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CN109261181A - Utilize the Ti of isopropylamine intercalation and layering3C2Fabricated in situ TiO2@Ti3C2Method and product - Google Patents

Utilize the Ti of isopropylamine intercalation and layering3C2Fabricated in situ TiO2@Ti3C2Method and product Download PDF

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CN109261181A
CN109261181A CN201811051653.7A CN201811051653A CN109261181A CN 109261181 A CN109261181 A CN 109261181A CN 201811051653 A CN201811051653 A CN 201811051653A CN 109261181 A CN109261181 A CN 109261181A
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isopropylamine
intercalation
tio
layered
temperature
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林道辉
柯涛
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Zhejiang University ZJU
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Zhejiang University ZJU
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/20—Carbon compounds
    • B01J27/22—Carbides

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Abstract

The present invention relates to a kind of Ti using isopropylamine intercalation and layering3C2Fabricated in situ TiO2@Ti3C2Method and product, synthetic method include: 1) by Ti3AlC2- MAX phase ceramics powder, which is dispersed in HF solution, to be performed etching, and Mxene-Ti is obtained3C2；2) by Mxene-Ti3C2It is dispersed in progress isopropylamine intercalation in the mixed solution of isopropylamine and water, obtains the Ti of isopropylamine intercalation3C2；3) by the Ti of isopropylamine intercalation3C2It is dispersed in water, is ultrasonically treated under an argon atmosphere, obtain the Ti of isopropylamine intercalation and layering after dry3C2；4) Ti of isopropylamine intercalation and layering3C2In-situ oxidation is carried out under Oxygen Condition to get TiO2@Ti3C2.This method improves Mxene-Ti using isopropylamine and ultrasonic treatment3C2Interlamellar spacing, for the TiO of generation2More attachment sites are provided, the catalytic degradation to pollutant is more advantageous to.

Description

Utilize the Ti of isopropylamine intercalation and layering3C2Fabricated in situ TiO2@Ti3C2Method and Product
Technical field
The present invention relates to Ti3C2Preparation field, and in particular to a kind of Ti using isopropylamine intercalation and layering3C2It is in situ Synthesize TiO2@Ti3C2Method and product.
Background technique
Since two-dimension nano materials graphene in 2004 is successfully stripped out from graphite, since it is very good each Kind performance, graphene have all obtained in-depth study in every field, also therefore cause people and grind to two-dimension nano materials Study carefully upsurge.
2011, by Univ Drexel of the U.S. (Drexel University) Yury Gogotsi professor and Michel W.Barsoum professor et al. cooperation has found a kind of New Two Dimensional structure nano material-two dimension transition metal carbide Or carbonitride, it and graphene have similar layer structure, have good electric conductivity and powerful charge storage, In terms of Li battery also with good application prospect.
Nano-titanium dioxide is due to its excellent spectrochemical property, such as: photochemical stability, thermo-chemical stability, well Dispersibility and weatherability, be widely used in the fields such as cosmetics, functional fibre, plastics, coating, paint, repaired in environmental pollution It during multiple, can be utilized to as photocatalyst for degrading pollutant, however titanium dioxide is due to the fault of construction (electricity of itself Sub- hole is easy compound) cause its catalytic performance to substantially reduce.Many scholars solve this problem using many methods, Such as: precious metal ion mixes, and nonmetallic ion mixes, and photosensitizer etc. all achieves good results.
Ti3C2In contain titanium elements in itself, many scholars attempt discovery, Ti3C2The catalytic performance having is very poor, but passes through The titanyl on surface can be melted into titanium dioxide by peroxidization, obtain a kind of new nano material TiO2@Ti3C2, due to Ti3C2 Fermi level it is more negative than titanium dioxide, and forbidden bandwidth is smaller than titanium dioxide, in the illumination by respective wavelength, can be used as The receptor in hole greatly reduces the compound of electron hole, and catalytic performance is greatly enhanced.
Currently, selecting the blocky Mxene-Ti that directly synthesis obtains mostly3C2It is made by hydro-thermal method or heat treatment TiO2@Ti3C2, directly pass through common etching agent HF, NH4HF2And the Ti that the mixed liquor of HCl and LiF obtains3C2Interlamellar spacing compared with It is small, finally influence TiO2@Ti3C2Catalytic performance.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of Ti using isopropylamine intercalation and layering3C2 Fabricated in situ TiO2@Ti3C2Method, improve Mxene-Ti using isopropylamine and ultrasonic treatment3C2Interlamellar spacing, for generation TiO2More attachment sites are provided, its catalytic performance is further increased.
A kind of Ti using isopropylamine intercalation and layering3C2Fabricated in situ TiO2@Ti3C2Method, include the following steps:
1) by Ti3AlC2- MAX phase ceramics powder, which is dispersed in HF solution, to be performed etching, and Mxene-Ti is obtained3C2；
2) by Mxene-Ti3C2It is dispersed in progress isopropylamine intercalation in the mixed solution of isopropylamine and water, isopropylamine is obtained and inserts The Ti of layer3C2；
3) by the Ti of isopropylamine intercalation3C2It is dispersed in water, is ultrasonically treated under an argon atmosphere, obtain isopropylamine after dry The Ti of intercalation and layering3C2；
4) Ti of isopropylamine intercalation and layering3C2In-situ oxidation is carried out under Oxygen Condition to get TiO2@Ti3C2。
Mxene-Ti is improved using isopropylamine and ultrasonic treatment in the present invention3C2Interlamellar spacing, for the TiO of generation2It provides Then more attachment sites utilize the Ti of isopropylamine intercalation and layering3C2It carries out in-situ oxidation and prepares TiO2@Ti3C2, in original Without adding any chemical agent in the oxidation process of position, TiO can be greatly improved2@Ti3C2Purity and crystallinity, be more advantageous to To the catalytic degradation of pollutant.
The mass concentration of HF solution is 40~55% in step 1) of the present invention.Preferably, the matter of the HF solution Measuring concentration is 48~50%.
Mxene-Ti in step 2) of the present invention3C2, isopropylamine and water feed ratio be 1g:15~30ml:70~ 90ml.Preferably, the Mxene-Ti3C2, isopropylamine and water feed ratio be 1g:18~22ml:78~82ml.
The intercalation time is 16~20h in step 2) of the present invention.
The frequency being ultrasonically treated in step 3) of the present invention is 40~50Hz, and power is 80~100%, temperature when ultrasonic Degree is 5~12 DEG C, and the time is 2~4h.
Original position oxidation package includes in step 4) of the present invention: by the Ti of isopropylamine intercalation and layering3C2It is put into tubular type Muffle furnace In, temperature programmed oxidation reaction is carried out under Oxygen Condition, obtains TiO after the reaction was completed2@Ti3C2。
The rate that is passed through of oxygen of the present invention is 50~150 ml/mins.Preferably, the oxygen is passed through speed Rate is 90~110 ml/mins.
Temperature programming of the present invention is 3~6 DEG C/min of heating rate, and the temperature of holding is 300~400 DEG C, and the time is 1~3h.Preferably, the temperature kept is 350~370 DEG C.
The present invention also provides a kind of TiO being prepared such as above-mentioned method2@Ti3C2。
Compared with the existing technology, the beneficial effects of the present invention are embodied in:
(1) Mxene-Ti of isopropylamine intercalation and layering is prepared in the present invention using isopropylamine and ultrasonic wave added3C2, improve Mxene-Ti3C2Interlamellar spacing, for the TiO of generation2Provide more attachment sites.
(2) TiO can be greatly improved without adding any chemical agent using in-situ oxidation in the present invention2@Ti3C2's Purity and crystallinity are more advantageous to the catalytic degradation to pollutant.
Detailed description of the invention
Fig. 1 is to utilize isopropylamine intercalation and layering Ti3C2With blocky Mxene-Ti3C2XRD diagram；
Fig. 2 is the XRD diagram of powder prepared by comparative example 1~6；
Fig. 3 is the XRD partial enlarged view of powder prepared by comparative example 1~6；
Fig. 4 is the XRD diagram of the powder of Examples 1 to 6 preparation；
Fig. 5 is the XRD partial enlarged view of the powder of Examples 1 to 6 preparation；
Fig. 6 is bulk Mxene-Ti3C2FESEM figure；
Fig. 7 is the Ti of isopropylamine intercalation and layering3C2FESEM figure；
Fig. 8 is the FESEM figure of powder prepared by comparative example 1；
Fig. 9 is the FESEM figure of powder prepared by comparative example 2；
Figure 10 is the FESEM figure of powder prepared by comparative example 3；
Figure 11 is the FESEM figure of powder prepared by comparative example 4；
Figure 12 is the FESEM figure of powder prepared by comparative example 5；
Figure 13 is the FESEM figure of powder prepared by comparative example 6；
Figure 14 is the FESEM figure of powder prepared by embodiment 1；
Figure 15 is the FESEM figure of powder prepared by embodiment 2；
Figure 16 is the FESEM figure of powder prepared by embodiment 3；
Figure 17 is the FESEM figure of powder prepared by embodiment 4；
Figure 18 is the FESEM figure of powder prepared by embodiment 5；
Figure 19 is the FESEM figure of powder prepared by embodiment 6；
Figure 20 is degradation kinetics figure of the powder to methylene blue of the preparation of comparative example 1~6；
Figure 21 is degradation kinetics figure of the powder to methylene blue of Examples 1 to 6 preparation.
Specific embodiment
Below with reference to specific embodiment, present invention will be explained in further detail.
Embodiment 1
1)15g Ti3AlC2- MAX phase ceramics powder is slowly added into the HF solution that 300mL mass concentration is 49%, 36h is reacted under the conditions of 50 DEG C of oil bath in magnetic stirring apparatus；
2) acquired solution after reaction, is centrifuged 5min under the revolving speed of 3000rpm, pours out supernatant, and spend from Sub- water cleans sediment, and concussion is centrifuged again with the same terms after shaking up, is repeated 6 times.Measure the pH of last supernatant 5~6 it Between, then with dehydrated alcohol washing precipitate, be centrifuged after concussion, keep identical revolving speed and centrifugation time to be repeated twice, after centrifugation Acquired solution is filtered and is precipitated, gained is deposited under the conditions of 60 DEG C and is dried in vacuo for 24 hours, Mxene-Ti is obtained3C2Material；
3) Mxene-Ti for obtaining step 2)3C2Material, isopropylamine and deionized water are 1g:20ml according to feed ratio: 80ml mixing, magnetic agitation reacts 18h at room temperature, and centrifuge washing twice, obtains solid precipitating after the reaction was completed；
4) the solid precipitating that step 3) obtains is dissolved in 300ml deionized water, under protection of argon gas low temperature ultrasonic 3h, Temperature setting is 10 DEG C, frequency 45Hz, power 100%.After the completion of ultrasound, acquired solution is uniformly poured into the training of glass It supports in ware, is dried in vacuo 36h under the conditions of 60 DEG C, obtains the Ti of isopropylamine intercalation and layering3C2Material (iPA-Ti3C2)；
5) by the Ti of step 4) obtained isopropylamine intercalation and layering3C20.2g is weighed to be uniformly dispersed in inside quartz boat, The flow for being passed through oxygen is 100 ml/mins, and temperature program control is 25 DEG C of initial temperature, by adjusting heating-up time control Heating rate is 5 DEG C/min, and the temperature finally kept is 300 DEG C, continues 1h, after EP (end of program) by the way of natural cooling, Sample is taken out when temperature drops to room temperature, obtains TiO2@Ti3C2Material.
Embodiment 2
Process in preparation process reference implementation example 1, the difference is that, the temperature finally kept in step 5) is 320 DEG C, continue 1h and takes out sample after EP (end of program) by the way of natural cooling when temperature drops to room temperature, obtain TiO2@Ti3C2 Material.
Embodiment 3
Process in preparation process reference implementation example 1, the difference is that, the temperature finally kept in step 5) is 340 DEG C, continue 1h and takes out sample after EP (end of program) by the way of natural cooling when temperature drops to room temperature, obtain TiO2@Ti3C2 Material.
Embodiment 4
Process in preparation process reference implementation example 1, the difference is that, the temperature finally kept in step 5) is 360 DEG C, continue 1h and takes out sample after EP (end of program) by the way of natural cooling when temperature drops to room temperature, obtain TiO2@Ti3C2 Material.
Embodiment 5
Process in preparation process reference implementation example 1, the difference is that, the temperature finally kept in step 5) is 380 DEG C, continue 1h and takes out sample after EP (end of program) by the way of natural cooling when temperature drops to room temperature, obtain TiO2@Ti3C2 Material.
Embodiment 6
Process in preparation process reference implementation example 1, the difference is that, the temperature finally kept in step 5) is 400 DEG C, continue 1h and takes out sample after EP (end of program) by the way of natural cooling when temperature drops to room temperature, obtain TiO2@Ti3C2 Material.
Comparative example 1
1)15g Ti3AlC2- MAX phase ceramics powder is slowly added into the HF solution that 300mL mass concentration is 49%, 36h is reacted under the conditions of 50 DEG C of oil bath in magnetic stirring apparatus；
2) acquired solution after reaction, is centrifuged 5min under the revolving speed of 3000rpm, pours out supernatant, and spend from Sub- water cleans sediment, and concussion is centrifuged again with the same terms after shaking up, is repeated 6 times.Measure the pH of last supernatant 5~6 it Between, then with dehydrated alcohol washing precipitate, be centrifuged after concussion, keep identical revolving speed and centrifugation time to be repeated twice, after centrifugation Acquired solution is filtered and is precipitated, gained is deposited under the conditions of 60 DEG C and is dried in vacuo for 24 hours, Mxene-Ti is obtained3C2Material；
3) the blocky Mxene-Ti for obtaining step 2)3C2It weighs 0.2g to be uniformly dispersed in inside quartz boat, is passed through oxygen Flow be 100 ml/mins, temperature program control be 25 DEG C of initial temperature, pass through adjust the heating-up time control heating rate It is 5 DEG C/min, the temperature finally kept is 300 DEG C, continues 1h, after EP (end of program) by the way of natural cooling, is dropped to temperature Sample is taken out when to room temperature, obtains TiO2@Ti3C2Material.
Comparative example 2
Preparation process refers to the process in comparative example 1, the difference is that, the temperature finally kept in step 3) is 320 DEG C, continue 1h.
Comparative example 3
Preparation process refers to the process in comparative example 1, the difference is that, the temperature finally kept in step 3) is 340 DEG C, continue 1h.
Comparative example 4
Preparation process refers to the process in comparative example 1, the difference is that, the temperature finally kept in step 3) is 360 DEG C, continue 1h.
Comparative example 5
Preparation process refers to the process in comparative example 1, the difference is that, the temperature finally kept in step 3) is 380 DEG C, continue 1h.
Comparative example 6
Preparation process refers to the process in comparative example 1, the difference is that, the temperature finally kept in step 3) is 400 DEG C, continue 1h.
Characterization experiment
(1) XRD characterization is carried out for embodiment and comparative example
It is respectively as follows: the Ti that isopropylamine (iPA) intercalation and layering are utilized in embodiment 4 as shown in Figure 13C2, in comparative example 4 not The blocky Mxene-Ti of intercalation and layering3C2。
Know the Ti using isopropylamine intercalation and layering3C2, the corresponding angle in the position of main peak becomes smaller, after illustrating layering Ti3C2Interlamellar spacing becomes larger, and the comparison of interlamellar spacing and lattice constant parameter is as shown in table 1:
The comparison of the interlamellar spacing and lattice constant parameter of 4 intermediate product of table 1, embodiment 4 and comparative example
As shown in Fig. 2, comparing Ti3C2(blocky Mxene-Ti prepared by comparative example 43C2), anatase TiO2, rutile TiO2 And the XRD diagram of the material powder of the preparation of comparative example 1~6, it is known that with the rising of temperature, the content of titanium dioxide increases in sample Add, Ti3C2Content reduce, after temperature is higher than 360 DEG C, anatase and rutile generate simultaneously, and temperature is higher, generate golden Red stone increases.
As shown in enlarged drawing Fig. 3, when more than 360 DEG C, Ti3C2Peak all disappears, and illustrates there was only titanium dioxide in powder at this time In the presence of.
As shown in figure 4, comparing the Ti of isopropylamine layering and intercalation3C2It, can with the XRD diagram of the powder of Examples 1 to 6 preparation Know in selected temperature range, only generates anatase, there is no rutile generations.
By the amplification graph discovery of Fig. 5, in selected temperature range, there is also Ti3C2Peak, illustrate Ti at this time3C2With two Titanium oxide coexists.
It summarizes, utilizes the Ti of isopropylamine intercalation and layering3C2Than blocky Mxene-Ti3C2With bigger interlamellar spacing, simultaneously To Ti3C2Structure also produce change.The Ti of isopropylamine layering and intercalation3C2Only anatase generates in selected temperature range. And bulk Mxene-Ti3C2When more than 360 DEG C, anatase and rutile generate simultaneously, Ti3C2Peak has but all disappeared, only Titanium dioxide exists.
(2) FESEM characterization is carried out for embodiment and comparative example
As shown in figs. 6-7, bulk Mxene-Ti is shown in Fig. 6 (4 intermediate product of comparative example)3C2Interlamellar spacing is smaller and layer Number is more；Display isopropylamine intercalation and layering Ti in Fig. 7 (4 intermediate product of embodiment)3C2There is part curling, the number of plies is reduced.
As depicted in figures 8-13, bulk Ti is shown in Fig. 8 (1 product of comparative example)3C2Under the conditions of 300 DEG C almost not how by Oxidation, layer structure are obvious；In Fig. 9 (2 product of comparative example) under the conditions of 320 DEG C of display, there is a small amount of titanium dioxide to generate；Figure 10 It is shown under the conditions of 340 DEG C in (3 product of comparative example), in Ti3C2Surface has apparent titanium dioxide to generate；Figure 11 (comparative example 4 Product) in be shown under the conditions of 360 DEG C, Ti3C2Surface is nearly all titanium dioxide, and layer structure is not apparent；Figure 12 is (right 5 product of ratio) displays temperature is when being raised to 380 DEG C, Ti3C2Layer structure destroy completely, and the diameter of titanium dioxide granule Obviously become larger, discovery has rutile generation；Figure 13 (6 product of comparative example) is shown under the conditions of 400 DEG C, and titanium dioxide granule is into one Step becomes larger.
As shown in Figure 14~19, the display Ti of isopropylamine intercalation and layering in Figure 14 (1 product of embodiment)3C2At 300 DEG C Under the conditions of oxidation there is a small amount of titanium dioxide to generate, Ti3C2Layer structure is still obvious；It is shown in Figure 15 (2 product of embodiment) Under the conditions of 320 DEG C, content of titanium dioxide is greatly increased, Ti3C2Layer structure is unobvious；It is shown in Figure 16 (3 product of embodiment) Under the conditions of 340 DEG C, temperature rises, and titanium dioxide granule becomes larger；It is shown under the conditions of 360 DEG C in Figure 17 (4 product of embodiment), two Titanium oxide content continues growing, but Ti3C2Layer structure still exists；380 DEG C of items are shown in Figure 18 (5 product of embodiment) Ti under part3C2Layer structure slowly disappears；Ti is shown in Figure 19 (6 product of embodiment)3C2Layer structure has completely disappeared.
(3) the photo-catalysis capability test of methylene blue is carried out for embodiment and comparative example
10mg catalyst, the magnetic force under dark condition is added into the methylene blue solution that 50ml concentration is 20 mg/litres 1h is stirred, adsorption equilibrium is reached, then opens light source (ultraviolet lamp, power 500w, the optical filter containing 365nm), every 10 points Clock takes a sample, and supernatant methylene blue concentration is surveyed after centrifugation, draws kinetics of photocatalytic degradation curve.
As shown in figure 20, the product that prepared by comparative example 1~6 carries out the photo-catalysis capability test of methylene blue, for block Shape Mxene-Ti3C2The TiO of synthesis2@Ti3C2, with the rising of temperature, TiO2@Ti3C2Catalytic capability present inverted " V " type, Catalytic effect is best at 360 DEG C.
As shown in figure 21, the product of Examples 1 to 6 preparation carries out the photo-catalysis capability test of methylene blue, utilizes isopropyl The Ti of amine layering3C2The TiO of synthesis2@Ti3C2, with the rising of temperature, TiO2@Ti3C2Catalytic capability first rise, it is rear to decline, At 360 DEG C, catalytic effect is best.

Claims (8)

1.一种利用异丙胺插层和分层的Ti3C2原位合成TiO2@Ti3C2的方法，其特征在于，包括如下步骤：A method for in situ synthesis of TiO 2 @Ti 3 C 2 by using isopropylamine intercalation and layering of Ti 3 C 2 , characterized in that it comprises the following steps: 1)将Ti3AlC2-MAX相陶瓷粉末分散在HF溶液中进行刻蚀，得到Mxene-Ti3C2；1) Dispersing Ti 3 AlC 2 -MAX phase ceramic powder in HF solution for etching to obtain Mxene-Ti 3 C 2 ; 2)将Mxene-Ti3C2分散在异丙胺与水的混合溶液中进行异丙胺插层，得到异丙胺插层的Ti3C2；2) Dispersing Mxene-Ti 3 C 2 in a mixed solution of isopropylamine and water to intercalate with isopropylamine to obtain Ti 3 C 2 intercalated with isopropylamine; 3)将异丙胺插层的Ti3C2分散在水中，在氩气气氛下超声处理，干燥后得到异丙胺插层和分层的Ti3C2；3) dispersing Ti 3 C 2 intercalated with isopropylamine in water, sonicating under an argon atmosphere, and drying to obtain isopropylamine intercalation and layered Ti 3 C 2 ; 4)异丙胺插层和分层的Ti3C2在氧气条件下进行原位氧化，即得TiO2@Ti3C2。4) The isopropylamine intercalation and the layered Ti 3 C 2 are oxidized in situ under oxygen to obtain TiO 2 @Ti 3 C 2 . 2.根据权利要求1所述的利用异丙胺插层和分层的Ti3C2原位合成TiO2@Ti3C2的方法，其特征在于，所述步骤1)中HF溶液的质量浓度为40～55％。The method for in-situ synthesis of TiO 2 @Ti 3 C 2 by using isopropylamine intercalation and layered Ti 3 C 2 according to claim 1, characterized in that the mass concentration of the HF solution in the step 1) It is 40 to 55%. 3.根据权利要求1所述的利用异丙胺插层和分层的Ti3C2原位合成TiO2@Ti3C2的方法，其特征在于，所述步骤2)中Mxene-Ti3C2、异丙胺与水的投料比为1g:15～30ml:70～90ml。The method for in-situ synthesis of TiO 2 @Ti 3 C 2 by using isopropylamine intercalation and layered Ti 3 C 2 according to claim 1, wherein the step 2) is Mxene-Ti 3 C 2 , the ratio of isopropylamine and water is 1g: 15 ~ 30ml: 70 ~ 90ml. 4.根据权利要求1所述的利用异丙胺插层和分层的Ti3C2原位合成TiO2@Ti3C2的方法，其特征在于，所述步骤3)中超声处理的频率为40～50Hz，功率为80～100％，超声时的温度为5～12℃，时间为2～4h。The method for in-situ synthesis of TiO 2 @Ti 3 C 2 by using isopropylamine intercalation and layered Ti 3 C 2 according to claim 1, wherein the frequency of the ultrasonic treatment in the step 3) is 40 to 50 Hz, the power is 80 to 100%, the temperature at the time of ultrasound is 5 to 12 ° C, and the time is 2 to 4 hours. 5.根据权利要求1所述的利用异丙胺插层和分层的Ti3C2原位合成TiO2@Ti3C2的方法，其特征在于，所述步骤4)中原位氧化包括：将异丙胺插层和分层的Ti3C2放入管式马弗炉中，在氧气条件下进行程序升温氧化反应，反应完成后得TiO2@Ti3C2。The method for in-situ synthesis of TiO 2 @Ti 3 C 2 by using isopropylamine intercalation and layered Ti 3 C 2 according to claim 1, wherein the in-situ oxidation in the step 4) comprises: The isopropylamine intercalation and layered Ti 3 C 2 were placed in a tubular muffle furnace, and a temperature-programmed oxidation reaction was carried out under oxygen conditions, and TiO 2 @Ti 3 C 2 was obtained after completion of the reaction. 6.根据权利要求5所述的利用异丙胺插层和分层的Ti3C2原位合成TiO2@Ti3C2的方法，其特征在于，所述氧气的通入速率为50～150毫升/分钟。The method for in-situ synthesis of TiO 2 @Ti 3 C 2 by using isopropylamine intercalation and layered Ti 3 C 2 according to claim 5, wherein the oxygen gas permeation rate is 50-150. ML/min. 7.根据权利要求5所述的利用异丙胺插层和分层的Ti3C2原位合成TiO2@Ti3C2的方法，其特征在于，所述程序升温为升温速率3～6℃/分钟，保持的温度为300～400℃，时间为1～3h。The method for in-situ synthesis of TiO 2 @Ti 3 C 2 by using isopropylamine intercalation and layered Ti 3 C 2 according to claim 5, wherein the temperature is increased to a temperature rising rate of 3 to 6 ° C. /min, the temperature maintained is 300 to 400 ° C, and the time is 1 to 3 h. 8.一种如权利要求1～7任一所述的方法制备得到的TiO2@Ti3C2。8. TiO 2 @Ti 3 C 2 prepared by the method according to any one of claims 1 to 7.
CN201811051653.7A 2018-09-10 2018-09-10 Utilize the Ti of isopropylamine intercalation and layering3C2Fabricated in situ TiO2@Ti3C2Method and product Withdrawn CN109261181A (en)

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CN112038601A (en) * 2020-08-31 2020-12-04 贝特瑞新材料集团股份有限公司 Negative electrode active material, its preparation method and use
CN112933958A (en) * 2021-02-10 2021-06-11 广西大学 Method for photocatalytic carbon dioxide reduction
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