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Trimethyl phosphite adsorbed on silica: An NMR and infrared study

Journal Article · · Journal of Physical Chemistry; (United States)
DOI:https://doi.org/10.1021/j100156a061· OSTI ID:5234485
 [1]; ;  [2]
  1. Simon Fraser Univ., Burnaby, British Columbia (Canada)
  2. Univ. of Ottawa, Ontario (Canada)

Infrared spectroscopy and phosphorus-31 magic angle spinning nuclear magnetic resonance spectroscopy have been used to study the adsorption of trimethyl phosphite (TMP) on silica. At 23 C TMP reacts rapidly with surface silanol groups to give SiOCH{sub 3} as a chemisorbed product and liquid dimethyl phospite (DMP). However, formation of DMP ceases when about half of the SiOH groups have been consumed because DMP strongly hydrogen bonds to the remaining silanols thereby inhibiting further reaction between TMP and SiOH. TMP also undergoes isomerization to dimethyl methylphosphonate (DMMP) which is catalyzed by SiOH. As the number of initial silanol groups is decreased (by using higher temperatures of vacuum activation) the quantity of DMP produced decreases whereas that of DMMP increases. A mechanism for formation of DMP and DMMP has been suggested. At 100C isomerization does not occur, all SiOH groups are consumed, and the major product is DMP/SiOCH{sub 3} accompanied by a small quantity of a chemisorbed phosphorus-containing species having the proposed structure (SiO){sub 2}P-H({double bond}O). The latter is stable up to 400C. If TMP is heated with silica from 100 to 400C, in addition to SiOCH{sub 3}, the major new chemisorbed product of the reaction which can be identified by IR and NMR is (SiO){sub 2}P-Me({double bond}O) (Me = CH{sub 3}). The advantages of a combined IR-NMR approach is discussed.

OSTI ID:
5234485
Journal Information:
Journal of Physical Chemistry; (United States), Journal Name: Journal of Physical Chemistry; (United States) Vol. 95:3; ISSN JPCHA; ISSN 0022-3654
Country of Publication:
United States
Language:
English