Abstract: A process for the preparation of ethyltrifluoroacetoacetate is provided. In this first step, ethyltrifluoroacetate is condensed with ethyl acetate in the presence of sodium ethoxide in cyclohexane. In a second step, the condensation product is neutralized with a protonic acid, such as formic acid, to release an enol. In the third step, the ethyltrifluoroacetoacetate obtained is separated by distillation. The ethyltrifluoroacetoacetate is used as an intermediate in syntheses in the pharmaceutical or plant protection industry.

Abstract: Formate salts of nitrogenous bases containing a tertiary nitrogen atom are prepared by reacting the nitrogenous base with carbon dioxide and hydrogen in the presence of a solvent and a catalyst comprising an inorganic or organometallic compound of rhodium and an organophosphorus compound. The catalysts disclosed effect the reaction at a lower temperature and at higher productivities relative to the Group VIII metal catalysts of the prior art.

Abstract: Formic acid cannot be completely removed from formic acid and water mixtures by distillation because of the presence of the maximum azeotrope. Formic acid can be readily removed from formic acid--water mixtures by extractive distillation in which extractive agent is a dicarboxylic acid mixed with certain high boiling organic compounds. Examples of effective agents are: itaconic acid and diethylene glycol diethyl ether; azelaic acid, heptanoic acid and 2-hydroxyacetophenone.

Abstract: 2-Pentanone cannot be completely removed from 2-pentanone and formic acid mixtures by distillation because of the presence of the maximum azeotrope. 2-Pentanone can be readily removed from 2-pentanone-formic acid mixtures by extractive distillation in which the extractive agent is a ketone, either alone or mixed with certain high boiling organic compounds. Examples of effective agents are cyclohexanone; diisobutyl ketone and octanoic acid; isophorone, hexanoic acid and butyl ether.

Abstract: An integrated process for the production of formic acid from carbon dioxide and hydrogen. The process comprises for example, a reactor in which the formate salt of a nitrogenous base is produced together with subsequent purification and formic acid recovery stages. In the process described formic acid is recovered from the formate salt by using a base interchange reaction in which there is generated a thermally decomposable formate salt of a high boiling base. The high boiling base can be for example an imidazole and the nitrogenous base can be triethylamine.

Abstract: 3-Methyl-2-butanone cannot be removed from 3-methyl-2-butanone and formic acid mixtures by distillation because of the presence of the maximum azeotrope between 3-methyl-2-butanone and formic acid. 3-Methyl-2-butanone can be readily removed from 3-methyl-2-butanone - formic acid mixtures by extractive distillation in which the extractive agent is dimethylacetamide, dimethylformamide or these with certain high boiling organic compounds.

Abstract: Pure hydroxylammonium salts of fatty acids of 1 to 4 carbon atoms are prepared by reacting hydroxylammonium sulfate and alkali metal salts of fatty acids with 1 to 4 carbon atoms in solution at elevated temperatures and separating off the hydroxylammonium salts of fatty acids of 1 to 4 carbon atoms by(a) reacting hydroxylammonium sulfate and alkali metal salts of fatty acids of 1 to 4 carbon atoms in solution in water or alkanols of 1 to 3 carbon atoms or mixtures thereof at 20.degree.-70.degree. C.,(b) evaporating the solvent out of the reaction mixture to obtain a dry residue,(c) isolating the hydroxlammonium salts of fatty acids of 1 to 4 carbon atoms from the dry residue thus obtained by sublimation under reduced pressure.

Abstract: A process of regenerating a palladium salt catalyst comprising, in combination, steps of:(I) heating an organic residue containing a palladium salt catalyst which has been separated from a reaction solution, at a temperature of not lower than 330.degree. C. under an inert gas atmosphere to produce a reduced and thermally decomposed porous product;(II) firing the porous product produced in the step I under an oxygen-containing atmosphere; and(III) treating the product fired in the step II with an acid to produce a palladium salt.

Abstract: Dioxane cannot be completely removed from dioxane and formic acid mixtures by distillation because of the presence of the maximum azeotrope. Dioxane can be readily removed from dioxane - formic acid mixtures by extractive distillation in which the extractive agent is dimethylsulfoxide, either alone or admixed with certain high boiling organic compounds. Examples of effective agents are dimethylsulfoxide; DMSO and octanoic acid; DMSO, neodecanoic acid and methyl salicylate.

Abstract: 2-Pentanone cannot be completely removed from 2-pentanone and formic acid mixtures by distillation because of the presence of the maximum azeotrope. 2-Pentanone can be readily removed from 2-pentanone formic acid mixtures by extractive distillation in which the extractive agent is dimethylsulfoxide, either alone or mixed with certain high boiling organic compounds. Examples of effective agents are dimethylsulfoxide; DMSO and octanoic acid; DMSO, hexanoic acid and isophorone.

Abstract: Formic acid cannot be completely removed from formic acid and water mixtures by distillation because of the presence of the maximum azeotrope. Formic acid can be readily removed from formic acid - water mixtures by extractive distillation in which the extractive agent is ethylene carbonate or propylene carbonate, either alone or mixed with certain high boiling organic compounds. Examples of effective agents are ethylene carbonate and heptanoic acid; propylene carbonate, benzoic acid and isophorone; propylene carbonate, heptanoic acid and 2-hydroxyacetophenone.

Abstract: Impure formic acid cannot be completely removed from formic acid-water-impurity mixtures by distillation because of the presence of the maximum azeotrope between formic acid and water. Formic acid can be readily removed from mixtures containing it, water and impurities of the ether, ester, ketone or diketone type by using extractive distillation in which the extractive agent is a higher boiling oxygenated, nitrogenous or sulfur containing organic compound or a mixture of these. Examples of effective agents are adiponitrile; sulfolane and salicyclic acid; dimethylformamide, N,N-dimethylacetamide and ethylene glycol ethyl ether acetate.

Abstract: The invention relates to a process for the extraction of carboxylic acids from aqueous solutions with a carboxylic acid content below 8% by weight. A mixture of an aliphatic amine with a total carbon number of at least 10 and a phenol or naphthol is used as extracting agent. The molar ratio of phenol:amine or alkylated phenol:amine or naphthol:amine is in the range from 0.1:1 to around 1.1:1.

Abstract: Formic acid cannot be easily removed from acetic acid by distillation because of the closeness of their vapor pressures. Formic acid can be readily removed from acetic acid by extraction distillation. Typical extractive distillation agents are carboxylic acids in the range of hexamoic acid to neodecanoic acid with or without solvents such as methyl benzoate, acetophenone and nitrobenzene.

Abstract: An improved process for the preparation of primary terpenoid alcohols, e.g. 6,7-dihydrogeraniol and phytol, and of their esters with formic acid. The terpenoid formates are obtained very advantageously by reacting the corresponding tert.-vinylcarbinols with more than 2 moles, per mole of vinylcarbinol, of aqueous formic acid of more than 70 percent strength by weight, or with anhydrous formic acid, at from 5.degree. to 100.degree. C. The primary terpenoid alcohols themselves are obtained from their formates by trans-esterification with a low-boiling alcohol in the presence of a catalytic amount of a strong base. The products are valuable compounds. For example, 6,7-dihydrogeraniol is used as a scent and phytol is used as a perfume fixative and as a starting material for the synthesis of naturally occurring materials.

Abstract: Formic acid cannot be completely removed from formic acid - water mixtures by distillation because of the presence of the maximum azeotrope. Formic acid can be readily removed from mixtures containing it and water by using extractive distillation in which the extractive distillation agent is a sulfone. Typical examples of effective agents are thiophan sulfone; dimethyl sulfone and adiponitrile; phenyl sulfone, adiponitrile and acetophenone.

Abstract: C.sub.2 to C.sub.10 monocarboxylic acids are co-produced with formic acid by reacting at an elevated temperature below 250.degree. C. a C.sub.1 to C.sub.9 alkyl formate with carbon monoxide and water in the presence as catalyst of a Group VIII noble metal component and an iodine or bromine-containing promoter, the partial pressure of carbon monoxide being in the range 1 to 300 bar, the concentration of noble metal component being in the range from 100 to 5000 ppm and the atomic ratio of noble metal to iodine or bromine being in the range from 1:50 to 1:1000 and thereafter recovering the co-produced C.sub.2 to C.sub.10 monocarboxylic acid and formic acid. In a preferred embodiment, the alkyl formate is methyl formate and the recovered acids are acetic acid and formic acid.

Abstract: This invention provides a process for improving the separation and recovery of metal formate and pentaerythritol as crystalline products, from an aqueous waste stream of a pentaerythritol manufacturing operation which involves the reaction of formaldehyde with acetaldehyde in the presence of a metal hydroxide catalyst.The pentaerythritol process waste stream is passed through a macroreticular resin bed to remove organic byproducts, and the purified waste stream is then evaporatively concentrated to produce crystalline sodium formate product. The resultant mother liquor is diluted with water-miscible alkanol to precipitate a pentaerythritol-metal formate mixture. The precipitate is washed with a portion of waste stream feed to dissolve the metal formate and yield undissolved crystalline pentaerythritol as a product.At least about 85 percent of the metal formate and at least about 90 percent of the pentaerythritol contained in the original waste stream are recovered as products of the process.

Abstract: Formic acid is recovered, by distillation, from its mixtures with solvents of the general formula I ##STR1## where R.sup.1 is hydrogen, methyl, ethyl or vinyl and R.sup.2 and R.sup.3 are each alkyl, cycloalkyl, aryl or aralkyl, or R.sup.2 and R.sup.3 together form a 1,4- or 1,5-alkylene group, in each case of not more than 8 carbon atoms, with the provisos that the sum of the number of carbon atoms in R.sup.2 and R.sup.3 is 7 to 14 and that only one of these radicals is aryl, by a method in which the distillation is carried out in the presence of a carboxamide II which is selected from the group consisting of formamide, acetamide, propionamide and the same compounds substituted by N-methyl or N,N-dimethyl, and which has a boiling point lower than that of the solvent I.

Abstract: Prepare hydroxyaromatic ethers by contacting an oxidizing agent with an acylaromatic ether in the presence of an acid catalyst.

Abstract: Novel polymers having high activity as cationic surface-active agents are prepared by the addition polymerization of ethylenically unsaturated aromatic sulfonium salts, e.g., ##STR1## When such polymers are heated and/or dried, they are irreversibly converted to inert, nonionic residues without the elimination of odorous by-products.The novel sulfonium salt polymers having relatively low molecular weight and low charge density are particularly useful as surfactants or emulsifiers in the emulsion polymerization of ethylenically unsaturated monomers such as styrene, butadiene, alkyl acrylates and the like. The polymers having high molecular weight and high charge density are useful as thickeners and flocculants.

Abstract: Formate salts of nitrogenous bases containing tertiary nitrogen are prepared by reacting the nitrogenous base with carbon dioxide and hydrogen using a soluble transition metal catalyst. For example triethylamine is reacted with carbon dioxide and hydrogen using ruthenium trichloride as catalyst and an isopropanol/water mixture as solvent to yield triethylammonium formate which was separated from the reaction mixture by distillation.

Abstract: The invention relates to a process for making 1-aminoalkane-1,1-diphosphonic acids of the general formula (I): ##STR1## in which R stands for an aliphatic hydrocarbon radical having from 1 to 12 carbon atoms.To this end, the invention provides:(a) for tetraphosphorus hexoxide to be reacted with at least one compound of the general formula (II) ##STR2## in which R has the meaning given above and X stands for an --ONH.sub.4 or NH.sub.2 -radical, in inert gas atmosphere at elevated temperature, the molar ratio of tetraphosphorus hexoxide to the compound of general formula (II) being about 1 to 2-6; and(b) for 1-aminoalkane-1,1-diphosphonic acid to be crystallized from the reaction mixture.

Abstract: Hydrogen is generated by contacting an alkaline aqueous solution of formaldehyde with at least one catalyst selected from the group consisting of molybdenum, tungsten, molybdenum carbides, tungsten carbides, molybdenum nitrides, tungstenum borides, copper, silver, gold and compounds of copper, silver and gold.Hydrogen can be generated at ambient temperature under atmospheric pressure and, therefore, complicated steps or complicated devices are unnecessary.

Abstract: A method of recovering or extracting chemicals, such as furfural, formic acid, acetic acid and other organic compounds from acidic hydrolysates of plants or vegetable matter, especially spent sulfite liquors after conversion of the pentosans into pentoses and then into furfural by heating the hydrolysate in an acidic environment. The conversion of the pentosans pentoses into furfural, preferably with acidulation, is accomplished in a counterflow or countercurrent flow heat exchanger and a reactor, preferably a tubular reactor. The hydrolysate which has additionally been heated and converted in the reactor is used as a heating medium or heat carrier for heating up the hydrolysate which is converted in the counterflow heat exchanger, whereupon there is recovered as the distillate furfural in conjunction with the formic acid, acetic acid and the like.

Abstract: A process for the recovery of carboxylic acids from mixtures containing glycol esters derived from these acids. The process comprises reacting these mixtures at boiling with water to form carboxylic acid and entraining the carboxylic acid formed by means of the water by azeotropic distillation, so as to separate off a mixture of carboxylic acid and water. This mixture is subjected to extractive distillation by means of an organic solvent which is insoluble in water and in which water is insoluble. A mixture of water and organic solvent is thereby separated from a solution of carboxylic acid in the organic solvent.

Abstract: This invention provides a process for recovery of sodium formate from an aqueous waste stream which is a byproduct mother liquor derived from a reaction system in which pentaerythritol is produced by the reaction of formaldehyde with acetaldehyde in the presence of sodium hydroxide catalyst.As one of its important features, the invention process involves contacting the mother liquor with a monoalkylamine solvent which is highly selective for extraction of organic materials to the exclusion of sodium formate.

Abstract: A method for making water-soluble potassium formate substantially free of water-insoluble salts selectively and in high yield at temperatures at or below about 100.degree. C., includes contacting potassium sulfate, potassium carbonate or a mixture of potassium and sodium carbonate and potassium and sodium sulfate with calcium formate, forming water-soluble potassium formate and water-insoluble calcium sulfate, calcium carbonate, or mixtures thereof, thus permitting recovery of substantially potassium-free calcium sulfate, calcium carbonate or both, and substantially calcium sulfate-free calcium carbonate-free potassium formate from the aqueous media.

Abstract: Anhydrous or substantially anhydrous formic acid is obtained by hydrolysis of methyl formate, in a process wherein(a) methyl formate is hydrolyzed,(b) the methanol and excess methyl formate are distilled from the hydrolysis mixture obtained,(c) the bottom product of distillation (b), consisting of formic acid and water, is extracted, in a liquid-liquid extraction, with an extractant which in the main takes up the formic acid,(d) the resulting extract phase, consisting of formic acid, the extractant and a part of the water, is subjected to distillation,(e) the top product obtained from this distillation and consisting of all or part of the water introduced into the distillation, and part of the formic acid, is recycled, as vapor, into the lower part of the distillation column of stage (b),(f) the bottom product of distillation stage (d), consisting of the extractant, with or without part of the water, and the greater part of the formic acid, is separated by distillation into anhydrous or substantially anhydrou

Abstract: A process for recovering carboxylic acids with a material of which the main component is a polymeric compound having a pyridine skeletal structure and a crosslinked structure, followed by desorbing the captured carboxylic acids by use of a desorbing agent.

Abstract: Formic acid is produced in a continuous process by hydrolyzing methyl formate with water at high temperature and pressure in the presence of a formic acid catalyst. Methanol is also formed. The reesterification of the reaction products to methyl formate (a reaction favored by high temperatures) is minimized by flashing the reaction product at relatively low pressure and temperature and thereafter distilling the residual liquid under vacuum. This procedure separates the methyl alcohol from the formic acid with a minimum contact time and at a low temperature which does not favor the reesterification reaction. The flashed vapor, primarily unreacted methyl formate, is recycled to the reaction zone. High purity formic acid, i.e., 85%, is obtained by subjecting the bottom from the vacuum distillation to a second distillation step. The distillate from the vacuum distillation is distilled to separate residual methyl formate for recycle from the co-product methyl alcohol.

Abstract: A process for the preparation of a 4-acyloxy-2-methyl-crotonaldehyde of the formula ##STR1## where R is hydrogen or an aliphatic radical of 1 to 5 carbon atoms, by reacting a 1,1,4-triacyloxy-2-methyl-but-2-ene of the formula ##STR2## where R.sup.1 and R.sup.2 are each hydrogen or an aliphatic radical of 1 to 5 carbon atoms, with water in the presence of a carboxylic acid of the formulaR--COOH III.

Abstract: This invention provides a process for recovery of sodium formate from an aqueous waste stream which is a byproduct mother liquor derived from a reaction system in which pentaerythritol is produced by the reaction of formaldehyde with acetaldehyde in the presence of metal hydroxide catalyst.Among its important features, the invention process involves evaporative crystallization of the mother liquor to separate out a major proportion of metal formate; dilution of the resultant secondary aqueous waste stream with methanol to precipitate metal formate/pentaerythritol solids; contact of the solids with a portion of the primary aqueous waste stream feed to dissolve metal formate; and recycle of the metal formate-enriched aqueous stream to the evaporative crystallization step of the process.

Abstract: A process for the production of anhydrous or substantially anhydrous formic acid by hydrolysis of methyl formate which is carried out in a column having an upper fractionating section, a middle hydrolysis section and a lower extraction section and in which(a) the hydrolysis is carried out in the middle section of the columm, with water and methyl formate in countercurrent,(b) the resulting formic acid is extracted, in the lower section of the column, by means of a carboxylic acid amide which is fed into the lower end of the middle section of the column,(c) the extract phase, consisting in the main of formic acid and the carboxylic acid amide, is distillatively dehydrated, or substantially dehydrated, in the lower section of the column,(d) the methanol and uncovered methyl formate are removed by fractional distillation in the upper section of the column and(e) the pure formic acid or concentrated aqueous formic acid is distilled from the anhydrous or substantially anhydrous extract phase in a second column, le

Abstract: A process for the production of isocyanates by the addition of carbon monoxide to a metal or aryl carbamate.

Abstract: In a process for the manufacture of sodium dithionite by reacting sulfur dioxide with sodium formate and aqueous sodium hydroxide solution in the presence of methanol, an aqueous methanolic solution of sodium formate is first produced by reacting carbon monoxide with sodium hydroxide solution in an aqueous medium, containing from 1 to 50% by weight of methanol, based on the amount of water, at from 80 to 120.degree. C. under a pressure of from 10 to 40 bars. The resulting aqueous methanolic solution can be reacted directly, in the conventional manner, with sulfur dioxide and aqueous sodium hydroxide solution to give sodium dithionite.

Abstract: Formic acid is prepared by hydrolyzing methyl formate, the hydrolysis being carried out in the presence of from 0.5 to 3.0 moles, per mole of methyl formate, of a base which contains tertiary nitrogen atoms, boils at not less than 180.degree. C. under atmospheric pressure and has a pKa from 4 to 9, N-substituted imidazole derivatives being the preferred bases.

Abstract: Carboxylic acids of the general formula IR.sup.1 -COOH Iwhere R.sup.1 is hydrogen, methyl, ethyl or vinyl, are isolated from their dilute aqueous solutions by extraction followed by distillation of the mixtures obtained, the extractant used being a secondary amide of the general formula II ##STR1## where R.sup.2 and R.sup.3 are alkyl, cycloalkyl, aryl or aralkyl or conjointly are 1,4- or 1,5-alkylene, in each case of not more than 8 carbon atoms, with the proviso that the sum of the carbon atoms of R.sup.2 and R.sup.3 is from 7 to 14 and that only one of these radicals is aryl, and where R.sup.4 is one of the radicals R.sup.1.

Abstract: An ammonium salt of an alkanoic acid having about 1-10 carbon atoms per molecule is prepared by reacting ammonia with an excess of the alkanoic acid in an aqueous system in a tubular reactor.An ammonium salt of an alkanoic acid having about 12-18 carbon atoms per molecule is prepared by reacting ammonia with the alkanoic acid in a tubular reactor. The reaction can be conducted in the presence or absence of water.

Abstract: Isobutylene, hydrogen cyanide and sulfuric acid are reacted to produce tertiary butyl formamide, which is hydrolyzed by sodium hydroxide to produce tertiary butyl amine. The tertiary butyl amine is removed by vaporization and the residue is treated with sulphuric acid and methanol and is distilled to recover formate values as methyl formate or sodium formate. There is additionally recovered crystalline sodium sulfate and a water immiscible yellow organic phase.