Abstract: Caprolactam is obtained from mixtures which contain polymers or thermoplastic molding materials having the repeating unit--N(H)--(CH.sub.2).sub.5 --C(O)--(a) by cleavage at elevated temperatures in the presence of a base under reduced pressure or (b) in the presence of water, by using a mixture essentially comprisingfrom 50 to 99.9% by weight of a polymer or of a thermoplastic molding material having the repeating unit--N(H)--(CH.sub.2).sub.5 --C(O)--from 0.1 to 50% by weight of additives selected from the group consisting of inorganic fillers, organic and inorganic pigments and dyes,from 0 to 10% by weight of organic and/or inorganic additives,from 0 to 40% by weight of non-polyamide-containing polymers andfrom 0 to 20% by weight of polyamides, with the exception of polycaprolactam and copolyamides prepared from caprolactam,and carrying out the cleavage in the presence of a base under reduced pressure, the water content of the mixture used being not more than 0.

Abstract: Tertiary-butyldiethanolamine subject to color deterioration is purified and stabilized against color formation by vacuum distilling said amine at a pressure within the range of 1 to 50 mm.

Abstract: The present invention relates to a method of reacting polyamides or mixtures thereof with ammonia to obtain a mixture of monomers. The reaction is carried out in the presence of certain Lewis Acid catalyst precursors.

Abstract: The present invention relates to a process for the reduction of the color of polyamines by reacting at elevated temperature, e.g. 120.degree.-170.degree. C., and pressure, e.g. 500 to 6000 psig. the colored polyamines, e.g. triethylenetetramine and tetraethylenepentamine, in the presence of a ruthenium on alumina hydrogenation catalyst. The catalyst for the polyamine decolorization process preferably has at least 0.5 wt. % Ru. In the process of the present invention, the polyamines can either be distilled into a narrow product composition and then hydrogenareal, or a crude polyamine product can be hydrogenated and then distilled to produce the desired product composition.

Abstract: The present invention relates to a process for the reduction of the color of polyamines by reacting at elevated temperature, e.g. 120.degree.-170.degree. C., and pressure, e.g. 500 to 6000 psig. the colored polyamines, e.g. triethylenetetramine and tetraethylenepentamine, in the presence of a cobalt on alumina hydrogenation catalyst promoted with copper and chromium. In the process of the present invention, the polyamines can either be distilled into a narrow product composition and then hydrogenated, or a crude polyamine product can be hydrogenated and then distilled to produce the desired product composition.

Abstract: A process for the purification of a perfluorochemical composition comprises continuously mixing the perfluorochemical composition, comprising a liquid mixture of inert perfluorochemicals (e.g., perfluoroalkanes, perfluoroethers, perfluoroaminoethers, or perfluoroalkyl tertiary amines) and isomeric fluorohydrochemicals, with a stabilization composition comprising water-miscible alkanol and an aqueous solution of base (such as potassium hydroxide) made by dissolving the base in an amount of water sufficient to dissolve or disperse the fluoride salt by-products of the subsequent reaction of the base with the fluorohydrochemicals to form fluoroolefins, the amount of the alkanol in the stabilization composition being in stoichiometric excess of the amount needed to completely convert the fluoroolefins to alkoxyvinyl ethers. The process can be utilized to purify the product mixtures resulting from fluorination methods such as direct fluorination or ECF.

Abstract: Color-containing alkanolamines or alkyleneamines, having color numbers of up to 100 PtCo or higher, can be treated with inorganic solid acidic catalysts. Inorganic support materials having bonded inorganic acid functionalities may be used as the inorganic solid acidic catalysts. In the presence of water, these inorganic solid acidic catalysts produce decolorized alkanolamines or alkyleneamines having color numbers of 20 PtCo or less. The process of decolorization can be carried out in batch or continuous mode processes thus providing low cost, high quality and high purity end products.

Abstract: Useful monomeric products are obtained in the reaction of nylon 6,6 with ammonia. Increased yield of monomer products from nylon 6,6 is obtained from ammonolysis when a mixture with nylon 6 is employed.

Abstract: A process is disclosed for simultaneously depolymerizing nylon 6 and nylon 6,6 and reclaiming the monomer values by steam distillation.

Abstract: A process for decolorizing polyalkylene polyamines, which comprises contacting one or more polyalkylene polyamines having an average molecular weight of greater than about 200 and less than about 1000 with carbon at a temperature greater than or equal to about 100.degree. C. and less than or equal to about 300.degree. C. under conditions effective to reduce the color rating of the one or more polyalkylene polyamines.

Abstract: A continuous method of preparing N-monoalkyl alkylenediamines, uncontaminated by the N,N'-dialkyl alkylenediamine, is based on the observation that the disubstituted material selectively precipitates from aqueous media. A scheme is presented where an aqueous alkylenediamine is reacted with a suitable carbonyl component and hydrogen over a supported platinum catalyst. Where the alkylenediamine forms an azeotrope with water it can be conveniently recycled to the reactor.

Abstract: Waste or scrap polyurethane may be conveniently and economically converted to useful active-hydrogen containing polyethers and polyamines by contacting the polyurethane with water, strong base, and an activating agent such as a quaternary ammonium compound containing at least 15 carbon atoms or an organic sulfonate containing at least 7 carbon atoms. The activating agent helps to accelerate the rate of base catalyzed hydrolysis.

Abstract: O-substituted hydroxylamines (I)H.sub.2 N--O--CH.sub.2 --R(I)where R is H or an organic radical, and their salts are prepared by reacting a cyclic imidoether II of a 1,4- or 1,5-dicarboxylic acid, the said imidoether containing an ether group --O--CH.sub.2 --R, with a basic compound by a method in which a primary aliphatic aminoalcohol III is used as the basic compound and the compound I is, if required, converted to its salts.

Abstract: A process is disclosed for the extraction recovery of ethylene amines from an aqueous solution containing at least 10% by weight sodium chloride and not more than 5% by weight sodium hydroxide, the process comprised of mixing with said aqueous solution an extraction-effective amount of a polar organic solvent which is immiscible with an aqueous salt solution, miscible with water and having a boiling poing below about 105.degree. C. This mixture is allowed to form an organic phase and an aqueous salt solution phase. The organic phase, which contains at least a portion of the ethylene amines, is separated from the aqueous salt solution phase. The preferred polar organic solvent is n-propanol. The preferred temperature range for the process is between about 70.degree. C. and about 95.degree. C.

Abstract: A method of making ethylenediamine dinitrate comprising:(a) reacting ethylenediamine with aqueous nitric acid to form ethylenediamine dinitrate solution; and(b) adding said ethylenediamine dinitrate solution to a non-aqueous liquid, miscible with water in amounts of at least about 50 percent by weight, and in which ethylenediamine dinitrate is insoluble, to form solid ethylenediamine dinitrate with an average particle size of about 30 microns in diameter.

Abstract: Disclosed is a method for purification of polyamines which comprises contacting said polyamines with a treating agent selected from the group consisting of oxides, hydroxides or alkoxides of elements from the group consisting of silicon or Group IIA, IIIA, IIB, IIIB, IVB or VB at a temperature of about 150.degree. C. to 250.degree. C. and a pressure of subatomspheric to 10 atmospheres for a period of time sufficient to lower the hydroxyl impurity level of said amines.

Abstract: This invention relates to a process for separating mono-n-hexylamine from water and particularly to an improvement in a process for the recovery of mono-n-hexylamine from the reaction of n-hexanol with ammonia under amination conditions. In this process water is produced as a by-product and in the separation process an azeotrope is formed which comprises about 49% water and 51% hexylamine. The process for enhancing separation of the azeotrope of mono-n-hexylamine and water comprises contacting the azeotrope of mono-n-hexylamine and water with di-n-hexylamine or with a mixture of di-n-hexylamine and tri-n-hexylamine in sufficient amount to reduce the solubility of mono-n-hexylamine in water thus forming an organic phase and an aqueous phase which can be separated by simple techniques, e.g., decanting.

Abstract: High molecular weight amines having reduced low molecular weight amine contents are obtained by reacting a mixture of (1) a high molecular weight amine and (2) a low molecular weight amine with (3) an isocyanate in quantities such that from 0.5 to 10 equivalents of isocyanate are present for each equivalent of low molecular weight amine. The product of high molecular weight amines is particularly useful in the production of isocyanate addition products such as polyurethane plastics and foams.

Abstract: Process for the improvement of the quality of polyalkylene polyamines prepared by the reaction of (i) ammonia and/or an alkyleneamine compound having at least two amino groups and an alkanolamine compound having at least one amino group in the presence of a catalytically effective amount of a metal acid phosphate and at a temperature and pressure sufficient to form the polyalkylene polyamine.

Abstract: Recovery of bis(hexamethylene)triamine from still heels of hexamethylenediamine by extraction using an aliphatic hydrocarbon having a boiling point between about 34.degree. C. and 210.degree. C.

Abstract: The present invention relates to a process for the reduction of the color of polyamines by reacting at elevated temperature, i.e. 50.degree. to 175.degree. C., and pressure, i.e. 50 to 1500 psig, such colored polyamines, e.g. triethylenetetramine or tetraethylenepentamine, in the presence of a hydrogenation catalyst, e.g. Raney nickel or palladium on carbon, and a hydrogen atmosphere for a period of time sufficient to effectuate the desired reduction in color. In the process of the present invention, the polyamines can either be distilled into a narrow product composition and then hydrogenated or a crude polyamine product can be hydrogenated and then distilled to produce the desired product composition.

Abstract: A method of removing color from crude triethylenetetramine (TETA) is disclosed. In the preferred procedure, acid treated clay or acidic form zeolite are mixed with the TETA at elevated temperatures. After several hours exposure, the TETA is distilled to obtain a decolored product. The decoloration can be a continuous or batch process. The distillation is performed in the presence or absence of the catalyst.

Abstract: A process of decoloring crude triethylenetetramine (TETA) is disclosed. In the disclosed and preferred procedure, a sulfonic acid ion exchange resin acts on the crude TETA to enable subsequent distillation at elevated temperature to obtain decolored TETA.

Abstract: In the recovery of ethylene amines from aqueous solutions by alcohol extraction the alcoholic extract is treated with carbon dioxide so as to convert the extracted amines into carbamates, which are then back extracted with water and recovered by conventional decarbonation and dehydration. The double extraction technique results in an aqueous concentrate of at least twice the original amine concentration.

Abstract: A method is disclosed for separating alkyleneamines from a mixture of by-product alkali or alkaline earth metal chloride salt and alkyleneamines comprising the sequenced combination of the steps of: (a) washing said amine-chloride salt mixture with an aqueous alkali or alkaline earth metal hydroxide solution to form a washed amine-chloride salt mixture; and (b) treating a mixture of the amino and chloride salt to physically separate chloride salt from said amine of said mixture.

Abstract: Ethyleneamines are recovered from an aqueous solution of carbonates of ethyleneamines by distilling an aqueous solution of carbonates of ethyleneamines including ethylenediamine, in which the molar ratio of the carbon dioxide component to the ethyleneamines including ethylenediamine is 0.01 to 0.5, whereby ethylenediamine is distilled out together with water. The aqueous solution to be distilled is advantageously prepared by heating an aqueous solution of carbonates of ethyleneamines including ethylenediamine to effect decarboxylation.

Abstract: There is disclosed a process for reducing the reaction time in the hydrolysis of a condensation polymer wherein molten condensation polymer is intimately admixed with a depolymerizing agent which is either (i) one of the products resulting from the complete hydrolytic depolymerization of the condensation polymer; or (ii) water. The depolymerization agent is present in the mixture in an amount which is less than the weight of the condensation polymer and the materials are intimately admixed for a time sufficient that the molecular of the condensation polymer is reduced by at least 50%. The treated condensation polymer of lower molecular weight is thereafter subjected to neutral hydrolysis. In addition to decreasing the overall time required to effect complete hydrolytic depolymerization, this process additionally permits the use of a smaller hydrolysis vessel, thereby reducing the fabrication cost of the hydrolysis unit.

Abstract: A process for decolorizing polyethylene polyamines using a chlorinated hydrocarbon. The discolored polyethylene polyamine and chlorinated hydrocarbon are contacted to form a decolorizing mixture, and the mixture is distilled. The decolored polyethylene polyamine is collected from the distillate.

Abstract: A process for the neutral hydrolytic depolymerization of condensation polymers is described. The process is conducted in a continuous manner and comprises introducing condensation polymer waste material into an aqueous hydrolysis zone at a temperature of between 200.degree. C. and 300.degree. C. and superatmospheric pressure of at least 15 atmospheres. High pressure steam is introduced into the lower portion of the hydrolysis zone underneath the level of the condensation polymer waste material. The steam serves as the principal source of heat for the hydrolysis zone. By being introduced underneath the level of the condensation polymer waste material, the steam agitates the waste material to provide heat transfer to accelerate the hydrolysis reaction. Further, a portion of the steam condenses to provide water which is a reactant in the hydrolysis reaction. An aqueous solution of the product(s) of the hydrolysis reaction is withdrawn from an upper portion of the hydrolysis zone.

Abstract: Copper-diamine complexes such as copper(II)-di-t-butylethylenediamine dibromide are prepared by the reaction of a dihalide such as 1,2-dibromoethane with an amine such as t-butylamine and a basic copper(II) compound such as cupric oxide in a nitrile solvent. The diamine can be liberated from the complex by reacting it with a complexing agent such as an ethylenediaminetetraacetic acid salt.

Abstract: Ethyleneamines are efficiently recovered from an aqueous solution thereof by extracting them from the aqueous solution into an organic phase with an extractant selected from carbonyl group-containing organic solvents, benzyl alcohol, carboxylic acids and salts thereof, alkylphosphoric acids and salts thereof, and mixed solvents containing at least one of these extractants. The ethyleneamines in the organic phase is recovered preferably from the organic phase to the aqueous phase by incorporating an acid therein, followed by phase separation.

Abstract: A process is provided which may be run continuously for producing polyethylene polyamines having improved color characteristics which comprises treating discolored polyethylene polyamines with polyethylene polyamine hydrochloride in the presence of water at elevated temperatures for the time necessary to reduce the color of said polyethylene polyamines and then flash evaporating the decolorized polyethylene polyamines from the treating mixture.

Abstract: The present invention relates to a method for purifying N,N-dimethylaminopropylamine containing 1,3-diaminopropane as an impurity. Dimethylaminopropionitrile is formed by adding dimethylamine to acrylonitrile, and is then converted by subsequent hydrogenation and distillation into N,N-dimethylaminopropylamine. The impurity 1,3-diaminopropane is removed by adding a metal salt of a transition element which forms a stable complex with the 1,3-diaminopropane.

Abstract: A process for purifying crude polyether polyols which are prepared by anionic polymerization of alkylene oxides in the presence of basic catalysts. The polyols are mixed with water and ortho-phosphoric acid in certain quantity ratios, an adsorption agent is incorporated in the reaction mixture, the mixture is filtered and the water is removed from the polyether polyol by distillation.

Abstract: There is described a continuous process for the manufacture of ethylenediamine from the products of the reaction of ethylene oxide and ammonia, provision of a continuous recycle stream of monoethanolamine to the products of the reaction of ethylene oxide and ammonia, the amination of such products of the reaction of ethylene oxide and ammonia combined with the monoethanolamine recycle in which the feed stream to the amination reaction zone contains at least 70 weight percent monoethanolamine as well as diethanolamine and triethanolamine, the moles of ammonia provided to the amination reaction exceeds the molar concentration of alcoholic hydroxyl groups present in the amination feed, and the feed to the amination reactor contains at least a 5% increase in the concentration of monoethanolamine over the concentration of monoethanolamine in the reaction product stream from the reaction of ethylene oxide and ammonia.

Abstract: A process for preparing noncyclic polyalkylene polyamine compounds is disclosed wherein ammonia, an alkylene polyamine compound and an alkanolamine compound are reacted in the presence of an effective amount of a phosphorus-containing substance or a salt of a sulfur-containing substance or its corresponding acid at a temperature from about 200.degree. to 350.degree. C. under a pressure sufficient to maintain the reaction mixture essentially in liquid phase. The polyalkylene polyamines thus formed are recovered from the reaction mixture.

Abstract: A method and apparatus are disclosed for extracting amine compounds from air samples without loss due to formation of nitrosamine artifacts. The apparatus includes a cartridge having a separation zone between a first port and a second port. The separation zone contains an air pervious packing of a granular, solid phase amine complexing agent. The method includes a first step of driving an air sample through the separation zone of the cartridge from the first port to the second port, and a second step of driving an eluent through the separation zone from the second port to the first port, or backflushing the cartridge. To extract amine compounds, the eluent is a solvent for the amine complexing agent in the separation zone of the cartridge. The method may contain the further step of determining the amine compound concentration of at least a portion of the eluate which passes from the separation zone following the second step of the method.

Abstract: This is an improvement in a process for the production of an amine such as hexamethylenediamine from a nitrile such as adiponitrile where the nitrile is hydrogenated under pressure in the presence of a Raney nickel catalyst, the reaction being conducted in a reactor from which is discharged a product stream containing both the amine and the Raney nickel catalyst. The improvement comprises charging to the process discharge stream containing the product amine and the Raney nickel catalyst, an inorganic base, whereby the Raney nickel catalyst is passivated and catalytic decomposition of the amine is substantially decreased.

Abstract: Hexamethylenediamine (HMD) is purified by dissolving ammonia in crude molten HMD under pressure, directing the solution thus prepared to a reduced pressure zone where the ammonia is vaporized thereby causing a portion of the HMD to crystallize following which the crystals in the slurry are washed with essentially pure HMD. This purified HMD is suitable for conversion into polyamide fibers.

Abstract: A process for producing 1,17-diamino-9-azaheptadecane, which comprises adding nitric acid, hydrochloric acid, p-toluenesulfonic acid or sulfanilic acid to octamethylenediamine, and heating the mixture to eliminate ammonia therefrom.

Abstract: The invention is a process for reducing residual organic chloride in a hydrocarbyl amine by contacting the hydrocarbyl amine with a chlorine-displacing nucleophile selected from NaSCN, NaCN, and NaSPH where a portion of the residual organic chloride is converted to an inorganic chloride, and removing the inorganic chloride.