Preparation of Bis[(3-ethyl-3-methoxyoxetane)propyl]diphenylsilane and Investigation of Its Cationic UV-Curing Material Properties

Round 1

Reviewer 1 Report

In this work by Liu and co-workers, the authors prepared certain chemical compounds, which they used for UV-facilitated polymerization. The results are in line with the aims and scope of the journal, but the paper contains several issues, which must be tackled before it could be recommended for publication. Please find the suggestions below:
1) The abstract is repetitive and does not represent well the content of the article. Please improve it. 
2) The state of the art is not described with a sufficient level of detail. Some findings are supported with numerous references* while the important works of others in the area of this manuscript are disregarded. Please balance the introduction. 
* Example: "The advantages of cationic photopolymerization is wear resistance, high hardness ,small volume shrinkage, strong adhesion, and it does not exhibit oxygen inhibition like radical-based systems[17-23]"
3) Importantly, the "in this work" section of the introduction lacks statements regarding the novelty factor of this contribution. The authors should clearly say what is new in this work that was not done by others before to enable readers to quickly judge the impact of this contribution.
4) The experimental part is mixed up with results. Please exclude the information regarding the synthesis from this section. 
5) Characterization parameters are not given. 
6) Features should be denoted in the FTIR spectrum in Figs. 3, 5, and 8. 
7) Formatting of the article is poor. Please unify the size of the plots and remove the redundant empty space. 
8) The most serious shortcoming is the lack of statistics, which puts in doubt if the presented results are statistically significant.
9) Conclusions should be extended and more research insight in the form of interpretation and hypotheses should be included in the text. 

Author Response

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Author Response File: Author Response.docx

Reviewer 2 Report

First of all, the manuscript needs a complete review in terms of writing, because there are many typos that make it seem unfinished. Thus, there are many words pasted, doubled words, punctuation marks are distant from words, and there are unfinished phrases, such as for example, in Introduction section, lines 39-40: “In this paper, This experiment intended to improve the photosensitivity of a kind of oxetane by adding silico-benzene compounds”. English must also be revised, so authors should contact a native speaker or a professional.

The FT-IR spectra presented in Figures 2, 4 and 6 have rather poor quality, so figures with improved quality should be provided by the authors. In order to make these figures easier to read, the characteristic bands discussed in the text should be marked on the FT-IR graphs. The standard spectrum of these compounds should also be superimposed in order to better highlight the band concordances.

The quality of Figures 3, 5 and 7 is also poor ad should be improved by the authors. In this case, the characteristic peaks should be also marked on the graphs for easier understanding.

In fact, all the figures have poor quality and should be replaced with some with better resolution.

After reading the manuscript carefully, my impression is that the experimental data are presented descriptively, without being discussed or compared. In addition, 3 different materials are synthesized, but the manuscript does not clearly understand the purpose of these syntheses. The authors must explain in detail what each synthesized compound is used for. What is the role of these compounds in the study?

In my opinion, the manuscript must be completely reorganized, and the experimental data fully exploited through complete and critical discussions. What is the novelty and originality of the study? This aspect is not highlighted by the authors.

In this form the study cannot be recommended for publication in the journal Polymers being a routine study.

Author Response

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Author Response File: Author Response.docx

Reviewer 3 Report

The authors present an interesting report on a synthesis route for a UV-curable oxetane silane compound, the characterization of the product and a few tested parameters for the cured film. Overall, the article is interesting for UV-curable coatings and the results are well supporting the drawn conclusions. In order to provide complete details, the authors should still add the purity of the used materials in sect. 2.1.

Author Response

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Author Response File: Author Response.docx

Reviewer 4 Report

Dear Editor and Authors,

 

After reviewing the manuscript submitted for review, I recommend publication with minor changes not requiring reviewer approval. 

 

Please pay attention to the formatting of the chemical formulas. The quality and style of the chemical structures drawn should be improved. Additionally, please indicate:

• How did the authors determine monomer conversion by the photo-DSC method and the theoretical heat for complete conversion?

 

 

Author Response

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Author Response File: Author Response.docx

Round 2

Reviewer 1 Report

The authors addressed the concerns raised. 

Author Response

Thank you for reviewing our manuscript, and thank you for your valuable comments.

Reviewer 2 Report

The quality of the manuscript has been improved from all points of view: scientific content, quality of figures, and cited literature.
The authors responded to all the observations made and modified/completed/corrected the corresponding data in the manuscript.

In this form, the manuscript may be recommended for publication in the  Polymers journal.

Author Response

Thank you for reviewing our manuscript, and thank you for your valuable comments.

Reviewer 3 Report

The manuscript was improved by the authors as suggested in previous reviews and is suitable now for publishing.

Author Response

Thank you for reviewing our manuscript, and thank you for your valuable comments.

This manuscript is a resubmission of an earlier submission. The following is a list of the peer review reports and author responses from that submission.

Round 1

Reviewer 1 Report

I have reviewed a manuscript entitled “Preparation of bis[(3-ethyl-3-methoxyoxetane)propyl]diphenylsilane and investigation of its cationic UV-curing material properties”. they successfully synthesized a UV-curing product and characterized it in terms of mechanical properties. I think this work can be published after addressing the following comments:

• Please have a separate paragraph at the end of the introduction about the aim of the work.
• Please add details about the source of chemicals.
• Figure 1 is too simple with no useful info. please add more details about the steps of experiments or the mechanism of the reaction.
• Please add an error bar to your figures!
• Please merge figures 2, 3, and 4.
• Please merge figures 7, 8, and 9.
• Please merge figure 5.1. and 5.2.
• What is the significance of this product compared to the previously developed product?

Reviewer 2 Report

Dear Editor and Authors,

In the manuscript received for review, the authors, try to explicitly demonstrate the relationship between influencing factors, the yield of reaction between 3-ethyl-3-al-8lylmethoxyoxetane and diphenylsilane. The authors' work is contained in 11 manuscript pages. The manuscript is not well prepared in terms of its component parts moreover lacks adequate text editing to give an additional good impression of the diligence of the research carried out.

Main concerns for the Authors:

1) Please indicate the manufacturers for the materials described and the purity of the compounds. (for example in the section materials: Toluene, cationic photoinitiator (UV-6976, namely triarylsulfonium hexafluoroantimonate), diphenylsilane, 3-ethyl-3-allylmethoxyoxetane, tris(triphenylphosphine) rhodium chloride) .

2) All chemical formulas included in the manuscript need improvement. Please use proper formatting; as it stands, the formulas are drawn incorrectly.

3) All FT-IR plots included in the manuscript need to be described, and if specific bands on the FT-IR spectra are compared, then the spectra should be normalized so that the change in band intensity can be discussed. 

5) Functional group conversions should be calculated from the photo-DSC experiments. All curves should be overlaid on one plot. Data related to the analysis of DSC waveforms should be tabulated (maximum heat, conversion, tmax, Hmax, induction time, etc.).

6) Indicate how the yield of the synthesis was calculated.  How was the yield calculated from the HNMR analysis? 

7) What conditions during photopolymerization were used? 
What were sample sizes tested? Was an inert gas used? 
What was the distance of the light source from the sample surface? 

8) Is the intensity of the light the intensity at the sample surface or the intensity of the light source? (photo-DSC experiments)

The above comments do not detract in any way from the authors' work but merely show an additional way to complete and improve their manuscript. 

I, therefore, ask the Editor to reject the manuscript (additional experiments are needed to improve the quality of the presented manuscript).