CN102218296A - Method for preparing carbon nanofiber-supported carbon foam and method for applying nanofiber-supported carbon foam to adsorption of greasy dirt - Google Patents
Method for preparing carbon nanofiber-supported carbon foam and method for applying nanofiber-supported carbon foam to adsorption of greasy dirt Download PDFInfo
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Abstract
The invention discloses a method for preparing nanofiber-supported carbon foam and a method for applying the nanofiber-supported carbon foam to adsorption of greasy dirt, and belongs to the technical field of inorganic non-metallic carbon material science. Carbon nanofibers are supported on the surface of carbon foam by a chemical vapor deposition technology to form a composite material; and the composite material serving as an adsorbing material is applied to sewage containing greasy dirt, and the removal rate of the greasy dirt is 100 percent. The invention has the characteristics of simple process, low production cost, environmental friendliness, high capacity of removing the greasy dirt, wide application range, simple separation, cycle use and the like.
Description
Technical field
The present invention relates to a kind of preparation of Carbon foam loaded with nano carbon fiber and the application process of absorption greasy dirt thereof, belong to inorganic non-metallic carbon material science and technology field.
Background technology
Current society, oil occupies and consequence as the energy.Yet, in oil exploitation, processing, transportation and use, have a considerable amount of oil to reveal, discard in the Yu Haiyang.The whole world enters the petroleum pollution of ocean every year more than 1,000 ten thousand tons, and these pollute for marine ecosystems and bring destructive disaster, and therefore the improvement to greasy dirt in the seawater becomes the task of top priority.At present in the world the improvement of greasy dirt there are chemical method and physical method.What chemical method adopted is the chemical detergent that comprises emulsifying dispersant, oil-collecting agent, fuel thickener etc.The chemistry detergent can effectively be cleared up less than the oil film of 1mm thickness.But chemical method can consume a large amount of medicines, also may produce secondary pollution in addition.Physical method generally adopts the oil fence, contamination removing ship and attached retracting device, oil absorption material (comprising macromolecular material, inorganic porous material and fiber etc.) cleaning greasy dirt.Physical method is with its environmental friendliness, removes advantages such as speed oil is fast and is subjected to paying attention to widely.Mainly based on the polypropylene-base oil absorption material, the market price is at the 3500-4000 dollar per tonne at present, and cost is higher relatively.In addition, form because polypropylene-base washing oil material mostly is flexible material greatly, so oil-retaining is poor after the oil suction, slightly a pressurization leakage of oil again.Simultaneously,, therefore can only carry out de-oiling, make it be difficult to be repeatedly used by extruding because the polypropylene material softening temperature is lower than 150 ℃.Usually the access times of polypropylene-base oil absorption material are 2-3 time.The existence of these shortcomings makes their application be restricted, and the development of new oil absorption material becomes the task of top priority.Studies show that the large pore material with super hydrophobic surface can effectively carry out water-oil separating (Angewandte Chemie-International Edition, 2004.43 (15): 2012-2014; Advanced Materials, 2006.18 (23): 3063-3078.).
Carbon foam is a kind of have high porosity, low-density, strong acid-fast alkali-proof resistance to chemical attack, higher thermal conductivity factor and heat endurance, higher mechanical strength and macropore foam-like raw material of wood-charcoal material of high opening pore structure.These characteristics have Carbon foam becomes the possibility of excellent oil absorption material.For example, Carbon foam has guaranteed that up to 97% porosity it can adsorb the mink cell focus doubly above own wt 20-30; The low-density of Carbon foam makes it all float on the sea before and after greasy dirt absorption, is convenient to it is handled; The strong corrosion resistant performance has guaranteed that it can use for a long time in seawater even high corrosive environment; Higher thermal conductivity factor might separate it by the greasy dirt of heating treatment method to absorption with heat endurance, and has guaranteed its reusable possibility; Oil-retaining after higher mechanical strength has guaranteed the feasibility of Carbon foam practical application and increased its oil suction; And macroporous structure helps adsorbing as high viscosity greasy dirts such as oil, mink cell focuses.But Carbon foam is not still reported so far as the research that oil absorption material is applied to seawater greasy dirt improvement aspect.This may be owing to due to the following reason: 1, Carbon foam mainly is that presoma is synthetic by foaming with the mesophase pitch at present.Though resulting Carbon foam has the excellent specific property of himself, raw material mesophase pitch cost is higher relatively, needs HTHP when synthetic simultaneously, therefore is difficult to the large batch of seawater greasy dirt improvement aspect that is applied to.2, resulting Carbon foam percent opening is lower, and the aperture is less, is unfavorable for the absorption and the desorption of high viscosity greasy dirt.Though 3, what is more important raw material of wood-charcoal material itself has certain hydrophobicity, contact angle is less, therefore is difficult to reach oil-water separation efficiently.By changing the Carbon foam surface wettability, make it become the super-hydrophobicity material at Carbon foam superficial growth carbon nano-fiber.Yet, though the report of Carbon foam superficial growth carbon nano-fiber (Fuel, 2009.88 (1): 46-53 of common occurrence; Journal of Materials Chemistry, 2008.18 (21): 2426-2436), but its super-hydrophobicity and water-oil separating performance were not also carried out deep research.In addition, because mostly being greatly on synthetic Carbon foam surface by concentrated acid oxidation and metal salt solution impregnating technology, existing technology carries out the CNT required catalyst loading of growing, the time-consuming tediously long and product quality of this process is difficult to guarantee that the use of concentrated acid simultaneously will increase cost and bring environmental problem.Therefore, we propose a kind of simple and can realize large-scale production Carbon foam loaded with nano carbon fiber preparation and absorption greasy dirt method.
Summary of the invention
In order to overcome above-mentioned problems of the prior art, the invention provides a kind of preparation of Carbon foam loaded with nano carbon fiber and the application process of absorption greasy dirt.This method technology is simple, with low cost, Carbon foam area load carbon nano-fiber composite material surface has super-hydrophobicity, the greasy dirt adsorption rate fast, sorbing material is easy to reclaim.
The technical solution used in the present invention is: a kind of preparation method of Carbon foam loaded with nano carbon fiber is as follows:
(1) be 0.1-4 in nickel element and polyamic acid solid content ratio: 100 ratio takes by weighing nickel salt, nickel salt is dissolved in the dimethylacetamide solution of polyamic acid, form the dimethylacetamide solution of nickel salt and polyamic acid, to in above-mentioned solution, flood 2-5min as the high polymer foam of template, take out the template foam after flooding, the dimethylacetamide solution that squeezes out excessive nickel salt and polyamic acid obtains the compound foam, compound foam after the extruding is put into insulating box, solidify at 60 ℃ of down dry 5-10h, compound foam after solidifying is placed quartz boat, in tube type resistance furnace with 1-10 ℃/min temperature programming to 700-1500 ℃, 0.5-10h is handled in charing, obtains carrying a nickel foam charcoal after being cooled to room temperature;
The nickel foam charcoal that carries that (2) will obtain prepares Carbon foam loaded with nano carbon fiber through chemical vapour deposition technique, and process is as follows: will carry the nickel foam charcoal and place the tube furnace flat-temperature zone, and under inert gas shielding, be warming up to 500-600 ℃, switching gas is N
2/ H
2Gaseous mixture, sample reduction 30-60min, 1-100 ℃/min temperature programming is to 700-900 ℃ under this atmosphere, and mist switches to H
2/ N
2/ C
2H
4, after question response carried out 3-60min, gas switched to inert gas, is cooled to room temperature, made Carbon foam loaded with nano carbon fiber.
The aperture of described year nickel foam charcoal is the 80-1200 micron, and carbon nano-fiber length is the 0.5-700 micron.
Polyamic acid solid content in the dimethylacetamide solution of described polyamic acid is 5-15%.
Described nickel salt is selected from nickel nitrate, nickel chloride, nickelous sulfate.
Described template foam is selected from polyurethane foam, melamine foamed plastic or phenolic resin foam.
0.01-5000g is had integrally-built Carbon foam area load carbon nano-fiber composite put into the waste water that contains greasy dirt as sorbing material, in temperature be-10-105 ℃, pressure is to adsorb under the 50-8000KPa condition, adsorption time is 1-900 second, and the water-oil separating degree is 70%-100%.
The mixture that consists of aromatic hydrocarbons, aliphatic hydrocarbon or aromatic hydrocarbons and aliphatic hydrocarbon of described greasy dirt.
The salt content of described waste water is 0-100000ppm.
The present invention compared with prior art has following advantage:
(1) the present invention can regulate pore structure, percent opening and density and the complete Carbon foam surface that is covered in of carbon nano-fiber of foams integral composite easily.
(2) Carbon foam loaded with nano carbon fiber has excellent oil and water separation capability.
(3) preparation process is simple, less demanding to equipment, and parameter is controlled easily, processing ease, is easy to amplify.
The specific embodiment
The invention will be further described below by embodiment.
Embodiment one
In nickel element and polyamic acid solid content ratio is that 4: 100 ratio takes by weighing nickel salt, nickel salt is dissolved in the dimethylacetamide solution of polyamic acid, form the dimethylacetamide solution of nickel salt and polyamic acid, to in above-mentioned solution, flood 2-5min as polyamine fat, take out the template foam after flooding, the dimethylacetamide solution that squeezes out excessive nickel nitrate and polyamic acid obtains the compound foam, compound foam after the extruding is put into insulating box, solidify at 60 ℃ of down dry 5-10h, compound foam after solidifying is placed quartz boat, in tube type resistance furnace with 1-10 ℃/min temperature programming to 700 ℃, 1h is handled in charing, obtains carrying a nickel foam charcoal after being cooled to room temperature;
The nickel foam charcoal that carries that obtains is prepared Carbon foam loaded with nano carbon fiber through chemical vapour deposition technique, and process is as follows: will carry the nickel foam charcoal and place the tube furnace flat-temperature zone, and under inert gas shielding, be warming up to 500 ℃, switching gas is N
2/ H
2Gaseous mixture, sample reduction 30min, 10 ℃/min temperature programming to 800 ℃ under this atmosphere, mist switches to H
2/ N
2/ C
2H
4, after question response carried out 30min, gas switched to inert gas, is cooled to room temperature, made Carbon foam loaded with nano carbon fiber.
1g is had integrally-built Carbon foam area load carbon nano-fiber composite put into the waste water (salt content 50ppm) that contains gasoline as sorbing material, in temperature is 20 ℃, pressure is to adsorb under the 100KPa condition, and adsorption time is 1 second, and the water-oil separating degree is 100%.
Embodiment two
In nickel element and polyamic acid solid content ratio is that 0.5: 100 ratio takes by weighing nickel chloride, nickel chloride is dissolved in the dimethylacetamide solution of polyamic acid, form the dimethylacetamide solution of nickel chloride and polyamic acid, to in above-mentioned solution, flood 5min as phenol formaldehyde foam, take out the template foam after flooding, the dimethylacetamide solution that squeezes out excess chlorination nickel and polyamic acid obtains the compound foam, compound foam after the extruding is put into insulating box, solidify at 60 ℃ of down dry 5h, compound foam after solidifying is placed quartz boat, in tube type resistance furnace with 10 ℃/min temperature programming to 1200 ℃, 1h is handled in charing, obtains carrying a nickel foam charcoal after being cooled to room temperature;
The nickel foam charcoal that carries that obtains is prepared Carbon foam loaded with nano carbon fiber through chemical vapour deposition technique, and process is as follows: will carry the nickel foam charcoal and place the tube furnace flat-temperature zone, and under inert gas shielding, be warming up to 600 ℃, switching gas is N
2/ H
2Gaseous mixture, sample reduction 30min, 10 ℃/min temperature programming to 700 ℃ under this atmosphere, mist switches to H
2/ N
2/ C
2H
4, after question response carried out 60min, gas switched to inert gas, is cooled to room temperature, made Carbon foam loaded with nano carbon fiber.
10g is had integrally-built Carbon foam area load carbon nano-fiber composite put into the waste water (salt content 0ppm) that contains light oil as sorbing material, in temperature is 5 ℃, pressure is to adsorb under the 1000KPa condition, and adsorption time is 5 seconds, and the water-oil separating degree is 100%.
Embodiment three
In nickel element and polyamic acid solid content ratio is that 1: 100 ratio takes by weighing nickel nitrate, nickel nitrate is dissolved in the dimethylacetamide solution of polyamic acid, form the dimethylacetamide solution of nickel nitrate and polyamic acid, to in above-mentioned solution, flood 5min as melamine foamed plastic, take out the template foam after flooding, the dimethylacetamide solution that squeezes out excessive nickel nitrate and polyamic acid obtains the compound foam, compound foam after the extruding is put into insulating box, solidify at 60 ℃ of down dry 10h, compound foam after solidifying is placed quartz boat, in tube type resistance furnace with 10 ℃/min temperature programming to 900 ℃, 1h is handled in charing, obtains carrying a nickel foam charcoal after being cooled to room temperature;
The nickel foam charcoal that carries that obtains is prepared Carbon foam loaded with nano carbon fiber through chemical vapour deposition technique, and process is as follows: will carry the nickel foam charcoal and place the tube furnace flat-temperature zone, and under inert gas shielding, be warming up to 600 ℃, switching gas is N
2/ H
2Gaseous mixture, sample reduction 60min, 10 ℃/min temperature programming to 800 ℃ under this atmosphere, mist switches to H
2/ N
2/ C
2H
4, after question response carried out 60min, gas switched to inert gas, is cooled to room temperature, made Carbon foam loaded with nano carbon fiber.
10g is had integrally-built Carbon foam area load carbon nano-fiber composite put into the waste water (salt content 1200ppm) that contains coal tar as sorbing material, in temperature is 80 ℃, pressure is to adsorb under the 1000KPa condition, and adsorption time is 120 seconds, and the water-oil separating degree is 97%.
Embodiment four
In nickel element and polyamic acid solid content ratio is that 4: 100 ratio takes by weighing nickel nitrate, nickel nitrate is dissolved in the dimethylacetamide solution of polyamic acid, form the dimethylacetamide solution of nickel nitrate and polyamic acid, to in above-mentioned solution, flood 5min as polyamine fat vacuole foam, take out the template foam after flooding, the dimethylacetamide solution that squeezes out excessive nickel nitrate and polyamic acid obtains the compound foam, compound foam after the extruding is put into insulating box, solidify at 60 ℃ of down dry 8h, compound foam after solidifying is placed quartz boat, in tube type resistance furnace with 10 ℃/min temperature programming to 900 ℃, 1h is handled in charing, obtains carrying a nickel foam charcoal after being cooled to room temperature;
The nickel foam charcoal that carries that obtains is prepared Carbon foam loaded with nano carbon fiber through chemical vapour deposition technique, and process is as follows: will carry the nickel foam charcoal and place the tube furnace flat-temperature zone, and under inert gas shielding, be warming up to 600 ℃, switching gas is N
2/ H
2Gaseous mixture, sample reduction 60min, 100 ℃/min temperature programming to 900 ℃ under this atmosphere, mist switches to H
2/ N
2/ C
2H
4, after question response carried out 10min, gas switched to inert gas, is cooled to room temperature, made Carbon foam loaded with nano carbon fiber.10g is had integrally-built Carbon foam area load carbon nano-fiber composite put into the waste water (salt content 1200ppm) that contains mink cell focus as sorbing material, in temperature is 80 ℃, pressure is to adsorb under the 80KPa condition, and adsorption time is 500 seconds, and the water-oil separating degree is 98%.
Claims (8)
1. the preparation method of a Carbon foam loaded with nano carbon fiber is characterized in that:
(1) be 0.1-4 in nickel element and polyamic acid solid content ratio: 100 ratio takes by weighing nickel salt, nickel salt is dissolved in the dimethylacetamide solution of polyamic acid, form the dimethylacetamide solution of nickel salt and polyamic acid, to in above-mentioned solution, flood 2-5min as the high polymer foam of template, take out the template foam after flooding, the dimethylacetamide solution that squeezes out excessive nickel salt and polyamic acid obtains the compound foam, compound foam after the extruding is put into insulating box, solidify at 60 ℃ of down dry 5-10h, compound foam after solidifying is placed quartz boat, in tube type resistance furnace with 1-10 ℃/min temperature programming to 700-1500 ℃, 0.5-10h is handled in charing, obtains carrying a nickel foam charcoal after being cooled to room temperature;
The nickel foam charcoal that carries that (2) will obtain prepares Carbon foam loaded with nano carbon fiber through chemical vapour deposition technique, and process is as follows: will carry the nickel foam charcoal and place the tube furnace flat-temperature zone, and under inert gas shielding, be warming up to 500-600 ℃, switching gas is N
2/ H
2Gaseous mixture, sample reduction 30-60min, 1-100 ℃/min temperature programming is to 700-900 ℃ under this atmosphere, and mist switches to H
2/ N
2/ C
2H
4, after question response carried out 3-60min, gas switched to inert gas, is cooled to room temperature, made Carbon foam loaded with nano carbon fiber.
2. the preparation method of a kind of Carbon foam loaded with nano carbon fiber according to claim 1 is characterized in that: the aperture of described year nickel foam charcoal is the 80-1200 micron, and carbon nano-fiber length is the 0.5-700 micron.
3. the preparation method of a kind of Carbon foam loaded with nano carbon fiber according to claim 1 is characterized in that: the polyamic acid solid content in the dimethylacetamide solution of described polyamic acid is 5-15%.
4. the preparation method of a kind of Carbon foam loaded with nano carbon fiber according to claim 1 is characterized in that: described nickel salt is selected from nickel nitrate, nickel chloride, nickelous sulfate.
5. the preparation method of a kind of Carbon foam loaded with nano carbon fiber according to claim 1 is characterized in that: described template foam is selected from polyurethane foam, melamine foamed plastic or phenolic resin foam.
6. the application process of a kind of Carbon foam loaded with nano carbon fiber absorption greasy dirt according to claim 1, it is characterized in that: 0.01-5000g is had integrally-built Carbon foam area load carbon nano-fiber composite put into the waste water that contains greasy dirt as sorbing material, in temperature be-10-105 ℃, pressure is to adsorb under the 50-8000KPa condition, adsorption time is 1-900 second, and the water-oil separating degree is 70%-100%.
7. the application process of a kind of Carbon foam loaded with nano carbon fiber absorption greasy dirt according to claim 6 is characterized in that: the mixture that consists of aromatic hydrocarbons, aliphatic hydrocarbon or aromatic hydrocarbons and aliphatic hydrocarbon of described greasy dirt.
8. the application process of a kind of Carbon foam loaded with nano carbon fiber absorption greasy dirt according to claim 6, it is characterized in that: the salt content of described waste water is 0-100000ppm.
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| CN105499595A (en) * | 2014-09-25 | 2016-04-20 | 江苏格业新材料科技有限公司 | Preparing method of foamed silver material carrying nano silver |
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Application publication date: 20111019 |