Petrarch Systems, Inc

The starting allyltrimethylsilane can be prepared in satisfactory yield by the procedure of Sommer. It can also be purchased from PCR Inc., Aldrich Chemical Company, Inc., Fluka A. G., Petrarch Systems Inc., and Tokyo Kasei Kogyo Co., Ltd. The checkers employed material from Petrarch. 

Chiorotrimethyl si 1ane was supplied by Petrarch Systems, Inc., and used without further purification. 

Silicon Compounds Registrar and Review, Petrarch Systems, Inc., Bristol, PA 1984... 

Materials. Methyl methacrylate was a product of Rohm and Haas, and t-butyl methacrylate was obtained from Polvsciences, Inc. Potassium trimethylsilanolate (PTMS) was obtained from Petrarch Systems, Inc. Anhydrous lithium iodide, trimethylsilyl iodide (TMSI), and n-butyllit.ium (in hexanes) were purchased from Aldrich Chemical Co. 

Chloromethyltrimethylsilane, obtained from Petrarch Systems Inc., was purified by distillation at 97 C under atmospheric pressure. 

Chlorotriraethylsilane was obtained from Petrarch Systems, Inc., or Shin-etsu Kagaku Co., and distilled from calcium hydride before use. 

PS118, PS160, PS340, PS463, PS537, and PS732) were obtained from Petrarch Systems, Inc. For the IR spectra a Nicolet MX-10 FT-IR spectrometer was used at a resolution of 1 cm". The UV spectra were measured on a Model DMS 90 Varian Associates UV-Visible spectrophotometer which was connected to an Apple 11+ desktop computer, equipped with an in-house modified Varian Associates software package. Other experimental details are described elsewhere(3). 

N,N-Oimethylaminotrimethylsilane is available from Petrarch Systems, Inc. Care should be taken to assure that there is no free dimethyl amine present. Commercial samples can be purified by distillation through a 6"-Vigreux column, bp 86-87°C. The submitters used a spinning band column for removal of hexamethyldisiloxane, bp 99-100°C, which is present as a contami nant. 

Trimethylchlorosilane was from Petrarch System Inc. (Bristol, PA), whereas n-octyl-dimethylchlorosilane, pyridine (anhydrous, water content below 0.003%) and solvents were from Aldrich Chemical Co. (Milwaukee, Wl). All materials were used without additional purification. The MCM-41 sample used in the current study was a previously reported large-pore MCM-41 prepared by post-synthesis hydrothermal restructuring [21]. 

Standard solutions of methanol were prepared in distilled water using GR methanol (EM Science, 99.8%). Trimethylmonomethoxysilane (TMMS), methyl-trimethoxysilane (MTMS), and ethyltrimethoxysilane (ETMS) were obtained from Petrarch Systems Inc., Bristol, PA. All the silanes were distilled under vacuum prior to use and stored at 5°C. A liquid-phase, 3C-NMR spectrum of each silane showed no presence of methanol, which indicates little or no hydrolysis of the methoxy groups. 

The precursor used to create the 3-APTHS solutions was 3-aminopropyl-triethoxysilane (3-APTES). Commercial 3-APTES obtained from Huls Petrarch Systems Inc. was twice vacuum-distilled. Individual ampules were filled with the distilled precursor and sealed for later use. Triply-distilled HPLC grade water was used to prepare the 3-APTHS solutions used for sample treatment. For isotopically labelled 3-APTHS studies, we used 99 atom % 15N labelled 3-APTES, and 97.8 atom % l80 labelled water. Both compounds were obtained from MSD Isotopes [12]. The substrates used were polished Si wafers 1.5 cm in diameter. The Cr was sputter-deposited to a thickness of 1000 A onto one half of the Si wafer so that both the Si and Cr surfaces had identical preparation histories up to and including the analysis for every sample prepared. 

Cold-rolled steel panels were purchased from Advanced Coating Technologies, Inc. (Hillsdale, Michigan). Silane chemicals (methylsilane, trimethylsilane, and tetramethylsilane) were purchased from Petrarch Systems, Inc. The silane plasma-deposited steel was then dip-coated with a polymer film 10-25 pim thick. The polymer coating resins used were silane-modified polymers with functionalities such as hydroxyl, acrylate, or amine. 

Materials. Trimethylsilylmethyl methacrylate (Sl) and chloro-methylstyrene (CMS) (mixed m,p isomers) were obtained from Petrarch Systems Inc. and Dow Chemical Co. Inc., respectively. Both monomers were purified by distillation at reduced pressure. Copolymers were prepared by free-radical solution polymerization at 85 C in toluene. Reactions were initiated using benzoyl peroxide. 

Trimethylsilylmethylphenol and o-cresol were obtained from Petrarch Systems, Inc. and Aldrich Chem. Co. Inc., respectively. Silylated novolac (Sl-novolac) resins were prepared by condensation polymerization of p-trimethylsilylmethyl phenol, o-cresol and formaldehyde. Poly(2-methyl-l-pentene-sulfone) (PMPS) was prepared as described in the literature (12). 

The commercially available adhesion promoters (Petrarch Systems Inc.) tested were applied as dilute solutions 0.3 - 7% by weight in acetone or xylene, or as for hexamethyldisilazane (HMDS), either as a liquid or vapor (Imtec Star 2000). 

Synthesis. Synthesis of the copolymers was performed by a hydrosilylation reaction of poly(dimethylsiloxane-co-methylhydrosiloxane) (Petrarch System, Inc.) and a-olefins of various lengths (Aldrich). A round-bottomed flask equipped with a magnetic stirring bar, condenser, and calcium chloride tube was charged with a 50% solution of the reactants (up to 10% molar excess of a-olefin) in dry toluene. A solution of hydrogen hexachloroplatinate(IV) in diglyme-isopropyl alcohol (150 ppm Pt) was then added to the reaction mixture. The reaction mixture was stirred at 60 °C for 3 h. At the end of this period, the mixture was refluxed with activated charcoal for 1 h and filtered while hot. Finally the solvent and excess a-olefins were removed under reduced pressure (67 Pa at 100 °C). The reaction proceeded to completion as evidenced by the absence of the Si-H absorption at 2130 cm" in the IR spectra. Residual a-olefin in the purified polymers was determined by gas-liquid chromatography. In all polymers, residual a-olefin was less than 1.5 wt %. 

Materials. Octamethylcyclotetrasiloxane, D4, was generously supplied hy General Electric Company. l,3-Bis(3-aminopropyl)tetramethyldisiloxane (to be referred to subsequently as aminopropyldisiloxane) was obtained from Petrarch Systems, Inc. These materials were dried over calcium hydride and vacuum distilled prior to use. Potassium hydroxide, tetramethylammonium hydroxide pentahydrate, and tetrabutylphosphonium bromide used in the preparation of the siloxanolate catalysts were used as received from Aldrich. 

The PD MS chains used were hydroxyl terminated and were obtained from Petrarch Systems, Inc. (Bristol, PA). Their number-average molecular weights (MJ were 660 and 880 g/mol for the short chains and 21.3 X 10 g/mol for the long chains (7). Their polydispersity indices would be expected to be 2. 

Nippon Carbon Company, Ltd., 619 Nippon Telegraph and Telephone Corporation, 515 North Dakota State University, 3 Petrarch Systems, Inc., 181 S. C. Johnson and Son, Inc., 91 Sandia National Laboratories, 227, 241, 341, 379, 459... 

Diphenylmethylchlorosilane was purchased from Petrarch Systems, Inc., and distilled from calcium hydride (bp 85°C/0.1 mm) prior to use. A 187.5-mmol scale reaction using diphenylmethylchlorosilane purchased from Petrarch Systems and used without purification gave an 89% yield of the a-silyl ester. 

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