Synthesis of Silicon Hybrid Phenolic Resins with High Si-Content and Nanoscale Phase Separation Structure

Round 1

Reviewer 1 Report

After minor revision the present contribution can be published in the journal “Processes”.

• Whole paper: Check the whole paper carefully if there are redundant spaces which must be deleted. Insert spaces where necessary (for example between numerical value and unit, etc.).
• The arrangement between text and figures/tables has to be optimized (see page 2, 6 and 7).
• Figure captions must be on the same page than the figures (see Figure 2, Figure 8 and Figure 14).
• The y-axis of Figure 1 should be reformatted in a logarithmic scale because the phase domain length spans three orders of magnitude.
• Line 136 “Φ 30 ×10 mm”. Not clear, maybe: “approximately 30 mm ×10 mm”.
• Line 157 “reaction33”: What is the meaning of “33”?
• Line 158 “Mn and Mw”: Define “Mn” and “Mw” in detail. “n” and “w” subscript (also in Figure 3).
• Line 174 “Fig. 1s”: Maybe “Fig. 2“?
• Line 195-197 “94 m/z” ... “304 m/z”: What does it mean?
• Figure 6: The letters in the left picture are much too small.
• Page 10: Define “I”.
• Line 251: Replace “Fig. 11” with “Figure 11.”.
• Table 1: Replace “AIR” with “Air”.
• Line 317/318 “The maximum intensity of volatilized CO2 for PF was about 27.53, and that for SPF-4 decreased to 10.59.”: Not clear. What’s about the unit (see also Figure 16).
• Figure 16: The picture are too small.
• Page 15: Replace “Fig. 17ab”, “Fig. 17cd” and “Fig. 17 ef” with “Fig. 17a,b”, “Fig. 17c,d” and “Fig. 17 e,f”.
• Line 361: Replace “table 3” with “Table 3”.
• Table 3: Check the units. Maybe “kw” must be replaced with “kW”. Define “TTI” and “MLR”.
• Line 387/388: Line spacing.
• Check the references carefully. They must be according to the instructions to the authors.

Author Response

your comments are all valuable and very helpful for revising and improving our paper. We have studied comments carefully and have made correction which we hope meet with approval. Revised portion are marked in the paper. The main corrections in the paper and the responds to the reviewer’s comments are as flowing:

Responds to your comments:

1. We have optimized the arrangement between text and figures/table
2. Thanks for your advice, the y-axis of Figure 1 have been reformatted in a logarithmic scale.
3. Line 139 “Φ 30 ×10 mm” were corrected as “approximately Φ 30 mm (diameter) ×10 mm (thickness)”.
4. Response to comment: Line 159 “reaction33”: What is the meaning of “33”?

  Response: 33 are the number of the reference.

5. Line 161 “Mn and Mw” were corrected and “M_n” and “M_w” was defined in detail. (also in Figure 3)
6. Line 178 “Fig. 1s” was shown in supplementary information.
7. Line 195-197 “94 m/z” ... “304 m/z” mean ion fragment peaks.
8. Figure 6 and Figure 16 have been corrected.
9. Line 227 “I” was scattering intensity”.
10. Line 260: “Fig. 11” has been replaced with “Figure 11.”.
11. Table 1: “AIR” has been replaced with “Air”.
12. Line 326/327 “The maximum absorption intensity of volatilized CO₂ for PF was about 27.53, and that for SPF-4 decreased to 10.59.” Absorption strength commonly has no unit in IR spectra.
13. Page 15: “Fig. 17ab”, “Fig. 17cd”, “Fig. 17 ef” and table 3 (Line 373) were corrected.
14. Table 3: MLR was mass loss rate and TTI was time to ignition, and they have been corrected in the manuscript.

    Special thanks to you for your good comments and we are sorry for our carelessness.

We appreciate for your warm work earnestly, and hope that the correction will meet with approval.

Reviewer 2 Report

Manuscript entitled “Synthesis of silicon hybrid phenolic resins with high Si-content and nanoscale phase separation structure” by W. Yuan, F. Chen, S. Li, Y. Du, Z. Luo, Y. Sun, H. Li and T. Zhao.

In this work silicone hybrid phenolic resin, with potential application in ablative materials, was prepared by mixing phenolic and self-synthesized silicone resin. Firstly, high silicone content silicone resins with different molecular structure were prepared controlling the hydrolytic polymerization of polysiloxane, by using ethanol as inhibitor. In a second step, the silicone resins were mixed with phenolic resin. The hybrid resin obtained using 400% ethanol by weight of siloxane (sample SPF-4) presented nanoscale phase separation, as proved by SAXS. The structure of the hybrids was confirmed by FTIR and Nuclear Magnetic Resonance. It was observed an increase in thermal stability (TGA measurement under nitrogen) and oxidation resistance of SPF-4 compared with phenolic resin. In addition, it was found an improvement in flame resistance and ablative property given by the compact Si-rich layer formed because of the high Si content and nanoscale phase structure.

In my opinion, the manuscript is well written and presented. The experimental results are clearly explained and the results support the conclusions. Therefore, I think that the paper is worthy for publication as it is.

Author Response

Thank you for your nice comments on our article.