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Sulfur Recovery

Chapter 16
Based on presentation by Prof. Art Kidnay

Plant Block Schematic

Adapted from Figure 7.1,

Fundamentals of Natural Gas Processing, 2nd ed.

Kidnay, Parrish, & McCartney

Updated: January 4, 2019 Copyright © 2019 John Jechura ([email protected])
2

Topics

Introduction Properties of sulfur Sulfur recovery processes

▪ Claus Process ▪ Claus Tail Gas Cleanup

Sulfur storage Safety and environmental considerations

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3

Introduction &

Properties of Sulfur

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Sulfur Crystals

http://www.irocks.com/minerals/specimen/34046 http://www.mccullagh.org/image/10d-5/sulfur.html

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5

Molten Sulfur

http://www.kamgroupltd.com/En/Post/7/Basic-info-on-elemental-Sulfur(HSE)

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6

World Consumption of Sulfur

Primary usage of sulfur to make sulfuric acid

(90 – 95%)

▪ Other major uses are rubber processing, cosmetics, & pharmaceutical

applications

China primary market

Ref: https://ihsmarkit.com/products/sulfur-chemical-economics-handbook.html

Report published December 2017

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7

Sulfur Usage & Prices

Natural gas & petroleum

production accounts for the

majority of sulfur production Primary consumption is agriculture & industry

▪ 65% for farm fertilizer: sulfur → sulfuric acid → phosphoric acid → fertilizer

$50 per ton essentially disposal cost

▪ Chinese demand caused runup in 2007-2008

Ref: http://ictulsa.com/energy/

Updated December 24, 2018

“Cleaning up their act”, Gordon Cope,

Hydrocarbon Engineering, pp 24-27, March 2011

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U.S. sulfur production

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Sulfur Chemical Structure

Pure sulfur exists as SX where X = 1 to 8

▪ The dominant species are S2, S6, &

S8

May be in ring structure or open chain

Species determined by temperature

This composition greatly affects its properties!

Octasulfur, S8

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Sulfur Vapor Species

1.0

S8

0.8

S2

0.6 0.4

S6

0.2 0.0

  • 200
  • 400
  • 600
  • 800
  • 1000
  • 1200
  • 1400

Temperature, °F

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Viscosity of Molten Sulfur

105

Pure Sulfur

104 103 102 101 100

  • 400
  • 600

Temperature, °C
300

  • 500
  • 700
  • 800

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Viscosity of Molten Sulfur

105

Pure Sulfur

H2S Partial Pressure,

104

psia
0.0015

0.015

103

0.15 1.5

102

14.7

101 100

  • 400
  • 600

Temperature, °C

  • 300
  • 500
  • 700
  • 800

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Viscosity of liquid sulfur

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14

Sulfur recovery processes

Updated: January 4, 2019 Copyright © 2017 John Jechura ([email protected])

Sulfur Recovery

Typically a modified Claus process

▪ H2S rich stream burned with 1/3 stoichiometric air. Hot gases are then

passed over alumina catalyst to produce free sulfur

  • Combustion:
  • H2S + 1.5·O2 H2O + SO2

Claus Reaction: 2·H2S + SO2 D 2·H2O + 3·S

▪ Sulfur formation reaction mildly exothermic

▪ Sulfur conversion reactors kept above 400oF (sulfur dew point)

The Claus reaction is reversible – therefore, 100% conversion can

never be achieved

▪ Practically, Claus units are limited to about 96% recovery ▪ Tail gas units are used to provide improved conversion

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16

Modified Claus Process

Petroleum Refining Technology & Economics – 5th Ed.

by James Gary, Glenn Handwerk, & Mark Kaiser, CRC Press, 2007

Converters 400 – 700oF
Burner & Reactor above 1800oF

2300-2700oF for NH3 destruction

GPSA Engineering Data Book, 13th ed.,

Fig. 22-2, 2012

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Temperature Regimes for the Claus Process

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Straight-through Claus Process

gas reheat gas reheat

450°F

gas reheat waste heat

boiler

  • 420°F
  • 400°F

Claus #3
HP steam
Claus #1

590°F

Claus #2 acid

gas
LP

  • 453°F
  • 300°F 407°F

LP steam
LP

600°F
270°F

steam

375°F

steam 350°F

110°F 8 psig

condens condenser er

  • condenser
  • condenser

condenser

boiler feed air

water (BFW)
BFW
BFW

sulfur
BFW reaction

furnace

  • sulfur
  • sulfur
  • sulfur

1700 - 2400°F

tail gas

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Equilibrium Conversion of H2S to S

Temperature, o C

  • 204
  • 427
  • 871
  • 1316
  • 1538

  • 649
  • 1093

100
80 60 40

melting point boiling point

  • 0
  • 400
  • 800
  • 1200
  • 1600
  • 2000
  • 2400
  • 2800

Temperature, °F

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Equilibrium Conversion of H2S to S

100

Claus #3
Furnace & waste heat boiler
Claus #2

  • 1700 - 2400F
  • Claus #1

80 60 40

melting point boiling point

  • 0
  • 400
  • 800
  • 1200
  • 1600
  • 2000
  • 2400
  • 2800

Temperature, °F

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21

Hydrocarbons in the Claus Process

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Claus Process

Use multiple stages to obtain highest conversion

▪ Typically three

Various flow patterns

▪ Straight-through – best, used whenever possible

▪ Split flow – best at low H2S feed concentrations (5 to 30 mol% H2S)

▪ Sulfur recycle < 5% H2S ▪ Direct oxidation < 5% H2S

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23

Claus Process

Claus unit feed usually contains H2S and CO2 High concentrations of noncombustible components (CO2, N2)

▪ Lower flame temperature ▪ Difficult to maintain stable combustion furnace flame temperatures below
1700oF

Solutions include

▪ Preheating air ▪ Preheating acid gas feed ▪ Enriching oxygen in air ▪ Using split-flow process

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24

Split-flow Claus Process

gas reheat gas reheat gas reheat

HP steam

  • Claus #3
  • Claus #2

  • Claus #2
  • Claus #1
  • 2/3 flow

1/3 flow

  • LP
  • LP

steam
LP steam steam acid gas

condenser

BFW ccoonnddeennsseerr

  • condenser
  • condenser
  • condenser
  • condenser

air

boiler feed water (BFW)

BFW

  • sulfur
  • sulfur
  • sulfur

reaction

furnace sulfur tail gas

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25

Typical Claus Configurations

Approximate

concentration of
Process variation

H2S in feed
(mol%)

55 - 100
30 - 55

15 - 30

10 - 15
5 - 10
Straight-through Straight-through + acid gas and/or air preheat

Split-flow or acid gas and/or air preheat

Split-flow with acid gas and/or air preheat Split-flow with fuel added, O2 enrichment, or with acid gas and air preheat

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Tail Gas Clean Up

Three process categories: Direct oxidation of H2S to sulfur (Superclaus)

2 H2S + O2 → 2 S + 2 H2O

Sub-dew point Claus processes (Cold Bed Adsorption) SO2 reduction and recovery of H2S (SCOT)

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27

Claus Tail Gas Cleanup

Conventional 3-stage Claus units recover 96 to 97.5% of sulfur

▪ Remainder was burned to SO2 and vented

▪ Adding fourth stage results in 97 to 98.5% recovery

Regulations now require 99.8 to 99.9% recovery

Meeting regulations requires modified technology

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Shell Claus Offgas Treating (SCOT)

Four step process:

▪ Mix feed with reducing gas (H2 and CO)

▪ Convert all sulfur compounds to H2S ▪ Cool the reactor gas ▪ Strip H2S using amine

To Stack
Claus Tail Gas
H2S Recycle

Reducing Gas
Catalytic Reactor
Air

Furnace
Fuel

  • Low Pressure
  • Low Pressure

Steam
H2O
Steam Reboiler

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SCOT Process

To Stack
Claus Tail Gas

Reducing Gas
H2S Recycle
Catalytic Reactor
Air

Furnace
Fuel

Low Pressure
Steam
Low Pressure Steam Reboiler
H2O

Mix Claus tail

gas with H2 and sulfur compounds to H2S

CO and heat in Reactions:

Catalytically convert all

Cool reactor gas

Strip H2S from gas & recycle to

(exiting at ~570oF Claus in waste heat

Typically use MDEA – can get to

SO2 + 3H2 → H2S + 2H2O

S2 + 2H2 → 2H2S COS + H2O → CO2+ H2S CS2 + 2H2O → CO2 + H2S

inline burner

exchanger and

water wash to complete cooling.

low H2S levels in Stack Gas &

slip CO2 so it doesn’t build up in

the recycle gas

Updated: January 4, 2019 Copyright © 2019 John Jechura ([email protected])
30

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  • Economical Sulfur Removal for Fuel Processing Plants Challenge Sulfur Is Naturally Present As an Impurity in Fossil Fuels

    Economical Sulfur Removal for Fuel Processing Plants Challenge Sulfur Is Naturally Present As an Impurity in Fossil Fuels

    SBIR Advances More Economical Sulfur Removal for Fuel Processing Plants Challenge Sulfur is naturally present as an impurity in fossil fuels. When the fuels are burned, the sulfur is released as sulfur dioxide—an air pollutant responsible for respiratory problems and acid rain. Environmental regulations have increasingly restricted sulfur dioxide emissions, forcing fuel processors to remove the sulfur from both fuels and exhaust gases. The cost of removing sulfur from natural gas and petroleum in the United States was about DOE Small Business Innovation $1.25 billion in 2008*. In natural gas, sulfur is present mainly as hydrogen sulfide gas (H2S), Research (SBIR) support while in crude oil it is present in sulfur-containing organic compounds which are converted enabled TDA to develop and into hydrocarbons and H2S during the removal process (hydrodesulfurization). In both cases, commercialize its direct oxidation corrosive, highly-toxic H2S gas must be converted into elemental sulfur and removed for sale or process—a simple, catalyst-based safe disposal. system for removing sulfur from At large scales, the most economical technology for converting hydrogen sulfide into sulfur is natural gas and petroleum—that the Claus process. This well-established process uses partial combustion and catalytic oxidation was convenient and economical enough for smaller fuel processing to convert about 97% of the H2S to elemental sulfur. In a typical application, an amine treatment plants to use. unit concentrates the H2S before it enters the Claus unit, and a tail gas treatment unit removes the remaining 3% of the H2S after it exits the Claus unit. This multi-step process has low operating costs but high capital costs—too expensive for TDA Research, Inc.