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Article
Peer-Review Record

Study on the Shale Hydration Inhibition Performance of Triethylammonium Acetate

Minerals 2022, 12(5), 620; https://doi.org/10.3390/min12050620
by Yuanzhi Qu 1, Ren Wang 1,2,*, Shifeng Gao 1, Hongjun Huang 1, Zhilei Zhang 1, Han Ren 1, Yuehui Yuan 1, Qibing Wang 1,2, Xiangyun Wang 3 and Weichao Du 3,*
Reviewer 1: Anonymous
Minerals 2022, 12(5), 620; https://doi.org/10.3390/min12050620
Submission received: 13 April 2022 / Revised: 5 May 2022 / Accepted: 6 May 2022 / Published: 13 May 2022

Round 1

Reviewer 1 Report

The manuscript “Study on the shale hydration inhibition performance of tri-ethylammonium acetate on shale” introduced the preparation, performance and inhibitive mechanism of a novel shale inhibitor. This research shows a certain degree of novelty and significance, but, authors need to address the following issues to make this paper better.

  1. Some writing errors should be corrected in your manuscript, for example: hour-h, minute-min.
  2. The words “on shale” in the title should be deleted.
  3. In abstract part, the word “into” should be deleted, the word “effect” should be changed to “performance”, the word “new” should be changed to “novel”, the sentence “with acetic acid and triethylamine as raw materials” should be changed to “by using acetic acid and triethylamine as raw materials”,
  4. Please add another Keywords
  5. Please add a description of the importance of drilling fluid to wellbore stability in the first paragraph.
  6. Please describe the amine inhibitor appropriately in abstract part.
  7. -CH2- and -CH3 in line 115 should be changed to -CH2- and -CH3
  8. The word expansion in line 131 and 133 should be changed to swelling
  9. The reason for swelling of Na-MMT in the Linear Expansion Tests part should place in the beginning of this paragraph.
  10. Na MMT should be changed to swelling Na-MMT in the full paper.
  11. The format of words in your manuscript should be amended, for example: cm-1 should be corrected to cm-1.
  12. Some words have been repeated, and the expressions of some sentences in this article need to be further improved.

Author Response

Responses to the comments of Reviewer 1#

  1. Some writing errors should be corrected in your manuscript, for example: hour-h, minute-min.

Response: Thank you for your comments concerning our manuscript, we have corrected our mistakes.

  1. The words “on shale” in the title should be deleted .

Response: Thank you for your comments concerning our manuscript, we have deleted it.

  1. In abstract part, the word “into” should be deleted, the word “effect” should be changed to “performance”, the word “new” should be changed to “novel”, the sentence “with acetic acid and triethylamine as raw materials” should be changed to “by using acetic acid and triethylamine as raw materials”.

Response: Thanks for reviewer’s comments, we have corrected our mistakes..

  1. Please add another Keywords.

Response: Thank you for your comments concerning our manuscript, we have added one.

  1. 5. Please add a description of the importance of drilling fluid to wellbore stability in the first paragraph.

Response: Thanks for reviewer’s comments. We have added it.

  1. Please describe the amine inhibitor appropriately in abstract part.

Response:  Thanks for reviewer’s academic background, according to the reviewer's comments, we have added it.

  1. -CH2- and -CH3 in line 115 should be changed to -CH2- and -CH3

Response: Thanks for reviewer’s academic background, we have corrected our mistakes.

  1. The word expansion in line 131 and 133 should be changed to swelling.

Response: Thanks for reviewer’s comments. we have corrected our mistakes.

  1. The reason for swelling of Na-MMT in the Linear Expansion Tests part should place in the beginning of this paragraph.

Response: Thanks for reviewer’s comments. We have added it.

  1. Na MMT should be changed to swelling Na-MMT in the full paper.

Response: Thanks for reviewer’s academic background. we have corrected our mistakes.

  1. The format of words in your manuscript should be amended, for example: cm-1 should be corrected to cm-1..

Response: Thanks for reviewer’s academic background. we have corrected our mistakes.

  1. Some words have been repeated, and the expressions of some sentences in this article need to be further improved.

Response: Thanks for reviewer’s academic background. we have corrected our mistakes.

Special thanks to you for your good comment

Author Response File: Author Response.pdf

Reviewer 2 Report

Presented work related to a such important problem as shale hydration and collapse of wellbore. The triethylammonium acetate (TEYA) was chosen as ionic shale inhibitor. Obtained inhibitor and the inhibition mechanism was studied by infrared spectroscopy and X-Ray diffraction methods.

My several remarks are listed below:

Page 2, Line 47

triethylammonium acetate

Please add chemical formula.

Page 2, Lines 55-57

A certain amount of triethylamine was added into a three-neck flask, a certain amount of acetic acid was slowly added with stirring, and then heated at the temperature required until the reaction was completed.

“A certain amount” should be replaced with exact values.

Page 2, Line 63 and Line 72

50 g of calcium-based bentonite/50 g 40-mesh shale samples

It is not good to start the sentence from the numbers.

Page 2, Line 68

A total of 10 g Na-MMT

The abbreviation must be deciphered on first use.

Page 3, Lines 88-89

The prepared sample powder was mixed with KBr and pressed into pellets for FT-IR analysis

The prepared sample powder was mixed with KBr and pressed into pellets for FT-IR analysis.

Page 3, Line 90

XRD analysis

Information about equipment should be added.

Page 3, Line 97

TEYA was characterized by WQF-520 FT-IR Fourier transform infrared spectrometer.

This information should be placed in section 2.4.1. FT-IR analysis.

Page 3, Line 105

was the target product [27-30].

I think that it is better to put each reference to explanation of exact spectral band. Is the reference spectrum of the studied acetate presented in the literature? X-ray diffraction analysis was not performed at all?

Page 3, Figure 2.

We don’t know the initial shape of mud balls.

Page 5, Line 143

k2SiO3

K2SiO3

Figure1, Figure 5

Horizontal axis should be: Wavenumber/cm-1

Page 6, Line 168

peak of bentonite

What is bentonite and where is it in the spectra?

Page 7, Line 191

In this paper, a new ionic shale inhibitor TEYA was obtained

Why you call this compound new? As I see, triethylammonium acetate is already known (CH3CH2)3NHOCOCH3.

Author Response

Responses to the comments of Reviewer 2#

  1. Page 2, Line 47 triethylammonium acetate Please add chemical formula.

Response: Thank you for your comments concerning our manuscript, we have added it in Scheme 1 .

 

  1. Page 2, Lines 55-57, certain amount” should be replaced with exact values.

Response: Thank you for your comments concerning our manuscript, we have modified it.

 

  1. Page 2, Line 63 and Line 72 50 g of calcium-based bentonite/50 g 40-mesh shale samples  It is not good to start the sentence from the numbers.”.

Response: Thanks for reviewer’s comments, we have corrected our mistakes..

 

  1. Page 2, Line 68 A total of 10 g Na-MMT  The abbreviation must be deciphered on first use..

Response: Thank you for your comments concerning our manuscript, we have added it in” Materials” part.

 

  1. 5. Page 3, Lines 88-89 The prepared sample powder was mixed with KBr and pressed into pellets for FT-IR analysis.

Response: Thanks for reviewer’s comments. We have corrected our mistakes.

 

  1. Page 3, Line 90 XRD analysis  Information about equipment should be added.

Response:  Thanks for reviewer’s academic background, according to the reviewer's comments, we have added it in the 2.4.2. XRD analysis part .

 

  1. Page 3, Line 97 TEYA was characterized by WQF-520 FT-IR Fourier transform infrared spectrometer. This information should be placed in section 2.4.1. FT-IR analysis.

Response: Thanks for reviewer’s academic background, according to the reviewer's comments, we have added it in 2.4.1. FT-IR analysis part .

 

  1. Page 3, Line 105 was the target product [27-30]. I think that it is better to put each reference to explanation of exact spectral band. Is the reference spectrum of the studied acetate presented in the literature? X-ray diffraction analysis was not performed at all?.

Response: Thanks for reviewer’s comments. we have added two references here.

 

  1. Page 3, Figure 2. We don’t know the initial shape of mud balls.

Response: Thanks for reviewer’s comments. We have re-done the mud ball experiment, and the photos of the mud ball in its initial state have been put in Figure 2.

 

  1. Page 5, Line 143 k2SiO3  .

Response: Thanks for reviewer’s comments. We have corrected our mistakes.

 

  1. Figure1, Figure 5 Horizontal axis should be: Wavenumber/cm-1.

Response: Thanks for reviewer’s academic background. we have corrected our mistakes.

  

  1. Page 6, Line 168 peak of bentonite What is bentonite and where is it in the spectra?.

Response: Thanks for reviewer’s academic background. the crystal layer spacing of dry Na-MMT is 1.28 nm, and we have corrected the Figure 6.

 

  1. Page 7, Line 191 In this paper, a new ionic shale inhibitor TEYA was obtained Why you call this compound new? As I see, triethylammonium acetate is already known (CH3CH2)3NHOCOCH3..

Response: Thanks for reviewer’s academic background. Indeed, CH3CH2)3NHOCOCH3 is not a new compound, but its application in drilling fluid has not been reported. It is the first time to report it as a shale inhibitor

Special thanks to you for your good comment

Round 2

Reviewer 2 Report

The authors worked on the manuscript. At this moment I have couple of remarks.

Page 2, Line 70

Page 3, Line 89

Page 3, Line 114

You should never begin a sentence with a numeral. Try to reword the sentence. If you find it unwieldy to reorder your words, spell out the number.

Page 3, Lines 104-105 and Lines 110-111

It is the same sentence. It just written twice.

Page 3, Line 117

diffract meter

diffractometer

Author Response

Response to Reviewer 2 Comments

 

Point 1:  Page 2, Line 70 Page 3, Line 89Page 3, Line 114  You should never begin a sentence with a numeral. Try to reword the sentence. If you find it unwieldy to reorder your words, spell out the number..

Response 1: Thank you for pointing out the mistake to us. We have revised it and checked the whole article. Thank you

 

Point 2: Page 3, Lines 104-105 and Lines 110-111.It is the same sentence. It just written twice.

Response 2: Thank you for pointing out the mistake to us. We have revised it. Thank you

 

Point 3: diffract meter   diffractometer.

Response 3: Thank you for pointing out the mistake to us. We have revised it. Thank you

Author Response File: Author Response.pdf

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