Allied Chemical Corporation

Alliedsignal Inc.

Allied Corporation

Francis E Evans

Martin A Robinson

Richard E Eibeck

Morris B Berenbaum

Robert E Booth

Kenneth B Gilleo

Charles J Lind

William J Wagner

Eugene B Recla

Charles J Felice, Jr

Joel P Guptill

Kenneth H Schroeder

The present invention provides a process for recovering boron trifluoride from an impure gaseous boron trifluoride residue. The process comprises: (a) feeding an impure gaseous boron trifluoride residue containing sulfur dioxide as an impurity into a mixture of boric and sulfuric acids wherein the acid mixture absorbs boron trifluoride from the impure boron trifluoride residue and slightly absorbs or does not absorb sulfur dioxide from the impure gaseous boron trifluoride residue; and (b) removing the unabsorbed sulfur dioxide from the acid mixture. The present invention also provides a boron trifluoride preparation and purification process. The process comprises the steps of (a) reacting boric acid and fluorosulfuric acid in surfuric acid to form a product; (b) distilling the product from step (a) to yield pure boron trifluoride and impure gaseous boron trifluoride; (c) feeding the impure gaseous boron trifluoride residue containing sulfur dioxide as an impurity into a mixture of boric and sulfuric acids wherein the acid mixture absorbs boron trifluoride from the impure gaseous boron trifluoride residue and only slightly absorbs sulfur dioxide from the impure gaseous boron trifluoride residue; and (d) removing the unabsorbed sulfur dioxide from the acid mixture. The recovered boron trifluoride may be used as a catalyst.

Process for recovering boron trifluoride from an impure gaseous boron

Sulfuric acid contaminated with boron and fluoride values such as the waste acid of a boron trifluoride process is purified by contacting the contaminated acid with an inert gas to desorb boron trifluoride, and the inert gas is stripped by contacting with an absorbing liquid including concentrated sulfuric acid. Hydrogen fluoride and/or fluorosulfuric acid are added to contaminated sulfuric acid as agents to spring non-volatile boron value. In addition, the water content of the contaminated acid is adjusted within a narrow concentration range, to improve the efficiency of both the stripping and the absorption operations. The absorption of boron trifluoride into the absorbing sulfuric acid is improved when it contains boric acid. Preferably the contaminated sulfuric acid to be purified is one portion of the waste liquid and the absorbing liquid is another portion of the waste liquid of a boron trifluoride manufacturing process. Boric acid is added to the absorbing liquid, then boron trifluoride is stripped from the inert gas and absorbed into the absorbing liquid. The absorbing liquid along with stripped boron trifluoride is recycled to a boron trifluoride manufacturing process. The inert gas can be recycled to the desorbing step.

Process for removing boron from sulfuric acid

A process for the conversion of boron trifluoride dimethyl ether complex to boron trifluoride dialkyl ether complex substantially free of dimethyl ether impurities, which comprises reacting the boron trifluoride-dimethyl ether complex, in the liquid phase, in the presence of dialkyl ether wherein at least one of the alkyl groups contains at least two carbon atoms, in a restricted vapor equilibration region, while simultaneously sweeping the said vapor equilibration region with a substantially inert gas, and heating to distill off the dimethyl ether. High purity of the boron trifluoride dialkyl ether complex is attained with this method, with only minimal traces of the boron trifluoride dimethyl ether complex, dimethyl ether remaining. The preferred product is boron trifluoride diethyl ether.

Process for the conversion of boron trifluoride dimethyl ether complex

Sulfuric acid contaminated with boron and fluoride values such as the waste acid of a boron trifluoride process is purified by contacting the contaminated acid with an inert gas to desorb boron trifluoride, and the inert gas is stripped by contacting with an absorbing liquid including concentrated sulfuric acid. Fluosulfonic acid is added to contaminated sulfuric acid at levels approximately three times the molar values of boric acid contaminant as an agent to spring non-volatile boron values. The absorption of boron trifluoride into the absorbing sulfuric acid is improved when it contains boric acid. Preferably the contaminated sulfuric acid to be purified is one portion of the waste liquid and the absorbing liquid is another portion of the waste liquid of a boron trifluoride manufacturing process. Boric acid is added to the absorbing liquid, then boron trifluoride is stripped from the inert gas and absorbed into the absorbing liquid. The absorbing liquid along with stripped boron trifluoride is recycled to a boron trifluoride manufacturing process. The inert gas can be recycled to the desorbing step.

Purification of boron-containing sulfuric acid

When saturated with boron trifluoride, certain polyhydric alcohols form adducts which catalyze hydrocarbon alkyl transfer reactions for which boron trifluoride is catalytic. The adduct is recovered from the reaction mixture and recycled, greatly reducing boron and fluoride values in the product and in any effluent. Examples include propylation of toluene in the presence of a recycled adduct of boron trifluoride with mannitol or sorbitol, and the oligomerization of decene by a recycled adduct of boron trifluoride with mannitol or butanediol. Some of the catalysts become viscous on cooling and are thus more easily separated from the reaction products which remain in a separate liquid phase.

Recyclable boron trifluoride catalyst and method of using same

High purity tetrahydrocarbylammonium tetrahydridoborates are prepared under anhydrous conditions by reacting tetrahydrocarbylammonium salts with at least 8% molar excess of an alkali metal hydroxide in the presence of ethanol to produce the corresponding tetrahydrocarbylammonium hydroxides and alkali metal salts, removing the alkali metal salts and adding an alkali metal borohydride to the solution to produce the corresponding tetrahydrocarbylammonium tetrahydridoborates and alkali metal hydroxides.

Preparation of high purity tetrahydrocarbylammonium tetrahydridoborates

When saturated with boron trifluoride, certain polyhydric alcohols form adducts which catalyze reactions for which boron trifluoride is catalytic. The adduct is recovered from the reaction mixture and recycled, greatly reducing boron and fluoride values in the product and in any effluent. Examples include propylation of toluene in the presence of a recycled adduct of boron trifluoride with mannitol or sorbitol.

Fluoroorganic compounds are prepared by reacting a haloorganic starting material in which at least one halo atom is replaceable with a fluorine atom by metathetical exchange, with calcium fluoride in the presence of a crown ether and an anhydrous, polar, basic organic solvent which complexes with the calcium ion and contains no --OH groups, at a temperature and for a period of time adequate to effect fluorination.

Preparation of fluoroorganic compounds with calcium fluoride

Dry calcium fluoborate suitable for use in the manufacture of boron trifluoride is produced by reacting, in an aqueous medium, calcium fluoride, hydrofluoric acid and boric acid followed by removing water from the calcium fluoborate reaction product by purging the reaction product with a dry inert gas such as nitrogen, at a temperature between about 140.degree. to 160.degree. C.

Process for producing calcium fluoborate

A stabilized heat exchange medium is disclosed including a fluorocarbon, an absorbant and a tribasic phosphite stabilizer. The preferred absorbants are assymetrical furan derivatives containing at least 1 oxygen with a single bond to an adjacent carbon, and is most preferably an alkyl tetrahydrofurfuryl ether. The fluorocarbon contains 1 or 2 carbons, 1 or 2 hydrogens and the remainder chlorine and fluorine. The tribasic phosphites are of the formula (R.sub.1 'O)(R.sub.2 'O)(R.sub.3 'O)P, wherein R.sub.1 ', R.sub.2 ' and R.sub.3 ' are each independently alkyl, alkenyl, phenyl, alkylene phenyl, alkylene alkylphenyl or alkylphenyl.

Stabilized heat activated heat exchange absorption pair

A composition for increasing flame resistance of a step-reaction polymer comprising a metal salt of certain organic acids in combination with certain organic acids or their ammonium salts, the method of treating the step-reaction polymer with the composition and the resulting treated polymer.

Synergistic compositions for increasing flame resistance of polymers

A flame resistant organic polymer which decomposes into fragments containing acidic and/or basic groups and the process for making same comprising treating an organic polymer which decomposes into said fragments with from about 0.5 to about 25 weight percent of a compound which contains at least one functional radical selected from --0--, --S-- and --N-- and at least one carboxyl or mercapto group which is able to dissociate in water to provide a free positively charged ion.

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Hamburg, NY, United States of America

Francis E Evans