Method for the manufacture of cyclododecasulfur
US-10011485-B2 · Jul 3, 2018 · US
US2022169505A1 · US · A1
| Field | Value |
|---|---|
| Publication number | US-2022169505-A1 |
| Application number | US-202017437930-A |
| Country | US |
| Kind code | A1 |
| Filing date | Mar 5, 2020 |
| Priority date | Mar 13, 2019 |
| Publication date | Jun 2, 2022 |
| Grant date | — |
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Methods for producing cyclododecasulfur are disclosed that include the steps of: reacting a metallasulfur derivative with a molecular halogen to produce cyclododecasulfur and a metallahalide derivative; and reacting the metallahalide derivative with a sulfide or polysulfide to produce the metallasulfur derivative and a halide.
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That which is claimed is: 1 . A method for producing cyclododecasulfur, comprising: reacting a metallasulfur derivative with a molecular halogen to produce cyclododecasulfur and a metallahalide derivative; and reacting the metallahalide derivative with a sulfide or polysulfide to produce the metallasulfur derivative and a halide. 2 . The method of claim 1 , wherein the metallahalide comprises zinc. 3 . The method of claim 1 , wherein the metallahalide derivative is reacted with sulfide or polysulfide in the presence of elemental sulfur. 4 . The method of claim 1 , wherein the halide comprises one or more of a metal halide or a quaternary halide. 5 . The method of claim 1 , wherein the metallahalide derivative is reacted with a polysulfide, wherein the polysulfide comprises a higher rank polysulfide dianion, and wherein the reacting of the metallahalide derivative with the polysulfide also produces a lower rank polysulfide dianion. 6 . The method of claim 1 , further comprising oxidizing the halide to produce a mixture of molecular halogen, a trihalide, and a halide. 7 . The method of claim 6 , further comprising a step of reducing a polysulfide comprising a higher rank polysulfide dianion to produce a lower rank metal polysulfide dianion. 8 . The method of claim 7 , wherein the step of oxidizing the halide and the step of reducing the polysulfide are carried out together in an electrochemical cell comprising a catholyte chamber and an anolyte chamber separated by an ion-selective membrane which is permeable to cations, wherein the polysulfide is reduced by electrons in the catholyte chamber, and wherein the halide is oxidized in the anolyte chamber by loss of electrons to produce molecular halogen. 9 . The method of claim 6 , further comprising recovering the molecular halogen from the mixture and using the molecular halogen to produce the cyclododecasulfur. 10 . The method of claim 7 , further comprising recovering the halide from the mixture and using the halide in the step of oxidizing the halide. 11 . The method of claim 1 , wherein the polysulfide is present and is obtained by reacting a sulfide with elemental sulfur to produce the polysulfide. 12 . The method of claim 11 , wherein the sulfide that is reacted with the elemental sulfur is obtained by reacting hydrogen sulfide with a hydroxide to produce the sulfide. 13 . A method for producing cyclododecasulfur, comprising: reacting (TMEDA)Zn(S 6 ) with molecular bromine to produce cyclododecasulfur and (TMEDA)ZnBr 2 ; and reacting (TMEDA)ZnBr 2 with Na 2 S x , wherein x is from about 1.0 to about 8, to produce (TMEDA)Zn(S 6 ) and NaBr. 14 . The method of claim 13 , wherein the step of reacting (TMEDA)ZnBr 2 with Na 2 S x is carried out in the presence of elemental sulfur. 15 . The method of claim 13 , further comprising oxidizing the NaBr to produce a mixture of molecular halogen, NaBr 3 , and NaBr. 16 . The method of claim 15 , further comprising reducing the Na 2 S x comprising a higher rank polysulfide dianion to produce a lower rank polysulfide dianion. 17 . The method of claim 15 , further comprising recovering the molecular bromine from the mixture and using the molecular bromine to produce the cyclododecasulfur. 18 . The method of claim 16 , wherein the oxidizing and the reducing steps are carried out in an electrochemical cell comprising a catholyte chamber and an anolyte chamber separated by an ion-selective membrane which is permeable to cations, wherein the Na 2 S x is reduced by electrons in the catholyte chamber, and wherein the NaBr is oxidized in the anolyte chamber by loss of electrons to produce molecular bromine. 19 . The method of claim 13 , wherein the Na 2 S x comprises a higher rank polysulfide dianion, and wherein the step of reacting (TMEDA)ZnBr 2 with the Na 2 S x also produces a lower rank polysulfide dianion; and wherein the method further comprises a step of reacting the lower rank polysulfide dianion with elemental sulfur to obtain a higher rank polysulfide dianion. 20 . A method comprising reacting a metallahalide derivative with an alkali metal polysulfide to obtain a metallasulfur derivative and an alkali metal halide, optionally in the presence of elemental sulfur.
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