Synthetic Routes to Crystalline Complex Metal Alkyl Carbonates and Hydroxycarbonates via Sol–Gel Chemistry—Perspectives for Advanced Materials in Catalysis

Round 1

Reviewer 1 Report

The article can be published in the present form

Author Response

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Author Response File: Author Response.pdf

Reviewer 2 Report

Hanf, Schunk and coworkers revealed a novel synthetic route using metal alkoxides as single-source precursors for layered inorganic functional materials. It is interesting to me that when using such metal alkoxides precursors can influence the catalytic properties of the final material after hydrolysis. Further the size, shape and composition of some of the materials can be adjusted in various ways. Of course this manuscript was well-written and well-developed. Thus, I think this work is worthy of publication in Catalysts after the minor revisions, and the comments are attached.

1. When chemically defined crystalline carbonates and hydroxycarbonates were formed, 20 times of water washing was required. Could the use of increasing the amount of water and reducing the number of water washes proceed smoothly?
2. Metal alkyl carbonates could be used as catalyst precursors for the synthesis of methanol from CO/CO₂ and H₂. Is there a mechanism for this and how does the catalytic action take place?
3. Some chemical formula writing specifications require attention, for example, the last paragraph on page 15, where the 2 and 3 in Al₂O₃ need to be subscripted. There are also many minor problems with writing, for example, the writing of H₂ As well as deleting the second sentence on page 13, the redundant Figure 12.
4. The content in Figure 14 looks very blurry, can you provide a clearer analysis of the graph? At the same time, the explanation of this part was not thorough and I did not understand it.

Author Response

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Author Response File: Author Response.pdf

Reviewer 3 Report

The article 'Synthetic routes to crystalline complex metal alkyl carbonates and hydroxycarbonates via sol-gel chemistry – perspectives for advanced materials in catalysis' is devoted to the study of the reacion of metal alkoxides with CO₂, followed by hydrolysis, on examples of the syntheses of hydrotalcite Mg₆Al₂CO₃(OH)₁₆·4H₂O and Cu/ZnO/Al₂O₃ phases. However, in the present form the manuscript cannot be accepted, the text should be reorganized and rewritten.

The introductory part of the Abstract seems wordy, significant results are missed (e.g. solubilization strategies for metal alkoxide precursors, the synthesis of hydrotalcite).

In the Introduction, the authors cite and show Table 1 (weird classification, it's all mixed up) and cover many issues irrelevant to the subject of the study ('Ziegler-Alfol' process, DFT modeling of CO₂ insertion etc). The objectives of the investigation are unclear. I recommend to shorten and concretize this section, and remove the Table 1.

The title of the Section 2.2 is bad, the Section is wordy. The chemical equation for the synthesis of hydrotalcite is needed, the role of carbonate is missed in Fig. 7. The Table 3 contains photos of the reaction mixtures but it's not clear which was the reason for the choice of the photos presented and why other photos were missed. The caption under Fig. 7 does not contain information about the chemical nature of the crystalline compound under study. 'Cu/ZnO/Al₂O₃' catalyst is mentioned in the text, why not CuO?

Section 4.2 don't have any proof of the composition of metal alkoxides and Cu/ZnO/Al₂O₃ phases. Section 4.3 (Catalyst testing) does not contain any useful information and must be completely rewritten. In general, in the present form Materials and Methods section is not acceptable.

Conclusion section also contains a lot of words without short and clear formulation of the problem, methods and results.

The article prepared in sloppy manner, the text needs editing. Taking into account the overall assessment, detailed analysis of the manuscript makes no sense.

Author Response

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Author Response File: Author Response.pdf

Round 2

Reviewer 3 Report

The authors had taken into account all comments and have made the necessary changes in the manuscript.

Please correct technical error (line 78). 

Author Response

Dir Sir or Madam,

the required change is made in the manuscript.

Kind regards

Schirin Hanf