Refinement of sulfonated hydrocarbons

Claim 2

A process of enhancing the separation of unreacted hydrocarbons from the sulfonated product mixture obtained by contacting about 5 to about 30 grams sulfur trioxide per 100 kilograms of a hydrocarbon selected from the group consisting of crude oils, top crude oils, gas oils and mixtures thereof in a reaction zone at a temperature of from about 27° C. to about 121° C. and a pressure from about 0.01 to about 150 atmospheres for a reaction time of from about 0.001 to about 3600 seconds to form a sulfonated product mixture from which a raffinate comprising free unreacted hydrocarbons separates, said method comprising the steps of: (a) removing a portion of said raffinate thereby leaving the remainder of said raffinate with said sulfonated product mixture; (b) neutralizing with a base said sulfonated product mixture containing said remainder of said raffinate to form a neutralized sulfonated product mixture and a second raffinate; and (c) thereafter removing said second raffinate from the neutralized sulfonated product mixture, the remainder of said raffinate in step (a) being in an amount sufficient to enhance the separation rate of said second raffinate and said neutralized sulfonated product mixture thereby enabling the removing of step (c) to take place at a rate faster than that which would take place if substantially all of said raffinate had been removed prior to step (b).

Claim 3

The process of claim 1 wherein step (a) comprises removing substantially all of said raffinate and thereafter adding a portion of the raffinate as said remainder to said sulfonated product mixture prior to the neutralizing of step (b).

Claim 4

The process of claim 1 or claim 2 further comprising adding an extraction solvent to the sulfonated product mixture prior to step (a).

Claim 5

The process of claim 1 or claim 3 wherein the sulfonate product mixture prior to its neutralization contains an amount of said remainder of said raffinate which will cause a separation between the neutralized sulfonate product and free unreacted hydrocarbon to occur at a rate of from about 0.3 to about 0.6 hours per foot of emulsion.

Claim 6

The process of claim 1 or claim 3 wherein the sulfonate product mixture prior to its neutralization contains from about 7 to about 12 percent by volume of said remainder of said raffinate.

Claim 7

The process of claim 3 wherein the extraction solvent is used in an amount of from about 0.1 to about 3 killograms per kilogram of sulfonated product mixture.

Claim 8

The process of claim 6 wherein the extraction solvent is selected from the group consisting of water and a low molecular weight aqueous alcohol.

Claim 9

The process of claim 7 wherein the hydrocarbon to be sulfonated is selected from the group consisting of crude oils and topped crude oils and the extraction solvent is water.

Claim 10

The process of claim 7 wherein the hydrocarbon to be sulfonated is a gas oil and the extraction solvent is a low molecular weight aqueous alcohol.

Claim 11

In a process for the preparation of petroleum sulfonates useful in the preparation of micellar dispersions for supplemental recovery of oil, said sulfonates having an average equivalent weight of from about 350 to about 525, by contacting sulfur trioxide with hydrocarbon selected from the group consisting of crude oils, topped crude oils, gas oils and mixtures thereof at a temperature of from about 38° C. to about 93° C. and a pressure of from about 0.15 to about 75 atmospheres for a reaction time of from about 0.1 to about 360 seconds wherein from about 7 to about 20 kilograms of sulfur trioxide are contacted with each 100 kilograms of hydrocarbon, the improvement comprising: (a) partially extracting free unreacted hydrocarbon from the sulfonated product mixture with from about 0.1 to about 3.0 kilograms of an extraction solvent per kilogram of sulfonated product mixture to obtain sulfonated product mixture containing from about 7 to about 12 percent by volume of the free unreacted hydrocarbon; (b) neutralizing with a monovalent base the sulfonated product mixture containing from about 7 to about 12 percent free unreacted hydrocarbon; (c) permitting the sulfonate product mixture and free unreacted hydrocarbon to separate; and (d) removing all of the free unreacted hydrocarbon from the neutralized sulfonated product.

Claim 12

In a process for the preparation of petroleum sulfonates useful in the preparation of micellar dispersions for supplemental recovery of oil, said sulfonates having an average equivalent weight of from about 350 to about 525, by contacting sulfur trioxide with hydrocarbon selected from the group consisting of crude oils, topped crude oils, gas oils and mixtures thereof at a temperature of from about 38° C. to about 93° C. and a pressure of from about 0.15 to about 75 atmospheres for a reaction time of from about 0.1 to about 360 seconds wherein from about 7 to about 20 kilograms of sulfur trioxide are contacted with each 100 kilograms of hydrocarbon, the improvement comprising: (a) partially extracting free unreacted hydrocarbon from the sulfonated product mixture with from about 0.1 to about 3.0 kilograms of an extraction solvent per kilogram of sulfonated product mixture to obtain sulfonated product mixture containing from about 7 to about 12 percent by volume of the free unreacted hydrocarbon; (b) neutralizing with a monovalent base the sulfonated product mixture containing from about 7 to about 12 percent free unreacted hydrocarbon; (c) permitting the sulfonate product mixture and free unreacted hydrocarbon to separate; and (d) removing all of the free unreacted hydrocarbon from the neutralized sulfonated product.

Claim 13

The process of claim 10 wherein the extraction solvent is used in an amount of from about 0.3 to about 1.5 kilograms per kilogram of the sulfonated product mixture.

Claim 14

The process of claim 10 or claim 11 wherein the extraction solvent is selected from the group consisting of water or a low molecular weight aqueous alcohol solution.

Claim 15

The process of claim 12 wherein the hydrocarbon sulfonated is selected from the group consisting of crude oils and topped crude oils and the extraction solvent is water.

Claim 16

The process of claim 12 wherein the hydrocarbon feedstock sulfonate is a gas oil and the extraction solvent is a low molecular weight aqueous alcohol selected from the group consisting of aqueous ethanol and aqueous propanol.

Claim 17

In a process for the preparation of petroleum sulfonates comprising contacting sulfur trioxide with a hydrocarbon selected from the group consisting of crude oils, topped crude oils, gas oils and mixtures thereof in a reaction zone at a temperature of from about 27° C. to about 121° C. and a pressure of from about 0.1 to about 150 atmospheres for a reaction time of from about 0.001 to about 3600 seconds wherein from about 5 to about 30 kilograms of sulfur trioxide are contacted with each 100 kilograms of hydrocarbon, the improvement comprising: (a) allowing the sulfonate product mixture to separate into a free unreacted hydrocarbon phase and an acid sulfonated product phase; (b) separating the sulfonate product mixture into a phase containing a portion of the free unreacted hydrocarbon and an acid sulfonated product phase containing the remainder of the free unreacted hydrocarbon such that the remainder of free unreacted hydrocarbon causes a faster separation between unreacted hydrocarbon and neutralized sulfonate product than is possible if a complete separation were effected between the free unreacted hydrocarbon and the sulfonated product mixture to be neutralized; (c) neutralizing with a base the acid sulfonated product mixture containing the remainder of the free unreacted hydrocarbon of step (b); and (d) thereafter removing all of the free unreacted hydrocarbon from the neutralized sulfonated product mixture at a rate of from about 0.3 to about 0.6 hours per foot of emulsion.

Claim 18

In a process for the preparation of petroleum sulfonates comprising contacting sulfur trioxide with a hydrocarbon selected from the group consisting of crude oils, topped crude oils, gas oils and mixtures thereof in a reaction zone at a temperature of from about 27° C. to about 121° C. and a pressure of from about 0.1 to about 150 atmospheres for a reaction time of from about 0.001 to about 3600 seconds wherein from about 5 to about 30 kilograms of sulfur trioxide are contacted with each 100 kilograms of hydrocarbon, the improvement comprising: (a) allowing the sulfonate product mixture to separate into a free unreacted hydrocarbon phase and an acid sulfonated product phase; (b) separating the sulfonate product mixture into a phase containing a portion of the free unreacted hydrocarbon and an acid sulfonated product phase containing the remainder of the free unreacted hydrocarbon such that the remainder of free unreacted hydrocarbon causes a faster separation between unreacted hydrocarbon and neutralized sulfonate product than is possible if a complete separation were effected between the free unreacted hydrocarbon and the sulfonated product mixture to be neutralized; (c) neutralizing with a base the acid sulfonated product mixture containing the remainder of the free unreacted hydrocarbon of step (b); and (d) thereafter removing all of the free unreacted hydrocarbon from the neutralized sulfonated product mixture at a rate of from about 0.3 to about 0.6 hours per foot of emulsion.