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Peer-Review Record

Selective Carbon Enrichment from Micro/Nano Silicon–Carbon Ores via Sodium Hexametaphosphate: Mechanistic Insights and Structural Characterization

Minerals 2025, 15(4), 329; https://doi.org/10.3390/min15040329
by Xi Xu 1, Gaoxiang Du 1,2,*, Xianguang Wang 3, Jiao Wang 4, Huan Shuai 1 and Shujin Shi 1
Reviewer 1: Anonymous
Reviewer 2: Anonymous
Minerals 2025, 15(4), 329; https://doi.org/10.3390/min15040329
Submission received: 12 February 2025 / Revised: 17 March 2025 / Accepted: 19 March 2025 / Published: 21 March 2025
(This article belongs to the Section Clays and Engineered Mineral Materials)

Round 1

Reviewer 1 Report

Comments and Suggestions for Authors

This manuscript has to be improved in the following aspects before possible publication.

  1. The introduction of this manuscript has to be improved.
  2. Proper citations are recommended for section ‘Introduction’.
  3. The highlights of this manuscript should be described clearly.
  4. A detailed section 2.2 is recommended.
  5. The formula in section 2.3 needs a more detailed description.
  6. The sentence in line 149-150 should be revised.
  7. 2 (b) can be removed.
  8. Section 4 should be rewritten to give a concise conclusion.
Comments on the Quality of English Language

Some English writing in this manuscript can be improved.

Author Response

Reviewer #1:

Reviewer Comments and Suggestions for Authors:

Comments and Suggestions for Authors

This manuscript has to be improved in the following aspects before possible publication.

  1. The introduction of this manuscript has to be improved.
  2. Proper citations are recommended for section ‘Introduction’.
  3. The highlights of this manuscript should be described clearly.
  4. A detailed section 2.2 is recommended.
  5. The formula in section 2.3 needs a more detailed description.
  6. The sentence in line 149-150 should be revised.
  7. 2 (b) can be removed.
  8. Section 4 should be rewritten to give a concise conclusion.

Comments on the Quality of English Language.

Some English writing in this manuscript can be improved.

(R1Q1) The introduction of this manuscript has to be improved.

>>AUTHORS’ REPLY:

Thanks for your valuable feedback. We are fully aware that the introduction section indeed requires improvement. We have made revisions and added a comprehensive literature review (Line33-87).

 

(R1Q2) Proper citations are recommended for section ‘Introduction’

>>AUTHORS’ REPLY:

We sincerely appreciate your meticulous review and valuable feedback. We have added appropriate citations of relevant literature in the introduction section (Line33-87).

 

(R1Q3) The highlights of this manuscript should be described clearly.

>>AUTHORS’ REPLY:

Thanks for your valuable feedback. Upon reviewing the manuscript, we are aware that the highlights of this article are indeed not very prominent. The highlights of this article mainly include the following points. Firstly, the effective separation of quartz and carbonaceous matter in silicon-carbon ores was achieved through physical methods, and the mechanism of sodium hexametaphosphate (SHMP) in the separation process was deeply explored. In addition, the structure and types of carbonaceous matter in silicon-carbon ores were characterized by infrared spectroscopy, Raman spectroscopy and transmission electron microscopy (TEM), and the pore structure characteristics of carbonaceous matter were studied in detail by BET analysis (Line23-31).

 

(R1Q4) A detailed section 2.2 is recommended.

>>AUTHORS’ REPLY:

Thanks for your valuable feedback. We have thoroughly revised section 2.2 to ensure it is detailed, comprehensive, and clearly articulated. The specific revision details have been clearly marked in the submitted manuscript (Line 99-130).

 

(R1Q5) The formula in section 2.3 needs a more detailed description.

>>AUTHORS’ REPLY:

Thanks for your valuable suggestions. In response, we have already provided explanations for the formulas in section 2.3 in the submitted manuscript (Line152-153).

 

(R1Q6) The sentence in line 149-150 should be revised.

>>AUTHORS’ REPLY:

Thanks for your valuable suggestions. We have revised the sentence in the manuscript to ensure its smooth expression and logical consistency with the context (Line225-226).

 

(R1Q7) 2 (b) can be removed..

>>AUTHORS’ REPLY:

Thanks for your valuable suggestions. We have removed 2(b) from the manuscript (Line227-228).

 

(R1Q8) Section 4 should be rewritten to give a concise conclusion.

>>AUTHORS’ REPLY:

Thanks for your valuable suggestions. We have simplified and revised the conclusion part of the manuscript(Line 495-524).

 

(R1Q9) Some English writing in this manuscript can be improved.

>>AUTHORS’ REPLY:

Thanks for your valuable suggestions. We have conducted a detailed review of the entire manuscript and made revisions and adjustments to inappropriate sentences to ensure that the sentences are accurate, comply with academic norms, and are semantically consistent with the context.

Author Response File: Author Response.pdf

Reviewer 2 Report

Comments and Suggestions for Authors

The manuscript entitled ‘Selective Carbon Enrichment from Micro/Nano Silicon-carbon ores via Sodium Hexametaphosphate: Mechanism insight,  Structural characterization, and Potential Applications’ discusses the enrichment of carbon from a silicon-carbon deposit and the characterisation of deposit samples.

My specific comments are as follows:

  1. The title says ‘Potential Applications’ - there are no studies proving the applications of enriched carbon in the manuscript. In general, carbons have many applications, but no research has been done in this direction. Please change the title or remove ‘Potential Applications’.
  2. Fig 6: Raman spectra - please label which spectrum applies to which samples.
  3. Fig 7: Please state in the title of the figure what images a-h refer to.
  4. Fig 9 and line 328-332: on what basis do the authors conclude that there are 2 types of carbonaceous substances.
  5. why was reagent sodium hexametaphosphate chosen to enrich carbon from the ore?

Author Response

Reviewer #2:

Comments and Suggestions for Authors

The manuscript entitled ‘Selective Carbon Enrichment from Micro/Nano Silicon-carbon ores via Sodium Hexametaphosphate: Mechanism insight, Structural characterization, and Potential Applications’ discusses the enrichment of carbon from a silicon-carbon deposit and the characterisation of deposit samples.

My specific comments are as follows:

  1. The title says ‘Potential Applications’ - there are no studies proving the applications of enriched carbon in the manuscript. In general, carbons have many applications, but no research has been done in this direction. Please change the title or remove ‘Potential Applications’.
  2. Fig 6: Raman spectra - please label which spectrum applies to which samples.
  3. Fig 7: Please state in the title of the figure what images a-h refer to.
  4. Fig 9 and line 328-332: on what basis do the authors conclude that there are 2 types of carbonaceous substances.
  5. why was reagent sodium hexametaphosphate chosen to enrich carbon from the ore?

 

(R2Q1) The title says ‘Potential Applications’ - there are no studies proving the applications of enriched carbon in the manuscript. In general, carbons have many applications, but no research has been done in this direction. Please change the title or remove ‘Potential Applications’.

>>AUTHORS’ REPLY:

Thanks for your valuable feedback. We have already modified the title.

 

(R2Q2) Fig 6: Raman spectra - please label which spectrum applies to which samples.

>>AUTHORS’ REPLY:

Thanks for your suggestion. We have already labeled the Raman spectrum graph in Figure 6 in the manuscript (Line 344).

 

(R2Q3) Fig 7: Please state in the title of the figure what images a-h refer to.?

>>AUTHORS’ REPLY:

Thank you for your valuable suggestions. We have labeled and provided detailed explanations for each image in Figure 7 based on your suggestions (Line 443).

 

(R2Q4) Fig 9 and line 328-332: on what basis do the authors conclude that there are 2 types of carbonaceous substances.

>>AUTHORS’ REPLY:

Thanks for your valuable suggestions. This is an oversight in our description. The spectroscopic characterization in Figure 6 reveals critical structural insights: Fourier-transform infrared (FTIR) and Raman analyses collectively demonstrate that the carbonaceous matter exists predominantly as amorphous carbon and contains two functional groups (Tang, S. W.; Shuai, H.; Zhao, R. T.; Du, G. X.; Wang, X. G.; Wang, J., Process Mineralogy of Micro/Nano Silicon-Carbon Ore Obtained from Jiangxi, China. Minerals 2022, 12, (6); Tucureanu, V.; Matei, A.; Avram, A. M., FTIR Spectroscopy for Carbon Family Study. Critical Reviews in Analytical Chemistry 2016, 46, (6), 502-520.). Complementing these spectroscopic findings, high-resolution transmission electron microscopy (HR-TEM) observations in Figure 9 disclose a dual-phase carbon architecture. The matrix consists of a highly disordered amorphous carbon network, while localized domains exhibit short-range graphitic ordering with interfacial lattice fringes (Li, K.; Liu, Q. F.; Cheng, H. F.; Hu, M. S.; Zhang, S., Classification and carbon structural transformation from anthracite to natural coaly graphite by XRD, Raman spectroscopy, and HRTEM (vol 249, 119286, 2021). Spectroc. Acta Pt. A-Molec. Biomolec. Spectr. 2023, 303; Li, K.; Zhang, H.; Wu, Y. T.; Hu, M. S.; Liu, Q. F., Graphite microcrystals growth in naturally graphitized coal from Hunan, China. Journal of Crystal Growth 2022, 582.).

Figure 6. Infrared (FTIR) and Raman spectra of silicon carbide ore before and after treatment with sodium hexametaphosphate

Figure 9. TEM image of carbon-silicon-carbon ore sample (SC-2) after SHMP treatment

 

(R2Q5) why was reagent sodium hexametaphosphate chosen to enrich carbon from the ore?

>>AUTHORS’ REPLY:

Thanks for your valuable questions and suggestions. In our preliminary investigations employing sodium polyacrylate (PAAS) as an organic grinding aid, we observed limited separation efficiency during subsequent extraction processes. This inefficiency likely stems from the amphiphilic nature of polymeric dispersants - while their anionic carboxyl groups (-COO⁻) preferentially adsorb onto quartz surfaces, the hydrophobic polymer backbone simultaneously engages with aromatic domains in carbonaceous matter. This dual interaction mechanism induces co-dispersion of both mineral phases.

Based on this, we selected sodium hexametaphosphate (SHMP) as the inorganic dispersant to selectively disperse the inorganic minerals in the silicon-carbon ore slurry, thereby effectively separating the organic and inorganic components. Judging from the separation phenomenon and results, the use of sodium hexametaphosphate to separate carbon and quartz in silicon-carbon ore is effective.

Author Response File: Author Response.pdf

Reviewer 3 Report

Comments and Suggestions for Authors

The manuscript titled "Selective Carbon Enrichment from Micro/Nano Silicon-carbon 2 ores via Sodium Hexametaphosphate: Mechanism insight, 3 Structural characterization, and Potential Applications" is highly interesting, but it requires major revisions.

 

Abstract

The abstract is well-written.

 

Keywords

suggestion: add structural features and carbonaceous material

 

Introduction

Recommendation: Include a literature review

 

Materials and Methods

Recommendation: Include a diagram

Page 3: Line 124: Replace "specific surface area and pore size (BET)" with "textural analysis, with BET as one of the methods used."

 

Results and discussion

3.1 Exploration of the Grinding and Separation Mechanism of Silicon-Carbon Ore

This section is thoroughly discussed and the quality of the Figures is excelente.

 

3.2 Characterization and Identification of Carbonaceous Materials in Silicon-carbon Ore

This section is well discussed and the quality of the Figures is excellent.

 

3.3 BET analysis of carbonaceous in Silican-Carbon Ore and its application prospects

Replace "BET analysis" with "textural analysis"

 

Page 11: Lines 337-345

Page 12: Lines 346-347

The content on pages 11 and 12, along with the aforementioned lines, should be moved to the introduction.

The specific surface area value must be an integer. Replace 92.12 with 92 m²/g. Is this value high or low compared to the literature?

 

Page 12: lines 358-361: This text should be in the conclusion.

 

Conclusion

Page 13: Line 380: Replace: BET specific surface area analysis with textural analysis

Page 13: Line 382: Replace 95.12 with 92 m²/g.

 

References

Standardize and revise the references.

 

Author Response

Reviewer #3:

Comments and Suggestions for Authors

The manuscript titled "Selective Carbon Enrichment from Micro/Nano Silicon-carbon 2 ores via Sodium Hexametaphosphate: Mechanism insight, 3 Structural characterization, and Potential Applications" is highly interesting, but it requires major revisions.

 

Abstract

The abstract is well-written.

 

Keywords

suggestion: add structural features and carbonaceous material

 

Introduction

Recommendation: Include a literature review

 

Materials and Methods

Recommendation: Include a diagram

Page 3: Line 124: Replace "specific surface area and pore size (BET)" with "textural analysis, with BET as one of the methods used."

 

Results and discussion

3.1 Exploration of the Grinding and Separation Mechanism of Silicon-Carbon Ore

This section is thoroughly discussed and the quality of the Figures is excellent.

 

3.2 Characterization and Identification of Carbonaceous Materials in Silicon-carbon Ore

This section is well discussed and the quality of the Figures is excellent.

 

3.3 BET analysis of carbonaceous in Silican-Carbon Ore and its application prospects

Replace "BET analysis" with "textural analysis"

 

Page 11: Lines 337-345

Page 12: Lines 346-347

The content on pages 11 and 12, along with the aforementioned lines, should be moved to the introduction.

The specific surface area value must be an integer. Replace 92.12 with 92 m²/g. Is this value high or low compared to the literature?

 

Page 12: lines 358-361: This text should be in the conclusion.

 

Conclusion

Page 13: Line 380: Replace: BET specific surface area analysis with textural analysis

Page 13: Line 382: Replace 95.12 with 92 m²/g.

 

References

Standardize and revise the references.

 

(R3Q1) Abstract:

The abstract is well-written.

>>AUTHORS’ REPLY:

Thanks for your recognition of our work.

 

(R3Q2) Keywords

suggestion: add structural features and carbonaceous material

>>AUTHORS’ REPLY:

Thanks for your suggestion. We have added "structural features" and "carbonaceous materials" to the keywords (Line21).

 

(R3Q3) Introduction

Recommendation: Include a literature review

>>AUTHORS’ REPLY:

Thank you for your valuable suggestions. We are fully aware that the introduction section indeed requires improvement. We have made revisions and added a comprehensive literature review (Line 32-87).

 

(R2Q4) Materials and Methods

Recommendation: Include a diagram

Page 3: Line 124: Replace "specific surface area and pore size (BET)" with "textural analysis, with BET as one of the methods used."

>>AUTHORS’ REPLY:

We appreciate your valuable questions and suggestions. We have made the revisions in the submitted manuscript as per your suggestions (Line 189).

 

(R2Q5) Results and discussion

3.1 Exploration of the Grinding and Separation Mechanism of Silicon-Carbon Ore

This section is thoroughly discussed and the quality of the Figures is excelente.

>>AUTHORS’ REPLY:

Thanks for your recognition of our work.

 

(R2Q6) Results and discussion

3.2 Characterization and Identification of Carbonaceous Materials in Silicon-carbon Ore

This section is well discussed and the quality of the Figures is excellent.

>>AUTHORS’ REPLY:

Thanks for your recognition of our work.

 

(R2Q7) Results and discussion

3.3 BET analysis of carbonaceous in Silican-Carbon Ore and its application prospects

Replace "BET analysis" with "textural analysis"

>>AUTHORS’ REPLY:

We appreciate your valuable questions and suggestions. We have already made the necessary revisions to this part in the manuscript (Line 466).

 

(R2Q8) Results and discussion

Page 11: Lines 337-345

Page 12: Lines 346-347

The content on pages 11 and 12, along with the aforementioned lines, should be moved to the introduction.

The specific surface area value must be an integer. Replace 92.12 with 92 m²/g. Is this value high or low compared to the literature?

>>AUTHORS’ REPLY:

①We appreciate your valuable questions and suggestions. We have revised this section by relocating the relevant introductory content to the Introduction and adjusting the significant figures.

②The initial specific surface area of the carbonaceous material in the silicon-carbon ores was 92 m²/g, which is considered relatively low according to literature reports and primarily restricted to adsorption applications. However, in our study, following purification and activation treatments, the specific surface area of the carbonaceous material was enhanced to over 400 m²/g, thereby significantly broadening its potential applications in areas such as adsorption and catalysis.

 

(R2Q9) Results and discussion

Page 12: lines 358-361: This text should be in the conclusion.

>>AUTHORS’ REPLY:

We appreciate your valuable questions and suggestions. We have made adjustments to this part and moved it to the conclusion section.

 

(R2Q10) Conclusion

Page 13: Line 380: Replace: BET specific surface area analysis with textural analysis

Page 13: Line 382: Replace 95.12 with 92 m²/g.

>>AUTHORS’ REPLY:

We appreciate your valuable questions and suggestions. We have incorporated the suggested revisions into the manuscript.

 

(R2Q10) References

Standardize and revise the references.

>>AUTHORS’ REPLY:

We appreciate your valuable questions and suggestions. We have revised the reference section in accordance with the requirements of your journal.

Author Response File: Author Response.pdf

Round 2

Reviewer 1 Report

Comments and Suggestions for Authors

a Figures at line 184 should be removed.

b The sentence 'These results indicate that SHMP substantially decreases the absolute value of the ζ potential of the silicon-carbon ore slurry.' should be revised as 'These results indicate that SHMP substantially increases the absolute value of the ζ potential of the silicon-carbon ore slurry.'

Author Response

Comments and Suggestions for Authors

a Figures at line 184 should be removed.

b The sentence 'These results indicate that SHMP substantially decreases the absolute value of the ζ potential of the silicon-carbon ore slurry.' should be revised as 'These results indicate that SHMP substantially increases the absolute value of the ζ potential of the silicon-carbon ore slurry.'

(R1Q1)Figures at line 184 should be removed.

>>AUTHORS’ REPLY:

Thanks for your valuable feedback. We have removed the Figure on line 184 as per your request. The specific changes can be found on line 185.

 

(R1Q1)The sentence 'These results indicate that SHMP substantially decreases the absolute value of the ζ potential of the silicon-carbon ore slurry.' should be revised as 'These results indicate that SHMP substantially increases the absolute value of the ζ potential of the silicon-carbon ore slurry.'

>>AUTHORS’ REPLY:

Thanks for your valuable suggestions. There was an obvious mistake in this sentence, and we have already made the correction. The specific change is on line 183.

Author Response File: Author Response.pdf

Reviewer 3 Report

Comments and Suggestions for Authors

All the suggestions and corrections I requested have been incorporated in accordance with the authors' response letter and the revised manuscript. I have reviewed everything and approve of the revised manuscript.

Author Response

Comments and Suggestions for Authors

All the suggestions and corrections I requested have been incorporated in accordance with the authors' response letter and the revised manuscript. I have reviewed everything and approve of the revised manuscript.

(R3Q1) All the suggestions and corrections I requested have been incorporated in accordance with the authors' response letter and the revised manuscript. I have reviewed everything and approve of the revised manuscript.

>>AUTHORS’ REPLY:

We sincerely appreciate your recognition of our work. 

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