Vacuum laboratory

In the development of thiophene chemistry three periods can be clearly distinguished the Victor Meyer era, the Steinkopf period, and the modem development starting with the discovery of the synthesis of thiophene from butane and sulfur, making thiophene potentially available in unlimited amounts. Hartough in his well-known monograph, has reviewed the intense and hectic thiophene research toward the end of the 1940 s carried out mainly at the Socony-Vacuum laboratories, but also at many academic institutions. An article by Nord et al. appeared in 1955 in which the research work in thiophene chemistry at Fordham University, as well as progress in general up to 1954, was reviewed. 

Vacuum may be natural or artificially produced. Natural vacuum, for example, occurs on the lunar surface or in the interstellar space where one should however speak of numerical density of particles ( 1 particle/cm3) instead of pressure. In the intergalactic space, the density is around 1 particle/m3. Natural vacuum laboratories in use are, for example, the Space Shuttle or Space Stations, but we will deal only with artificial vacuum, produced by pumps inside a container. 

Actual tests on a sample of Sovacide F outdoor fog oil, according to data furnished by Socony-Vacuum Laboratories, showed the following characteristics ... 

Research and Development Department, Socony-Vacuum Laboratories, Paulsboro, N. J. 

Determined spectrographically from measurements made in these laboratories Humble Oil and Refining Co., Baytown, Tex. Socony-Vacuum Laboratories, Paulsboro, N. J. Standard Oil Development Co., Elizabeth, N. J. Sun Oil Co., Norwood, Pa. 

From 1943 to 1948 he was consultant to Hydrocarbon Research, Inc., and from 1948 until his death a consultant to the Socony-Vacuum laboratories in connection with the synthesis of gasoline and the cracking and re-forming of petroleum by catalytic processes. 

Rejtrmces. Blicke and Burckhalter, J. Am. Chem. Sec., 44, 478 (1942). The method has been checked in the Socony-Vacuum Laboratories. In cases where di-(2-thienyl)methane can be conveniently separated irom the end-products, the crude reaction mixture can be conveniently utilized without resorting to distillation of the 2-thenyl chloride. Over-all yields normally are improved in this manner. The author has found that it is convenient to prepare this compound using equimolar quantities of hydrochloric acid, thiophene, and formaldehyde, omitting the use of hydrogen chloride. The yields tire comparable when the above proced ire is employed. 

Rejereme. Hartough and Conley, J. Am, Chem. Soc., 69, 3096 (1947). The procedure has been checked by H. E. Rasmussen, Socony-Vacuum Laboratories, on scmipilot-plant scale operations in a 30-gal. Pfaudler kettle. The yields are slightly improved on larger scale production. 

Rejerences. The procedure above is a modification of the method of Steinkopf and Hopner, Ann., 501, 174 (1933), adapted by R. Smith, Socony-Vacuum Laboratories. Burton and Davy, J. Chem. Soc., 1948, 525, obtained a 50% yield of 2-thiophene-sulfonyl chloride by Steinkopf and Hopner s method. 

Rejmnee. The method was developed in the Socony-Vacuum Laboratories from the method of Rinkes, Rec, trad, chim., 53, 648 (1934) 55, 991 (1936). See Chapter VII for other references. 

Rejerence. This procedure is a modification of the method of Stcinkopf and Haiiskc, Ann., 527, 247 (1937), used in the Socony-Vacuum Laboratories. Sec also Stcinkopf, Die Chemie des TIuophens, page 43, for a modification of a method to introduce the iodine evenly to the reaction mixture. 

Reference. Hartough and Kosak, J. Am. Chem. Soc., 69, 3093 (1948). See also, Kosak and Hartough, Organic Synthe.m, 28, 1 (1948). This reaction has been checked by L. G. Conley, Socoiiy-Vacuum Laboratories. It has been successfully extended to the preparation of 2-propanoyl- and 2-butanoylthiophene without modification. The yields tire in the range of 85-95% of theory. 

Reference. This is a modification of the method of Steinkopf, Jacob, and Pena, Ann., 512, 136 (1934), adapted by Caesar, Socony-Vacuum Laboratories. 

Sncony-Vacuum Laboratories (A Division of Socony-Vacuum Oil Co., Inc.), Research and Development Department, Paulsboro, New Jersey... 

C. D. Prater, Socony-Vacuum Laboratories A Division of Socony-... 

Samples were melt pressed in a vacuum laboratory hot press (Carver Press, Model C) at 160°C for 30 min. The molded films were then allowed to cool to room temperature under vacuum. A dual temperature chamber for the melt crystallization experiments consists of two large thermal chambers maintained at the melt temperature (Ti = 160°C) and the crystallization temperature (Ts = 81°C, 83°C, 86°C, 89°C, 92°C or 96°C). After 5-10 min at Ti, the copper sample cell was transferred rapidly ( 2 s) to the other chamber by means of a metal rod connected to a pneumatic device. A detailed description of the arrangement of the sample and of the two detectors used to measure WAXS and SAXS simultaneously has been provided previously [32]. Each polymer sample within the copper cell was 1.5 mm thick and 7 mm in diameter and was contained between two 25 im thick Kapton films. The actual sample temperature during crystallization (T2) and melting (Ti) was monitored by means of a thermocouple inserted into the sample cell. The crystallization temperature was usually reached 120 s after transfer without overshooting. Under isothermal conditions the fluctuations in the sample temperature are less than 0.5°C. Unless stated otherwise, all references to time are times elapsed after transferring the sample to the crystaUization chamber. 

After extrusion the obtained granulates should be dried in a vacuum laboratory drier at a temperature of 50 °C for 6 hours until a humidity of 4-6% is achieved (Figure 11.4). 

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