Abstract: Novel benzothioxepanone and benzothioxepane thione compounds are characterized by the formula ##STR1## wherein Z is: ##STR2## R is Cl, Br, F, C.sub.1 to C.sub.8 alkyl, or C.sub.1 to C.sub.8 alkoxy; X and Y are each hydrogen, or taken together form a fused cyclopentyl or cyclohexyl ring, with the proviso that when Z is ?1!, X and Y represent a fused cyclopentyl or cyclohexyl ring; and n is 0, 1, or 2. The compounds are useful as co-catalysts in the para-directed nuclear chlorination of toluene.
Type:
Grant
Filed:
October 22, 1997
Date of Patent:
October 6, 1998
Assignee:
Occidental Chemical Corporation
Inventors:
Ramesh Krishnamurti, Sandor Nagy, Thomas F. Smolka
Abstract: An adsorbent-based air conditioning system for conditioning an air supply to an enclosed space, such as a building, room, or the passenger compartment of a motor vehicle, aircraft, or the like, utilizes interchangeable adsorbent-containing vessels. Two of the vessels are employed to condition the air supply with respect to temperature and humidity while, at the same time a third and, optionally, a fourth vessel are regenerated by drying and cooling to provide replacements vessels as needed. In operation, ambient air is dehumidified by passing through vessel 1 and the moisture collected in the vessel by adsorption. The exiting air may be cooled by means of a heat exchanger, then directed through vessel 2, containing moist adsorbent, for further cooling and humidification. The air is then supplied to the room, or other space to be conditioned.
Abstract: Disclosed is a method of reducing the UV absorption of a solvent that comprises water, an ethylene glycol, or a mixture thereof, where the solvent contains at least 0.1 ppm of a dione, particularly 3-methyl-2-hydroxy cyclopent-2-eneone or its tautomer, 3-methyl-1, 2-cyclopentanedione. The solvent is passed through an anionic exchange resin containing strong base sites. The UV absorbance of the effluent from the anionic exchange resin can be monitored and, when it increases, the resin can be reactivated by passing an aqueous solution of a base through it.
Abstract: A cleaning solvent comprising(A) about 3 to about 20 wt % of a fluorinated compound selected from the group consisting of(1) fluorocarbons having the general formulaC.sub.m H.sub.n F.sub.2m+2-nwhere m is 4 to 8, and n is 0 to m/2 if m is even and 0 to (m+1)/2 if m is odd;(2) C.sub.5 F.sub.11 NO;(3) alkyl perfluoroethers having the general formulaR.sub.1 OR.sub.2where R.sub.1 is C.sub.3 F.sub.7 or C.sub.4 F.sub.9 and R.sub.2 is CH.sub.3 or C.sub.2 H.sub.5 ; and(4) fluorochlorocarbons having the general formulaC.sub.p H.sub.q Cl.sub.r F.sub.2p+2-q-rwhere p is 3, 4, or 5, q is 1 to p-1, and r is 1 to p-1;(B) up to about 15 wt % of a C.sub.1 to C.sub.4 alkanol; and(C) the remainder benzotrifluoride.
Abstract: Disclosed is a method of making a polyimide pattern on a substrate. A solution is prepared in an organic solvent of a polyamic acid and about 1 to about 10 wt. % of a photosensitizer that becomes more water soluble when exposed to actinic light. A coating is formed of the solution on a substrate and solvent is evaporated from the coating. A positive photoresist is applied over the coating and is exposed to a pattern of actinic light. The exposed portions of the photoresist are removed as well as the exposed portions of the polyamic acid coating thereunder. The remaining photoresist is removed and the polyamic acid coating is imidized.
Abstract: Disclosed is a single phase liquid composition comprising 0.5 to 30 wt % of a benzotrifluoride solvent, about 0.5 to about 50 wt % of a glycol ether cosolvent, up to about 50 wt % of an alkanol, up to about 10 wt % of a surfactant, and the remainder water. The composition is effective in cleaning hard surfaces, stripping paint, and as a carrier.
Type:
Grant
Filed:
November 25, 1996
Date of Patent:
April 28, 1998
Assignee:
Occidental Chemical Corporation
Inventors:
Edward A. Rowe, Hang-Chang Bobby Chen, Mark E. Lindrose
Abstract: A process for the pare-directed nuclear chlorination of an alkylbenzene, such as toluene, comprises reacting the alkylbenzene with chlorine in the presence of a Lewis acid catalyst and a novel co-catalyst of the formula: ##STR1## where Z is ##STR2## and R is Cl, Br, F, C.sub.1 to C.sub.8 alkyl to C.sub.1 to C.sub.8 alkoxy; x and y are each hydrogen, or taken together form a fused cyclopentyl or cyclohexyl ring; n is 0, 1 or 2, with the proviso that when Z is ?3!, n is 0 or 1.
Type:
Grant
Filed:
December 2, 1996
Date of Patent:
February 3, 1998
Assignee:
Occidental Chemical Corporation
Inventors:
Ramesh Krishnamurti, Sandor Nagy, Thomas F. Smolka
Abstract: Disclosed is a method of making a chlorobenzene having the general formulas ##STR1## where X is Cl or F, and X' is X or CF.sub.3. A compound having the formula ##STR2## is sulfonated using at least 2 moles per mole of said compound of a sulfonating agent selected from the group consisting of sulfuric acid, chlorosulfonic acid, and mixtures thereof, to produce a sulfonated compound. The sulfonated compound is chlorodesulfonated to produce a chlorobenzene, such as 1,2,4-trichlorobenzene. Preferably, the starting material is ortho-dichlorobenzene.
Abstract: Disclosed are bis-meta-benzotrifluoride compounds having the general formula ##STR1## where each A is independently selected from the group consisting of NO.sub.2, NH.sub.2, and NH.sub.3.sup.+ Z.sup.-, Z.sup.- is an anion and B is selected from the group consisting of O, CO, S, SO, and SO.sub.2. The diamine compounds are useful as monomers in making polyimides, polyamide-imides, and polyamides.
Type:
Grant
Filed:
April 15, 1996
Date of Patent:
October 7, 1997
Inventors:
Jeffrey S. Stults, Henry C. Lin, Robert A. Buchanan
Abstract: A method of in-service cleaning an operating column by inserting into the column a lance through which a compatible liquid is dispensed at a pressure of at least about 5000 psig. Also disclosed is apparatus which comprises a column through which a fluid can pass, nozzles mounted on the outside of the column, where each nozzle comprises a flange welded to the column and a valve bolted to the flange, a lance which can be inserted through the nozzles into the column and means for dispensing a liquid through the lance at a pressure of at least about 5000 psig.
Abstract: Disclosed is a method of determining whether a solvent contains a tautomeric cyclic 1,2-dione. It is first determined whether the pH of the solvent is acidic (<5), basic (>9), or neutral (5 to 9). If the pH is neutral, an acid or a base is added to make the pH acidic or basic, respectively. The UV absorbance at a first wavelength between about 230 nm and about 270 nm and at a second wavelength between about 280 and about 320 nm is determined. If the pH is acid, it is changed to basic and, if it is basic, it is changed to acidic. The UV absorbance at the first and second wavelengths is again determined. The presence of a tautomeric cyclic 1,2-dione is indicated if the absorbance at the first wavelength was greater when the solvent was acidic and the absorbance at the second wavelength was greater when the solvent was basic. The concentration of the tautomeric cyclic 1,2-dione can be determined by multiplying the change in absorbance by a constant.
Type:
Grant
Filed:
June 10, 1996
Date of Patent:
August 26, 1997
Inventors:
Jian Steven Qi, David E. Albright, Garra C. Lester
Abstract: Disclosed is a method of making a glycol ether acetate. Acetic acid is reacted with a glycol ether at a molar ratio of about 1.1 to about 2, in a mixture with a catalyst and an azeotropic agent which can be either butyl acetate or dibutyl ether. The mixture is heated to a temperature and pressure sufficient to vaporize an azeotrope of water and the azeotropic agent. In another embodiment of the invention, a glycol ether acetate is made by preparing a reaction mixture of acetic acid and a glycol ether in a molar ratio of about 1.1 to about 1.2, about 5 to about 25 wt % n-butanol, an additional amount of acetic acid stoichiometric with the amount of n-butanol, and a catalyst. The reaction mixture is heated to form a glycol ether acetate, water, and butyl acetate. The azeotrope, excess acetic acid, butyl acetate, and glycol ether are successively removed by distillation.
Abstract: Disclosed is a method of reducing the corrosion of a carbon steel reboiler in which a reboiler fluid containing nitrogen trichloride is heated to decompose the nitrogen trichloride. About 1 to about 100 ppm, based on the reboiler fluid weight, of a source of iodine, is added to the reboiler.
Type:
Grant
Filed:
August 2, 1996
Date of Patent:
June 17, 1997
Assignee:
Occidental Chemical Corporation
Inventors:
Chao-Peng Chen, Tilak V. Bommaraju, Paul C. Williams
Abstract: Disclosed is a method of selecting a gas oil feedstock for use in manufacturing olefins. The feedstock is analyzed for the presence of benzothiophenes and is used to manufacture olefins only if it contains less than 50 ppm (as sulfur) of benzothiophenes. The concentration of benzothiophenes can be reduced by distilling the feedstock and removing the fraction of the feedstock that boils between about 45.degree. and about 60.degree. C. under reduced pressure of about 0.05 to about 0.1 mmHg. The concentration of benzothiophenes can also be reduced by passing the feedstock through a benzothiophene adsorber such as activated alumina or activated carbon.
Abstract: Disclosed is a method of making 3,5-diaminobenzotrifluoride from 4-chloro-3,5-dinitrobenzotrifluoride. A solution of 4-chloro-3,5-dinitrobenzotrifluoride in an alcohol is prepared. Separately, a slurry is prepared of a palladium catalyst on a suitable substrate, at least one equivalent of magnesium oxide per equivalent of 4-chloro-3,5-dinitrobenzotrifluoride, sufficient hydrogen-donating reducing agent to reduce the 4-chloro-3,5-dinitrobenzotrifluoride to 3,5-diaminobenzotrifluoride, and an amount of alcohol sufficient to make the slurry stirrable. The solution is added to the slurry with stirring at a rate that does not exceed the reaction rate of the 4-chloro-3,5-dinitrobenzotrifluoride so that no unreacted 4-chloro-3,5-dinitrobenzotrifluoride accumulates in the slurry. The reaction mixture is heated at about 75.degree. to about 100.degree. C.
Abstract: A process for the para-directed nuclear chlorination of an alkylbenzene, such as toluene, comprises reacting the alkylbenzene with chlorine in the presence of a Lewis acid catalyst and a novel co-catalyst of the formula: ##STR1## where Z is ##STR2## ; and R is Cl, Br, F, C.sub.1 to C.sub.8 alkyl to C.sub.1 to C.sub.8 alkoxy; x and y are each hydrogen, or taken together form a fused cyclopentyl or cyclohexyl ring; n is 0, 1 or 2, with the proviso that when Z is [3], n is 0 or 1.
Type:
Grant
Filed:
April 21, 1995
Date of Patent:
April 15, 1997
Assignee:
Occidental Chemical Corporation
Inventors:
Ramesh Krishnamurti, Sandor Nagy, Thomas F. Smolka
Abstract: Disclosed is a method of making a free-standing polyimide film. A solution is prepared of a polyamic acid 20 to 98% imidized in an organic solvent and a coating of the solution is applied to a non-stick substrate. The coating is heated to a temperature high enough to evaporate all but 1 to 20 wt % of the solvent and form a film. The film is removed from the substrate and is heated to evaporate the solvent to less than 1000 ppm.
Abstract: Crude mixtures of dioxydiphthalic anhydride containing alkali metal salts are purified by treating the crude mixture with an alkanol, such as n-butanol, to form the dioxydiphthalic acid diester; removing the insoluble alkali metal salts by filtration; removing the excess alkanol; and reconverting the dioxydiphthalic acid diester to dioxydiphthalic anhydride.
Type:
Grant
Filed:
March 31, 1995
Date of Patent:
April 30, 1996
Assignee:
Occidental Chemical Corporation
Inventors:
Willis T. Schwartz, Frank J. Dinan, Jeffrey S. Stults
Abstract: 3,5-Diaminobenzotrifluoride is prepared by reaction of 4-chloro-3,5-dinitrobenzotrifluoride with sodium formate in acetic acid, in the presence of sodium acetate and palladium on charcoal.
Type:
Grant
Filed:
December 10, 1990
Date of Patent:
August 9, 1994
Assignee:
Occidental Chemical Corporation
Inventors:
Ramesh Krishnamurti, Mahendra K. Dosi, Henry C. Lin
Abstract: A process for the selective hydrodefluorination of a tetrafluorophthalimide compound of the formula ##STR1## where X is 1 and R is a monovalent organo group; or X is 2 and R is a divalent organo group; comprises reacting (I) the tetrafluorophthalimide with zinc in an aqueous alkali metal hydroxide medium. The product may be hydrolyzed to form 3,4,6-trifluorophthalic acid.
Type:
Grant
Filed:
April 3, 1992
Date of Patent:
March 15, 1994
Assignee:
Occidental Chemical Corporation
Inventors:
Jeffrey S. Stults, Lawrence B. Fertel, William S. Derwin