Method for the manufacture of polymeric sulfur

Patent metadata

Field	Value
Publication number	US-10000380-B2
Application number	US-201715440007-A
Country	US
Kind code	B2
Filing date	Feb 23, 2017
Priority date	Mar 2, 2016
Publication date	Jun 19, 2018
Grant date	Jun 19, 2018

Abstract

The present invention relates to a method for the manufacture of polymeric sulfur. The method includes reacting a metallasulfur derivative with an oxidizing agent to form polymeric sulfur.

First claim

The invention claimed is:

1. A method for the manufacture of polymeric sulfur, comprising reacting a metallasulfur derivative with an oxidizing agent in a reaction zone to form polymeric sulfur in a polymeric sulfur-containing reaction mixture.

2. 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.

3. The method of claim 2 , 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.

4. The method of claim 3 , wherein the stoichiometric ratio of the oxidizing agent to the metallasulfur derivative is selected so that less than one equivalent of the oxidizing agent is present for every two M-S bonds in the metallasulfur derivative.

5. The method of claim 3 , wherein X and X′ are chlorine or bromine.

6. The method claim 1 , wherein the reacting is carried out at a temperature greater than ambient temperature.

7. The method claim 1 , wherein the reacting is carried out at a temperature from about 40° C. to about 60° C.

8. The method of claim 1 , further comprising 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.

9. The method of claim 1 , further comprising isolating the polymer from the polymer-containing reaction mixture by:
(i) dissolving impurities from the polymer-containing mixture by treating the polymer-containing mixture with a solvent for the impurities to form a dissolution liquor, followed by separating polymer particles from the dissolution liquor to obtain mother-liquor-wet polymer particles; and
(ii) drying the mother-liquor-wet polymer particles from step (i) to produce purified polymer.

10. The method of claim 1 , further comprising isolating the polymer from the polymer-containing reaction mixture by:
(i) contacting the polymer-containing mixture with a sedimentation solvent to produce a suspended slurry mixture and a settled particle layer;
(ii) dissolving impurities from the settled particle layer by treating the settled particle layer with a solvent for the impurities to form a dissolution liquor, followed by separating polymer particles from the dissolution liquor to obtain mother-liquor-wet particles; and
(iii) drying the mother-liquor-wet polymer particles to produce purified polymer.

11. The method of claim 1 , further comprising isolating the polymer from the polymer-containing reaction mixture by:
(i) dissolving impurities from the polymer-containing mixture by treating the polymer-containing mixture with a solvent for the impurities to form a dissolution liquor, followed by separating polymer particles from the dissolution liquor;
(ii) contacting the polymer particles with a sedimentation solvent to produce a suspended slurry mixture and a settled particle layer; and
(iii) separating the settled particle layer from the suspended slurry mixture to obtain purified polymer.

12. The method of claim 8 , further comprising forming a slurry of the sulfur templating agent in a solvent prior to the reacting step.

13. The method of claim 8 , further comprising forming a solution of the sulfur templating agent in a solvent prior to the reacting step.

14. A method for the manufacture of a polymeric sulfur compound, the method comprising:
(i) reacting cyclooctasulfur, tetramethylethylenediamine, and zinc in the presence of water to form a tetramethylethylenediamine/Zn(S 6 ) complex; and
(ii) reacting the complex with an oxidizing agent in the presence of a solvent for the complex at a temperature greater than ambient temperature.

Assignees

• Eastman Chem Co

Inventors

• Barnicki Scott Donald
• Hembre Robert Thomas
• Laningham Michael Richard
• Chakraborty Sumit
• Bhamidi Venkateswarlu

Classifications

• C07F3/06

  Zinc compounds · CPC title

• C07D341/00

  Heterocyclic compounds containing rings having three or more sulfur atoms as the only ring hetero atoms · CPC title

• C01B17/12

  Insoluble sulfur (mu-sulfur) · CPC title

• C01B17/0253 Primary

  from non-gaseous sulfur compounds other than sulfides or materials containing such sulfides · CPC title

• C01B17/0243

  Other after-treatment of sulfur · CPC title