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Peer-Review Record

Roasting Pretreatment Combined with Ultrasonic Enhanced Leaching Lead from Electrolytic Manganese Anode Mud

Reviewer 1: Anonymous
Reviewer 2: Maria Letizia Ruello
Reviewer 3: Anonymous
Metals 2019, 9(5), 601; https://doi.org/10.3390/met9050601
Received: 1 May 2019 / Revised: 13 May 2019 / Accepted: 21 May 2019 / Published: 24 May 2019
(This article belongs to the Special Issue Metal Removal and Recycling)

Round  1

Reviewer 1 Report

Manuscript entitled “Roasting pretreatment combined with ultrasonic enhanced leaching lead from electrolytic manganese anode mud submitted by Huimin Xie, Shiwei Li, Libo Zhang, Yongmi Wang and Hailin Long, can be accepted for publishing in the Metals Journal, after a minor revision.

In this study, ultrasound was introduced into the process of leaching of lead from the electrolytic manganese anode mud to enhance the recovery of lead, also making experimental conditions milder. The manuscript presents original results, which are well organized and systematized. In my opinion, this manuscript should be accepted for publication after a minor revision.

 

            Here is a list of my specific comments:

General comment: The practical      applicability of this study should be highlighted more. Add some      advantages of this procedure compared with the traditional one.

Page 2, line 54: “Ultrasonic waves are sound waves with      special frequency higher than 20 kHz.” Add here a reference.

Page 2,      lines 64-71: At the end of Introduction, the main objectives of this study      should be formulated more clearly.

Page 3,      2.2. Experimental procedure and instrument: Experimental details (volume,      concentration, time, temperature, etc.) required to perform the      experiments related to the influence of “The effects of concentration,      liquid-solid ratio, and temperature on the leaching process under      conventional and ultrasonic conditions…” (as is mentioned in Abstract)      must be added here.


Author Response

Response to Reviewer 1 Comments

 

Point 1: Page 2, line 54: “Ultrasonic waves are sound waves with special frequency higher than 20 kHz.” Add here a reference.

Response 1: I have revised the sentence and added a reference according to the reviewer’s suggestion .

Point 2:  Page 2,lines 64-71: At the end of Introduction, the main objectives of this study      should be formulated more clearly.

Response 2: I have revised the sentence and corrected the inappropriate place according to the reviewer’s suggestion. .

Point 3: Page 3, 2.2. Experimental procedure and instrument: Experimental details (volume,      concentration, time, temperature, etc.) required to perform the experiments related to the influence of “The effects of concentration,  liquid-solid ratio, and temperature on the leaching process under  conventional and ultrasonic conditions…” (as is mentioned in Abstract) must be added here.

Response 3: I have revised the manuscript and and added experimental details according to the reviewer’s suggestion.


Author Response File: Author Response.pdf

Reviewer 2 Report

Sorry, I am not English mother tongue, but I think that a deep language revision needs.


Lines 21, 22 "Keywords: Electrolytic manganese anode mud; Ultrasound enhance; Roasting; Dynamics modeling"

Could be improved. Avoid repetition of words already presented in the title, and introduce others (eg. reducing environmental pollution; sustainable development; hydrometallurgical recovery process)


Line 29 "...the lead content about 7% ..." Please check, the predicate "is" should be missed.


Line 31 "...pre-evaporation of lead causes the precision of manganese to decrease[3,4] ..."  precision??? sure?


Lines 390, 391 Please correct: andmanganese(II); withmanganese


Line 75 (and others) "The raw material is ground ..." Please use other words instead of "raw material", since this words refer to a feedstock, unprocessed material, or primary commodity, (for example; crude oil is a raw material)


Line 128 please use the word mass instead of "quality"


Lines 134 - 136 "The results are shown in Fig. 5 that the leaching rate of lead in electrolytic manganese anode mud pretreated by roasting is obviously higher than that in non-roasting process." Please rephrase (ex. The results (Fig. 5) show  that the leaching rate of lead in electrolytic manganese anode mud pretreated by roasting is obviously higher than that in non-roasting process.)


Lines 154, 155 " ... indicating that the phase transformation of the electrolytic manganese anode mud after 1123K high temperature roasting." Please rephare (ex. ... indicating that a phase transformation of the electrolytic manganese anode mud occurs after 1123K high temperature roasting.).


Lines 158, 159 "As shown in Fig. 7 that the dense structure in which the raw materials exists in the "mineral phase" is destroyed." Please rephare (ex. ... As shown in Fig. 7, the dense structure, in which the materials exists in the mineral phase, is destroyed.).


Line 262 "ultrasonic optimized process conditions" please resume here, or in the header of fig. 12  what are this conditions

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Author Response

Response to Reviewer Comments

 

Point 1: Line 29 "...the lead content about 7% ..." Please check, the predicate "is" should be missed.

Response 1: I have revised the sentence according to the reviewer’s suggestion .

Point 2: Line 31 "...pre-evaporation of lead causes the precision of manganese to decrease[3,4] ..."  precision??? sure?

Response 2: I have revised the part and corrected the inappropriate place according to the reviewer’s suggestion.

Point 3: Lines 390, 391 Please correct: andmanganese(II); withmanganese

Response 3: I have revised the references according to the reviewer’s suggestion.

Point 4: Line 75 (and others) "The raw material is ground ..." Please use other words instead of "raw material", since this words refer to a feedstock, unprocessed material, or primary commodity, (for example; crude oil is a raw material)

Response 4: I have revised the manuscript and instead of "raw material" according to the reviewer’s suggestion.

Point 5: Line 128 please use the word mass instead of "quality"

Response 5: I have revised the part and corrected the inappropriate place according to the reviewer’s suggestion.

Point 6: Lines 134 - 136 "The results are shown in Fig. 5 that the leaching rate of lead in electrolytic manganese anode mud pretreated by roasting is obviously higher than that in non-roasting process." Please rephrase (ex. The results (Fig. 5) show  that the leaching rate of lead in electrolytic manganese anode mud pretreated by roasting is obviously higher than that in non-roasting process.)

Response 6: I have revised the sentence according to the reviewer’s suggestion .

Point 7: Lines 154, 155 " ... indicating that the phase transformation of the electrolytic manganese anode mud after 1123K high temperature roasting." Please rephare (ex. ... indicating that a phase transformation of the electrolytic manganese anode mud occurs after 1123K high temperature roasting.).

Response 7: I have revised the sentence according to the reviewer’s suggestion .

Point 8: Lines 158, 159 "As shown in Fig. 7 that the dense structure in which the raw materials exists in the "mineral phase" is destroyed." Please rephare (ex. ... As shown in Fig. 7, the dense structure, in which the materials exists in the mineral phase, is destroyed.).

Response 8: I have revised the sentence according to the reviewer’s suggestion .

Point 9: Line 262 "ultrasonic optimized process conditions" please resume here, or in the header of fig. 12  what are this conditions

Response 9: I have revised the sentence according to the reviewer’s suggestion .


Author Response File: Author Response.pdf

Reviewer 3 Report

Roasting pretreatment combined with ultrasonic enhanced leaching lead from electrolytic manganese anode mud was proposed to solve the difficult Problem of lead in electrolytic manganese anode mud

My Remarks in text:

Line 13- leaching with Ammonium Acetate

Line 22-Lead

Line 43: which impurities?

Line 64: leaching of lead with Ammonium Acetate

Line 67: Which process? Leaching process of lead?

Line 76. What is grain size after milling, Filtration and drying?

Line 84: You mentioned the presence of PbSO4, but at Figure 1 at X-ray Analysis we found PbO2. What is correct?

Line 89- based (instead biased)

Line 138. Roasting conditions (923-1123 K, time ?, flow rate of gas? Initial weight of sample?) Which gas was introduced in the Furnace? Which reactor? (Muffle furnace?)

Line 172: Relased from the Crystal lattice of mud. (this is not complete sentence,..)

It is difficult to accept, that Pb-O is destroyed

Line 174: What is difference between Figure 1 and Figure 6 concerning to lead?

line 188. In which time?

Line 196: What is the leaching rate of  other elements:Fe, Mn, Ca,..

Why did you not present a leaching Efficiency of lead  in time? Without kinetics of leaching you can not give real Explanation of leaching process

line 217: Figure 9 (in which time)

Line 224. the mass Transfer effect can be increased using higher stirring Speed, but you did not investigate it

Line 243: What is ultrasound frequency at 150 W and 450 W?

Line 262. You have written " conditions conditions". Please to correct it

Line 263-CAn you write the chemical reaction for Dissolution of CaSO4 and PbSO4

Line 272, 272-"and Migration behaviour of lead have obvious leaching effect lead". CAn you check this sentence?

Line 296: The presence of slag is not connected with your leaching process. CAn you delete it.

Line 297. CAn you give Information about leaching of lead at Figure 16 starting from PbSO4

Line 313, 314-"x-is the leaching rate of electrolytic manganese mud", or x is the leaching rate of lead from the electrolytic manganese mud

Line 330,331-  "A high pressure of about 5 x 107 Pa" ( or a high pressure of about 5 x 107 Pa). What is correct?

Line 339, 342-conventional (not conventionl)


General comments

The pH-Values of leaching process shall be mentioned

The stirring Speed was constant, but this is most important Parameter for Diffusion controlled process

CAn you give the values of particle size Distribution of used sample

What is chemism of the roasting and leaching process. Can you give chemical equations in order to present the studied processes

Diagramm of leaching Efficiency of lead (manganese, iron, calcium) in time is missing

Can you propose your model for lead removal from anode mud

What is selectivity of leaching process

What is final product after your Treatment

Is it possible to make a scale up of your process with roasting and ultrasound leaching

What is with gas Analysis after the roasting?


Author Response

Response to Reviewer 2 Comments

Reviewer 2:

Question 1: Line 13- leaching with Ammonium Acetate

Response:  I have revised the manuscript according to the reviewer’s suggestion .

Question 2: Line 22-Lead

Response:  I have revised the manuscript and added the keywords according to the reviewer’s suggestion .

Question 3: Line 43: which impurities?

Response: The impurities is lead, and I have revised the manuscript according to the reviewer’s suggestion .

Question 4: Line 64: leaching of lead with ammonium acetate

Response: I have revised the sentence and corrected the inappropriate place according to the reviewer’s suggestion .

Question 5: Which process? Leaching process of lead?

Response: The process is leaching process of lead, and I have revised the sentence

Question 6: Line 76. What is grain size after milling, Filtration and drying?

Response: I have revised the manuscript and corrected the inappropriate place according to the reviewer’s suggestion .

Question 7:You mentioned the presence of PbSO4, but at Figure 1 at X-ray Analysis we found PbO2. What is correct?

Response: The author had made a mistake because of negligence and had already correct the mistake.

Question 8: Line 89- based (instead biased)

Response: I have revised the manuscript according to the reviewer’s suggestion .

Question 9: Line 138. Roasting conditions (923-1123 K, time ?, flow rate of gas? Initial weight of sample?) Which gas was introduced in the Furnace? Which reactor? (Muffle furnace?)

Response: The roasting pretreatment process is carried out in tubular resistance furnace (SK-G06123K, Tianjin Zhonghuan Laboratory Furnace Co., Ltd.). N2 is fed into the furnace at 100L/h  rate and kept for 30 minutes at the specified temperature.

Question 10: Line 172: Relased from the Crystal lattice of mud. (this is not complete sentence,..)

Response: I have revised the sentence according to the reviewer’s suggestion .

 

Question 11: Line 174: What is difference between Figure 1 and Figure 6 concerning to lead?

Response: The lead in Figure 1 and Figure 6 exists in the form of PbSO4, but after roasting pretreatment, the PbSO4 comes out of the crystal, which is conducive to subsequent leaching treatment.

Question 12: line 188. In which time?

Response: In 60min, and I have revised the manuscript according to the reviewer’s suggestion .

Question 13: What is the leaching rate of other elements:Fe, Mn, Ca,..

Response: The authors added quantitative analysis of the element to the leaching residue and found that the content of Pb and S decreased significantly compared with the raw material, and the removal effect was better. However, the content of Mn and Fe remained unchanged basically, and the Ca element was promoted leaching in the form of calcium sulfate, while part is still present in the leaching residue, so the ammonium acetate selected herein selectively leaches Pb.

Element

Pb

Mn

S

Ca

Fe

Content(wt.%)

0.362

55.92

0.126

0.934

0.987

Question 14: Why did you not present a leaching efficiency of lead in time? Without kinetics of leaching you can not give real Explanation of leaching process

Response: I have revised the manuscript and studied the effects of leaching time on leaching rate of Pb according to the reviewer’s suggestion

Question 15: line 217: Figure 9 (in which time)

Response: The experimental process is a process of gradual optimization of single factor experimental conditions. 60 minutes is chosen as the time for the study of liquid-solid ratio.

Question 16: Line 224. the mass Transfer effect can be increased using higher stirring Speed, but you did not investigate it

Response: I have revised the manuscript and added experimental study on rotating speed according to the reviewer’s suggestion

Question 17: Line 243: What is ultrasound frequency at 150 W and 450 W?

Response: The frequency of the ultrasonic instrument used in this experiment is between 19Khz to 20.5kHZ, and five gear positions are set later. The ultrasonic frequency is not necessarily related to the power, but related to the diameter of the horn. All experiments in this experiment are fixed in 3 steps, and the operating frequency measured by the frequency meter is 19.8kHZ.

Question 18: Line 262. You have written " conditions conditions". Please to correct it

Response: The author had made a mistake because of negligence and had already correct the mistake.

Question 19: Line 263-can you write the chemical reaction for Dissolution of CaSO4 and PbSO4

Response: I have added the chemical reaction for dissolution of CaSO4 and PbSO4 according to the reviewer’s suggestion .

Question 20: Line 272, 272-"and Migration behaviour of lead have obvious leaching effect lead". can you check this sentence?

Response: The author had made a mistake because of negligence and had already correct the mistake.

Question 21: Line 296: The presence of slag is not connected with your leaching process. Can you delete it.

Response: I have revised the manuscript and replaced the figure according to the reviewer’s suggestion

Question 22: Line 297. can you give Information about leaching of lead at Figure 16 starting from PbSO4

Response: I have revised the manuscript and replaced the figure according to the reviewer’s suggestion

Question 23: Line 313, 314-"x-is the leaching rate of electrolytic manganese mud", or x is the leaching rate of lead from the electrolytic manganese mud

Response: The author had made a mistake because of negligence and had already correct the mistake.

Question 24: Line 330,331- "A high pressure of about 5 x 107 Pa" ( or a high pressure of about 5 x 107 Pa). What is correct?

Response: I have revised the manuscript and corrected the inappropriate place

Question 25: Line 339, 342-conventional (not conventionl)

Response: The author had made a mistake because of negligence and had already correct the mistake.

 

General comments

Question1: The pH-Values of leaching process shall be mentioned

Response: The author measured the pH of 2mol/L ammonium acetate solution and found pH is 6.9.

Question2: The stirring Speed was constant, but this is most important Parameter for Diffusion controlled process

Response: I have revised the manuscript and added experimental study on rotating speed according to the reviewer’s suggestion

Question3:Can you give the values of particle size Distribution of used sample

Response: I have revised the manuscript and added experimental study on particle size according to the reviewer’s suggestion

Question4: What is chemism of the roasting and leaching process. Can you give chemical equations in order to present the studied processes

Response: I have revised the manuscript and supplemented the reaction formula according to the reviewer’s suggestion

Question5:Diagramm of leaching Efficiency of lead (manganese, iron, calcium) in time is missing

Response: I have revised the manuscript and supplemented the leaching efficiency of lead in time according to the reviewer’s suggestion

Question6: Can you propose your model for lead removal from anode mud

Response: In this paper, the restrictive link of the leaching process is studied by kinetics, and the model diagram of the leaching process is redrawn.

Question7: What is selectivity of leaching process

Response: The solvent used herein is a weak acid weak base salt, so that Pb+ and ACcoordination leaching, while other metal ions are not leached.

Question8: What is final product after your treatment

Response: The electrolytic manganese anode and mud after lead removal are obtained, which can be returned to the electrolytic system. The author added quantitative analysis of the element to the leaching residue

Element

Pb

Mn

S

Ca

Fe

Content(wt.%)

0.362

55.92

0.126

0.934

0.987

 

Question9: Is it possible to make a scale up of your process with roasting and ultrasound leaching

Response: Roasting pretreatment can change the phase of electrolytic manganese anode mud and release lead sulfate from the lattice, which is beneficial to leaching of lead. Therefore, there is no complex chemical reaction with air in the experimental process. In the later stage, the muffle furnace and the ultrasonic generator can be used in parallel to carry out the expanded experiment, and it has a promising application prospect.

Question10: What is with gas Analysis after the roasting?

Response: Since the roasting temperature does not reach the decomposition temperature of calcium sulfate and lead sulfate, after passing through the exhaust gas absorption device, the main component of the exhaust gas is N2, so there no special explanation is given in the manuscript.

 

Author Response File: Author Response.pdf

Round  2

Reviewer 3 Report

This improved version shall be published in present form in Metals. Thank you for your improvement.

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