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Investigations in Supercritical Fluids

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In situ NMR Methods in Catalysis

Part of the book series: Topics in Current Chemistry ((TOPCURRCHEM,volume 276))

Abstract

In recent years, supercritical fluids (SCF) have drawn substantial interest as modern solvents for chemical reactions, separations, and extractions in the area of basic research as well as in industrial processes. Especially, supercritical carbon dioxide (scCO 2) is a desirable replacement for organic solvents because it is inexpensive, nontoxic, nonflammable, environmentally benign, and exhibits ease of recycling and disposal. This contribution provides for an overview of the basic physical properties of SCFs, such as density tuning, diffusivity, viscosity and interaction with fluorinated compounds. In addition, in situ NMR spectroscopy in toroid cavity autoclaves and the specialized technique of parahydrogen-induced polarization are introduced as superior and beneficial for investigating physical properties and chemical reaction in SCFs. The concept of turnover frequencies and active sites in catalysis is reviewed, while specific examples are given for homogeneous hydrogenations and hydroformylations in scCO2. The emerging field of colloid catalysis in SCFs is illustrated with the ultrafast single-phase hydrogenation of alkynes using bimetallic colloids in inverted polymer micelles as the catalyst.

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Abbreviations

B 0 :

Static magnetic field in NMR spectroscopy

B 1 :

Alternating magnetic field of NMR radiofrequency pulses

BARF:

Tetrakis(3,5-bis(trifluoromethyl)phenyl) borate

C1 :

Compound with a single carbon atom

D :

Diffusion coefficient

E :

Energy

k :

Boltzmann's constant

MAGROFI:

Magnetization-grating rotating-frame imaging

M n :

Average molecular mass in atomic mass units

PEEK:

(Polyether)ether ketone

PHIP:

Parahydrogen-induced polarization

p c :

Critical pressure

p(CO2):

CO2 pressure

p(H2):

H2 pressure

p-H2 :

Parahydrogen

r A :

Hydrodynamic radius

scCO2 :

Supercritical carbon dioxide

SCF:

Supercritical fluid

SCR:

Substrate-to-catalyst ratio

t :

Time

T :

Temperature

T 1 :

Spin-lattice relaxation time constant

T c :

Critical temperature

TCA:

Toroid cavity autoclave

TCD:

Toroid cavity detector

TOF:

Turnover frequency

TON:

Turnover number

η:

Dynamic viscosity

ν:

NMR resonance frequency

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Authors and Affiliations

  1. Department of Neurology II, Otto von Guericke University, Leipziger Str. 44, 39120, Magdeburg, Germany

    Heiko G. Niessen

  2. Department of Chemistry, University of Missouri-Rolla, 1870 Miner Circle, 65409-0010, Rolla, MO, USA

    Klaus Woelk

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  1. Heiko G. Niessen
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  2. Klaus Woelk
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Correspondence to Klaus Woelk .

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Joachim Bargon Lars T. Kuhn

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Niessen, H.G., Woelk, K. (2005). Investigations in Supercritical Fluids . In: Bargon, J., Kuhn, L.T. (eds) In situ NMR Methods in Catalysis. Topics in Current Chemistry, vol 276. Springer, Berlin, Heidelberg. https://doi.org/10.1007/b135837

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