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Article
Peer-Review Record

Catalytic Oxidation of Flax Shives into Vanillin and Pulp

Catalysts 2022, 12(9), 1003; https://doi.org/10.3390/catal12091003
by Valery E. Tarabanko *, Dmitrii O. Vigul, Konstantin L. Kaygorodov, Yulia V. Chelbina and Elena V. Mazurova
Reviewer 2: Anonymous
Reviewer 3: Anonymous
Reviewer 4: Anonymous
Catalysts 2022, 12(9), 1003; https://doi.org/10.3390/catal12091003
Submission received: 23 June 2022 / Revised: 31 August 2022 / Accepted: 2 September 2022 / Published: 6 September 2022
(This article belongs to the Special Issue Catalysis for Flavours and Fragrances)

Round 1

Reviewer 1 Report

ï‚· Major reference [Number 8] for the synthesis of vanillin was not opening. Doi not found

ï‚· The role of the catalyst is to initiate the reaction, however, the catalyst used here is almost equal to starting material.

ï‚· Cu being heavy metal used in this quantity and not recovering may harm the environment.

ï‚· Not enough characteristic data to support the production and quantification of Vanillin production.

Author Response

Dear Reviewer,

many thanks for the thorough revision of our manuscript,  the very useful remarks, and recommendations.

We made additional experiments and added corresponding discussion to the manuscript.

Encloised are our responses for you remarks.

  Once more thank you for the useful revision.

Sincerely yours.

Valery E. Tarabanko

Author Response File: Author Response.pdf

Reviewer 2 Report

The work investigated several factors that affect the catalytic oxidation of flax shives to vanillin and pulp, but it’s more like an experiment report than a research work. And there are several obvious mistakes as shown below. Therefore, I suggest reject this manuscript.

1.     What’s the meaning of “… starting from 70ths of XX century” ?? in the first paragraph?

2.     The paragraph structure of the introduction is strange.

3.     The whole work only presented the experimental data and was lack of insightful investigation or discussion.

4.     How did the author know copper oxide was obtained in situ during the oxidation process just by SEM?

5.     I didn’t see the data on acid prehydrolysis on the efficiency of subsequent pine wood.

Author Response

Dear Reviewer,

many thanks for the thorough revision of our manuscript,  the very useful remarks, and recommendations.

We made additional experiments and added corresponding discussion to the manuscript.

Encloised are our responses for you remarks.

  Once more thank you for the useful revision.

Sincerely yours.

Valery E. Tarabanko

Author Response File: Author Response.pdf

Reviewer 3 Report

Tarabanko et. al investigated a process of catalytic oxidation of flax shives to vanillin and pulp. It was considerable for bio-vanillin yield at 12 wt. % per lignin and pulp. This research contains some interesting results, which is into the scope of the journal. Some major issues must be addressed before publication.

 

1.      The description for Fig. 1 & Fig. 1 were losing.

2.      The description for Fig.2c was losing. Simultaneously, the catalyst had regular shape at 100 μm scale comparing with that of Fig.2a&2b at 10 μm and 30 μm scale, the author should explain the reason.

3.      The Fig. 2 didn’t coincident with the descript in the sentence: “Change in the volume of the reaction mass from 300 ml [8] to 400 ml (Fig. 2) leads to an increase in this tangent to the value tg= 2.81 ± 0.2.”

4.      The research contents for the title “2.3. Influence of stirring speed on the vanillin accumulation kinetics and its yield” was poor. The author should add corresponding content to explain the influence of stirring speed for reaction kinetics.

5.      The analysis for Table 1 was not specific and particular. Only three variates was unreasonable to discuss the reaction conditions, I suggest the authors should added the result under  the stirring speed at 400 rpm and 600 dpm. Simultaneously, the result in NaOH concentration at 25% should be added.

6.      Under 500 rpm, the Oxygen consumption(mol/mol of vanillin) in 75% NaOH was smaller than that in 100% NaOH and 50% NaOH, the authors should give the reasonable explain.

7.      Some mistake should be corrected:

“xx century” in Line 22 on Page 1

“ofherbaceous “ in Line 143 on Page 5

Author Response

Dear Reviewer,

many thanks for the thorough revision of our manuscript,  the very useful remarks, and recommendations.

We made additional experiments and added corresponding discussion to the manuscript.

Encloised are our responses for you remarks.

  Once more thank you for the useful revision.

Sincerely yours.

Valery E. Tarabanko

Author Response File: Author Response.pdf

Reviewer 4 Report

The manuscript entitled "Catalytic Oxidation of Flax Shives into Vanillin and Pulp" by Tarabanko et al. reports on the oxidative conversion of an underexplored residue, flax shives, into valuable chemicals such as vanillin. Overall the paper reads well and is scientifically sound. Some suggestions for improvement is provided below:

- Page 1, line 9: is the yield provided based on initial lignin basis or also pulp input? and was the catalyst CuO provided as particles, it is mentioned as homogeneous catalyst (sulfate form later in the text).

- Page 1, line 20: XX century, the number is missed; also, any reference for the first paragraph in the introduction?

-Page 2, line 42: 25-28 wt. % vanillin yield from softwood lignins, any literature supporting this figure?

- Literature on relevant copper catalyst systems is missing in the introduction, the authors should cite relevant and recent reports on this topic.

- Page 3, line 115: you start with Fig. 2a, where is the insertion text of Fig. 1?

- Page 7, line 202: use superscript in min -1

- Page 8: In Table 1 vanillin yield is reported as wt% on lignin then in the conclusions reported as per lignin and pulp, can the authors clarify this? also are you using ',' separators instead of '.'?

- Page 8: The methods section should be expanded significantly: what are the chemicals used, any sample preparation done prior to GLC analysis? how did the authors quantify the vanillin yield? in case of calibration curves, could be added in an appendix

- Page 8: line 248-249:  the term 'on the other hand' is used twice in successive lines

- An important aspect is if the authors have performed any blank experiment, without using copper catalyst, to compare with its performance? otherwise the role of the catalyst is yet to be confirmed

- Page 9: Literature should be updated with more recent references

Author Response

Dear Reviewer,

many thanks for the thorough revision of our manuscript,  the very useful remarks, and recommendations.

We made additional experiments and added corresponding discussion to the manuscript.

Encloised are our responses for you remarks.

  Once more thank you for the useful revision.

Sincerely yours.

Valery E. Tarabanko

Author Response File: Author Response.pdf

Round 2

Reviewer 1 Report

In the introduction why it is 50ths-70ths. This is not correct it must be 70th for example. Correct it please.

Author Response

Dear Reviewer,

Thanks for the revision. We corrected the indexes. 

Best regards. 

Valery E. Tarabanko 

Reviewer 2 Report

Be careful with the revisions mode in the final version of the manuscript, there are still comment in it.

Author Response

Dear Reviewer,

thank you for your remark.

The comments concerned the already made revisions and are deleted in the final version. 

Kind regards.

Valery E Tarabanko

 

Reviewer 3 Report

The author has answered all the questions.  I suggest to accept the manuscript in present form.

Author Response

Dear Reviewer, 

thank you for the useful remarks on our manuscript and for your work on it. 

Best regards. 

Valery E. Tarabanko

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