Retraction Watch

Tracking retractions as a window into the scientific process

Chemists lose JACS silicone paper over data dispute

with 6 comments

Journal of the American Chemical SocietyA pair of chemists at Ball State University in Indiana has lost their paper in the Journal of the American Chemical Society on silicone in a dispute over the provenance of the data.

The article, “Silicone Electrosynthesis from Silica Raw Materials at Room Temperature,” was written by Jeffrey E. Dick, a grad student, and Daesung Chong. It appeared in JACS in March.

As the abstract explained:

Here, we describe a method of synthesizing silicones at room temperature in a one step, one pot electrochemical reaction. The current energy intensive method to produce silicones involves carbothermic reduction at temperatures exceeding 2000 °C over coal, which consequentially produces environmentally harmful gases, CO and CO2. Even after this, the metallic Si is subjected to follow up chemical reactions described by Eugene Rochow in 1945 to produce the final silicones. The electrochemical synthesis is achieved by bulk cathodic electrolysis of methanol in the presence of raw SiO2 materials (sand or quartz) at Eappl = -2.7 – -3.0 V vs Fc/Fc+ couple in two organic solvent/electrolyte systems. Electrodes are a nickel wire cloth, a nickel-chromium wire, a graphite plate, or a Pt basket. The major products in order of relative yields were octamethylcyclotetrasiloxane (D4), hexamethylcyclotrisiloxane (D3), and decamethylcyclopentasiloxane (D5). Ranges for relative yields, or the ratio of the D3, D4, or D5 to the total amount of silicones produced, are 17-28%, 64-80%, and 5-8%, respectively. We also provide evidence for a possible mechanistic pathway involving the initiation of a methyl radical followed by radical propagation to the final products through the intermediate dimethyldimethoxysilane. To the best of our knowledge, this is the first report of the reduction of silicon-containing raw materials at room temperature to yield silicones.

According to the retraction notice, however, that last line was premature:

This Communication has been retracted at the request of the authors and Ball State University. The publication has been removed due to intellectual property rights concerns.

Alth0ugh we’re not chip makers, the economic potential of a simpler way to make silicones seems pretty clear — and we can see why someone, or an institution, might be eager to protect a nascent royalty stream for such a technology. We’ve asked the authors for more information about the nature of the “concerns” and will update this post if we hear from them.

Hat tip: Rolf Degen

Comments
  • FX Coudert (@fxcoudert) May 2, 2014 at 1:34 pm

    For IP purposes, can you really un-publish something? I mean, once it’s been made public even for a day, doesn’t it count as published?

    • DocMartytn May 3, 2014 at 9:05 am

      Exactly. We lost our world IP rights because a journal ‘helpfully’ posted the proof copy of an accepted paper online on Friday afternoon instead of Monday, as promised.

    • Kenrod May 3, 2014 at 9:28 am

      In the US a patent must be filed within one year of publication by the inventor. After one year the publication will be used by the examiner as prior art.

      • DocMartytn May 3, 2014 at 11:45 am

        That is the US position, the rest of the world demands that the Patent is filed before public disclosure; you basically lose all your foreign rights if the basis of the IP is published anywhere; this includes posters at conferences or even talks in an institution with people present who do not have a NDA agreement (typically people within an institution have a standing NDA), so a lab talk with a ‘visitor’ can count as a public disclosure.

  • Kenrod May 2, 2014 at 2:56 pm

    According to Chong’s page at Ball State (link above) he was at Dow Corning’s “Siloxane site” prior to joining the Ball State faculty. I suspect that this has something to do with the retraction and IP issues.

  • Andrew P July 10, 2014 at 5:36 pm

    I have a copy of the paper that I saved before it was retracted.

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