Vol.3 No.2 2010

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Research paper : Establishment of compact processes (A. Suzuki et al.)−161−Synthesiology - English edition Vol.3 No.2 (2010) Discussions with Reviewers1 OverallComment (Koh Harada, AIST Tohoku)Please explain why you used both words of “integration” and “concert” in the subtitle.Answer (Akira Suzuki)The subtitle “Integration and concert of high-pressure microengineering and supercritical fluid”, expresses the point that these integrations are not merely “1+1=2”, but the property of supercritical fluid may become 3 or 4 or anything by using microengineering. Recently, in the world of chemistry, the phrase, “concerted reaction field”, comes into use. The word “integration” does contain the element that it is more than simply getting together, and therefore to enhance the reader’s understanding, I deleted “concert”, and the subtitle shall be “Integration of high-pressure microengineering and supercritical fluid”.Comment (Yoshiro Owadano, Research Coordinator, AIST)For non-specialist readers, I think you should write clearly to which category the compact process described in this paper belongs:1) Makes possible the synthesis that was conventionally impossible2) Achieves lower environmental load or higher yield compared to the conventional methodIf 2) is the case, please indicate as much as possible, what the volume of production (possibility) or rate of energy saving is in quantitative terms, or what are the figures set as the goal. For example, I think you should describe a more specific future image, such as what manufacturing method and in which industry this will be used in the sections, “Numbering up strategy” and “Future development”.Answer (Akira Suzuki)The compact process described in this paper is a high-speed, highly controllable process to convert the bulk chemicals that were produced conventionally by large-scale concentrated production to low-volume distributed production for producing the necessary amount at the necessary place. Therefore, it is not a process for synthesizing products that were conventionally impossible, but is a process that has low environmental load and realizes high yield compared to the conventional processes. In this paper, two reactions (Beckmann rearrangement and nitration) are given as examples of organic synthesis. While both reactions conventionally use concentrated sulfuric acid as the acid catalyst, in the compact process, high-temperature and high-pressure water plays the role of concentrated sulfuric acid, and it is now possible to establish a process that uses no catalyst (no sulfuric acid low environmental load) and has high speed (microreaction high yield).To clarify the above discussion, we described the superiority of the micro heat exchange compared to the conventional technology in the “Numbering up strategy”. We described the possibility of increasing the production volume using the example of -caprolactam synthesis in the “Future development”.Comment (Koh Harada)I think that the phrase “compact process” used in this paper has a narrower meaning that is used specifically in the chemical industry, compared to the general usage. Please define what is the “compact process” for non-specialist readers.Answer (Akira Suzuki)In the text, we added: “The compact process here means a safe, flexible, and efficient process with low environmental load, where the cycling of resource and energy can be done easily. It also is high-speed and has highly controllable performance, and enables low-volume distributed production”.2 Balance in establishing a circulating systemQuestion (Koh Harada)In the discussion of “1 Background and objective of the research”, you state the “balance or recovery and reuse” are important. Is this a requirement to establish the circulating system?Answer (Akira Suzuki)In the large-scale concentrated production method, the amount handled is extremely high. Although reuse in other processes or at other plants may be done through the recovery of the byproduct or recycling of waste products produced in certain processes, I don’t think they provided realistic solutions due to the balance of supply and demand and the problem of transportation. The establishment of the circulating system was difficult in the large-scale concentrated production method.3 Comparison with conventional methodQuestion (Koh Harada)You would be better to mention about a comparison of your method with the conventional method at the beginning of the discussion of “2 Integration and concert of microreactor and supercritical water”.Answer (Akira Suzuki)The caprolactam synthesis by Beckmann rearrangement using concentrated sulfuric acid is a high-yield process of 98 %. On the other hand, the yield by high-temperature and high-pressure water described in Table 1 is 83 %, and is inferior in terms of numbers, but is superior in the fact that it does not use concentrated sulfuric acid at all. Here, to emphasize that the yield can be dramatically increased using supercritical water alone by precisely controlling the reaction time, we intentionally did not mention the yield of the conventional method.4 Advantage of electromagnetic inductionQuestion (Koh Harada)In “3.2 High-pressure micro heat exchanger”, what is the advantage of the electromagnetic induction method? It was written that it was not employed due to its size, but in what case would it be more advantageous?Answer (Akira Suzuki)Compared to direct energization application, the advantage of the electromagnetic induction may be that there is no need to take measures against electric leaks, and the heating intensity can be changed by how the induction coil is wound. Which is better is a case-by-case consideration, but I think for a microdevice, direct energization application is better because it does not require the induction coil.

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