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CN114436676A - Production method of carbon nano tube composite porous ceramic capable of adsorbing toxic substances - Google Patents

Production method of carbon nano tube composite porous ceramic capable of adsorbing toxic substances Download PDF

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CN114436676A
CN114436676A CN202210111821.7A CN202210111821A CN114436676A CN 114436676 A CN114436676 A CN 114436676A CN 202210111821 A CN202210111821 A CN 202210111821A CN 114436676 A CN114436676 A CN 114436676A
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porous ceramic
carbon nano
nano tube
toxic substances
stirring
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李蕾蕾
吴功松
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Shenzhen Zhongke Nanotechnology Co ltd
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Abstract

The invention provides a production method of carbon nano tube composite porous ceramic capable of adsorbing toxic substances, which relates to the technical field of adsorbing materials and comprises the following steps: s1: preparing proper amount of polyvinyl alcohol, acrylic acid, carbon nano tube, cross-linking agent, initiator, yttrium chloride catalyst, surfactant and porous ceramic according to the proportion. According to the invention, the carbon nano tube is mixed with polyvinyl alcohol, a cross-linking agent, acrylic acid and an initiator are added for reaction, and porous ceramic, a yttrium chloride catalyst and a surfactant are added, so that the carbon nano tube can be fully compounded with the porous ceramic, and a finished product composite porous ceramic material is obtained, and the carbon nano tube can be attached to the hole of the porous ceramic, so that the contact area of the carbon nano tube and a toxic substance is effectively increased, and the whole finished product composite porous ceramic material can quickly adsorb the toxic substance and simultaneously can maintain the adsorption effect for a long time, so that a better adsorption effect is achieved.

Description

Production method of carbon nano tube composite porous ceramic capable of adsorbing toxic substances
Technical Field
The invention relates to the technical field of adsorption materials, in particular to a production method of carbon nano tube composite porous ceramic capable of adsorbing toxic substances.
Background
In the daily decoration and the manufacturing process, often produce the noxious material, and in order to handle the noxious material, often can adopt chemical decomposition method or physical adsorption method to handle, and because the physical adsorption method has easy operation, advantages such as convenient to use, by extensive application in daily life and manufacturing, and current physical adsorption method often uses adsorption material such as active carbon to adsorb, but the active carbon often is less with the area of contact of harmful substance, often be difficult to reach comparatively effective quick adsorption effect, and use a period, the adsorption effect is discounted greatly easily, be difficult to reach better result of use.
Chinese patent No. CN102802764A discloses a cross-linked polymer-carbon adsorbent for removing heavy metals, toxic substances and carbon dioxide, which comprises a carbonaceous adsorbent material and a cured amine-containing polymer, and sulfur. The formation of the polymer-carbon sorbent by curing a curable amine-containing polymer in the presence of a carbonaceous sorbent material, a sulfur crosslinking agent, a cure accelerator, and optionally a cure activator, enables the removal of heavy metals and toxic pollutants from flue gas and the absorption of carbon dioxide, but is difficult to effectively adsorb toxic substances for extended periods of time, and improvements are needed.
Chinese patent No. CN109663564A discloses a gas adsorbing material and a preparation method thereof, wherein the gas adsorbing material is prepared from 90-260 parts by weight of graphene aqueous solution and 79-81 parts by weight of activated carbon, and the adsorption capacity of the activated carbon to toxic substances is enhanced by mixing the graphene aqueous solution with the activated carbon, but the adsorption capacity of the activated carbon to toxic substances is limited, and it is difficult to rapidly adsorb toxic substances, and improvement is required.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a production method of a carbon nano tube composite porous ceramic capable of adsorbing toxic substances.
In order to achieve the purpose, the invention adopts the following technical scheme: a method for producing carbon nano tube composite porous ceramic capable of adsorbing toxic substances comprises the following steps:
s1: preparing a proper amount of polyvinyl alcohol, acrylic acid, carbon nano tubes, a cross-linking agent, an initiator, a yttrium chloride catalyst, a surfactant and porous ceramic according to a proportion;
s2: pouring the carbon nano tube and polyvinyl alcohol into a reaction kettle together, and then adding the mixture in a mass ratio of 1: and (6-9) heating and stirring the deionized water at the stirring temperature of 55-70 ℃, the stirring speed of 150-220 rpm and the stirring time of 30-40 minutes to obtain an initial mixed solution.
S3: simultaneously dripping a cross-linking agent, acrylic acid and an initiator into the initial mixed solution obtained in S1, maintaining the stirring speed in S1 in the dripping process, continuously stirring for 10-15 minutes after finishing dripping, raising the temperature in the reaction kettle to 75-90 ℃, stirring at the stirring speed of 120-180 revolutions per minute for 3-4 hours, and thus obtaining a secondary mixed solution;
s4: carrying out ultrasonic oscillation on the secondary mixed solution for 60-90 seconds, standing for 5-8 minutes after oscillation, and repeating for 3-5 times to obtain a carbon source solution for later use;
s5: adding the porous ceramic into a carbon source solution, then adding a yttrium chloride catalyst and a surfactant, heating and stirring at the stirring temperature of 240-280 ℃, the stirring speed of 30-60 revolutions per minute and the stirring time of 30-40 minutes, and then standing at constant temperature for 2-3 hours to obtain the finished product of the composite porous ceramic material.
In order to produce the finished composite porous ceramic material, the improvement of the invention is that the composition mass fraction of each material in the S1 is as follows: 4-8% of polyethylene, 3-5% of acrylic acid, 16-21% of carbon nano tube, 1-2.5% of cross-linking agent, 1-2% of initiator, 1-2% of yttrium chloride catalyst, 0.5-1.5% of surfactant and 54-76% of porous ceramic.
In order to achieve a better adsorption effect, the invention has the improvement that the tube diameter of the carbon nano tube in the S1 is 20-60nm, and the length is 50-100 um.
In order to make the reaction normally proceed, the invention improves that the cross-linking agent in the S1 is N, N' -methylene bisacrylamide.
In order to have a larger contact area with toxic substances, the improvement of the invention is that the material of the porous ceramic in S1 is one of boron carbide ceramic, beryllium oxide ceramic, zirconium oxide ceramic, silicon carbide ceramic and alumina ceramic, the diameter of the porous ceramic is 1-2cm, the pore diameter is 200-400 mu m, and the through-hole rate is 60-80%.
In order to ensure that the reaction normally occurs, the improvement of the invention is that the initiator in S1 is one of potassium persulfate and ammonium persulfate.
In order to activate the surface of the porous ceramic, the improvement of the invention is that the surfactant in the S1 is one of dimethyl ethyl allyl ammonium chloride, methyl cellulose copolymer, polyvinyl alcohol, sodium petroleum sulfonate, lignosulfonate, sodium alkyl sulfate and polyvinyl amine.
In order to achieve different effects, the invention has the improvement that the mass fractions of the components of the materials are as follows: 6% of polyethylene, 4% of acrylic acid, 18% of carbon nano tube, 2.1% of cross-linking agent, 1.4% of initiator, 1.5% of yttrium chloride catalyst, 0.9% of surfactant and 66.1% of porous ceramic.
In order to achieve different effects, the invention has the improvement that the mass fractions of the components of the materials are as follows: 7% of polyethylene, 4% of acrylic acid, 19% of carbon nano tube, 1.8% of cross-linking agent, 1.6% of initiator, 1.5% of yttrium chloride catalyst, 0.9% of surfactant and 64.2% of porous ceramic.
In order to achieve different effects, the invention has the improvement that the mass fractions of the components of the materials are as follows: 8% of polyethylene, 5% of acrylic acid, 20% of carbon nano tube, 1.8% of cross-linking agent, 1.5% of initiator, 1.4% of yttrium chloride catalyst, 1.2% of surfactant and 61.1% of porous ceramic.
Compared with the prior art, the invention has the advantages and positive effects that,
according to the invention, the carbon nano tube is mixed with polyvinyl alcohol, and a cross-linking agent, acrylic acid and an initiator are added for reaction, the carbon nano tube is modified by an active group carried by the polyvinyl alcohol, so that the carbon nano tube can have a better adsorption effect on toxic substances, and the porous ceramic, the yttrium chloride catalyst and the surfactant are added, so that the carbon nano tube can be fully compounded with the porous ceramic, and a finished product of the composite porous ceramic material is obtained, and the carbon nano tube can be attached to holes of the porous ceramic, so that the contact area of the carbon nano tube and the toxic substances is effectively increased, and the adsorption effect can be maintained for a long time while the toxic substances are quickly adsorbed by the whole finished product of the composite porous ceramic material, so that a better adsorption effect is achieved.
Drawings
FIG. 1 is a flow chart of a method for producing a carbon nanotube composite porous ceramic capable of adsorbing toxic substances according to the present invention.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, the present invention will be further described with reference to the accompanying drawings and examples. It should be noted that the embodiments and features of the embodiments of the present application may be combined with each other without conflict.
In the description of the present invention, it is to be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, and are used merely for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, are not to be construed as limiting the present invention. Further, in the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1, the present invention provides a method for producing a carbon nanotube composite porous ceramic capable of adsorbing toxic substances, comprising the following steps:
s1: preparing a proper amount of polyvinyl alcohol, acrylic acid, carbon nano tubes, a cross-linking agent, an initiator, a yttrium chloride catalyst, a surfactant and porous ceramic according to a proportion;
s2: pouring the carbon nano tube and polyvinyl alcohol into a reaction kettle together, and then adding the mixture in a mass ratio of 1: and (6-9) heating and stirring the deionized water at the stirring temperature of 55-70 ℃, the stirring speed of 150-220 rpm and the stirring time of 30-40 minutes to obtain an initial mixed solution.
S3: simultaneously dripping a cross-linking agent, acrylic acid and an initiator into the initial mixed solution obtained in S1, maintaining the stirring speed in S1 in the dripping process, continuously stirring for 10-15 minutes after finishing dripping, raising the temperature in the reaction kettle to 75-90 ℃, stirring at the stirring speed of 120-180 revolutions per minute for 3-4 hours, and thus obtaining a secondary mixed solution;
s4: performing ultrasonic oscillation on the secondary mixed solution for 60-90 seconds, standing for 5-8 minutes after oscillation, and repeating for 3-5 times to obtain a carbon source solution for later use;
s5: adding the porous ceramic into a carbon source solution, then adding a yttrium chloride catalyst and a surfactant, heating and stirring at the stirring temperature of 240-280 ℃, the stirring speed of 30-60 revolutions per minute and the stirring time of 30-40 minutes, and then standing at constant temperature for 2-3 hours to obtain the finished product of the composite porous ceramic material.
The mass fractions of the components of S1 are as follows: 4-8% of polyethylene, 3-5% of acrylic acid, 16-21% of carbon nano tube, 1-2.5% of cross-linking agent, 1-2% of initiator, 1-2% of yttrium chloride catalyst, 0.5-1.5% of surfactant and 54-76% of porous ceramic, wherein the tube diameter of the carbon nano tube in S1 is 20-60nm, the length of the carbon nano tube is 50-100um, the carbon nano tube can have good adsorption effect on toxic substances, an active group of polyvinyl alcohol can modify the carbon nano tube under reaction, so that the carbon nano tube can have better adsorption effect on the toxic substances, the cross-linking agent in S1 is N, N' -methylene bisacrylamide, the initiator in S1 is one of potassium persulfate and ammonium persulfate, the cross-linking agent and the initiator can stably perform the reaction, the porous ceramic in S1 is made of boron carbide ceramic, carbon nano tube, and the like, One of beryllium oxide ceramic, zirconium oxide ceramic, silicon carbide ceramic and aluminum oxide ceramic, the diameter of which is 1-2cm, the aperture of which is 200-400um, and the through-hole rate of which is 60-80%, the porous ceramic has a large surface area, so that the carbon nano tube can be compounded on the surface of the porous ceramic, thereby effectively contacting with toxic substances and effectively adsorbing the toxic substances.
The surfactant in the S1 is one of dimethyl ethyl allyl ammonium chloride, methyl cellulose copolymer, polyvinyl alcohol, petroleum sodium sulfonate, lignosulfonate, sodium alkyl sulfate and polyvinylamine, can activate the surface of the porous ceramic, and can be matched with yttrium chloride catalyst to compound the carbon nano tube on the surface of the porous ceramic, so that the contact area of the carbon nano tube and toxic substances is effectively increased, a better adsorption effect is achieved, and a longer effective adsorption time is prolonged.
Example one
The mass fraction of each material is as follows: 6% of polyethylene, 4% of acrylic acid, 18% of carbon nano tube, 2.1% of cross-linking agent, 1.4% of initiator, 1.5% of yttrium chloride catalyst, 0.9% of surfactant and 66.1% of porous ceramic.
A method for producing carbon nano tube composite porous ceramic capable of adsorbing toxic substances comprises the following steps:
s1: preparing a proper amount of polyvinyl alcohol, acrylic acid, carbon nano tubes, a cross-linking agent, an initiator, a yttrium chloride catalyst, a surfactant and porous ceramic according to a proportion;
s2: pouring the carbon nano tube and polyvinyl alcohol into a reaction kettle together, and then adding the mixture in a mass ratio of 1: 7, and then heating and stirring the mixture at 59 ℃, the stirring speed of 180 revolutions per minute and the stirring time of 39 minutes to obtain an initial mixed solution.
S3: simultaneously dripping a cross-linking agent, acrylic acid and an initiator into the initial mixed solution obtained in the step S1, maintaining the stirring speed in the step S1 in the dripping process, continuously stirring for 12 minutes after finishing dripping, raising the temperature in the reaction kettle to 85 ℃, stirring at the stirring speed of 160 revolutions per minute for 3 hours, and thus obtaining a secondary mixed solution;
s4: carrying out ultrasonic oscillation on the secondary mixed solution, wherein the oscillation time is 70 seconds, standing for 6 minutes after oscillation, and repeating for 4 times to obtain a carbon source solution for later use;
s5: adding the porous ceramic into a carbon source solution, then adding a yttrium chloride catalyst and a surfactant, heating and stirring at 260 ℃, stirring at 40 rpm for 36 minutes, and standing at constant temperature for 2.5 hours to obtain the finished composite porous ceramic material.
Example two
The mass fraction of each material is as follows: 7% of polyethylene, 4% of acrylic acid, 19% of carbon nano tube, 1.8% of cross-linking agent, 1.6% of initiator, 1.5% of yttrium chloride catalyst, 0.9% of surfactant and 64.2% of porous ceramic.
A method for producing carbon nano tube composite porous ceramic capable of adsorbing toxic substances comprises the following steps:
s1: preparing a proper amount of polyvinyl alcohol, acrylic acid, carbon nano tubes, a cross-linking agent, an initiator, a yttrium chloride catalyst, a surfactant and porous ceramic according to a proportion;
s2: pouring the carbon nano tube and polyvinyl alcohol into a reaction kettle together, and then adding the mixture in a mass ratio of 1: 8, and then heating and stirring the mixture at the stirring temperature of 68 ℃, the stirring speed of 160 revolutions per minute and the stirring time of 40 minutes to obtain an initial mixed solution.
S3: simultaneously dripping a cross-linking agent, acrylic acid and an initiator into the initial mixed solution obtained in the step S1, maintaining the stirring speed in the step S1 in the dripping process, continuously stirring for 14 minutes after finishing dripping, raising the temperature in the reaction kettle to 82 ℃, stirring, and obtaining a secondary mixed solution, wherein the stirring speed is 150 revolutions per minute, and the stirring time is 4 hours;
s4: carrying out ultrasonic oscillation on the secondary mixed solution for 60 seconds, standing for 5 minutes after oscillation, and repeating for 5 times to obtain a carbon source solution for later use;
s5: adding the porous ceramic into a carbon source solution, then adding a yttrium chloride catalyst and a surfactant, heating and stirring at the stirring temperature of 270 ℃, the stirring speed of 350 revolutions per minute for 36 minutes, and then standing at a constant temperature for 3 hours to obtain the finished product composite porous ceramic material.
EXAMPLE III
The mass fraction of each material is as follows: 8% of polyethylene, 5% of acrylic acid, 20% of carbon nano tube, 1.8% of cross-linking agent, 1.5% of initiator, 1.4% of yttrium chloride catalyst, 1.2% of surfactant and 61.1% of porous ceramic.
A method for producing carbon nano tube composite porous ceramics capable of adsorbing toxic substances comprises the following steps:
s1: preparing a proper amount of polyvinyl alcohol, acrylic acid, carbon nano tubes, a cross-linking agent, an initiator, a yttrium chloride catalyst, a surfactant and porous ceramic according to a proportion;
s2: pouring the carbon nano tube and polyvinyl alcohol into a reaction kettle together, and then adding the mixture in a mass ratio of 1: 8, and then heating and stirring the mixture at the stirring temperature of 60 ℃, the stirring speed of 200 revolutions per minute and the stirring time of 40 minutes to obtain an initial mixed solution.
S3: simultaneously dripping a cross-linking agent, acrylic acid and an initiator into the initial mixed solution obtained in the step S1, maintaining the stirring speed in the step S1 in the dripping process, continuously stirring for 12 minutes after finishing dripping, raising the temperature in the reaction kettle to 80 ℃, stirring at the stirring speed of 140 revolutions per minute for 3 hours, and thus obtaining a secondary mixed solution;
s4: performing ultrasonic oscillation on the secondary mixed solution, wherein the oscillation time is 90 seconds, standing for 5 minutes after oscillation, and repeating for 3 times to obtain a carbon source solution for later use;
s5: adding the porous ceramic into a carbon source solution, adding a yttrium chloride catalyst and a surfactant, heating and stirring at the stirring temperature of 280 ℃, the stirring speed of 50 revolutions per minute for 32 minutes, and standing at a constant temperature for 3 hours to obtain the finished composite porous ceramic material.
According to the invention, the carbon nano tube is mixed with polyvinyl alcohol, and a cross-linking agent, acrylic acid and an initiator are added for reaction, the carbon nano tube is modified by an active group carried by the polyvinyl alcohol, so that the carbon nano tube can have a better adsorption effect on toxic substances, and the porous ceramic, the yttrium chloride catalyst and the surfactant are added, so that the carbon nano tube can be fully compounded with the porous ceramic, and the finished product composite porous ceramic material is obtained, and the carbon nano tube can be attached to the holes of the porous ceramic, so that the contact area between the carbon nano tube and the toxic substances is effectively increased, and the adsorption effect can be maintained for a long time while the toxic substances are quickly adsorbed by the whole finished product composite porous ceramic material, so that a better adsorption effect is achieved.
The above description is only a preferred embodiment of the present invention, and not intended to limit the present invention in other forms, and any person skilled in the art may apply the above modifications or changes to the equivalent embodiments with equivalent changes by using the technical contents disclosed in the above description to other fields, but any simple modification, equivalent change and change made to the above embodiments according to the technical essence of the present invention still belong to the protection scope of the technical solution of the present invention.

Claims (10)

1. A production method of carbon nano tube composite porous ceramic capable of adsorbing toxic substances is characterized by comprising the following steps: the method comprises the following steps:
s1: preparing a proper amount of polyvinyl alcohol, acrylic acid, carbon nano tubes, a cross-linking agent, an initiator, a yttrium chloride catalyst, a surfactant and porous ceramic according to a proportion;
s2: pouring the carbon nano tube and polyvinyl alcohol into a reaction kettle together, and then adding the mixture in a mass ratio of 1: and (6-9) heating and stirring the deionized water at the stirring temperature of 55-70 ℃, the stirring speed of 150-220 rpm and the stirring time of 30-40 minutes to obtain an initial mixed solution.
S3: simultaneously dripping a cross-linking agent, acrylic acid and an initiator into the initial mixed solution obtained in S1, maintaining the stirring speed in S1 in the dripping process, continuously stirring for 10-15 minutes after finishing dripping, raising the temperature in the reaction kettle to 75-90 ℃, stirring at the stirring speed of 120-180 revolutions per minute for 3-4 hours, and thus obtaining a secondary mixed solution;
s4: performing ultrasonic oscillation on the secondary mixed solution for 60-90 seconds, standing for 5-8 minutes after oscillation, and repeating for 3-5 times to obtain a carbon source solution for later use;
s5: adding the porous ceramic into a carbon source solution, then adding a yttrium chloride catalyst and a surfactant, heating and stirring at the stirring temperature of 240-280 ℃, the stirring speed of 30-60 revolutions per minute and the stirring time of 30-40 minutes, and then standing at constant temperature for 2-3 hours to obtain the finished product of the composite porous ceramic material.
2. The method for manufacturing a carbon nanotube composite porous ceramic with adsorbed toxic substances as set forth in claim 1, wherein: the S1 comprises the following materials in percentage by mass: 4-8% of polyethylene, 3-5% of acrylic acid, 16-21% of carbon nano tube, 1-2.5% of cross-linking agent, 1-2% of initiator, 1-2% of yttrium chloride catalyst, 0.5-1.5% of surfactant and 54-76% of porous ceramic.
3. The method for producing carbon nanotube composite porous ceramic having adsorbed toxic substances according to claim 1, wherein: the pipe diameter of the carbon nano-tube in the S1 is 20-60nm, and the length is 50-100 um.
4. The method for producing carbon nanotube composite porous ceramic having adsorbed toxic substances according to claim 1, wherein: the cross-linking agent in the S1 is N, N' -methylene-bis-acrylamide.
5. The method for producing carbon nanotube composite porous ceramic having adsorbed toxic substances according to claim 1, wherein: the material of the porous ceramic in the S1 is one of boron carbide ceramic, beryllium oxide ceramic, zirconium oxide ceramic, silicon carbide ceramic and alumina ceramic, the diameter of the porous ceramic is 1-2cm, the pore diameter is 200-400 mu m, and the through-hole rate is 60-80%.
6. The method for producing carbon nanotube composite porous ceramic having adsorbed toxic substances according to claim 1, wherein: the initiator in the S1 is one of potassium persulfate and ammonium persulfate.
7. The method for producing carbon nanotube composite porous ceramic having adsorbed toxic substances according to claim 1, wherein: and the surfactant in the S1 is one of dimethyl ethyl allyl ammonium chloride, methyl cellulose copolymer, polyvinyl alcohol, petroleum sodium sulfonate, lignosulfonate, alkyl sodium sulfate and polyvinylamine.
8. The method for producing carbon nanotube composite porous ceramic having adsorbed toxic substances according to claim 1, wherein: the mass fraction of each material is as follows: 6% of polyethylene, 4% of acrylic acid, 18% of carbon nano tube, 2.1% of cross-linking agent, 1.4% of initiator, 1.5% of yttrium chloride catalyst, 0.9% of surfactant and 66.1% of porous ceramic.
9. The method for producing carbon nanotube composite porous ceramic having adsorbed toxic substances according to claim 1, wherein: the mass fraction of each material is as follows: 7% of polyethylene, 4% of acrylic acid, 19% of carbon nano tube, 1.8% of cross-linking agent, 1.6% of initiator, 1.5% of yttrium chloride catalyst, 0.9% of surfactant and 64.2% of porous ceramic.
10. The method for producing carbon nanotube composite porous ceramic having adsorbed toxic substances according to claim 1, wherein: the mass fraction of each material is as follows: 8% of polyethylene, 5% of acrylic acid, 20% of carbon nano tube, 1.8% of cross-linking agent, 1.5% of initiator, 1.4% of yttrium chloride catalyst, 1.2% of surfactant and 61.1% of porous ceramic.
CN202210111821.7A 2022-01-29 2022-01-29 Production method of carbon nano tube composite porous ceramic capable of adsorbing toxic substances Pending CN114436676A (en)

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