Facile Synthesis of Iron-Titanate Nanocomposite as a Sustainable Material for Selective Amination of Substitued Nitro-Arenes
Round 1
Reviewer 1 Report
The authors presented a good work concerning the preparation of iron-titanium mixed oxides active in the reduction of nitroarenes.
The authors provide to improve the quality of TEM images evidencing the fringes measures.
The SEM images are redundant, please move it to supplementary.
The quality of XRD figure must be improved and the peaks must be marked in order to simplify the readers understanding.
Author Response
We thank reviewers for their valuable input and giving us a chance to submit a revised version. We have now addressed all the queries raised by the Reviewers and Editor. Following are our responses,
Reviewer 1
The authors presented a good work concerning the preparation of iron-titanium mixed oxides active in the reduction of nitroarenes.
Q1. The authors provide to improve the quality of TEM images evidencing the fringes measures.
Author response:
We have now included better resolution Figure for TEM and carried our IFFT analysis to better measure the inter-planar distances. Previous Figure is now replaced with the new one. (Figure 3, Page 7).
Q2. The SEM images are redundant, please move it to supplementary.
Author response:
We moved SEM to supplementary information and changed Figure numbering accordingly.
Q3. The quality of XRD figure must be improved and the peaks must be marked in order to simplify the readers understanding.
Author response:
We have clarified and labelled peaks in a better way in the XRD Figure. We also incorporated high quality figure now. (Figure 1, Page 5).
Author Response File: 
Author Response.pdf
Reviewer 2 Report
The paper reports Facile Synthesis of Iron-Titanate nanocomposite as a Sustainable Material for Selective Amination of Substitued nitro-arenes. The following comments and recommendations must be considered by the authors before publication this paper.
- Introduction
1.1 Sol-gel method has been chosen by the authors to prepare iron and titanium nanomaterial. I think that the authors should update the results (based iron -TiO2 prepared by sol-gel using for catalysis). Here are some examples: 10.1039/C9CY02292A, 10.1016/j.jcat.2019.05.008, 10.1002/anie.201911153
1.2 What is the speciality of Fe9Tio19@TiO2? Have it been reported by others studies?
- Results & Discussion
2.1 The section “2.1 synthesis “ could move into the section ‘3 experimental”.
2.2 In fig.1 “Fe9TiO15.TiO2” should be corrected as “Fe9TiO15@TiO2”. Please standardize this formula for all the texts.
2.3 The information provided by two SEM images in Fig. 2 are quite similar and a higher magnification is better for one image
2.4 Line 125-131, this paragraph has been presented in Line 118-124.
2.5 Line 159-160, “Along with this material, we also tested newly prepared Fe2O3 and TiO2 and found that these materials are not active.” Some detail of Fe2O3 and TiO2 such as the preparation method, the size, the crystal structure…
2.6 Line 160-161 , ‘This clearly indicates that either the Fe- or Ti-particles alone are not active (Table 1, entries 2 and 3)’ . I don’t agree with this purpose. For example, it was shown (10.1002/ange.201205792) that the use of hydrazine hydrate as a reducing reagent, combined with the rapid generation in situ of colloidal Fe3O4 nanocrystals with high catalytic activity.
Author Response
We thank reviewers for their valuable input and giving us a chance to submit a revised version. We have now addressed all the queries raised by the Reviewers and Editor. Following are our responses,
Reviewer 2
The paper reports Facile Synthesis of Iron-Titanate nanocomposite as a Sustainable Material for Selective Amination of Substitued nitro-arenes. The following comments and recommendations must be considered by the authors before publication this paper.
Introduction
Q.1 1.1 Sol-gel method has been chosen by the authors to prepare iron and titanium nanomaterial. I think that the authors should update the results (based iron -TiO2 prepared by sol-gel using for catalysis). Here are some examples: 10.1039/C9CY02292A, 10.1016/j.jcat.2019.05.008, 10.1002/anie.201911153
1.2 What is the speciality of Fe9Tio19@TiO2? Have it been reported by others studies?
Author response:
We thank reviewer for the above comment and suggesting us recent references. We have now added the references mentioned by the Reviewers. Synthesis of this material has been reported earlier as an intermediate phase but has never been separated. Further, first time we explored its utilization as a heterogeneous catalyst. No application of this material has been reported earlier.
Results & Discussion
Q2. 2.1 The section “2.1 synthesis “ could move into the section ‘3 experimental”.
Author response:
We have now merged this section in the experimental part.
Q.3 2.2 In fig.1 “Fe9TiO15.TiO2” should be corrected as “Fe9TiO15@TiO2”. Please standardize this formula for all the texts.
Author response:
We have now corrected the formula throughout the manuscript.
Q.4 2.3 The information provided by two SEM images in Fig. 2 are quite similar and a higher magnification is better for one image
Author response:
We have moved SEM images to supplementary data as suggested by Reviewer 1 also.
Q5. 2.4 Line 125-131, this paragraph has been presented in Line 118-124.
Author response:
Q6. 2.5 Line 159-160, “Along with this material, we also tested newly prepared Fe2O3 and TiO2 and found that these materials are not active.” Some detail of Fe2O3 and TiO2 such as the preparation method, the size, the crystal structure…
Author response:
All the materials prepared for comparative studies such as Fe2O3 and TiO2 were prepared by the same sol-gel method and their XRD are provided in the Figure 1. XRD data shows change in crystallite sizes but at this stage we don’t have their TEM data.
Q7. 2.6 Line 160-161 , ‘This clearly indicates that either the Fe- or Ti-particles alone are not active (Table 1, entries 2 and 3)’ . I don’t agree with this purpose. For example, it was shown (10.1002/ange.201205792) that the use of hydrazine hydrate as a reducing reagent, combined with the rapid generation in situ of colloidal Fe3O4 nanocrystals with high catalytic activity.
Author response:
Fe3O4 nanocrystals are active, but in our method we got Fe2O3 nanostructures. Fe2O3 nanostructures might be active too but in our system either Fe2O3 is less active or has negligible activity in the conditions Fe9TiO15@TiO2 is active.
Author Response File: Author Response.pdf
Round 2
Reviewer 2 Report
it could be accepted as all the suggestions were considered.
