Improved Regioselective Mononitration of Naphthalene over Modified BEA Zeolite Catalysts
Round 1
Reviewer 1 Report
This manuscript reported the nitration of naphthalene over different HBEA zeolite catalysts. The prepared catalysts were characterized by several techniques for revealing the physiochemical properties changes before and after reaction. The effect of reaction temperature and the amount of zeolites on 1-nitronapthalene was investigated. This manuscript can be accepted with major revision. The detailed comments are as follows:
1. The introduction is quite simple, and more recent work on the use of zeolites in the nitration of naphthalene should be introduced.
2. The novelty of this work should be highlighted. The date reported in this work should be compared with other reported work.
3. The detailed preparation of catalysts should be provided.
4. In the 2.2 Nitration with nitric acid and acetic anhydride: what’s the role of acetic anhydride?
5. The results of catalytic performance with catalysts should be discussed.
6. As shown in Table 2, the addition of HBEA-280/500 and HZSM-5 will lead to a low yield. The author should be explained this.
7. How about the experimental error as shown in Table 2-3.
8. As shown in Table,5 the increase of amount of zeolite will lead to high yield. Why not further increase of amount of zeolite?
Author Response
Response to Reviewer 1 Comments
- The introduction is quite simple, and more recent work on the use of zeolites in the nitration of naphthalene should be introduced.
Response 1: Introduction revised
- The novelty of this work should be highlighted. The date reported in this work should be compared with other reported work.
Response 2: The novelty of this work should be highlighted in the introduction and conclusion, The date reported in this work should be compared with other reported work in the introduction.
- The detailed preparation of catalysts should be provided.
Response 3: The preparation of the catalysts has been added.
- In the 2.2 Nitration with nitric acid and acetic anhydride: what’s the role of acetic anhydride?
Response 4: The role of acetic anhydride has been added.
- The results of catalytic performance with catalysts should be discussed.
Response 5: The results of catalytic performance with catalysts have been discussed.
- As shown in Table 2, the addition of HBEA-280/500 and HZSM-5 will lead to a low yield. The author should be explained this.
Response 6: The a low yield has been explained.
- How about the experimental error as shown in Table 2-3.
Response 7: Error in Table 2-3 has been corrected.
- As shown in Table,5 the increase of amount of zeolite will lead to high yield. Why not further increase of amount of zeolite?
Response 8: Increase of amount of zeolite was investigated.
All modified parts are marked in red colour.
Reviewer 2 Report
This work reports on the nitration of naphthalene using beta zeolite catalysts. The authors characterized the catalysts before and after the nitration reaction by N2-isotherm, XRD, FT-IR, SEM and EDS. The results showed the HBEA-25 catalyst retained its structure after the reaction. The authors evaluated the catalytic performance of the zeolitic catalysts and revealed that the HBEA-25 catalyst was recyclable and gave the good regioselectivity in 1-nitronaphthalene by the nitration reaction.
However, the title may not be appropriate as the metal-modified zeolites are less selective than the unmodified zeolite.
Other comment shown below.
Introduction
It is desirable to mention the importance of selectivity in nitronaphthalene synthesis. For example, naphthylamine is obtained by reduction of nitronaphthalene. 1-naphthylamine is useful but 2-naphthylamine is carcinogenic and highly toxic.
Experimental
There seems to be a lack of description about preparation of the catalysts.
Table 3
‘CeBEA-25’ may be fixed to ‘CuBEA-25’.
Line 171
‘entry 5 in Table 2’ may be fixed to ‘entry 5 in Table 3’.
Line 178
‘H-type BEA-zeolite’ may be fixed to ‘H-form BEA-zeolite’.
Table 6
‘2:3 ration’ may be fixed to ‘2:3 ratio’.
Author Response
Response to Reviewer 2 Comments
Point 1: However, the title may not be appropriate as the metal-modified zeolites are less selective than the unmodified zeolite.
Response 1: the title is changed to“Improved regioselective mononitration of naphthalene over modified BEA zeolite catalysts”
Point 2: Introduction
Response 2: Introduction revised
Point 3: Experimental
Response 3: The preparation of the catalysts has been added.
Point 4: Table 3
Response 4: Table 3 has been revised
Point 5: Line 171 ‘entry 5 in Table 2’ may be fixed to ‘entry 5 in Table 3’.
Line 178 ‘H-type BEA-zeolite’ may be fixed to ‘H-form BEA-zeolite’.
Response 5: Line 171 and Line 178 had been revised.
Point 6: Table 6 ‘2:3 ration’ may be fixed to ‘2:3 ratio’.
Response 6: Error in Table 6 has been corrected.
All modified parts are marked in red colour.
Round 2
Reviewer 1 Report
This manuscript can be accepted.
