# US 2017/0253484 A1 · Method for the manufacture of cyclododecasulfur > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 2017/0253484 A1 - Document ID: US20170253484A1 - Status: Published application - Kind: A1 - Application number: 15/440,056 - Filed: 2017-02-23 - Published: 2017-09-07 - Earliest claimed: 2016-03-02 - Assignees: Eastman Chemical Company - Applicants: Eastman Chemical Company - Inventors: SCOTT DONALD BARNICKI; ROBERT THOMAS HEMBRE; ELAINE BEATRICE MACKENZIE; JOY LYNN LANINGHAM; MICHAEL RICHARD LANINGHAM; SHANE KIPLEY KIRK; LARRY WAYNE BLAIR; SUMIT CHAKRABORTY; VENKATESWARLU BHAMIDI; GUOXIONG HUA; JOHN DEREK WOOLLINS - Web page: https://patentgrep.com/patent/US20170253484A1 ## CPC - C01B 17/0253: {from non-gaseous sulfur compounds other than sulfides or materials containing such sulfides} - C01B 17/0243: {Other after-treatment of sulfur} - C01B 17/12: Insoluble sulfur (mu-sulfur) - C07D 341/00: Heterocyclic compounds containing rings having three or more sulfur atoms as the only ring hetero atoms - C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C} - C07D: HETEROCYCLIC COMPOUNDS (macromolecular compounds C08) ## Abstract The present invention relates to a method for the manufacture of cyclododecasulfur, a cyclic sulfur allotrope wherein the number of sulfur (S) atoms in the allotrope's homocyclic ring is 12. The method includes reacting a metallasulfur derivative with an oxidizing agent in a reaction zone to form a cyclododecasulfur-containing reaction mixture. ## Claims ### Claim 1 A method for the manufacture of cyclododecasulfur, comprising reacting a metallasulfur derivative with an oxidizing agent in a reaction zone to form a cyclododecasulfur-containing reaction mixture containing cyclododecasulfur. ### Claim 2 (depends on 1) The method of claim 1 wherein the metallasulfur derivative is characterized by the formula: wherein L is a monodentate or polydentate ligand species which may be the same or different when x>1; x is the total number of ligand species and is from 0 to 6 inclusive; M is a metal atom; y is the total number of metal atoms and is from 1 to 4 inclusive; S is a sulfur atom; z is the number of sulfur atoms, and is from 1 to 12 inclusive; u represents the charge of the metallasulfur derivative and may be from −6 to +6 inclusive; v is the number of metallasulfur derivative units in an oligomeric or polymeric structure; I is an ionic atom or group and may be cationic or anionic; and w is the number of cationic or anionic atoms or groups, as required to provide charge neutrality. ### Claim 3 (depends on 1) The method of claim 1 wherein the oxidizing agent is characterized by the formula: X-X′ wherein X and X′ are the same or different and are selected from the group consisting of halogens and pseudohalogens. ### Claim 4 (depends on 1) The method of claim 1, wherein the oxidizing agent comprises one or more of SO2Cl2 and SO2Br2. ### Claim 5 (depends on 1) The method of claim 1 wherein the oxidizing agent comprises one or more of O2, H2O2, an alkyl peroxide, and an acyl peroxide. ### Claim 6 (depends on 1) The method of claim 1, wherein the stoichiometric ratio of the oxidizing agent to the metallasulfur derivative is less than one equivalent of the oxidizing agent is present for every two M-S bonds in the metallasulfur derivative. ### Claim 7 (depends on 3) The method of claim 3, wherein X and X′ are one or more of chlorine and bromine. ### Claim 8 (depends on 1) The method of claim 1, further comprising a step of reacting elemental sulfur with a sulfur templating agent to form the metallasulfur derivative prior to the step of reacting the metallasulfur derivative with the oxidizing agent. ### Claim 9 (depends on 8) The method of claim 8, wherein the reacting the elemental sulfur with a sulfur templating agent to form the metallasulfur derivative is carried out in the presence of water. ### Claim 10 (depends on 1) The method of claim 1, further comprising a step of isolating the cyclododecasulfur from the cyclododecasulfur-containing reaction mixture. ### Claim 11 (depends on 10) The method of claim 10, wherein the step of isolating the cyclododecasulfur from the cyclododecasulfur-containing reaction mixture comprises one or more steps chosen from dissolving, heat treating, drying, acid treating, solvent washing, crystallizing, and sedimentation. ### Claim 12 (depends on 10) The method of claim 10, wherein the step of isolating the cyclododecasulfur comprises treating the cyclododecasulfur with a solvent for the cyclododecasulfur to form a dissolution liquor. ### Claim 13 (depends on 10) The method of claim 10, further comprising removing metal and metal-containing compounds from the cyclododecasulfur by sedimentation of the metal and the metal-containing compounds. ### Claim 14 (depends on 1) The method of claim 1, further comprising isolating cyclododecasulfur by heating a cyclododecasulfur-containing mixture in the presence of a solvent to decompose and dissolve in the solvent impurities that are present. ### Claim 15 (depends on 1) The method of claim 1, further comprising isolating cyclododecasulfur by treating a cyclododecasulfur-containing mixture with an acid to remove any metal or metal-containing compounds that are present. ### Claim 16 (depends on 12) The method of claim 12, further comprising crystallizing cyclododecasulfur from the dissolution liquor. ### Claim 17 A method for the manufacture of cyclododecasulfur, the method comprising: (i) reacting cyclooctasulfur, tetramethylethylenediamine, and zinc to form a tetramethylethylenediamine/Zn(S6) complex; and (ii) reacting the complex with an oxidizing agent. ### Claim 18 (depends on 17) The method of claim 17, wherein the step of reacting the cyclooctasulfur, the tetramethylethylenediamine, and the zinc to form a tetramethylethylene-diamine/Zn(S6) complex is carried out in the presence of water.