CN110548397B - Novel composite carbon reduction-oxidation nanotube forward osmosis membrane and preparation method thereof - Google Patents
Novel composite carbon reduction-oxidation nanotube forward osmosis membrane and preparation method thereof Download PDFInfo
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- CN110548397B CN110548397B CN201810564879.0A CN201810564879A CN110548397B CN 110548397 B CN110548397 B CN 110548397B CN 201810564879 A CN201810564879 A CN 201810564879A CN 110548397 B CN110548397 B CN 110548397B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/002—Forward osmosis or direct osmosis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/021—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/08—Polysaccharides
Abstract
The invention discloses a novel composite reduced carbon nanotube forward osmosis membrane and a preparation method thereof. The preparation method comprises the following steps: preparing the carbon oxide nanotube by adopting a modified Hummers method, reacting an aqueous solution of the carbon oxide nanotube with a reducing agent at 25-70 ℃ for 0.2-2 h, then adjusting the pH value of a reaction solution to be alkaline, and reacting at 40-80 ℃ for 0.5-3 h to obtain a reduced carbon oxide nanotube; and carrying out plasticizing reaction on the uniformly mixed reaction system containing the reduced-oxidized carbon nano tube, the plasticizer and the water at 70-100 ℃ to obtain the novel composite reduced-oxidized carbon nano tube forward osmosis membrane. The invention takes the carbon nanotube and the carbon nanotube as additives, can effectively improve the flux of the forward osmosis membrane, and simultaneously takes the natural polysaccharide as a plasticizer to be compounded with the carbon nanotube and the carbon nanotube to form a membrane, thereby having no toxicity, no harm, no pollution, higher mechanical strength and higher stability.
Description
Technical Field
The invention relates to a forward osmosis membrane, in particular to a novel composite reduction-oxidation carbon nanotube forward osmosis membrane and a preparation method thereof, and belongs to the technical field of forward osmosis water treatment membranes.
Background
Water is the source of life and is the most critical link in the global ecosystem. However, one of the most common problems that now afflicts global human development is the shortage of clean water and infrastructure. The water in China has two main problems: namely, water resource shortage and serious water pollution. Compared with the pressure driving process, the forward osmosis membrane separation process does not need to be operated under a high pressure condition, and only needs smaller pressure to maintain the flow of the solution at two sides of the membrane, so that the process has the potential advantages of low energy consumption, low pollution tendency, easy cleaning, high water recovery rate and the like. Forward osmosis is not only used in the fields of seawater desalination and wastewater treatment, but also in the processes of food industry, agriculture, controlled drug release, drug concentration and the like.
In the last decade, both the application of membrane processes and membrane preparation have developed rapidly, but the lack of high performance forward osmosis membranes remains one of the key issues to be solved in forward osmosis development. The traditional cellulose acetate membrane has thicker compact cortex, small permeability coefficient, inferior flux and inferior membrane stability in the aspects of membrane chemical property and the like, so that the research and development of high efficiency and high performance are the problems which are continuously solved at present.
The carbon nano tube is used as a one-dimensional nano material, has light weight, perfect connection of a hexagonal structure and a plurality of abnormal mechanical, electrical and chemical properties. In recent years, the extensive application prospect of the carbon nano-tube and the nano-material is continuously shown along with the research of the carbon nano-tube and the nano-material. In addition, the carbon nano tube also shows excellent water mass transfer characteristics, so the carbon nano tube has wide application prospect in the separation field.
Disclosure of Invention
The invention aims to provide a novel composite reduced carbon nanotube forward osmosis membrane and a preparation method thereof, so as to overcome the defects in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following steps:
the embodiment of the invention provides a preparation method of a novel composite reduced carbon nanotube forward osmosis membrane, which comprises the following steps:
providing reduced-oxidized carbon nanotubes;
and plasticizing the uniformly mixed reaction system containing the carbon nanotube, the plasticizer and the water at 70-100 ℃ for 0.5-8 h to obtain the novel composite carbon nanotube forward osmosis membrane.
In some preferred embodiments of the present invention, the preparation method comprises:
providing an aqueous solution of oxidized carbon nanotubes;
and (3) reacting the oxidized carbon nanotube aqueous solution with a reducing agent at 25-70 ℃ for 0.2-2 h, then adjusting the pH value of the reaction solution to be alkaline, and then heating and reacting at 40-80 ℃ for 0.5-3 h to obtain the reduced oxidized carbon nanotube.
The embodiment of the invention also provides the novel composite reduced carbon nanotube forward osmosis membrane prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
1) according to the preparation method of the novel composite reduction-oxidation carbon nanotube forward osmosis membrane, the carbon nanotubes are subjected to functional modification to prepare the carbon nanotubes, so that the defects of poor dispersibility in water and high possibility of agglomeration are effectively overcome;
2) the carbon nano tube in the novel composite carbon nanotube reduced and oxidized forward osmosis membrane provided by the invention has better water mass transfer characteristic, and the carbon nanotube reduced and oxidized and the carbon nano tube are taken as additives, so that the composite forward osmosis membrane can be endowed with better flux by the characteristic, and the flux of the forward osmosis membrane can be effectively improved;
3) the natural polysaccharide is used as a plasticizer, is compounded with the carbon nano tube and the reduction-oxidation carbon nano tube to form a film, is used as a film matrix material, is a natural, non-toxic and selectively-modified high polymer material, and is an ideal winding main body molecule. According to the invention, through a composite film forming process, the carbon nano tube and the reduced-oxidized carbon nano tube can form interaction with polysaccharide, and the polysaccharide can be wound on the surface of the carbon nano tube through a non-covalent effect, so that the novel nano composite forward osmosis membrane is prepared, and the composite membrane has high mechanical strength and stability and has wide application prospect.
Detailed Description
In view of the problem of low flux of the conventional forward osmosis membrane in the prior art, the inventors of the present invention have made extensive studies and extensive practices to provide the technical solution of the present invention. The technical solution, its implementation and principles, etc. will be further explained as follows.
As one aspect of the technical solution of the present invention, a method for preparing a novel composite reduced carbon nanotube forward osmosis membrane includes:
providing reduced-oxidized carbon nanotubes;
and plasticizing the uniformly mixed reaction system containing the carbon nanotube, the plasticizer and the water at 70-100 ℃ for 0.5-8 h to obtain the novel composite carbon nanotube forward osmosis membrane.
In some preferred embodiments of the present invention, the preparation method comprises:
providing an aqueous solution of oxidized carbon nanotubes;
and (3) reacting the oxidized carbon nanotube aqueous solution with a reducing agent at 25-70 ℃ for 0.2-2 h, then adjusting the pH value of the reaction solution to be alkaline, and then heating and reacting at 40-80 ℃ for 0.5-3 h to obtain the reduced oxidized carbon nanotube.
In some preferred embodiments of the present invention, the preparation method may specifically include:
adding the carbon oxide nanotube aqueous solution with a certain concentration into a three-necked flask, adding a reducing agent, stirring for a period of time, adding concentrated ammonia water to adjust the pH, and placing in a water bath for heating reaction to obtain the reduced carbon oxide nanotube. And then adding the carbon nano tube and the reduction-oxidation carbon nano tube in a certain proportion into water, adding a shaping agent, uniformly stirring, heating for shaping, and drying in a vacuum oven to obtain the novel composite reduction-oxidation carbon nano tube forward osmosis membrane.
In some embodiments, the concentration of the oxidized carbon nanotube aqueous solution is 0.1-2 mg/mL.
Furthermore, the concentration of the reducing agent in the reaction liquid is 5-50 g/L.
Further, the reducing agent includes any one or a combination of two or more of glucose, ascorbic acid, hydrazine hydrate, sodium borohydride, p-diphenol, and the like, but is not limited thereto.
Further, the preparation method comprises the following steps: and adjusting the pH value of the reaction solution to 9-13 by adopting concentrated ammonia water.
In some embodiments, the carbon nanotubes are prepared using a modified Hummers method.
Further, the preparation method comprises the following steps: and cleaning and centrifuging the oxidized carbon nanotube obtained by the modified Hummers method, and drying at 40-80 ℃ for 2-6 h.
The invention prepares the carbon oxide nanotube by functionally modifying the carbon nanotube, thereby effectively improving the defects of poor dispersibility in water and easy agglomeration.
In some embodiments, the mass ratio of carbon nanotubes to reduced-oxidized carbon nanotubes is 1: 5-5: 1.
further, the content of the carbon nano tube and the reduced carbon nano tube in the uniformly mixed reaction system is 1-10 wt%.
Further, the shaping agent includes any one or a combination of two or more of corn starch, potato starch, wheat flour, tapioca starch, and the like, but is not limited thereto.
Further, the concentration of the plasticizer in the uniformly mixed reaction system is 20-150 g/L.
In some preferred embodiments of the present invention, the preparation method further comprises: and after the plasticizing reaction is finished, drying the obtained solid at 30-60 ℃ for 5-10 h to obtain the novel composite reduction-oxidation carbon nano tube forward osmosis membrane.
Wherein, as a more specific embodiment, the preparation method may comprise the steps of:
step 1) preparing the carbon oxide nanotube by adopting a modified Hummers method, centrifuging the obtained carbon oxide nanotube by using deionized water, and drying a final product at 60 ℃ for 6 hours;
step 2) adding an aqueous solution of the carbon dioxide nanotube with a certain concentration into a three-necked flask, adding a certain amount of reducing agent, reacting for 0.2-2 h, adding concentrated ammonia water to adjust the pH value, then placing the reaction solution into a water bath, heating and reacting for 0.5-3 h, filtering after the reaction is finished, repeatedly cleaning for 10 times by using deionized water, and drying to obtain a reduced carbon dioxide nanotube;
and 3) adding a certain proportion of carbon nano tubes and reduced-oxidized carbon nano tubes into water, adding a plasticizer, uniformly stirring, heating to 70-100 ℃ for plasticizing, and then putting the plasticized carbon nano tubes into a vacuum oven to dry for 5-10 hours at 30-60 ℃ to obtain the novel composite reduced-oxidized carbon nano tube forward osmosis membrane.
As another aspect of the technical scheme of the invention, the invention also relates to a novel composite reduced carbon nanotube forward osmosis membrane prepared by the method.
Preferably, the thickness of the novel composite carbon nanotube forward osmosis membrane is 10-50 μm.
Preferably, the contact angle between the surface of the novel composite reduced carbon nanotube forward osmosis membrane and water is 39-55 degrees.
Preferably, when 2mol/L sodium chloride solution is used as an extraction solution, the pure water flux of the novel composite reduced carbon nanotube forward osmosis membrane is 25.8-36.2 L.m-2·h-1。
By the preparation process, the reduced-oxidized carbon nano tube and the carbon nano tube are used as additives, the flux of the forward osmosis membrane can be effectively improved, natural polysaccharide is used as a plasticizer to be compounded with the carbon nano tube and the reduced-oxidized carbon nano tube to form a membrane, the membrane is non-toxic, harmless and pollution-free, and the carbon nano tube and the reduced-oxidized carbon nano tube can form interaction with the polysaccharide, so that the membrane has high mechanical strength and stability and wide application prospect.
The technical solution of the present invention is explained in more detail below with reference to several preferred embodiments. However, the examples are chosen only for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention. In the examples, the apparatus and methods used are those conventional in the art, unless otherwise specified.
Example 1
Adding a certain 100mL of carbon oxide nanotube aqueous solution with the concentration of 2mg/mL into a three-necked bottle, adding 0.5g of glucose, reacting for 0.5h at 30 ℃, adding concentrated ammonia water to adjust the pH value to 9, then placing the reaction solution into a water bath, heating and reacting for 0.8h at 50 ℃, filtering after the reaction is finished, repeatedly washing for 10 times by deionized water, and drying for 3h at 50 ℃ to obtain the reduced carbon oxide nanotube. The ratio of 4g is 1: 3, adding the carbon nano tube and the reduced carbon nano tube into 100mL of water, adding 3g of corn starch, uniformly stirring, heating to 70 ℃ for shaping for 2h, and then putting the molded product into a vacuum oven for drying for 6h at 40 ℃ to obtain the novel composite reduced carbon nano tube forward osmosis membrane.
Through tests, the contact angle between the forward osmosis membrane prepared in the embodiment and water is 48 degrees, and 2mol/L sodium chloride solution is used as a drawTaking the solution, wherein the pure water flux is 32.1Lm-2h-1。
Example 2
Adding a certain 100mL of carbon oxide nanotube aqueous solution with the concentration of 0.1mg/mL into a three-necked bottle, adding 1g of ascorbic acid, reacting for 0.2h at 40 ℃, adding concentrated ammonia water to adjust the pH value to 11.5, then placing the reaction solution into a water bath, heating and reacting for 1h at 60 ℃, filtering after the reaction is finished, repeatedly washing for 10 times by deionized water, and drying for 3h at 60 ℃ to obtain the reduced carbon oxide nanotube. Mixing 6g of the mixture in a ratio of 1: and 5, adding the carbon nano tube and the reduced carbon nano tube into 100mL of water, adding 6g of corn starch, uniformly stirring, heating to 80 ℃ for shaping for 3h, and then putting the molded product into a vacuum oven for drying for 8h at 45 ℃ to obtain the novel composite reduced carbon nano tube forward osmosis membrane.
Through tests, the contact angle between the forward osmosis membrane prepared in the embodiment and water is 52 degrees, 2mol/L sodium chloride solution is used as an absorption liquid, and the pure water flux is 29.7Lm-2h-1。
Example 3
Adding a certain 100mL of carbon oxide nanotube aqueous solution with the concentration of 0.5mg/mL into a three-necked bottle, adding 2g of hydrazine hydrate, reacting for 1h at 50 ℃, adding concentrated ammonia water to adjust the pH value to 10, then placing the reaction solution into a water bath, heating and reacting for 0.5h at 50 ℃, filtering after the reaction is finished, repeatedly washing for 10 times by using deionized water, and drying for 5h at 80 ℃ to obtain the reduced carbon oxide nanotube. The ratio of 2g is 2: adding the carbon nanotube and the reduced-oxidized carbon nanotube of 1 into 100mL of water, adding 2g of corn starch, stirring uniformly, heating to 90 ℃ for shaping for 8h, and then putting the molded product into a vacuum oven for drying for 7 h at 60 ℃ to obtain the novel composite reduced-oxidized carbon nanotube forward osmosis membrane.
Through tests, the contact angle between the forward osmosis membrane prepared in the embodiment and water is 43 degrees, 2mol/L sodium chloride solution is used as an absorption liquid, and the pure water flux is 36.2Lm-2h-1。
Example 4
Adding 100mL of carbon oxide nanotube aqueous solution with the concentration of 1mg/mL into a three-necked bottle, adding 3g of sodium borohydride, reacting for 1.5h at 70 ℃, adding concentrated ammonia water to adjust the pH value to 12, then placing the reaction solution in a water bath, heating and reacting for 2.5h at 80 ℃, filtering after the reaction is finished, repeatedly washing for 10 times by deionized water, and drying for 2h at 70 ℃ to obtain the reduced carbon oxide nanotube. Mixing 5g of the mixture in a ratio of 1: adding the carbon nano tube and the reduced carbon nano tube of 1 into 100mL of water, adding 8g of corn starch, stirring uniformly, heating to 85 ℃ for shaping for 4h, and then putting the molded product into a vacuum oven for drying for 5h at 50 ℃ to obtain the novel composite reduced carbon nano tube forward osmosis membrane.
Through tests, the contact angle between the forward osmosis membrane prepared in the embodiment and water is 55 degrees, 2mol/L sodium chloride solution is used as an absorption liquid, and the pure water flux is 25.8Lm-2h-1。
Example 5
Adding 100mL of carbon oxide nanotube aqueous solution with the concentration of 1.5mg/mL into a three-necked bottle, adding 4g of p-diphenol, reacting for 2h at 60 ℃, adding concentrated ammonia water to adjust the pH value to 11, then placing the reaction solution into a water bath, heating at 70 ℃ for reacting for 2h, filtering after the reaction is finished, repeatedly washing for 10 times by using deionized water, and drying for 2.5h at 40 ℃ to obtain the reduced carbon oxide nanotube. The ratio of 10g is 5: 1, adding the carbon nano tube and the reduced carbon nano tube into 100mL of water, adding 15g of corn starch, uniformly stirring, heating to 75 ℃ for shaping for 0.5h, and then putting the molded product into a vacuum oven for drying for 10 hours at 55 ℃ to obtain the novel composite reduced carbon nano tube forward osmosis membrane.
Through tests, the contact angle between the forward osmosis membrane prepared in the embodiment and water is 44 degrees, 2mol/L sodium chloride solution is used as an absorption liquid, and the pure water flux is 30.5Lm-2h-1。
Example 6
Adding 100mL of oxidized carbon nanotube aqueous solution with the concentration of 2mg/mL into a three-necked flask, adding 5g of glucose, reacting for 0.8h at 25 ℃, adding concentrated ammonia water to adjust the pH value to 13, then placing the reaction solution in a water bath, heating and reacting for 3h at 40 ℃, filtering after the reaction is finished, repeatedly washing for 10 times by deionized water, and drying for 4.5h at 55 ℃ to obtain the reduced oxidized carbon nanotube. 1g is mixed into a mixture with the weight ratio of 1: 4, adding the carbon nano tube and the reduced carbon nano tube into 100mL of water, adding 10g of corn starch, uniformly stirring, heating to 100 ℃ for shaping for 1h, and then putting the molded product into a vacuum oven for drying for 7 hours at 30 ℃ to obtain the novel composite reduced carbon nano tube forward osmosis membrane.
Through tests, the contact angle between the forward osmosis membrane prepared in the embodiment and water is 39 degrees, 2mol/L sodium chloride solution is used as an absorption liquid, and the pure water flux is 35.3Lm-2h-1。
Comparative example 1: this comparative example is substantially the same as example 1 except that: reduced carbon oxide nanotubes were not added. The contact angle between the forward osmosis membrane obtained in this comparative example and water was 78 °, and the pure water flux was 8.6L · m when a 2mol/L sodium chloride solution was used as an extraction solution-2·h-1。
In addition, the inventors have also conducted experiments with other raw materials and conditions, etc. listed in the present specification, in the manner of examples 1 to 6, and also produced a novel composite reduced carbon nanotube forward osmosis membrane having a large flux, high mechanical strength and stability.
It should be understood that the above is only a specific application example of the present invention, and the protection scope of the present invention is not limited in any way. All the technical solutions formed by equivalent transformation or equivalent replacement fall within the protection scope of the present invention.
Claims (8)
1. A preparation method of a novel composite carbon nanotube forward osmosis membrane for reduction and oxidation is characterized by comprising the following steps:
providing an aqueous solution of oxidized carbon nanotubes;
reacting the oxidized carbon nanotube aqueous solution with a reducing agent at 25-70 ℃ for 0.2-2 h, then adjusting the pH value of the reaction solution to 9-13, and heating at 40-80 ℃ for reaction for 0.5-3 h to obtain a reduced oxidized carbon nanotube;
plasticizing a uniformly mixed reaction system containing the carbon nanotube, a plasticizer and water at 70-100 ℃ for 0.5-8 h to obtain a novel composite carbon nanotube forward osmosis membrane; wherein the mass ratio of the carbon nano tube to the reduced-oxidized carbon nano tube is 1: 5-5: 1, the content of carbon nanotubes and reduced-oxidized carbon nanotubes in the uniformly mixed reaction system is 1-10 wt%, the shaping agent is selected from any one or a combination of more than two of corn starch, potato starch, wheat flour and tapioca starch, and the concentration of the shaping agent in the uniformly mixed reaction system is 20-150 g/L;
in the composite film forming process of the novel composite carbon nanotube forward osmosis membrane, the carbon nanotube forward osmosis membrane and the shaping agent can form interaction, and the shaping agent is wound on the surface of the carbon nanotube through non-covalent interaction;
the thickness of the novel composite carbon nanotube forward osmosis membrane is 10-50 μm; the contact angle between the surface of the novel composite reduced-oxidized carbon nanotube forward osmosis membrane and water is 39-55 degrees.
2. The method of claim 1, wherein: the concentration of the oxidized carbon nanotube aqueous solution is 0.1-2 mg/mL.
3. The method of claim 1, wherein: the concentration of the reducing agent in the reaction liquid is 5-50 g/L.
4. The method of claim 1, wherein: the reducing agent is selected from any one or combination of more than two of glucose, ascorbic acid, hydrazine hydrate, sodium borohydride and p-diphenol.
5. The method of manufacturing according to claim 1, comprising: and adjusting the pH value of the reaction solution by adopting concentrated ammonia water.
6. The method of claim 1, wherein: the carbon oxide nanotube is prepared by adopting a modified Hummers method.
7. The method of manufacturing according to claim 6, comprising: and cleaning and centrifuging the oxidized carbon nanotube obtained by the modified Hummers method, and drying at 40-80 ℃ for 2-6 h.
8. The production method according to any one of claims 1 to 7, characterized by further comprising: and after the plasticizing reaction is finished, drying the obtained solid at 30-60 ℃ for 5-10 h to obtain the novel composite reduction-oxidation carbon nano tube forward osmosis membrane.
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