Sulfur separation process

Claim 2

A process for the removal of H 2 S from a sour gaseous stream comprising: (a) contacting the sour gaseous stream in a contacting zone with an aqueous reaction solution at a temperature below the melting point of sulfur, the solution containing an effective amount of a reactant comprising an oxidizing polyvalent metal chelate of an acid having the formula R1 ? ##STR3## from two to four of the groups Y are selected from acetic and propionic acid groups; from zero to two of the groups Y are selected from 2-hydroxy ethyl, 2-hydroxy propyl, and ##STR4## wherein X is selected from acetic acid and propionic acid groups; and R is ethylene, propylene or isopropylene or alternatively cyclohexane or benzene where the two hydrogen atoms replaced by nitrogen atoms are in the 1,2 position; and mixtures thereof, and producing a sweet gas stream and an aqueous admixture containing sulfur and reduced reactant; (b) removing aqueous admixture from the contacting zone; (c) contacting aqueous admixture in an extraction zone with a liquid composition selected from compounds having the formula C n H 2 (n+1), wherein n is a number from 4 through 8, and mixtures thereof, in an amount sufficient to remove at least the bulk of the sulfur from said admixture and form a separate phase containing sulfur and said composition, and forming a three phase mass comprising an upper mass containing solid sulfur and said liquid composition, and a lower phase in contact with said upper mass, said lower phase comprising aqueous admixture containing reduced reactant; (d) separating at least a portion of the upper mass, and recovering sulfur from the portion separated; (e) separating aqueous admixture containing reduced reactant from the lower phase, and regenerating said separated aqueous admixture in a regeneration zone to produce an aqueous admixture containing a regenerated reactant; (f) returning aqueous admixture from the regeneration zone to the contacting zone.

Claim 3

The process of claim 1 wherein at least a portion of the liquid recovered from the upper mass separated in step (d) is, after sulfur removal, returned to the extraction zone.

Claim 4

The process of claim 1 wherein at least a portion of the liquid composition in the upper mass of step (c) is decanted and returned for contact with aqueous admixture.

Claim 5

A process for the removal of H 2 S from a sour gaseous stream comprising (a) contacting the sour gaseous stream in a contacting zone with an aqueous reaction solution at a temperature below the melting point of sulfur, the solution containing an effective amount of a reactant comprising an oxidizing polyvalent metal chelate of an acid having the formula ##STR5## wherein from two to four of the groups Y are selected from acetic and propionic acid groups; from zero to two of the groups Y are selected from 2-hydroxy ethyl, 2-hydroxy propyl, and ##STR6## wherein X is selected from acetic acid and propionic acid groups; and R is ethylene, propylene or isopropylene or alternatively cyclohexane or benzene where the two hydrogen atoms replaced by nitrogen atoms are in the 1,2 position; and mixtures thereof, and producing a sweet gas stream and an aqueous admixture containing sulfur and reduced reactant; (b) removing aqueous admixture from the contacting zone, and regenerating the aqueous admixture to produce a regenerated aqueous admixture containing a regenerated reactant and sulfur; (c) contacting regenerated aqueous admixture in an extraction zone with a liquid composition selected from compounds having the formula C n H 2 (n+1), wherein n is a whole number from 4 through 8, and mixtures thereof, in an amount sufficient to remove at least the bulk of the sulfur from said regenerated aqueous admixture and form a separate phase containing sulfur and said composition, and forming a three phase mass comprising an upper mass containing solid sulfur and said liquid composition, and a lower phase in contact with said upper mass, said lower phase comprising regenerated aqueous reaction solution; (d) separating at least a portion of the upper mass, and recovering sulfur from the portion separated; (e) separating regenerated aqueous reaction solution from the lower phase, and returning regenerated aqueous reaction solution to the contacting zone.

Claim 6

A process for the removal of H 2 S from a sour gaseous stream comprising (a) contacting the sour gaseous stream in a contacting zone with an aqueous reaction solution at a temperature below the melting point of sulfur, the solution containing an effective amount of a reactant comprising an oxidizing polyvalent metal chelate of an acid having the formula ##STR5## wherein from two to four of the groups Y are selected from acetic and propionic acid groups; from zero to two of the groups Y are selected from 2-hydroxy ethyl, 2-hydroxy propyl, and ##STR6## wherein X is selected from acetic acid and propionic acid groups; and R is ethylene, propylene or isopropylene or alternatively cyclohexane or benzene where the two hydrogen atoms replaced by nitrogen atoms are in the 1,2 position; and mixtures thereof, and producing a sweet gas stream and an aqueous admixture containing sulfur and reduced reactant; (b) removing aqueous admixture from the contacting zone, and regenerating the aqueous admixture to produce a regenerated aqueous admixture containing a regenerated reactant and sulfur; (c) contacting regenerated aqueous admixture in an extraction zone with a liquid composition selected from compounds having the formula C n H 2 (n+1), wherein n is a whole number from 4 through 8, and mixtures thereof, in an amount sufficient to remove at least the bulk of the sulfur from said regenerated aqueous admixture and form a separate phase containing sulfur and said composition, and forming a three phase mass comprising an upper mass containing solid sulfur and said liquid composition, and a lower phase in contact with said upper mass, said lower phase comprising regenerated aqueous reaction solution; (d) separating at least a portion of the upper mass, and recovering sulfur from the portion separated; (e) separating regenerated aqueous reaction solution from the lower phase, and returning regenerated aqueous reaction solution to the contacting zone.

Claim 7

The process of claim 4 wherein at least a portion of the liquid recovered from the upper mass separated in step (d) is, after sulfur removal, returned to the extraction zone.

Claim 8

The process of claim 4 wherein at least a portion of the liquid composition in the upper mass of step (c) is decanted and returned for contact with aqueous admixture.

Claim 9

The process of claim 1 wherein the oxidizing polyvalent metal chelate compound is the Fe(III) chelate of N-(2-hydroxyethyl)ethylenediamine triacetic acid.

Claim 10

The process of claim 2 wherein the oxidizing polyvalent metal chelate compound is the Fe(III) chelate of N-(2-hydroxyethyl)ethylenediamine triacetic acid.

Claim 11

The process of claim 3 wherein the oxidizing polyvalent metal chelate compound is the Fe(III) chelate of N-(2-hydroxyethyl)ethylenediamine triacetic acid.

Claim 12

The process of claim 4 wherein the oxidizing polyvalent metal chelate compound is the Fe(III) chelate of N-(2-hydroxyethyl)ethylenediamine triacetic acid.

Claim 13

The process of claim 5 wherein the oxidizing polyvalent metal chelate compound is the Fe(III) chelate of N-(2-hydroxyethyl)ethylenediamine triacetic acid.

Claim 14

The process of claim 6 wherein the oxidizing polyvalent metal chelate compound is the Fe(III) chelate of N-(2-hydroxyethyl)ethylenediamine triacetic acid.

Claim 15

A process for the removal of H 2 S from a sour gaseous stream comprising (a) contacting the sour gaseous stream in a contacting zone with an aqueous reaction solution at a temperature below the melting point of sulfur, the solution containing an effective amount of a reactant comprising an oxidizing polyvalent metal chelate of an acid having the formula ##STR7## wherein from two to four of the groups Y are selected from acetic and propionic acid groups; from zero to two of the groups Y are selected from 2-hydroxy ethyl, 2-hydroxy propyl, and ##STR8## wherein X is selected from acetic acid and propionic acid groups; and R is ethylene, propylene or isopropylene or alternatively cyclohexane or benzene where the two hydrogen atoms replaced by nitrogen atoms are in the 1,2 position; and mixtures thereof, and producing a sweet gas stream and an aqueous admixture containing sulfur and reduced reactant; (b) removing aqueous admixture from the contacting zone; (c) separating removed aqueous admixture into an aqueous reactant solution having reduced sulfur content and an aqueous reactant slurry containing increased sulfur content; and regenerating aqueous reactant solution having reduced sulfur content and producing regenerated reaction solution, and returning regenerated reaction solution to the contacting zone; (d) concomitantly contacting aqueous reactant slurry in an extraction zone with a liquid composition selected from compounds having the formula C n H 2 (n+1), wherein n is a number from 4 through 8, and mixtures thereof, in an amount sufficient to remove at least the bulk of the sulfur from said slurry and form a separate phase containing sulfur and said composition, and forming a three phase mass comprising an upper mass containing solid sulfur and said liquid composition, and a lower phase in contact with said upper mass, said lower phase comprising aqueous admixture containing reduced reactant; (e) separating at least a portion of the upper mass, and recovering sulfur from the portion separated; (f) separating aqueous admixture containing reduced reactant from the lower phase, and regenerating said separated aqueous admixture in a regeneration zone to produce an aqueous admixture containing a regenerated reactant; (g) returning aqueous admixture from the regeneration zone to the contacting zone.

Claim 16

A process for the removal of H 2 S from a sour gaseous stream comprising (a) contacting the sour gaseous stream in a contacting zone with an aqueous reaction solution at a temperature below the melting point of sulfur, the solution containing an effective amount of a reactant comprising an oxidizing polyvalent metal chelate of an acid having the formula ##STR7## wherein from two to four of the groups Y are selected from acetic and propionic acid groups; from zero to two of the groups Y are selected from 2-hydroxy ethyl, 2-hydroxy propyl, and ##STR8## wherein X is selected from acetic acid and propionic acid groups; and R is ethylene, propylene or isopropylene or alternatively cyclohexane or benzene where the two hydrogen atoms replaced by nitrogen atoms are in the 1,2 position; and mixtures thereof, and producing a sweet gas stream and an aqueous admixture containing sulfur and reduced reactant; (b) removing aqueous admixture from the contacting zone; (c) separating removed aqueous admixture into an aqueous reactant solution having reduced sulfur content and an aqueous reactant slurry containing increased sulfur content; and regenerating aqueous reactant solution having reduced sulfur content and producing regenerated reaction solution, and returning regenerated reaction solution to the contacting zone; (d) concomitantly contacting aqueous reactant slurry in an extraction zone with a liquid composition selected from compounds having the formula C n H 2 (n+1), wherein n is a number from 4 through 8, and mixtures thereof, in an amount sufficient to remove at least the bulk of the sulfur from said slurry and form a separate phase containing sulfur and said composition, and forming a three phase mass comprising an upper mass containing solid sulfur and said liquid composition, and a lower phase in contact with said upper mass, said lower phase comprising aqueous admixture containing reduced reactant; (e) separating at least a portion of the upper mass, and recovering sulfur from the portion separated; (f) separating aqueous admixture containing reduced reactant from the lower phase, and regenerating said separated aqueous admixture in a regeneration zone to produce an aqueous admixture containing a regenerated reactant; (g) returning aqueous admixture from the regeneration zone to the contacting zone.

Claim 17

The process of claim 13 wherein at least a portion of the liquid recovered from the upper mass separated in step (e) is, after sulfur removal, returned to the extraction zone.

Claim 18

The process of claim 13 wherein at least a portion of the liquid composition in the upper mass of step (c) is decanted and returned for contact with aqueous admixture.

Claim 19

A process for the removal of H 2 S from a sour gaseous stream comprising (a) contacting the sour gaseous stream in a contacting zone with an aqueous reaction solution at a temperature below the melting point of sulfur, the solution containing an effective amount of a reactant comprising an oxidizing polyvalent metal chelate of an acid having the formula ##STR9## wherein from two to four of the groups Y are selected from acetic and propionic acid groups; from zero to two of the groups Y are selected from 2-hydroxy ethyl, 2-hydroxy propyl, and ##STR10## wherein X is selected from acetic acid and propionic acid groups; and R is ethylene, propylene or isopropylene or alternatively cyclohexane or benzene where the two hydrogen atoms replaced by nitrogen atoms are in the 1,2 position; and mixtures thereof, and producing a sweet gas stream and an aqueous admixture containing sulfur and reduced reactant; (b) removing aqueous admixture from the contacting zone, and regenerating the aqueous admixture to produce a regenerated aqueous admixture containing a regenerated reactant and sulfur; (c) separating the regenerated aqueous admixture into a regenerated aqueous reaction solution having reduced sulfur content and a regenerated aqueous reactant slurry containing increased sulfur content; (d) contacting regenerated aqueous reactant slurry in an extraction zone with a liquid composition selected from compounds having the formula C n H 2 (n+1), wherein n is a whole number from 4 through 8, and mixtures thereof, in an amount sufficient to remove at least the bulk of the sulfur from said regenerated reactant slurry and form a separate phase containing sulfur and said composition, and forming a three phase mass comprising an upper mass containing solid sulfur and said liquid composition, and a lower phase in contact with said upper mass, said lower phase comprising regenerated aqueous reaction solution; (e) separating at least a portion of the upper mass and recovering sulfur from the portion separated; (f) separating regenerated aqueous reaction solution from the lower phase, and returning regenerated aqueous reaction solution to the contacting zone.

Claim 20

A process for the removal of H 2 S from a sour gaseous stream comprising (a) contacting the sour gaseous stream in a contacting zone with an aqueous reaction solution at a temperature below the melting point of sulfur, the solution containing an effective amount of a reactant comprising an oxidizing polyvalent metal chelate of an acid having the formula ##STR9## wherein from two to four of the groups Y are selected from acetic and propionic acid groups; from zero to two of the groups Y are selected from 2-hydroxy ethyl, 2-hydroxy propyl, and ##STR10## wherein X is selected from acetic acid and propionic acid groups; and R is ethylene, propylene or isopropylene or alternatively cyclohexane or benzene where the two hydrogen atoms replaced by nitrogen atoms are in the 1,2 position; and mixtures thereof, and producing a sweet gas stream and an aqueous admixture containing sulfur and reduced reactant; (b) removing aqueous admixture from the contacting zone, and regenerating the aqueous admixture to produce a regenerated aqueous admixture containing a regenerated reactant and sulfur; (c) separating the regenerated aqueous admixture into a regenerated aqueous reaction solution having reduced sulfur content and a regenerated aqueous reactant slurry containing increased sulfur content; (d) contacting regenerated aqueous reactant slurry in an extraction zone with a liquid composition selected from compounds having the formula C n H 2 (n+1), wherein n is a whole number from 4 through 8, and mixtures thereof, in an amount sufficient to remove at least the bulk of the sulfur from said regenerated reactant slurry and form a separate phase containing sulfur and said composition, and forming a three phase mass comprising an upper mass containing solid sulfur and said liquid composition, and a lower phase in contact with said upper mass, said lower phase comprising regenerated aqueous reaction solution; (e) separating at least a portion of the upper mass and recovering sulfur from the portion separated; (f) separating regenerated aqueous reaction solution from the lower phase, and returning regenerated aqueous reaction solution to the contacting zone.

Claim 21

The process of claim 16 wherein at least a portion of the upper mass separated in step (e) is, after sulfur removal, returned to the extraction zone.

Claim 22

The process of claim 16 wherein at least a portion of the liquid composition in the upper mass of step (c) is decanted and returned for contact with aqueous admixture.

Claim 23

The process of claim 13 wherein the oxidizing polyvalent metal chelate compound is the Fe(III) chelate of N-(2-hydroxyethyl)ethylenediamine triacetic acid.

Claim 24

The process of claim 14 wherein the oxidizing polyvalent metal chelate compound is the Fe(III) chelate of N-(2-hydroxyethyl)ethylenediamine triacetic acid.

Claim 25

The process of claim 15 wherein the oxidizing polyvalent metal chelate compound is the Fe(III) chelate of N-(2-hydroxyethyl)ethylenediamine triacetic acid.

Claim 26

The process of claim 16 wherein the oxidizing polyvalent metal chelate compound is the Fe(III) chelate of N-(2-hydroxyethyl)ethylenediamine triacetic acid.

Claim 27

The process of claim 17 wherein the oxidizing polyvalent metal chelate compound is the Fe(III) chelate of N-(2-hydroxyethyl)ethylenediamine triacetic acid.

Claim 28

The process of claim 18 wherein the oxidizing polyvalent metal chelate compound is the Fe(III) chelate of N-(2-hydroxyethyl)ethylenediamine triacetic acid.