Influence of Concentration of Thiol-Substituted Poly(dimethylsiloxane)s on the Properties, Phases, and Swelling Behaviors of Their Crosslinked Disulfides
Round 1
Reviewer 1 Report
The authors present an interesting work in which they study the crosslinking of compounds based on thiolated poly(dimethylsiloxane) copolymers, with a comprehensive characterization and clearly analysing the most important results.
Although the manuscript is generally of acceptable quality for publication in Macromol, there is a reason why I suggest an additional review: the Supplementary Material is not attached to the manuscript, so the various references implying it can not be checked (at least, I could not access to it).
In the event that it was a platform error, and the SM could be revised for the other reviewers, I only have a few minor considerations for the manuscript:
1. Section 2.2: the characterization of the samples is set out in detail (which is a plus), but the preparation of the experiments is not detailed. In case it was in the SM, this part could be moved to the manuscript, or include a short summary with a scheme of the process.
2. Some of the information at the bottom of Figure 1 could be indicated in the text.
3. There seems to be a visual problem with the borders of table 3.
Author Response
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Author Response File: 
Author Response.docx
Reviewer 2 Report
The current work is a very high added value with many data reported in a systematic manner. I enjoyed reading the work. Below some minor suggestions.
Addition or removal of electrons. Please explain more in detail as there needs to be a general mechanism.
Ref 28 please highlight that with the longer building block intramolecular reactions for Si-O-Si formation are hampered making structure more flexible. The main reference for this is Nat. Mater. 2021 20, 1422. (later on intrachain and interchain are used as term)
L 116 the two series: suggestion to make an extra figure (or add it in Figure 1). Note Figure 1 should be placed higher.
Molecular weight should be mass average molecular weight or even better mass average molar mass
It should be stressed that the method of Figure 7 is very qualitative. More accurate is the complementary use of flattening yield data and e.g. solid state NMR data (if possible to obtain
Author Response
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Author Response File: Author Response.docx
Reviewer 3 Report
The work entitled: "Influence of Concentration of Thiol-Substituted Poly(dimethylsiloxane)s on the Properties, Phases, and Swelling Behaviors of Their Crosslinked Disulfides" is a very interesting and nicely written work that deals with the crosslinking of PDMS based polymers that are containing thiol functional groups. The use of I2 is mentioned for the crosslinking while extensive characterization of the materials is done. I can suggest the manuscript for publication after minor clarifications on the following points:
- It would be nice to have the opportunity to monitor the crosslinking process via the dynamic moduli. Was it possible to perform rheological measurements with in-situ monitoring of the crosslinking process?
-What is the mean crosslink molecular weight estimation based on the dynamic moduli?
- There are a few typos that need to be corrected (e.g., 1H instead of 1H). Please check once again. There are only a few.
Author Response
see attachment
Author Response File: Author Response.docx
Round 2
Reviewer 1 Report
After reviewing the SI file, I can say that the manuscript is completed, and can be accepted.
