WO2004056449A2 - Process for removal of so2 from off-gases by reaction with h202 - Google Patents

Process for removal of so2 from off-gases by reaction with h202 Download PDF

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Publication number
WO2004056449A2
WO2004056449A2 PCT/EP2003/013699 EP0313699W WO2004056449A2 WO 2004056449 A2 WO2004056449 A2 WO 2004056449A2 EP 0313699 W EP0313699 W EP 0313699W WO 2004056449 A2 WO2004056449 A2 WO 2004056449A2
Authority
WO
WIPO (PCT)
Prior art keywords
gas
removal
gases
reaction
filter
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/EP2003/013699
Other languages
French (fr)
Other versions
WO2004056449A3 (en
Inventor
Peter Schoubye
Kurt Agerbaek Christensen
Morten Thellefsen Nielsen
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Topsoe AS
Original Assignee
Haldor Topsoe AS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
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First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=32668631&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=WO2004056449(A2) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Priority to US10/539,604 priority Critical patent/US7776299B2/en
Priority to CA2511311A priority patent/CA2511311C/en
Priority to AU2003288228A priority patent/AU2003288228B2/en
Priority to JP2004561212A priority patent/JP2006512190A/en
Priority to EP03780121A priority patent/EP1578517B1/en
Application filed by Haldor Topsoe AS filed Critical Haldor Topsoe AS
Priority to DE60319738T priority patent/DE60319738T2/en
Priority to BRPI0317462-0A priority patent/BR0317462B1/en
Publication of WO2004056449A2 publication Critical patent/WO2004056449A2/en
Publication of WO2004056449A3 publication Critical patent/WO2004056449A3/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/48—Sulfur compounds
    • B01D53/50—Sulfur oxides
    • B01D53/507—Sulfur oxides by treating the gases with other liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/48—Sulfur compounds
    • B01D53/50—Sulfur oxides
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES 
    • F23J2215/00—Preventing emissions
    • F23J2215/20—Sulfur; Compounds thereof
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES 
    • F23J2217/00—Intercepting solids
    • F23J2217/10—Intercepting solids by filters
    • F23J2217/102—Intercepting solids by filters electrostatic
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES 
    • F23J2219/00—Treatment devices
    • F23J2219/40—Sorption with wet devices, e.g. scrubbers

Definitions

  • the present invention relates to a process for removal of S0 2 from off-gases by reaction with H 2 0 2 .
  • H 2 0 2 0.1-0.5% H 2 0 2 .
  • the absorption is typically carried out at a temperature of 50-80°C of the circulating solution.
  • H 2 0 2 is added either as a concentrated aqueous solution of H 2 0 2 to the circulating acid, or it is produced by electrolysis of a side stream of the circulating acid. The produced acid is drawn off from the circulating acid.
  • the known process usually requires installation of a low velocity aerosol filter downstream of the absorption tower to remove sulphuric acid aerosol (acid mist) in order to meet acid mist emission regulations requiring less than about 5 mol ppm HS0 4 in the stack gas.
  • Fine acid mist (aerosol) that may be present in the off-gas is not removed efficiently in the absorption tower. Fine acid mist is also formed in the absorption tower itself by reaction between S0 and H 2 0 2 vaporised from the absorbing liquid.
  • FIG. 1 A preferred embodiment of the invention is shown in Fig. 1.
  • a solution of 0.1-30% H 2 0 2 in line 1 is sprayed by the spray nozzles 3 into a stream of off-gas in line 2 containing typically between 100-1000 ppm S0 2 and having a temperature typically in the range of 50-120°C.
  • the nozzles are placed in duct 4, so that the spray is evenly distributed in the gas stream upstream of the mist filter 5 in which the gas is passed in parallel through a number of low velocity filter candles 6.
  • Even distribution of the droplets in the gas is desirable for the process and the most even distribution of the droplets is achieved by using air- atomising nozzles producing very small droplets.
  • the H 2 S0 formed in the process accumulates in the filter elements or candles from which it is drained off through line 7. Most or all of the mass of the droplets evaporate before the gas enters the filter candles, whereby most of the H 2 0 evaporates and reacts in the gas phase under formation of sul- phuric acid aerosol. However, it is not necessary that the droplets are completely evaporated before the gas enters the filter elements. The reaction between S0 2 and H 2 0 will be completed and the thermal equilibrium will be established in the mist filter elements without decreasing the efficiency of the S0-removal. Thus, the injection of the aqueous solution H 2 0 2 serves two purposes :
  • the water comprised in the solution cools off the off-gas in line 2 by evaporation of the droplets, whereby the off-gas is cooled off to a desired temperature of the filter elements or candles typically to a temperature between 50°C and 70°C.
  • the concentration of H 2 S0 4 in the produced acid will be the equilibrium concentration of H 2 S0 4 at the actual temperature and H 2 0 partial pressure in the gas phase.
  • An off-gas stream of 1000 Nm 3 /h at 100°C contains 200 ppm S0 2 + 10% H 2 0 and has a temperature of 100°C. 96% S0 2 removal is desired.
  • the aerosol filter is designed for opera- tion at maximum 70°C. Operation at 67-70°C is chosen in order to achieve the highest possible acid strength and low content of remaining H 2 0 2 in the produced acid.
  • the process is conducted as follows : 15.7 kg/h water con- taining 2.0 wt% H 2 0 2 is injected into the off-gas, whereby the off-gas is cooled to 65-70°C in thermal equilibrium.
  • the mist filter is 75 mm thick and has a flow area of 2.5 m 2 .
  • the diameter of the fibres is about 8 ⁇ m.
  • Experiments carried out under these conditions show that about 96% of the S0 2 is removed under production of 1.7 kg/h 50% H 2 S0 4 with about 500 ppm H 2 0 2 .
  • the treated gas contains less than 2 ppm H 2 S0 4 and the content of H 2 0 2 is below the detection limit .

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treating Waste Gases (AREA)
  • Gas Separation By Absorption (AREA)
  • Electrostatic Separation (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

A process for removal of SO2 in off-gases having a temperature of 30-150°C and containing 0.001-1 vol% SO2 in which the SO2 is oxidised to H2 SO4 by spraying an aqueous solution of H2O2 into the off-gas upstream of an aerosol filter removing the produced sulphuric acid from the off-gas.

Description

Process for Removal of S02 from Off-Gases by Reaction with H202
1
The present invention relates to a process for removal of S02 from off-gases by reaction with H202.
It has been known for more than 30 years that S02, as de- scribed in the publication 2164e from Lurgi/Sϋdchemie AG, August 1989, can be removed from off-gases by contacting the off-gas in an absorption tower with circulating solution of dilute sulphuric acid containing H202, whereby S02 is dissolved and oxidised to H2S04 in the solution. The circulating solution typically contains 30-60% HS04 and
0.1-0.5% H202. The absorption is typically carried out at a temperature of 50-80°C of the circulating solution. H202 is added either as a concentrated aqueous solution of H202 to the circulating acid, or it is produced by electrolysis of a side stream of the circulating acid. The produced acid is drawn off from the circulating acid.
The known process usually requires installation of a low velocity aerosol filter downstream of the absorption tower to remove sulphuric acid aerosol (acid mist) in order to meet acid mist emission regulations requiring less than about 5 mol ppm HS04 in the stack gas. Fine acid mist (aerosol) that may be present in the off-gas is not removed efficiently in the absorption tower. Fine acid mist is also formed in the absorption tower itself by reaction between S0 and H202 vaporised from the absorbing liquid.
It is a disadvantage of the known process that it requires installation of both an absorption tower and a low velocity mist filter. In the process according to the present invention, S02 in off-gases is removed by reaction with H202 without the use of an absorption tower by spraying a solution of H202 in water or dilute sulphuric acid into the off-gas upstream of a low velocity aerosol filter or wet electrostatic precipi- tator (WESP) .
A preferred embodiment of the invention is shown in Fig. 1. A solution of 0.1-30% H202 in line 1 is sprayed by the spray nozzles 3 into a stream of off-gas in line 2 containing typically between 100-1000 ppm S02 and having a temperature typically in the range of 50-120°C. The nozzles are placed in duct 4, so that the spray is evenly distributed in the gas stream upstream of the mist filter 5 in which the gas is passed in parallel through a number of low velocity filter candles 6. Even distribution of the droplets in the gas is desirable for the process and the most even distribution of the droplets is achieved by using air- atomising nozzles producing very small droplets. The H2S0 formed in the process accumulates in the filter elements or candles from which it is drained off through line 7. Most or all of the mass of the droplets evaporate before the gas enters the filter candles, whereby most of the H20 evaporates and reacts in the gas phase under formation of sul- phuric acid aerosol. However, it is not necessary that the droplets are completely evaporated before the gas enters the filter elements. The reaction between S02 and H20 will be completed and the thermal equilibrium will be established in the mist filter elements without decreasing the efficiency of the S0-removal. Thus, the injection of the aqueous solution H202 serves two purposes :
Firstly, it adds to the off-gas the amount of H202, which is required for achieving the desired conversion of S02 into H2S0 by the reaction
H202 + S02 = H2S04
Most of the conversion takes place by reaction in the gas phase between S02 and vaporised H202 under formation of acid mist or between S02 and H202 dissolved in the droplets. The reaction is completed in the aerosol filter in which remaining S02 is absorbed and reacts with remaining H202 con- tained in the dilute sulphuric acid wetting the fibre material .
Secondly, the water comprised in the solution cools off the off-gas in line 2 by evaporation of the droplets, whereby the off-gas is cooled off to a desired temperature of the filter elements or candles typically to a temperature between 50°C and 70°C. The concentration of H2S04 in the produced acid will be the equilibrium concentration of H2S04 at the actual temperature and H20 partial pressure in the gas phase.
Up to 98% S02-removal can be achieved at, typically, about 95% utilisation of the H202. EXAMPLE
An off-gas stream of 1000 Nm3/h at 100°C contains 200 ppm S02 + 10% H20 and has a temperature of 100°C. 96% S02 removal is desired. The aerosol filter is designed for opera- tion at maximum 70°C. Operation at 67-70°C is chosen in order to achieve the highest possible acid strength and low content of remaining H202 in the produced acid.
The process is conducted as follows : 15.7 kg/h water con- taining 2.0 wt% H202 is injected into the off-gas, whereby the off-gas is cooled to 65-70°C in thermal equilibrium. The mist filter is 75 mm thick and has a flow area of 2.5 m2. The diameter of the fibres is about 8 μm. Experiments carried out under these conditions show that about 96% of the S02 is removed under production of 1.7 kg/h 50% H2S04 with about 500 ppm H202. The treated gas contains less than 2 ppm H2S04 and the content of H202 is below the detection limit .

Claims

1. A process for removal of S02 in off-gases having a temperature of 30-150°C and containing 0.001-1 vol% S02 in which the SO2 is oxidised to H2S04 by spraying an aqueous solution of H202 into the off-gas upstream of an aerosol filter removing the produced sulphuric acid from the off- gas.
2. A process as in claim 1, in which the off-gas is cooled by evaporation of the water comprised in the solution being sprayed into the off-gas upstream of the filter,
3. A process as in claim 1, in which a wet electro- static separator us used in place of an aerosol filter.
PCT/EP2003/013699 2002-12-21 2003-12-04 Process for removal of so2 from off-gases by reaction with h202 Ceased WO2004056449A2 (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
BRPI0317462-0A BR0317462B1 (en) 2002-12-21 2003-12-04 process for the removal of so2 in outlet gases by reaction with h2o2.
CA2511311A CA2511311C (en) 2002-12-21 2003-12-04 Process for removal of so2 from off-gases by reaction with h2o2
AU2003288228A AU2003288228B2 (en) 2002-12-21 2003-12-04 Process for removal of SO2 from off-gases by reaction with H202
JP2004561212A JP2006512190A (en) 2002-12-21 2003-12-04 Method for removing SO2 from off-gases by reaction with H2O2
EP03780121A EP1578517B1 (en) 2002-12-21 2003-12-04 Process for removal of so2 from off-gases by reaction with h202
US10/539,604 US7776299B2 (en) 2002-12-21 2003-12-04 Process for removal of SO2 from off-gases by reaction with H2O2
DE60319738T DE60319738T2 (en) 2002-12-21 2003-12-04 PROCESS FOR REMOVING SO2 FROM EXHAUST GASES BY MITH2O2 REACTION

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DKPA200201992 2002-12-21
DKPA200201992 2002-12-21

Publications (2)

Publication Number Publication Date
WO2004056449A2 true WO2004056449A2 (en) 2004-07-08
WO2004056449A3 WO2004056449A3 (en) 2004-09-30

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ID=32668631

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Application Number Title Priority Date Filing Date
PCT/EP2003/013699 Ceased WO2004056449A2 (en) 2002-12-21 2003-12-04 Process for removal of so2 from off-gases by reaction with h202

Country Status (13)

Country Link
US (1) US7776299B2 (en)
EP (1) EP1578517B1 (en)
JP (1) JP2006512190A (en)
KR (1) KR20050084454A (en)
CN (1) CN100354028C (en)
AT (1) ATE388751T1 (en)
AU (1) AU2003288228B2 (en)
BR (1) BR0317462B1 (en)
CA (1) CA2511311C (en)
DE (1) DE60319738T2 (en)
ES (1) ES2300632T3 (en)
RU (1) RU2346731C2 (en)
WO (1) WO2004056449A2 (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007025948A1 (en) * 2005-09-02 2007-03-08 Basf Se Method and device for removing sulphur dioxide from a dry gas stream
CN107970911A (en) * 2017-12-01 2018-05-01 南京云高新型材料有限公司 A kind of environmental protection and energy saving high conversion rare earth catalyst and preparation method thereof
US10675585B2 (en) 2016-05-24 2020-06-09 Haldor Topsoe A/S Method for the removal of oxygen from an industrial gas
US10933372B2 (en) 2017-02-16 2021-03-02 Haldor Topsoe A/S Method for the removal of oxygen from an industrial gas feed

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CN100393393C (en) * 2006-03-30 2008-06-11 国电科技环保集团有限公司 Flue gas spray pre-washing device at the entrance of flue gas desulfurization absorption tower
CN100463847C (en) * 2006-06-23 2009-02-25 李开春 Method for preparing vitriol from flue gas
DE102007020141A1 (en) * 2007-04-26 2008-10-30 Bayer Materialscience Ag Recycle gas scrubber for the removal of SOx and sulfuric acid aerosols from chlorine-containing process gases
DE102007039926B4 (en) * 2007-08-23 2012-03-22 Götaverken Miljö AB Method and device for exhaust gas purification
KR101039715B1 (en) * 2009-01-23 2011-06-13 엘에스니꼬동제련 주식회사 Treatment method of copper smelting by-product gas
KR101341967B1 (en) * 2012-06-22 2013-12-16 한국에너지기술연구원 Method for producing hydrogen and sulfuric acid from sulfur dioxide using electrochemical process
US8877152B2 (en) * 2013-02-27 2014-11-04 Alstom Technology Ltd Oxidation system and method for cleaning waste combustion flue gas
CN103657375B (en) * 2014-01-07 2015-07-08 上海科洋科技股份有限公司 Method and system for removing trace SO2 in tail gas by gas phase oxidation
WO2018162471A1 (en) * 2017-03-08 2018-09-13 Shell Internationale Research Maatschappij B.V. Process for removing so2 from gas with so2 content that is temporarily very high
CN110407181B (en) * 2019-08-19 2024-12-17 广东新生环保科技股份有限公司 Tail gas sulfur dioxide acid making recovery system
US10940471B1 (en) 2019-10-30 2021-03-09 W. L. Gore & Associates, Inc. Catalytic efficiency of flue gas filtration
US11071947B2 (en) 2019-10-30 2021-07-27 W. L. Gore & Associates, Inc. Catalytic efficiency of flue gas filtration

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WO2007025948A1 (en) * 2005-09-02 2007-03-08 Basf Se Method and device for removing sulphur dioxide from a dry gas stream
US10675585B2 (en) 2016-05-24 2020-06-09 Haldor Topsoe A/S Method for the removal of oxygen from an industrial gas
US10933372B2 (en) 2017-02-16 2021-03-02 Haldor Topsoe A/S Method for the removal of oxygen from an industrial gas feed
CN107970911A (en) * 2017-12-01 2018-05-01 南京云高新型材料有限公司 A kind of environmental protection and energy saving high conversion rare earth catalyst and preparation method thereof
CN107970911B (en) * 2017-12-01 2020-10-13 南京云高新型材料有限公司 Environment-friendly energy-saving high-conversion-rate rare earth catalyst and preparation method thereof

Also Published As

Publication number Publication date
AU2003288228A1 (en) 2004-07-14
CA2511311C (en) 2011-09-20
BR0317462A (en) 2005-11-16
EP1578517A2 (en) 2005-09-28
US7776299B2 (en) 2010-08-17
WO2004056449A3 (en) 2004-09-30
JP2006512190A (en) 2006-04-13
CN1729039A (en) 2006-02-01
AU2003288228B2 (en) 2009-08-06
DE60319738D1 (en) 2008-04-24
BR0317462B1 (en) 2013-02-05
RU2005123041A (en) 2006-01-27
EP1578517B1 (en) 2008-03-12
CN100354028C (en) 2007-12-12
RU2346731C2 (en) 2009-02-20
CA2511311A1 (en) 2004-07-08
US20060057047A1 (en) 2006-03-16
ATE388751T1 (en) 2008-03-15
KR20050084454A (en) 2005-08-26
ES2300632T3 (en) 2008-06-16
DE60319738T2 (en) 2009-04-02

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