From: Dr Bob <drbob**At_Symbol_Here**FLOWSCIENCES.COM>
Subject: Re: [DCHAS-L] Hydrothermal and solvothermal reactor safety
Date: Tue, 27 Aug 2019 17:41:15 +0000
Reply-To: ACS Division of Chemical Health and Safety <DCHAS-L**At_Symbol_Here**PRINCETON.EDU>
Message-ID: e8329b8643624d59986d7b90ed7e21db**At_Symbol_Here**flowsciences.com
In-Reply-To


Hi Jeff!

 

These guys make pressure vessels and related equipment and instruments. They may have manuals on existing equipment highlighting procedures and safety steps.

 

https://www.parrinst.com/reactors-pressure-vessels/

 

Dr. Bob Haugen

Director of Product and Technology Development

Flow Sciences, Inc.

 

910 332 4878

 

Containment Products ¥ Get a Quote/Consultation ¥ Get Support/Replacement Parts

 

CONFIDENTIALITY NOTE: This e-mail, including all attachments, is directed in confidence solely to the person(s) to whom it is addressed, or an authorized recipient, and may not otherwise be distributed, copied or disclosed. The contents of this transmission may also be subject to intellectual property rights and all such rights are expressly claimed and are not waived. The contents of this e-mail do not necessarily represent the views or policies of Flow Sciences Inc. or its employees.

 

From: ACS Division of Chemical Health and Safety [mailto:DCHAS-L**At_Symbol_Here**PRINCETON.EDU] On Behalf Of Jeffrey Lewin
Sent: Tuesday, August 27, 2019 12:01 PM
To: DCHAS-L**At_Symbol_Here**PRINCETON.EDU
Subject: [DCHAS-L] Hydrothermal and solvothermal reactor safety

 

I'm looking for any information on the safe operation of hydrothermal and solvothermal reaction chambers.  They are sometimes also referred to as "autoclaves" (different than what this biologist thinks of) and "bombs." which might be the best description having recently viewed pictures of one that catastrophically failed (no injuries, plenty of damage).

 

From what I can find Googling - they've been around commercially for some time (10 or more years?); I found very little in written SOP's, but the discussion on researc- gate I've seen several comments that if not handled correctly, the results can be energetically problematic.

 

See https://www.toptionlab.com/Hydrothermal-synthesis-reactor/teflon-lined-hydrothermal-reactor.html for an example of a reactor.

 

So questions for the group:

 

Does your institution have specific guidance on using these such as limiting the size of reaction chambers?  

 

Do you have minimum engineering controls for containment (blast shielding, etc.)?  

 

Does your institution explicitly prohibit using them?

 

Two critical administrative controls I've seen are:

 

1) not overfilling the reaction chamber, allowing headspace for gas formation.  For hydrothermal reactions, this seems pretty well established since water expands about 25% at the temperatures these are operating at (190-220C).  For solvents, it doesn't seem to be as straight forward.  For example, I've not been able to find an expansion factor for dimethylformamide (DMF).

 

2) not heating and cooling too fast.  The instructions I've seen with reactors say things like don't heat or cool faster than 5C/min.  But I've seen instructions that go outside those guidelines (8C/min) and several that say "cool naturally" i.e. not at 5C/min (I've also seen discussions that specifically advise against quenching them).  

 

Any insight would be appreciated.

 

Jeff

 

 

--

Jeff Lewin

Chemical Safety Officer

Research Integrity Office

Laboratory Operations

207 Advanced Technology Development Complex (ATDC)

Michigan Technological University

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