in vacuum or inert gas environment.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108479701A (en) * | 2018-04-13 | 2018-09-04 | 同济大学 | A kind of super-hydrophobic super-oleophylic carbon material and preparation method thereof |
| CN111232950A (en) * | 2020-03-13 | 2020-06-05 | 陕西科技大学 | Method for preparing multifunctional elastic carbon material by carbonizing household paper |
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| JP2003066191A (en) * | 2001-08-29 | 2003-03-05 | Wakaida Eng:Kk | Processing method for radioactive gas and filter device for adsorbing radioactive gas |
| CN101045803A (en) * | 2006-03-27 | 2007-10-03 | 株式会社东芝 | Foaming composition and method of preparing foaming body |
| CN102500133A (en) * | 2011-10-15 | 2012-06-20 | 东南大学 | Application method of graphene sponge |
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Patent Citations (3)
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| JP2003066191A (en) * | 2001-08-29 | 2003-03-05 | Wakaida Eng:Kk | Processing method for radioactive gas and filter device for adsorbing radioactive gas |
| CN101045803A (en) * | 2006-03-27 | 2007-10-03 | 株式会社东芝 | Foaming composition and method of preparing foaming body |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108479701A (en) * | 2018-04-13 | 2018-09-04 | 同济大学 | A kind of super-hydrophobic super-oleophylic carbon material and preparation method thereof |
| CN111232950A (en) * | 2020-03-13 | 2020-06-05 | 陕西科技大学 | Method for preparing multifunctional elastic carbon material by carbonizing household paper |
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