# US 5,703,242 A · Preparation of solutions of imido-alkancarboxylic acids suitable for peroxidation processes > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,703,242 A - Document ID: US5703242A - Status: Granted - Kind: A - Application number: 08/777,699 - Filed: 1996-12-20 - Granted: 1997-12-30 - Earliest claimed: 1995-12-21 - Assignees: Ausimont S.p.A. - Inventors: Claudio Cavallotti; Gilberto Nucida; Claudio Troglia - Web page: https://patentgrep.com/patent/US5703242A ## CPC - C07D 209/48: with oxygen atoms in positions 1 and 3, e.g. phthalimide - C11D 3/3945: {Organic per-compounds (C11D3/3902 takes precedence)} - C07D: HETEROCYCLIC COMPOUNDS (macromolecular compounds C08) - C11D: DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL ## Abstract Purification process of imido-alkancaboxylic acids from contaminants represented by acid-carboxylic, lactam or aminoacids and water comprising: A) Preparation of the imido-alkancarboxylic acid precursor by reaction of an anhydride a1) or the corresponding acids, with an aminoacid b1) with water; or a1) with a lactam b2) and water; at temperatures comprised between 100.degree. and 250.degree. C., under pressure of an inert gas from 1 to 30 bar, for reaction times from 2 to 20 hours; wherein the ratio by moles between a1/(b1 or b2)/water is comprised between 1/1.05-1.1/0.5-2.5; optional addition of water such that it is at least, of 2 moles for mole of a1); B) discharge of the precursor obtained in phase A) in a solvent immiscible with water; C) separation of the aqueous phases from the organic phase; D) recovery of the organic phase for the successive peroxidation reaction. ## Claims ### Claim 1 Purification process of imido-alkancarboxylic acids from contaminants represented by carboxylic acid, lactam or aminoacids and water comprising: A) preparation of the imido-alkancarboxylic acid by reaction of: a1) an anhydride of formula ##STR5## or the corresponding acids, with b1) an aminoacid of formula ##STR6## with c1) water; or a1) with b2) a lactam of general formula ##STR7## with c1) water; at temperatures comprised betweeen 100.degree. C. and 250.degree. C., under pressure of an inert gas from 1 to 30 bar, for reaction times from 2 to 20 hours; wherein A indicates a group of formula ##STR8## n is an integer 0, 1 or 2, R.sup.1 is hydrogen, chlorine, bromine, alkyl C.sub.1 -C.sub.20, alkenyl C.sub.2 -C.sub.20, aryl or alkylaryl, R.sup.2 is hydrogen, chlorine, bromine or a group of formula--SO.sub.3 M, --CO.sub.2 M, --CO.sub.3 M, --OSO.sub.3 M, M indicates hydrogen, an alkaline metal or ammonium ion or the equivalent of an alkaline-earth metal ion and X indicates alkylene C.sub.1 -C.sub.19 or arylene; Y=X wherein the ratio by moles between a1/(b1 or b2)/c1 is comprised between 1/1.0-1.2/0.5-3; B) discharge of precursor obtained in phase A) in a solvent immiscible with water; C) separation of aqueous phases from an organic phase; D) recovery of the organic phase for the successive peroxidation reaction. ### Claim 2 (depends on 1) Purification process of imido-alkancarboxylic acids according to claim 1 wherein the ratio by moles a1/(b1 or b2)/C1 is comprised between 1/1.05-1.1/0.5-2.5. ### Claim 3 (depends on 2) Purification process of imido-alkancarboxylic acids according to claim 2 wherein the ratio by moles a1/(b1 or b2)/c1) is comprised betwwen 1/1.05-1.1/1-2. ### Claim 4 (depends on 1) Purification process of imido-alkancarboxylic acids according to claim 1 wherein the compounds of the type b) are those of class b2), the compounds of class a1) are selected from the following anhydrides or the corresponding acids: succinic, glutaric, maleic, trimellitic, phthalic, pyromellitic and alkyl- or alkenyl-succinic anhydride; the compounds of the class b1) are selected from: omega-aminobutyric acid, omega-aminovalerianic, omega-aminocaproic and omega-aminolauric acid; the compounds of class b2) are selected from: gamma-pyrrolidone, delta-piperidone, epsilon-caprolactam and omega-laurolactam. ### Claim 5 (depends on 4) Purification process of imido-alkancarboxylic acids according to claim 4 wherein the compound a1) is selected from phthalic anhydride or pthalic acid and the compound b2) is epsilon-caprolactam (CPL). ### Claim 6 (depends on 1) Purification process of imido-alkancarboxylic acids according to claim 1, wherein in phase A) the temperature is comprised between 130.degree. C. and 180.degree. C. and the pressure between 4 and 8 bar. ### Claim 7 (depends on 1) Purification process of imido-alkancarboxylic acids according to claim 1, wherein in phase B) a solvent immiscible with water is employed. ### Claim 8 (depends on 7) Purification process of imido-alkancarboxylic acids according to claim 7, wherein in phase B) the solvent is selected from CH.sub.2 Cl.sub.2 and CHCl.sub.3. ### Claim 9 (depends on 1) Purification process of imido-alkancarboxylic acids according to claim 1, wherein in reaction A) it is operated with an amount of water equal to at least 2 moles per mole of the compound a1). ### Claim 10 (depends on 9) Purification process of imido-alkancarboxylic acids according to claim 9, wherein the melt of the reaction A) is discharged in a solvent of phase B) at temperatures from 78.degree. to 95.degree. C. ### Claim 11 (depends on 1) Purification process of imido-alkancarboxylic acids according to claim 1, wherein in phase A) it is operated with an amount of water lower than 2 moles per mole of the compound a1) and water is added at the end of phase A up to a total amount of at least 2 moles per 1 mole of the compound a1). ### Claim 12 (depends on 1) Process for preparing peroxycarboxylic acids in the presence of hydrogen peroxide and a strong acid wherein the imido-alkancarboxylic acid obtained according to claim 1 is utilized as a precursor. ### Claim 13 (depends on 1) Purification process of imido-alkancarboxylic acids according to claim 1, wherein Y is an alkylene C.sub.3 -C.sub.19.