CN112023869B - Method for preparing mesoporous titanium disulfide adsorbent and application - Google Patents
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Abstract
The invention discloses a method for preparing a mesoporous titanium disulfide adsorbent and application thereof 2 . Mixing Ti and S powder (Ti: S molar ratio =1: 2) and template C 3 N 4 Mixing with ultrasonic oscillator, pouring into ceramic combustion boat, and adding iodine as transport agent. The boat was transferred to the tubular reactor and vented for 30 minutes. After heating at high temperature for 48 hours, the powder was washed with ethanol and dried at 100 ℃. Thus obtaining TiS 2 An adsorbent. The invention improves TiS by adding the template agent 2 The specific surface area and the porosity of the catalyst improve the adsorption quantity and the selectivity of the catalyst on carbon dioxide.
Description
Technical Field
The invention belongs to the technical field of gas separation, and particularly relates to a method for preparing a mesoporous titanium disulfide adsorbent and application thereof.
Background
In recent decades, with the increasing prominence of global warming, CO 2 Emission reduction becomes a research hotspot. Greenhouse gases (GHGs) in the atmosphere, mainly carbon dioxide (CO), are the main cause of the rise in temperature on the earth's surface 2 ) Chlorofluoroalkanes (CFCs), carbon monoxide (CO), methane (CH) 4 ) Ozone (O) 3 ) And nitrogen oxides, etc., wherein CO 2 Is a greenhouse gas with the largest influence on climate change, and converts CO into CO 2 The adsorption separation from the waste gas has important research significance, the adsorption method has the advantages of easy regeneration, low energy consumption, simple operation and the like, is widely researched and applied, and has low energySpent solid pore adsorbents are of great interest.
Post-combustion capture may be the first technology to be used for carbon dioxide removal, as existing combustion technologies can still be used without fundamental changes to them. Among various separation techniques such as absorption, adsorption, and membrane separation, adsorption is considered to be a promising technique. Its main advantages are easy regeneration of adsorbent and low cost of carbon dioxide capture. The application of adsorption requires that the adsorbent have a high CO 2 Adsorption capacity, easy regeneration and durability.
Many researchers have studied the CO of titanium-based materials 2 Adsorptive properties including potassium based TiO 2 Adsorbent, doped TiO 2 K of 2 CO 3 /Al 2 O 3 And mesoporous TiO 2 Graphene oxide nanocomposites. Also researchers have prepared amine modified titanium based CO 2 Adsorbents, e.g. TiO 2 Nanotube, mesoporous TiO 2 And a sulfur doped titanate. They all exhibit excellent CO 2 Adsorption capacity and good regenerability due to CO 2 Adsorption relies primarily on weak chemisorption provided by the amino groups, and regeneration can be effected efficiently.
Like graphite, titanium disulfide (TiS) 2 ) Has a layered (X-M-X) structure. The atoms in the S-Ti-S sheet are constrained by strong covalent interactions. The bonding between the layers is determined by weak van der waals forces. In recent years, TiS 2 And their intercalation compounds have attracted considerable theoretical and experimental interest for their interesting layer structures and anisotropic physical properties and their potential applications. For example, TiS due to the high density of free carriers in the layered material 2 At all temperatures, it shows a metallic electronic conductivity with an unusual temperature relationship of T2, which can be considered as a two-dimensional solid. LixTiS 2 Has been used as a positive electrode material for high energy density lithium batteries.
Disclosure of Invention
Aiming at the technical problem, the invention provides a method for preparing a mesoporous titanium disulfide adsorbent and application thereof, wherein the method adopts the addition of C 3 N 4 Mesoporous TiS prepared by solid-phase reaction method as template agent 2 To solve the problem of the existing solid-phase reaction method for preparing TiS 2 The specific surface area is not high, and the porosity is low.
A method for preparing a mesoporous titanium disulfide adsorbent comprises the following steps: step 1, uniformly mixing Ti powder, S powder and a template agent, adding the mixture into a ceramic combustion boat, and adding iodine as a transport agent, wherein the molar ratio of Ti to S is 1:2, and the template agent is C 3 N 4 And uniformly mixing the Ti powder and the S powder by using an ultrasonic oscillator; step 2, transferring the ceramic combustion boat into a tubular reactor, and emptying for 30 minutes; step 3, heating the mixture at the high temperature of 600-800 ℃ for 48 hours, and taking out the mixture after the product is cooled; step 4, cleaning the product with ethanol, and drying in a vacuum drying oven to obtain TiS 2 An adsorbent.
As a modification, the tubular reactor was purged with high-purity nitrogen for 30min before being subjected to the evacuation treatment in step 2.
As a modification, the heating rate of the heating reaction in the step 3 is 10 ℃/min.
As a modification, the drying temperature in step 4 is 100 ℃.
TiS prepared as described above 2 Use of an adsorbent for carbon dioxide adsorption.
Has the advantages that:
compared with the prior art, the method for preparing the mesoporous titanium disulfide adsorbent and the application thereof have the advantages that the mesoporous titanium disulfide adsorbent is prepared by adopting a solid-phase reaction method, and C is added in the preparation process 3 N 4 As templating agent, C 3 N 4 Decomposition temperature interval and TiS 2 The calcination temperature intervals of the precursors are overlapped, thereby ensuring that the temperature is in TiS 2 In the formation of (C) 3 N 4 Decomposition to realize pore-forming and improve TiS 2 The pore volume and the specific surface area of the adsorbent are improved, and the CO resistance of the material is improved 2 The amount of adsorption of (2).
Drawings
FIG. 1 is a drawing showing that 2 And CN-TiS 2 The SEM topography of (A) is TiS 2 -600, (b) isTiS 2 700 and (c) is TiS 2 800, (d) is CN-TiS 2 600, (e) is CN-TiS 2 700 and f is CN-TiS 2 -800。
Detailed Description
The invention is further described below with reference to the figures and the specific embodiments.
Example 1
A method for preparing a mesoporous titanium disulfide adsorbent comprises the following steps:
step 2, transferring the boat into a tubular reactor, firstly purging the tubular reactor for 30min by using high-purity nitrogen, and then emptying for 30 min;
step 3, heating the tubular reactor at 600 ℃ for 48 hours, wherein the heating rate of the heating reaction is 10 ℃/min, and taking out the product after the product is cooled;
step 4, washing the product with ethanol, and drying the product in vacuum at 100 ℃ to obtain CN-TiS 2 -600。
Example 2
A method for preparing a mesoporous titanium disulfide adsorbent comprises the following steps:
step 2, transferring the boat into a tubular reactor, firstly purging the tubular reactor for 30min by using high-purity nitrogen, and then emptying for 30 min;
step 3, heating the tubular reactor at 700 ℃ for 48 hours, wherein the heating rate of the heating reaction is 10 ℃/min, and taking out the tubular reactor after the product is cooled;
step 4, washing the product with ethanol, and drying the product in vacuum at 100 ℃ to obtain CN-TiS 2 -700。
Example 3
A method for preparing a mesoporous titanium disulfide adsorbent comprises the following steps:
step 2, transferring the boat into a tubular reactor, firstly purging the tubular reactor for 30min by using high-purity nitrogen, and then emptying for 30 min;
step 3, heating the tubular reactor at 800 ℃ for 48 hours, wherein the heating rate of the heating reaction is 10 ℃/min, and taking out the product after the product is cooled;
step 4, washing the product with ethanol, and drying the product in vacuum at 100 ℃ to obtain CN-TiS 2 -800。
Comparative example 1
A method for preparing a mesoporous titanium disulfide adsorbent comprises the following steps:
(1) step 1, uniformly mixing 2.4g of Ti and 3.2g S powder (Ti: S molar ratio is 1:2) in a ceramic combustion boat, and adding iodine as a transport agent;
(2) step 2, transferring the boat into a tubular reactor, firstly purging the tubular reactor for 30min by using high-purity nitrogen, and then emptying for 30 min;
(3) step 3, heating the tubular reactor at 600 ℃ for 48 hours at a heating rate of 10 ℃/min, and taking out the product after cooling;
(4) step 4, washing the product with ethanol to obtain powder, and drying the powder in vacuum at 100 ℃ to obtain TiS 2 -600。
Comparative example 2
A preparation method of mesoporous titanium disulfide comprises the following steps:
(1) step 1, uniformly mixing 2.4g of Ti and 3.2g S powder (Ti: S molar ratio is 1:2) in a ceramic combustion boat, and adding iodine as a transport agent;
(2) step 2, transferring the boat into a tubular reactor, firstly purging the tubular reactor for 30min by using high-purity nitrogen, and then emptying for 30 min;
(3) step 3, heating the tubular reactor at 700 ℃ for 48 hours, wherein the heating rate of the heating reaction is 10 ℃/min, and taking out the product after the product is cooled;
(4) step 4, washing the product with ethanol to obtain powder, and drying the powder in vacuum at 100 ℃ to obtain TiS 2 -700。
Comparative example 3
A preparation method of mesoporous titanium disulfide comprises the following steps:
(1) step 1, 2.4g of Ti and 3.2g S of powder (Ti: S molar ratio 1:2) were uniformly mixed in a ceramic combustion boat, and iodine was added as a transport agent;
(2) step 2, transferring the boat into a tubular reactor, firstly purging the tubular reactor for 30min by using high-purity nitrogen, and then emptying for 30 min;
(3) step 3, heating the tubular reactor at 800 ℃ for 48 hours, wherein the heating rate of the heating reaction is 10 ℃/min, and taking out the product after the product is cooled;
(4) step 4, washing the product with ethanol to obtain powder, and drying the powder in vacuum at 100 ℃ to obtain TiS 2 -800。
The low temperature nitrogen physisorption desorption isotherm of the material was tested at liquid nitrogen temperature (-196 ℃) using an ASAP2020M fully automated specific surface area and porosity analyzer (mack instruments usa) and its specific surface area and pore volume were calculated using the BET equation. CO 2 2 The adsorption performance is also tested in the above instrument, the test pressure is controlled between 0-0.12MPa through the pressure reducing valve of the steel cylinder and the electromagnetic valve, the temperature is controlled at room temperature by the method of immersing the sample tube in a thermostatic water bath, and the CO is measured under the above conditions 2 Adsorbing the isotherm to obtain the adsorption quantity.
TABLE 1 TiS prepared by different methods and temperatures 2 Specific surface area, pore volume and CO of physicochemical characteristics of 2 Amount of adsorption
As can be seen from Table 1, TiS 2 And CN-TiS 2 Specific surface area, pore volume and CO 2 The adsorption amount increases with the increase of the preparation temperature. When the preparation temperature is the same, CN-TiS 2 Specific surface area, pore volume and CO 2 The adsorption capacity is higher than TiS 2 This is due to C 3 N 4 The decomposition temperature of the titanium disulfide is 600-700 ℃, which is matched with the formation temperature interval of the titanium disulfide, and in the process of forming the titanium disulfide, the template agent C 3 N 4 TiS decomposed to form mesoporous structure 2 Improve TiS 2 Pore volume and specific surface area of adsorbent, thereby improving CO-to-CO ratio of material 2 The amount of adsorption of (3).
As can be seen from FIG. 1, TiS 2 And CN-TiS 2 The morphology of (a) changes with the increase of the preparation temperature. When the preparation temperature is 700 ℃, TiS 2 700 and CN-TiS 2 700 all exhibit a distinct layered structure, formed by electrostatic interactions, which is bound together, greatly increasing the CO 2 The amount of adsorption. And TiS 2 700 comparison, CN-TiS 2 The layer structure of-700 is more pronounced, so the specific surface area, pore volume and adsorption capacity of the latter are all higher than those of the former.
Claims (5)
1. A method for preparing a mesoporous titanium disulfide adsorbent is characterized by comprising the following steps: step 1, uniformly mixing Ti powder, S powder and a template agent, adding the mixture into a ceramic combustion boat, and adding iodine as a transport agent, wherein the molar ratio of Ti to S is 1:2, and the template agent is C 3 N 4 And uniformly mixing the Ti powder and the S powder by using an ultrasonic oscillator; step 2, transferring the ceramic combustion boat into a tubular reactor, and emptying for 30 minutes; step 3, heating at the high temperature of 600-800 ℃ for 48 hours, and taking out the product after the product is cooled; and 4, cleaning the product with ethanol, and drying in a vacuum drying oven to obtain the mesoporous titanium disulfide adsorbent.
2. The method for preparing the mesoporous titanium disulfide adsorbent according to claim 1, wherein the tubular reactor is purged with high-purity nitrogen for 30min before evacuation in step 2.
3. The method for preparing the mesoporous titanium disulfide adsorbent according to claim 1, wherein the heating rate of the heating reaction in step 3 is 10 ℃/min.
4. The method for preparing the mesoporous titanium disulfide adsorbent according to claim 1, wherein the drying temperature in step 4 is 100 ℃.
5. The application of the mesoporous titanium disulfide adsorbent prepared by the method of claim 1 in carbon dioxide adsorption.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103991900A (en) * | 2014-05-28 | 2014-08-20 | 南京理工大学 | Preparation method of high-purity and high-crystallinity titanium disulfide nanometer plates |
| CN107337233A (en) * | 2017-06-05 | 2017-11-10 | 陕西科技大学 | A kind of method of one step vulcanization method synthesis of titanium dioxide and titanium disulfide composite |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103991900A (en) * | 2014-05-28 | 2014-08-20 | 南京理工大学 | Preparation method of high-purity and high-crystallinity titanium disulfide nanometer plates |
| CN107337233A (en) * | 2017-06-05 | 2017-11-10 | 陕西科技大学 | A kind of method of one step vulcanization method synthesis of titanium dioxide and titanium disulfide composite |
Non-Patent Citations (1)
| Title |
|---|
| Synthetic Strategy and Structural and Optical Characterization of Thin Highly Crystalline Titanium Disulfide Nanosheets;Vladimir V. Plashnitsa, et al;《The Journal of Physical Chemistry Letters》;20120523;第3卷;第1554-1558页 * |
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