EP0532491A1 - Traitement de gaz contenant des composés organiques sulfurés spécialement dans des systèmes et procédés de lessivage kraft - Google Patents

Traitement de gaz contenant des composés organiques sulfurés spécialement dans des systèmes et procédés de lessivage kraft Download PDF

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Publication number
EP0532491A1
EP0532491A1 EP19920890034 EP92890034A EP0532491A1 EP 0532491 A1 EP0532491 A1 EP 0532491A1 EP 19920890034 EP19920890034 EP 19920890034 EP 92890034 A EP92890034 A EP 92890034A EP 0532491 A1 EP0532491 A1 EP 0532491A1
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European Patent Office
Prior art keywords
gas
gas stream
hydrogen
methane
catalyst
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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.)
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EP19920890034
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German (de)
English (en)
Inventor
Wayne J. Chamblee
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Kamyr Inc
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Kamyr Inc
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Publication of EP0532491A1 publication Critical patent/EP0532491A1/fr
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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/22—Other features of pulping processes
    • D21C3/26—Multistage processes
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C11/00—Regeneration of pulp liquors or effluent waste waters
    • D21C11/0064—Aspects concerning the production and the treatment of green and white liquors, e.g. causticizing green liquor
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C3/00—Pulping cellulose-containing materials
    • D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
    • D21C3/022—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes in presence of S-containing compounds

Definitions

  • a method for treatment of the off gases associated with kraft or sulfite pulping so as to change them from a source of pollution to a source of useful chemicals.
  • a method of acting on a first gas stream consisting essentially of off gases from a kraft or sulfite digester, off gases from a black liquor evaporator, and mixtures thereof, which comprises the steps of (a) treating the gases in the first gas stream to produce a second gas stream containing primarily hydrogen sulfide and methane, and then (b) separating the hydrogen sulfide from the methane.
  • Step (a) may be practiced by adding hydrogen to the gas in the first gas stream, and passing the first gas stream -- in the presence of the added hydrogen -- past a hydrogen desulfurization catalyst (e.g.
  • step (a) may be practiced by effecting substochiometric combustion of at least some of the gas in the first gas stream to produce a third gas stream, removing particulates from the gas in the third gas stream, and passing the gas in the third gas stream into contact with a dirty shift catalyst (e.g. one containing oxides of cobalt and molybdenum, or iron and chromium) to subject it to the water gas shift reaction namely: H2O + CO ⁇ H2 + CO2 to thereby produce the second gas stream.
  • Step (b) may be practiced by passing the gas in the second gas stream into contact with white liquor from kraft paper pulp being processed to remove the hydrogen sulfide therefrom, and increase the sulfidity of the white liquor.
  • a method of converting a first gas stream including water vapor and over 10% (e.g. about 15-80%) by weight organic sulfur compounds, into a second gas stream comprising primarily H2S and methane is provided.
  • the first gas stream is preferably composed of off gases from kraft or sulfite pulping processes containing methyl mercaptan, DMS, and hydrogen sulfide, but other sources may also be treated according to the invention.
  • the method comprises the steps of: (a) Adding hydrogen to the gas in the first gas stream. And, (b) passing the first gas stream, in the presence of the added hydrogen, past a hydrogen desulfurization catalyst to produce the second gas stream.
  • Step (a) may be practiced by: (a1) Removing hydrogen sulfide from the gas in the second gas stream to produce a third gas stream containing primarily methane and hydrogen. (a2) Reacting the gas in the third gas stream with steam, and then subjecting it to the water gas shift reaction in the presence of a catalyst to produce a fourth gas stream containing primarily hydrogen, methane, and carbon dioxide.
  • step (a3) separating the hydrogen from the fourth gas stream, to be added to the gas in the first gas stream, while producing a fifth gas stream containing primarily methane and carbon dioxide.
  • step (a3) separating the hydrogen from the fourth gas stream, to be added to the gas in the first gas stream, while producing a fifth gas stream containing primarily methane and carbon dioxide.
  • step (a2) separating the hydrogen from the fourth gas stream, to be added to the gas in the first gas stream, while producing a fifth gas stream containing primarily methane and carbon dioxide.
  • a method of converting a first gas stream including water vapor, and over 10% (e.g. about 15-80%) by weight organic sulfur compounds, into a third gas stream comprising primarily H2S and methane comprises the steps of: (a) Effecting substochiometric combustion of at least some the gas in the first gas stream to produce a second gas stream. (b) Removing particulates from the gas in the second gas stream. And, (c) passing the gas in the second gas stream into contact with a dirty shift catalyst to subject it to the water gas shift reaction and thereby produce a third gas stream comprising primarily hydrogen sulfide and methane, with some carbon dioxide.
  • Step (a) may be practiced to effect substochiometric combustion of only a first part of the gas in the first gas stream, and then there is a further step (d) of passing a second part of the gas in the first gas stream into the second gas stream before the practice of step (c).
  • step (a) may be practiced to effect substochiometric combustion of essentially all of the gas in the first gas stream.
  • FIGURES 1A and 1B schematically illustrate at 10 apparatus for practicing a method of converting a gas stream having a large amount of organic sulfur compounds therein into a second gas stream comprising primarily H2S and methane.
  • the off gas streams treated according to the invention include water vapor and over 10% (e.g. about 15-80%) by weight organic sulfur compounds.
  • the organic sulfur compounds typically present are methyl mercaptan, dimethyl sulfide (DMS), and hydrogen sulfide, the water vapor is in the form of steam, and additional organic and inorganic compounds are also present.
  • apparatus 10 is useful for the treatment of any gas stream having a high level of organic sulfur compounds, it is preferably utilized with -- and will be described with respect to herein -- the treatment of off gases from kraft (or sulfite) pulping processes in the production of paper pulp.
  • a digester 12 (FIGURE 1B) -- which may be a continuous digester such as that sold by Kamyr, Inc. of Glens Falls, New York, or a batch digester -- has a stream of off gases 13, and black liquor is withdrawn at an intermediate position as indicated at 14 in FIGURE 1B, while the kraft pulp produced is discharged at 15.
  • the black liquor in line 14 may be passed directly to black liquor evaporators, but preferably it is first subjected to a heat treatment process at step 17 to produce off gases in line 18.
  • the heat treatment of block 17 in FIGURE 1A is preferably that described in U.S. patent 4,929,307.
  • the black liquor passes to evaporators 19 which also produce off gases in line 20, then to a conventional recovery boiler 22, with conventional white liquor manufacture at block 23, to produce white liquor in line 24 having conventional sulfidity.
  • the off gases in line 18 which may include only those from the heat treatment 17, only those from the digester line 13, only those from the black liquor evaporators in line 20, or a combination of two or all of them -- are preferably first subjected to a drying or absorption stage (as indicated schematically at 27 in FIGURE 1) in order to remove a majority of the water vapor.
  • the removal of the water vapor increases the concentration of organic sulfur gases.
  • Step 27 is accomplished by drying the gas stream by any conventional means and/or by absorbing or adsorbing the organic portion of the gas onto a solid, or additionally by absorbing the off gas into one of any non-polar liquids (e.g. kerosene or mineral oil).
  • Treatment may be provided of a liquid mixture, but preferably according to the invention further treatment is of the concentrated gas.
  • the next steps in the practice of the invention as illustrated in FIGURE 1 are to add hydrogen, and then pass the gas in the presence of the added hydrogen past a hydrogen desulfurization catalyst.
  • This is accomplished in the hydrogen desulfurization (HDS) unit 28, with the hydrogen gas from line 29 added to the unit 28 along with the gas in line 18.
  • the hydrogen gas in line 29 can come from any source (e.g. be purchased , from water electroylsis, etc.).
  • the hydrogen desulfurization catalyst consist essentially of a transition metal-molybdenum alloy, particularly a nickel molybdenum or cobalt molybdenum alloy.
  • An example of the decomposition reaction that takes place in unit 28 is as follows: CH3SCH3 + 2 H2 ⁇ CH4 + H2S
  • the temperature conditions in the unit 28 must be at least 50°F over the dew point of the gas, and are typically 390-750°F, preferably about 410-700°F, and the pressure conditions are typically 150-300 psig, but can run from atmospheric pressure to 1,000 psig.
  • the hydrogen sulfide, methane, and other sulfur free gases may be stripped from the liquid phase.
  • the product gas stream in line 30 is further acted upon.
  • the gas stream in line 30 contains primarily methane, and hydrogen sulfide, with hydrogen also present.
  • the hydrogen sulfide is then separated out from the gas in stream 30. While the hydrogen sulfide may be separated as a gas and then used in its gaseous form in conventional pulping techniques, preferably it is fed to a scrubber 32 in which it is brought into contact with a caustic solution.
  • white liquor (although green liquor may also be advantageously utilized) from line 24 is passed into inlet 33 of scrubber 32, the hydrogen sulfide being absorbed in the white liquor and thereby significantly enhancing its sulfidity.
  • the significantly enhanced sulfidity white liquor then passes through the outlet 34 of the scrubber into line 35, to be used in the pulping process.
  • the gas stream that remains, in line 38, contains primarily methane, but also some hydrogen.
  • a feed water line 45 is provided through heat exchanger 46 in the hot gas exhaust conduit 47 of reformer 42.
  • the feed water is turned into steam in 46, which passes in line 48 to mix with the reformer feed gas in line 39, in the line 49.
  • the reformer 42 the following reaction occurs: C n H m + n H2O ⁇ n CO + (n + m/2) H2
  • the gas in line 50 thus is primarily hydrogen and carbon monoxide. From line 50 it passes to a shift converter 52.
  • the gas is reacted over an appropriate mixture of the oxides of iron and chromium which act as catalysts to promote the water gas shift reaction H2O + CO ⁇ H2 + CO2
  • the temperature conditions in the unit 52 are at least 50°F above the dew point of the gas, and are typically 450-950°F, and the pressure conditions are typically 150-300 psig, but can run from atmospheric to 1,000 psig.
  • the product gas mixture from the water gas shift reaction in line 54 contains primarily hydrogen and carbon dioxide, and this is added with the methane from line 40 to the PSA unit 43.
  • conventional adsorption or absorption methods are practiced to yield the pure hydrogen stream 29, and a second stream 56 which contains primarily methane and carbon dioxide.
  • the methane and carbon dioxide in line 56 may be split into a line 57 which is used as the fuel gas for the combustion chamber 58 of the methane/steam reformer 42 -- and thus providing the energy source for the reformer 42. If there is any excess fuel gas, it may be passed into storage at 60, or used as the combustion source for the lime kiln typically associated with a kraft pulping plant.
  • the white liquor in line 35 may be very advantageously used in pulp processing.
  • the liquor in line 35 has enhanced sulfidity compared to the conventional white liquor in line 24, and may be used in apparatus 62 (FIGURE 1B) which comprises a conventional chip feed system, and/or a conventional impregnation vessel.
  • the pulp slurry, with the increased sulfidity white liquor, in line 64 passes to the top of the digester 12 (typically a continuous digester), while white liquor of conventional sulfidity passes in line 66 to be added to a circulation loop in the digester 12.
  • the conventional sulfidity white liquor in line 66 can be used in the MCCTM process of Kamyr, Inc. of Glens Falls, New York.
  • the initial processing conditions selected were: 6.0 LHSV, 150 psig and 2500 SCFB reactor gas rate (based on total feed, not just DMS). These conditions were sufficient to convert the great majority of the DMS when the temperature was raised to an average of 640°F. Reducing the throughput to 3.0 LHSV resulted in a slight apparent increase in conversion. Reducing the reactor gas rate to 1600 SCFB did not slow the conversation of DMS (in fact it may have increased it), but reducing it to about 1000 SCFB did.
  • a reactor in a bench scale isothermal hydrotreating pilot plant was loaded with 87 ccs. of Criterion C324 nickel molybdenum hydrotreating catalyst.
  • the run feed was a 25/75 volume percent blend of DMS and kerosene. Assuming complete conversion of the DMS with no reaction of the kerosene, then the expected yield of H2S would be 14.2 wt% of the total feed and the yield of C1 would be 13.3 wt%. If there is some reaction of the kerosene it should not contribute more than 0.01 to 0.02 wt% to the H2S yield. The contribution of the kerosene to the methane yield is expected to be small.
  • the unit was lined out at the initial run conditions of 500°F, 6.0 LHSV, 150 psig and 2500 SCFB reactor gas rate (based on the total feed). The conversion of DMS was very low at these conditions, so the temperature was raised. Between 500°F and 520°F, the DMS began to convert in large quantities, which generated a large exotherm. Once the reactor temperatures were brought under control, the reactor inlet temperature was increased as much as possible (to about 560°F) so that the average reactor temperature was maximized at about 660°F while the hottest points were held to 734°F. Exceeding approximately 750°F was avoided so as to avoid extensive thermal cracking of the kerosene, which could possibly cause a much greater exotherm. At these conditions, the weight percent yields of hydrogen sulfide and methane were approximately 13.3 and 12.5, respectively.
  • the reactor gas rate was reduced to 1575 SCFB, which did not reduce conversion at all. H2S and C1 yields were 14.1 and 12.6, which indicate conversation is no lower and possibly even higher (perhaps due to increased residence time in the reactor). The reactor gas was then reduced to 1040 SCFB which did cause the H2S yield to drop to 13.4 although the C1 yield increased to about 13.5.
  • the temperature at which the reaction begins to proceed very quickly is between 510°F and 520°F (at the catalyst inlet).
  • a minimum gas rate of 1600 SCFB (based on total feed, the teat feed being at 75/25 volume percent blend of kerosene and DMS) is desirable to keep the reaction from being limited by hydrogen availability, but additional hydrogen may be necessary for long catalyst life.
  • FIGURE 2 Another embodiment according to the invention is schematically illustrated in FIGURE 2.
  • the off gases in line 18 are split into two streams, 71 and 72, with the stream 71 led to the partial oxidation block 73 in FIGURE 2. That is the gas in line 71 is reacted with a substochiometric amount of oxygen or air from line 74 (with or without steam) to produce a gas in line 75 rich in hydrogen and carbon monoxide, and also containing carbon dioxide, hydrogen sulfide, carbonyl sulfide, methane, sulfur dioxide, and other compounds including particulates (soot). Nitrogen will also be present if the gas from source 74 is air instead of essentially pure oxygen.
  • the gas in line 75 is preferably cleaned of soot by conventional techniques as indicated at 76, and feed gas in line 72 is recombined with the gas in line 75, either before or after the soot removal block 76. Then the gas in line 75 is passed over a special shift catalyst which can tolerate sulfur compounds, as indicated at 77 in FIGURE 2.
  • the dirty shift catalyst in 77 which preferably comprises an alumina catalyst containing oxides of an cobalt and molybdenum (commercially available from BASF under the trade name K8-11) -- promotes the water gas shift reaction H2O + CO ⁇ H2 + CO2 even in the presence of sulfur.
  • the temperature and pressure conditions in 77 are about 450-950°F, and about 150-300 psig.
  • a normal catalyst for the water gas shift reaction such as oxides of iron and chromium as described with respect to FIGURE 1A, is poisoned by sulfur compounds, but catalysts containing oxides of cobalt and molybdenum can effectively treat such gases.
  • This catalyst also promotes the hydrolysis of carbonyl sulfide into hydrogen sulfide as follows: COS + H2 ⁇ H2S + CO2
  • the primarily hydrogen and carbon dioxide gas stream 79 produced can then be used to treat the remaining sulfur containing off gases which are added in line 72.
  • the gases in line 72 may be added either as illustrated in FIGURE 2, or directly to the line 79.
  • the gases in line 79 may also be added to an HDS unit 28 to effect organic sulfur decomposition, as indicated at box 80 in FIGURE 2.
  • the latter reaction may also be accomplished by passing the hydrogen, carbon monoxide, and sulfur containing off gas mixtures through several sulfur tolerant carbon monoxide shift reactors in aeries.
  • the sulfur tolerant catalyst in the shift reactor can also promote the organic sulfur decomposition reaction as follows: CH3SCH3 + 2 H2 ⁇ 2 CH4 + H2S.
  • the gas mixture is then again separated into a stream containing hydrogen sulfide and a stream containing clean fuel gas. If this processing scheme is employed, the final gas mixture before separation will contain carbon dioxide, methane, hydrogen, and hydrogen sulfide.
  • the gas stream will also contain nitrogen if air was used as the oxygen source for the partial oxidation reaction.
  • the reaction then proceeds to the H2S recovery stage 81.
  • a simple acid gas scrubbing system may be used to separate the carbon dioxide and hydrogen sulfide from the gas mixture.
  • selective removal of the hydrogen sulfide by adsorption, absorption, or membrane may be employed. Scrubbing with a selective solvent such as methyldiethanolamine can remove essentially all of the hydrogen sulfide from the gas stream while removing only a small fraction of the carbon dioxide.
  • the hydrogen sulfide in line 82 may be used directly in pulping, or absorbed into white or green liquor as described with respect to FIGURE 1.
  • the gas in line 83 is primarily fuel gas, but it may contain nitrogen if air was used as the gas in line 74.
  • the nitrogen may optionally be removed -- as indicated by line box 84 -- by adsorption, membrane separation, or other viable techniques so as to increase the heat value of the product fuel gas.
  • the remaining gas may then be used as a fuel or the carbon dioxide and remaining hydrogen may be passed, at 06, over a methanation reactor containing an appropriate nickel catalyst where the carbon dioxide and hydrogen are converted into methane and water vapor as follows: CO2 + 4 H2 ⁇ CH4 + 2 H2O
  • the resulting fuel gas stream 88 can then be dehydrated at 87, and used as a clean fuel source.
  • FIGURE 3 illustrates a slightly modified form of the process of FIGURE 2.
  • components comparable to those in FIGURE 2 are shown by the same reference numeral.
  • the major distinction of the method of FIGURE 3 is that the substochiometric combustion is for the entire gas stream in line 71.
  • block 91 is provided indicating the heat value of the gas may be increased by passing it over a sulfur tolerant direct methanation catalyst (such as one available from Haldor Topsoe Company) which promotes the following reaction: 2 CO + 2 H2 ⁇ CH4 + CO2
  • the gas mixture may then be purified and the sulfur compounds isolated as described with respect to FIGURE 2.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Gas Separation By Absorption (AREA)
  • Paper (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)
  • Industrial Gases (AREA)
  • Treating Waste Gases (AREA)
EP19920890034 1991-09-10 1992-02-10 Traitement de gaz contenant des composés organiques sulfurés spécialement dans des systèmes et procédés de lessivage kraft Withdrawn EP0532491A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US75684991A 1991-09-10 1991-09-10
US756849 1991-09-10

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EP0532491A1 true EP0532491A1 (fr) 1993-03-17

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EP19920890034 Withdrawn EP0532491A1 (fr) 1991-09-10 1992-02-10 Traitement de gaz contenant des composés organiques sulfurés spécialement dans des systèmes et procédés de lessivage kraft

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EP (1) EP0532491A1 (fr)
JP (1) JPH05237344A (fr)
AU (2) AU643117B2 (fr)
BR (1) BR9201216A (fr)
CA (1) CA2060819A1 (fr)
FI (1) FI921516A (fr)
NO (1) NO920691L (fr)
ZA (1) ZA921042B (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012091906A3 (fr) * 2010-12-30 2012-09-13 Uop Llc Procédé de réduction d'un ou de plusieurs solides insolubles dans une liqueur noire
WO2012174094A1 (fr) * 2011-06-14 2012-12-20 Shell Oil Company Procédé de sulfuration aqueuse d'un catalyseur
US10870810B2 (en) 2017-07-20 2020-12-22 Proteum Energy, Llc Method and system for converting associated gas

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5234546A (en) * 1991-09-10 1993-08-10 Kamyr, Inc. Polysulfide production in white liquor

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0329301A2 (fr) * 1988-02-18 1989-08-23 Imperial Chemical Industries Plc Désulfuration
WO1992013994A1 (fr) * 1991-02-06 1992-08-20 A. Ahlstrom Corporation Procede de recuperation d'energie et de produits chimiques a partir de liqueur noire

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4067767A (en) * 1972-10-05 1978-01-10 Texaco Inc. Liquid phase coking of spent kraft pulping liquors
US4254094A (en) * 1979-03-19 1981-03-03 Air Products And Chemicals, Inc. Process for producing hydrogen from synthesis gas containing COS
US4839326A (en) * 1985-04-22 1989-06-13 Exxon Research And Engineering Company Promoted molybdenum and tungsten sulfide catalysts, their preparation and use

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0329301A2 (fr) * 1988-02-18 1989-08-23 Imperial Chemical Industries Plc Désulfuration
WO1992013994A1 (fr) * 1991-02-06 1992-08-20 A. Ahlstrom Corporation Procede de recuperation d'energie et de produits chimiques a partir de liqueur noire

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPIL Week 9113, Derwent Publications Ltd., London, GB; AN 91-089818 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012091906A3 (fr) * 2010-12-30 2012-09-13 Uop Llc Procédé de réduction d'un ou de plusieurs solides insolubles dans une liqueur noire
US8940129B2 (en) 2010-12-30 2015-01-27 Uop Llc Process for reducing one or more insoluble solids in a black liquor
WO2012174094A1 (fr) * 2011-06-14 2012-12-20 Shell Oil Company Procédé de sulfuration aqueuse d'un catalyseur
AU2012271758B2 (en) * 2011-06-14 2015-07-23 Shell Internationale Research Maatschappij B.V. Aqueous catalyst sulfiding process
US10870810B2 (en) 2017-07-20 2020-12-22 Proteum Energy, Llc Method and system for converting associated gas
US11505755B2 (en) 2017-07-20 2022-11-22 Proteum Energy, Llc Method and system for converting associated gas

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ZA921042B (en) 1992-12-30
BR9201216A (pt) 1993-04-13
AU1091192A (en) 1993-03-11
AU5310194A (en) 1994-03-03
JPH05237344A (ja) 1993-09-17
FI921516A0 (fi) 1992-04-07
NO920691L (no) 1993-03-11
NO920691D0 (no) 1992-02-21
CA2060819A1 (fr) 1993-03-11
FI921516A (fi) 1993-03-11
AU643117B2 (en) 1993-11-04

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