From: Richard Palluzi <000006c59248530b-dmarc-request**At_Symbol_Here**LISTS.PRINCETON.EDU>
Subject: Re: [DCHAS-L] Hydrothermal and solvothermal reactor safety
Date: Wed, 28 Aug 2019 05:50:05 -0400
Reply-To: ACS Division of Chemical Health and Safety <DCHAS-L**At_Symbol_Here**PRINCETON.EDU>
Message-ID: 003a01d55d85$f8d611b0$ea823510$**At_Symbol_Here**verizon.net
In-Reply-To


You may want to look at these articles which address some aspects of the general safety issues.

 

Spill Containment: An Often-Overlooked Hazard in Research (Chemical Engineering, Sept 2017)

Performance Analysis of Small Size Pilot Plant and Laboratory Relief Valves (Process Safety Progress, Sept 2003)

Temperature Control in High Pressure Continuously Stirred Reactors (Chemical Engineering, May 1990)

 

 

Richard Palluzi

PE, CSP

 

Pilot plant and laboratory consulting, safety, design,reviews, and training

www.linkedin.com/in/richardppalluzillc/

 

Richard P Palluzi LLC

72 Summit Drive

Basking Ridge, NJ 07920

rpalluzi**At_Symbol_Here**verizon.net

908-285-3782

 

From: ACS Division of Chemical Health and Safety <DCHAS-L**At_Symbol_Here**PRINCETON.EDU> On Behalf Of Jeffrey Lewin
Sent: Tuesday, August 27, 2019 4:43 PM
To: DCHAS-L**At_Symbol_Here**PRINCETON.EDU
Subject: Re: [DCHAS-L] Hydrothermal and solvothermal reactor safety

 

Thanks, Tilak,

 

I'm not personally using them - I'm trying to work through general safety concerns, especially using them for chemical reactions.  One example is creating Boron Quantum Dots using BN and DMF in 50ml reaction vessels.

 

See: https://www.ncbi.nlm.nih.gov/pubmed/26574683

 

Jeff

 

Jeff

 

 

On Tue, Aug 27, 2019 at 3:28 PM TILAK CHANDRA <0000058f112ac338-dmarc-request**At_Symbol_Here**lists.princeton.edu> wrote:

Hi Jeff:

If you can describe how you are going to use these vessels, I will be happy to provide you a SOP and other safety information.

Are you going to use these vessels for the digestion purpose or chemical reaction?

 

Please let me know.

 

Regards,

Tilak

 

From: ACS Division of Chemical Health and Safety <DCHAS-L**At_Symbol_Here**PRINCETON.EDU> On Behalf Of Jeffrey Lewin
Sent: Tuesday, August 27, 2019 11:01 AM
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.

 

 

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

--- For more information about the DCHAS-L e-mail list, contact the Divisional membership chair at membership**At_Symbol_Here**dchas.org Follow us on Twitter **At_Symbol_Here**acsdchas

--- For more information about the DCHAS-L e-mail list, contact the Divisional membership chair at membership**At_Symbol_Here**dchas.org Follow us on Twitter **At_Symbol_Here**acsdchas


 

--

Jeff Lewin

Chemical Safety Officer

Research Integrity Office

Laboratory Operations

207 Advanced Technology Development Complex (ATDC)

Michigan Technological University

--- For more information about the DCHAS-L e-mail list, contact the Divisional membership chair at membership**At_Symbol_Here**dchas.org Follow us on Twitter **At_Symbol_Here**acsdchas

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