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Process for desulphurisation of liquid hydrocarbon fuels

a technology of liquid hydrocarbon fuels and desulphurization, which is applied in the petroleum industry, petroleum industry, and treatment with plural serial refining stages, etc., can solve the problems of difficult removal, fuels are receiving intense scrutiny, and high consumption inevitably has a major impact on the global environmen

Inactive Publication Date: 2007-07-05
COUNCIL OF SCI & IND RES +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Benefits of technology

[0052] In yet another embodiment the use of continuous counter current oxidation reactor eliminate the need of settler as the settling zones are provided in the reactor itself.

Problems solved by technology

This high consumption inevitably has a major impact on global environment.
Most notably transport hydrocarbon fuels like diesel fuel, gasoline, jet fuels are receiving intense scrutiny due to increased environmental concerns.
Hydrodesulphurization can easily remove sulphur from several common classes of sulphur compounds such as sulphides, disulphides and thiols present in hydrocarbon fuels, because these are easily accessible to contact with hydrodesulphurization catalyst, however sulphur compounds like 4,6-dimethyldibenzothiophene (4,6-DMDBT) and others similar thiophene species are rigid to hydrodesulphurization and therefore are difficult to remove.
However to bring down sulphur content further below 100 ppm deep hydrodesulphurization of diesel requires very severe operating condition like the use of high temperature, high hydrogen pressure more active catalyst and long residence time.
Deep hydrodesulphurization yield negative effects such as reduce catalyst life, high hydrogen consumption and high yield loss thereby resulting in higher operating cost.
Apart from the cost involved, the energy requirement for implementation of hydro processing technology also leads to increased level of CO2 emission from refinery itself.
However large amounts of hydrogen peroxide were used for the oxidation of sulphur compounds present in gas oil.
This type of system is not convenient for the handling of the bulk product like hydrocarbon fuel.
The removal of sulphones, sulphoxides from bulk oxidized hydrocarbon fuel by adsorption method will involve handling and regeneration of large amount of solid adsorbent and therefore is likely to be very inconvenient and practically difficult process.
Hydrogen peroxide solution of more than 50% strength is not safe to handle at industrial scale.
Although NMP has very high capacity but not high selectivity.
However, incidentally, there are no literature report and use of NMP antisolvent like water mixture for solvent extraction / removal of sulphones / sulphoxides from oxidized hydrocarbon fuels.

Method used

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  • Process for desulphurisation of liquid hydrocarbon fuels
  • Process for desulphurisation of liquid hydrocarbon fuels

Examples

Experimental program
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Effect test

example 1

[0080] A series of experiments were carried out to optimize sulphur to oxidant mole ratio, carboxylic acid to hydrocarbon ratio and reaction time. All these experiments were carried out in a jacketed mixer settler equipped with mechanical stirrer, thermowell, neck for addition of reactant and drain valve. The temperature of reactants was maintained at desired level by circulating hot fluid in the jacket of the mixer settler. In the general experimental procedure, HDS diesel feedstock (I) (100 ml, 83.34 g) was added to the mixer settler and stirrer, hot fluid were started to keep the temperature of the reactant at 50° C. Desired amount of formic Acid (99-100%) was then added to the diesel followed by addition of fixed amount of 30% aqueous Hydrogen peroxide. The mixture was then stirred vigorously at 50° C. for a certain period and then taken out in the separating funnel through drain valves. The two layers namely hydrocarbon layer and formic acid layer were then separated. The diese...

example 2

[0082] After establishing the reaction parameters in mixer settler, experiments were carried out on oxidative desulphurization using HDS diesel feedstock (I) as feed as per the scheme shown in FIG. 1 in a blockout mode. The general discussion regarding FIG. 1 is given in Detailed description of the process. The oxidation of HDS diesel feedstock (I) was carried out in continuous counter current oxidation column B by using diesel as continuous phase at a flow rate 0.59 kg / hr and formic acid, 30% aqueous hydrogen peroxide mixture at a flow rate 0.29 kg / hr as disperse phase. The temperature of the continuous counter current oxidation column was maintained at 70° C. by passing hot water in the jacket of the column. The characteristics of the oxidized diesel obtained after acid neutralization column are given in Table 3. As seen from the Table 3 while there was no change in the cetane index of the HDS diesel after oxidation, the total sulphur present got reduced from 437 ppm to 365 ppm du...

example 3

[0087] Oxidative desulfurization of HDS diesel from another refinery (Feedstock II) was carried out in similar manner as described in Example 2 in a blockout mode. The oxidation of HDS diesel feedstock (II) was carried out in a continuous counter current oxidation column B by passing diesel as continuous phase at flow rate 0.59 kg / hr. and formic acid, 30% aqueous hydrogen peroxide mixture at a flow rate 0.29 kg / hr as discrete phase at 50° C. Characteristics of oxidised diesel obtained after and neutralization step is given in Table-5

TABLE 5CHARACTERISTICS OF OXIDIZED DIESEL FEEDSTOCK(II)Oxidized DieselCharacteristicsFeedstock (IT)R.I at 20° C.1.4678Density at 20° C., g / cc0.8446Aromatics wt % (ASTM 2549)26.2Total sulphur452 ppmCetane index53.7ASTM D 86IBP166 5% Recovered, ° C.211.810% Recovered, ° C.240.650% Recovered, ° C.293.990% Recovered, ° C.351.0FBP375.0Class type analysis wt %Total saturates72.6Mono AromaticsNDPoly AromaticsNDTotal Aromatics27.4

ND = not determined

[0088] Agai...

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Abstract

The present invention provides a process for oxidative desulphurization of liquid hydrocarbon fuels, such as diesel fuel, gasoline, jet fuel, fuel oils, coal liquids and similar petroleum products to ultra low sulphur hydrocarbon fuels with sulphur content less than 10 ppm. In this process, the sulfur compounds present in hydrocarbon fuel are first oxidised to more polar sulphones / sulphoxides and then removed by solvent extraction with NMP containing antisolvent followed by final polishing by passing through adsorption column.

Description

FIELD OF THE INVENTION [0001] The present invention relates to a process for the desulphurization of liquid hydrocarbon fuels. Particularly the invention relates to a process for oxidative desulphurization of liquid hydrocarbon fuels such as diesel fuel, gasoline, jet fuel, fuel oils, coal liquids and similar petroleum products to ultra low sulphur hydrocarbon fuels with sulfur content less than 10 ppm. More particularly, the present invention relates to oxidative desulphurization of liquid hydrocarbon fuels using carboxylic acid urea-H2O2 adduct, organosulphonic acid-H2O2 as oxidation system. BACKGROUND OF THE INVENTION [0002] Hydrocarbon fuels such as diesel fuel, gasoline, jet fuel, fuel oils and coal liquids are presently being consumed in vast quantities and their consumption continues to grow at alarming rates, due to their high energy densities and convenient physical form. This high consumption inevitably has a major impact on global environment. Most notably transport hydro...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C10G45/00C10G17/00
CPCC10G21/20C10G53/14C10G27/12C10G27/04
Inventor SAIN, BIRRAO, TUMULA VENKATESHWARNAUTIYAL, BHAGAT RAMNANOTI, SHRIKANT MADHUSUDANGARG, MADHUKAR ONKARNATHJAIN, LATA SUMANSHARMA, VISHAL BHARATDHARAM, PAULSHARMA, YOGENDRA KUMARGUPTA, ASHOK KUMAR
Owner COUNCIL OF SCI & IND RES
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