CN113912109A - Preparation method of nano titanium dioxide porous material - Google Patents
Preparation method of nano titanium dioxide porous material Download PDFInfo
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- CN113912109A CN113912109A CN202111393759.7A CN202111393759A CN113912109A CN 113912109 A CN113912109 A CN 113912109A CN 202111393759 A CN202111393759 A CN 202111393759A CN 113912109 A CN113912109 A CN 113912109A
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- C01G23/00—Compounds of titanium
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- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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Abstract
The invention discloses a preparation method of a nano titanium dioxide porous material, belonging to the technical field of nano material production. The invention prepares a core-shell structure from a nano material, and prepares a nano titanium dioxide porous material with a stable structure by using vanadium pentoxide and hydrogen peroxide as pore-forming materials, wherein the preparation method comprises the following steps: and (3) adding an SEBS thermoplastic elastomer for refining at the temperature of 140-180 ℃ of the double rods and the distance between the rollers of 0.5-1.5 mm, adding the coated nano titanium dioxide for refining, adding vanadium pentoxide for refining, and soaking the mixture into a mixed solution of sulfuric acid and hydrogen peroxide for reaction to obtain the catalyst. The method has low price and simple operation, can be used for large-scale production, and the nano titanium dioxide and the vanadium pentoxide can be uniformly dispersed in the high polymer material, and the vanadium pentoxide and the hydrogen peroxide are used as pore-forming materials, so that the obtained material has a stable structure.
Description
Technical Field
The invention belongs to the technical field of nano material production, and particularly relates to a preparation method of a nano titanium dioxide porous material.
Background
The titanium dioxide nano material has unique physical and chemical properties, so that the titanium dioxide nano material is widely applied to researches in the aspects of photocatalysis, antibiosis, solar batteries, lithium ion batteries and the like. The porous material has the advantages that the modification sites and the surface activity of the titanium dioxide can be improved due to the increase of the specific surface area, the expansion of a mass transfer path can increase the contact probability with the active sites, the size of a selected reactant is selected, and the like, so that the porous material becomes a research hotspot of the current porous material, and a series of materials with porous hollow structures, thin layers and nano self-organized structures are prepared.
At present, a material with a porous structure is often used as a framework or a template for preparing porous titanium dioxide, for example, "preparation of a porous titanium dioxide nano structure and application thereof in a solar cell (catalytic et al, university of Beijing information and technology, 2016, 6 months, volume 31, phase 3)" use open-cell polymer reticulated foam as a framework material to prepare the porous titanium dioxide nano structure; CN112429769A discloses a preparation method of ultra-low density titanium dioxide foam, which uses low density metal foam as a substrate to prepare a porous titanium dioxide product by using an atomic layer deposition method; however, the nano titanium dioxide porous material prepared by using the porous material as the skeleton has poor stability of the formed titanium dioxide network, and the porous structure is easy to collapse in the using process. CN113279248A discloses a nano titanium dioxide electrostatic spinning film and a preparation method thereof, wherein an electrostatic spinning technology is used for preparing a porous nano titanium dioxide film; however, this method is complicated and not suitable for industrial production.
Therefore, it is necessary to develop a method for preparing a nano titanium dioxide porous material with simple preparation technology and stable structure.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a nano titanium dioxide porous material with simple preparation technology and stable structure, which is characterized in that a nano material is dispersed in a high molecular material after being prepared into a core-shell structure, and then vanadium pentoxide and hydrogen peroxide are used as pore-forming materials to prepare the nano titanium dioxide porous material.
The invention provides a preparation method of a nano titanium dioxide porous material, which comprises the following steps:
A. adding an SEBS thermoplastic elastomer for first refining at the temperature of 140-180 ℃ of the double rollers and the distance between the rollers of 0.5-1.5 mm, then adding the coated nano titanium dioxide for second refining, adding vanadium pentoxide for third refining, and cooling to obtain a nano titanium dioxide/vanadium pentoxide/SEBS composite material;
B. and D, soaking the nano titanium dioxide/vanadium pentoxide/SEBS composite material obtained in the step A into a mixed solution of sulfuric acid and hydrogen peroxide for reaction, and washing and drying after the reaction is finished to obtain the nano titanium dioxide porous material.
In the preparation method of the nano titanium dioxide porous material, in the step A, the addition amount of the coated nano titanium dioxide is 15-40% of the mass of the SEBS thermoplastic elastomer.
In the preparation method of the nano titanium dioxide porous material, in the step A, the addition amount of the vanadium pentoxide is 15-40% of the mass of the SEBS thermoplastic elastomer.
In the preparation method of the nano titanium dioxide porous material, in the step A, the time for the first refining is 2-5 minutes; the time for the second refining is 15-30 minutes; the time for the third refining is 5-15 minutes.
In the preparation method of the nano titanium dioxide porous material, in the step B, the mixed solution of sulfuric acid and hydrogen peroxide is prepared by mixing 10-30% by mass of sulfuric acid and 15-30% by mass of hydrogen peroxide according to a volume ratio of 1: 1-3 mixing.
In the preparation method of the nano titanium dioxide porous material, in the step B, the reaction time is 4-8 hours.
In the preparation method of the nano titanium dioxide porous material, in the step B, the drying temperature is 60-80 ℃.
The invention has the beneficial effects that:
firstly, the SEBS thermoplastic elastomer is refined for the first time, then the nano titanium dioxide and the vanadium pentoxide with the core-shell structure are sequentially added for the second and third refining, so that the nano titanium dioxide and the vanadium pentoxide are uniformly dispersed in a high polymer material, and the nano titanium dioxide porous material is prepared by using the vanadium pentoxide and hydrogen peroxide as pore-forming materials. The method has low price and simple operation, can be used for large-scale production, and the obtained material has stable structure and can be applied to the related fields of laser inertial confinement fusion, hydrogen storage, purification, filtration, catalytic support and the like for a long time.
Detailed Description
Specifically, the preparation method of the nano titanium dioxide porous material comprises the following steps:
A. adding an SEBS thermoplastic elastomer for first refining at the temperature of 140-180 ℃ of the double rollers and the distance between the rollers of 0.5-1.5 mm, then adding the coated nano titanium dioxide for second refining, adding vanadium pentoxide for third refining, and cooling to obtain a nano titanium dioxide/vanadium pentoxide/SEBS composite material;
B. and D, soaking the nano titanium dioxide/vanadium pentoxide/SEBS composite material obtained in the step A into a mixed solution of sulfuric acid and hydrogen peroxide for reaction, and washing and drying after the reaction is finished to obtain the nano titanium dioxide porous material.
The vanadium pentoxide and SEBS used in the invention are commercially available products, and the preparation method of the coated nano titanium dioxide can adopt the prior art, such as' nano TiO2Research on seed emulsion polymerization coating, Sichuan chemical engineering, and in-situ coating method in 2014 2, volume 17.
In the step A, the temperature of the double rollers is controlled to ensure the processing temperature, the complete plasticization of the SEBS is ensured, the distance between the rollers is controlled to adjust the shearing force during processing, and the nano filler and the SEBS can be fully mixed.
In the step A, the addition amount of the coated nano titanium dioxide is 15-40% of the mass of the SEBS thermoplastic elastomer, and the addition amount of the vanadium pentoxide is 15-40% of the mass of the SEBS thermoplastic elastomer. The addition amount of the nano titanium dioxide is too small, the effective components in the formed porous material are insufficient, the effect cannot be achieved when the porous material is used, and the porous structure can be damaged when the addition amount is too large; the vanadium pentoxide is too little, the generated pores are too little, the performance of the porous material can be reduced in use, and the porous structure can be damaged due to the fact that the porous material is too much and too many pores are added.
In the step A, the time for the first refining is 2-5 minutes; the time for the second refining is 15-30 minutes; the time for the third refining is 5-15 minutes.
And (B) reacting vanadium pentoxide with hydrogen peroxide under an acidic condition, and forming pores by using a material, so that in the step B, the mixed solution of sulfuric acid and hydrogen peroxide is prepared by mixing 10-30% by mass of sulfuric acid and 15-30% by mass of hydrogen peroxide according to a volume ratio of 1: 1-3 mixing.
In the step B, the reaction time is 4-8 hours; the drying temperature is 60-80 ℃.
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Preparing the coated nano titanium dioxide: taking nano titanium dioxide with the particle size of 25-60 nm, stirring at a low speed at normal temperature, and then dropwise adding a monomer (methyl methacrylate or a methyl methacrylate-styrene mixture) by using a separating funnel at the dropwise adding speed of 1.2d/s to prepare a mixed solution of the nano titanium dioxide and a reaction monomer; heating water in a constant-temperature water bath kettle, heating to 86 ℃, and dropwise adding an initiator at the speed of 1.0 d/s; after the dripping is finished, reacting for half an hour at 86 ℃ under the condition of stirring at medium speed, then heating to 90 ℃, preserving heat for 2 hours, cooling to room temperature, filtering, extracting the solid part with acetone at 90 ℃ for 24 hours, drying, and grinding into fine powder.
SEBS number YH-502T, purchased from Baling petrochemical Co.
Example 1
The temperature of the two rollers is 140 ℃, the distance between the rollers is 0.5mm, after the SEBS thermoplastic elastomer is refined for 5 minutes, the coated nano titanium dioxide accounting for 15 percent of the mass of the SEBS thermoplastic elastomer is added, the mixture is refined for 15 minutes, then the vanadium pentoxide accounting for 40 percent of the mass of the SEBS thermoplastic elastomer is added, and the mixture is refined for 15 minutesThen, the obtained product is immersed in sulfuric acid with the mass percentage concentration of 30% and hydrogen peroxide with the mass percentage concentration of 30% according to the volume ratio of 1: 1, reacting for 8 hours, taking out the porous material, washing the porous material with distilled water for 3 times, putting the porous material into an oven, and drying the porous material at 60 ℃ to obtain the porous titanium dioxide with the specific surface area of 167.1m2Per g, porosity 73.2%.
Example 2
The temperature of the two rollers is 160 ℃, the distance between the rollers is 1.0mm, after the SEBS thermoplastic elastomer is refined for 3 minutes, the coated nano titanium dioxide with the mass of 25 percent of that of the SEBS thermoplastic elastomer is added, the refining is carried out for 20 minutes, then the vanadium pentoxide with the mass of 25 percent of that of the SEBS thermoplastic elastomer is added, after the refining is carried out for 10 minutes, the obtained product is immersed into sulfuric acid with the mass percent concentration of 20 percent and hydrogen peroxide with the mass percent concentration of 20 percent according to the volume ratio of 1: 2, reacting for 6 hours, taking out the porous material, washing the porous material with distilled water for 4 times, putting the porous material into an oven, and drying the porous material at 70 ℃, wherein the specific surface area of the prepared porous titanium dioxide is 155.1m2G, porosity 62.1%.
Example 3
The temperature of the two rollers is 180 ℃, the distance between the rollers is 1.5mm, after the SEBS thermoplastic elastomer is refined for 2 minutes, the coated nano titanium dioxide with the mass of 40 percent of that of the SEBS thermoplastic elastomer is added, the mixture is refined for 30 minutes, then the vanadium pentoxide with the mass of 15 percent of that of the SEBS thermoplastic elastomer is added, after the mixture is refined for 5 minutes, the obtained product is immersed into sulfuric acid solution and hydrogen peroxide with the mass percent concentration of 10 percent respectively according to the volume ratio of 1: 3 reacting for 4 hours, taking out the porous material, washing the porous material with distilled water for 5 times, putting the porous material into an oven to dry at 80 ℃, and obtaining the porous titanium dioxide with the specific surface area of 145.2m2(iii) per gram, porosity 55.2%.
Claims (7)
1. The preparation method of the nano titanium dioxide porous material is characterized by comprising the following steps: the method comprises the following steps:
A. adding an SEBS thermoplastic elastomer for first refining at the temperature of 140-180 ℃ of the double rollers and the distance between the rollers of 0.5-1.5 mm, then adding the coated nano titanium dioxide for second refining, adding vanadium pentoxide for third refining, and cooling to obtain a nano titanium dioxide/vanadium pentoxide/SEBS composite material;
B. and D, soaking the nano titanium dioxide/vanadium pentoxide/SEBS composite material obtained in the step A into a mixed solution of sulfuric acid and hydrogen peroxide for reaction, and washing and drying after the reaction is finished to obtain the nano titanium dioxide porous material.
2. The method for preparing a nano titanium dioxide porous material according to claim 1, characterized in that: in the step A, the addition amount of the coated nano titanium dioxide is 15-40% of the mass of the SEBS thermoplastic elastomer.
3. The method for preparing a nano titanium dioxide porous material according to claim 1, characterized in that: in the step A, the adding amount of the vanadium pentoxide is 15-40% of the mass of the SEBS thermoplastic elastomer.
4. The method for preparing a nano titanium dioxide porous material according to claim 1, characterized in that: in the step A, the time for the first refining is 2-5 minutes; the time for the second refining is 15-30 minutes; the time for the third refining is 5-15 minutes.
5. The method for preparing a nano titanium dioxide porous material according to claim 1, characterized in that: in the step B, the mixed solution of sulfuric acid and hydrogen peroxide is prepared by mixing 10-30% by mass of sulfuric acid and 15-30% by mass of hydrogen peroxide according to a volume ratio of 1: 1-3 mixing.
6. The method for preparing a nano titanium dioxide porous material according to claim 1, characterized in that: in the step B, the reaction time is 4-8 hours.
7. The method for preparing a nano titanium dioxide porous material according to any one of claims 1 to 6, characterized in that: in the step B, the drying temperature is 60-80 ℃.
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| CN102744050A (en) * | 2012-07-16 | 2012-10-24 | 黑龙江大学 | Method for preparing ordered mesoporous titanium dioxide photocatalyst |
| US20130029234A1 (en) * | 2011-07-26 | 2013-01-31 | Samsung Electronics Co., Ltd. | Porous carbonaceous composite material, positive electrode and lithium air battery including porous carbonaceous composite material, and method of preparing the same |
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- 2021-11-23 CN CN202111393759.7A patent/CN113912109B/en active Active
Patent Citations (8)
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| CN1515490A (en) * | 2003-08-26 | 2004-07-28 | 复旦大学 | Method for removing organic-inorganic composite porous material organic template agent |
| US20130029234A1 (en) * | 2011-07-26 | 2013-01-31 | Samsung Electronics Co., Ltd. | Porous carbonaceous composite material, positive electrode and lithium air battery including porous carbonaceous composite material, and method of preparing the same |
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| US20180069238A1 (en) * | 2013-06-21 | 2018-03-08 | Unist (Ulsan National Institute Of Science And Technology) | Porous silicon based negative electrode active material, method for manufacturing the same, and rechargeable lithium battery including the same |
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| CN106630835A (en) * | 2016-12-19 | 2017-05-10 | 马鞍山杰创塑胶科技有限公司 | Porous alumina aerogel modified regenerated EPS particle-Portland cement composite foamed heat retaining board and preparation method thereof |
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