Method of polyarylene sulfide precipitation
US-10106654-B2 · Oct 23, 2018 · US
US9562138B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-9562138-B2 |
| Application number | US-201615181136-A |
| Country | US |
| Kind code | B2 |
| Filing date | Jun 13, 2016 |
| Priority date | Apr 30, 2012 |
| Publication date | Feb 7, 2017 |
| Grant date | Feb 7, 2017 |
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The present invention relates to a method for separating volatile substances, particularly iodine, diiodized aromatic compounds and/or mixtures thereof, from material mixtures containing said compounds. The invention further relates to a device for producing polyarylene sulphides, by means of which volatile substances, particularly iodine and diiodized aromatic compounds, can be separated from the polymers.
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The invention claimed is: 1. A method for producing a polyarylene sulfide including at least one repeat unit of the following general formula I, the method comprising: performing a condensation of a di-iodized aromatic compound of the following general formula II using a sulfidation agent, wherein a material mixture comprising iodine and/or the at least one di-iodized aromatic compound of the general formula II is separated during the condensation step by a method, characterized in that a) a first part of the material mixture is separated at a pressure which is equal to or larger than the pressure which is present at the triple point of iodine; and b) a second part of the material mixture is separated at a pressure which is smaller than the pressure which is present at the triple point of iodine; wherein in both steps a) and b), the material mixture respectively has temperatures at which at least iodine is present in a gaseous state at the said pressures: A-S Formula I I-A-I Formula II In the Formulae I and II, A represents a bivalent aromatic radical. 2. The method in accordance with claim 1 , wherein the condensation step comprises: reacting the compound of the general formula II using the sulfidation agent to produce a prepolymer of the polyarylene sulfide of the general formula I; and condensation polymerizing the prepolymer. 3. The method in accordance with claim 2 , wherein the separation of the material mixture is performed during each of the steps of producing the prepolymer and polymerizing the prepolymer. 4. The method in accordance with claim 3 , wherein the step of producing the prepolymer and the separation of the first part therein takes place at a) the temperature of the material mixture of 250 to 320° C.; and/or b) at the pressure of ≧126 mbar (absolute pressure). 5. The method in accordance with claim 3 , wherein the step of polymerizing the prepolymer and the separation of the second part therein takes place at a) the temperature of the material mixture of 285 to 320° C.; and/or b) at the pressure of <126 mbar (absolute pressure). 6. The method in accordance with claim 2 , wherein the steps of producing the prepolymer and polymerizing the prepolymer are continuously performed, and the separation of material mixture is performed during each of the steps of producing the prepolymer and polymerizing the prepolymer, thereby continuously separating and draining the first and the second parts of the material mixture, respectively. 7. The method in accordance with claim 2 , wherein the first and/or the second parts of the separated material mixture are recycled to and re-used in the step of the producing the prepolymer. 8. The method in accordance with claim 7 , wherein the di-iodized aromatic compound of the general formula II in the first parts of the separated material mixture is recycled to and re-used in the step of the producing the prepolymer. 9. The method in accordance with claim 1 , wherein the first part of the separated material mixture is distilled and condensed, and liquefied. 10. The method in accordance with claim 1 , wherein the second part of the separated material mixture is desublimated and distilled. 11. The method in accordance with claim 1 , wherein the condensation step including the separation of the iodine is performed in a reactor. 12. The method in accordance with claim 1 , wherein the di-iodized aromatic compound of the following general formula II has at least one bivalent aromatic radical A selected from the group consisting of ortho-phenylene radical, meta-phenylene radical, para-phenylene radical, biphenylene radical, diphenylether radical, naphthylene radical and benzophenone radical. 13. The method in accordance with claim 1 , wherein the sulfidation agent is sulfur or alkali sulfide. 14. The method in accordance with claim 2 , wherein the prepolymer and the polyarylene sulfide include the repeat units of the general formula I, and at least one end of the repeat units are terminated with hydrogen. 15. The method in accordance with claim 2 , wherein the prepolymer has a viscosity of 0.1 to 10 Pas and the polyarylene sulfide has a viscosity of 15 to 400 Pas.
Recovery or purification · CPC title
derived from monomers containing one aromatic ring · CPC title
Stationary reactors without moving elements inside · CPC title
Stationary reactors without moving elements inside (B01J19/08, B01J19/26 take precedence; with stationary particles B01J8/02) · CPC title
Polysulfides · CPC title
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