WO1988007023A1 - Procede de transformation de sulfite et/ou de bisulfite en sulfate par oxydation catalytique au milieu aqueux - Google Patents

Procede de transformation de sulfite et/ou de bisulfite en sulfate par oxydation catalytique au milieu aqueux Download PDF

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Publication number
WO1988007023A1
WO1988007023A1 PCT/DK1988/000042 DK8800042W WO8807023A1 WO 1988007023 A1 WO1988007023 A1 WO 1988007023A1 DK 8800042 W DK8800042 W DK 8800042W WO 8807023 A1 WO8807023 A1 WO 8807023A1
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WO
WIPO (PCT)
Prior art keywords
sulphite
sulphate
oxidation
particles
enzyme
Prior art date
Application number
PCT/DK1988/000042
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English (en)
Inventor
Birger Borregaard
Anders Søren JOHANSEN
Johannes Jacobus Mallan
Mette Tingleff Skaanild
Original Assignee
Dansk Biologisk Produktion Amba
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
Application filed by Dansk Biologisk Produktion Amba filed Critical Dansk Biologisk Produktion Amba
Publication of WO1988007023A1 publication Critical patent/WO1988007023A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/96—Methods for the preparation of sulfates in general
    • 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
    • B01D53/501—Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound
    • 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
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/84—Biological processes
    • 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
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8603—Removing sulfur compounds
    • B01D53/8609—Sulfur oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/46—Sulfates
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

Definitions

  • the present invention relates to a method for the catalytic oxidation in aqueous medium of sulphite and/or bisulphite to form sulphate, which is removed for use or depositing.
  • the method is especially suitable for use in connection with the purification of effluent gases, such as flue gases or roast gases, for sulphur dioxide, in which method the sulphur dioxide is absorbed by one or more basic compounds of alkali metals, alkaline earth metals or ammonium in aqueous solution or suspension while forming sulphite or bisulphite, which is then oxidized in aqueous medium to form sulphate which is removed for use or precipitated for depositing.
  • effluent gases such as flue gases or roast gases
  • sulphur dioxide in which method the sulphur dioxide is absorbed by one or more basic compounds of alkali metals, alkaline earth metals or ammonium in aqueous solution or suspension while forming sulphite or bisulphite, which is then oxidized in aqueous medium to form sulphate which is removed for use or precipitated for depositing.
  • effluent gases such as flue gases or roast gases
  • sulphur dioxide
  • the invention is explained in the following in relation to use of the method for the desulphurization of S0 2 -containing flue and roast gases.
  • Several methods of this type are known. It is common to these methods that they are difficult to control and carry out optimally, and especially the oxidation of sulhite (SO ⁇ ) or bisulphite (HS0 3 ) to sulphate is causing difficulties.
  • SO ⁇ sulhite
  • HS0 3 bisulphite
  • the most important of the processes known are to be briefly mentioned.
  • the most commonly used method is the limestone process. According to this process the flue gases are usually scrubbed in power plants after the removal of, i.a., fly ash, using calcium carbonate (limestone) for removing SOshare in accordance with the reactions:
  • the formation of Ca in the limestone process depends on the concentration of H and CaCO-, and the process has its pH optimum typically about 6.
  • the formation of Ca depends only on the concentration of CaO, and its optimum pH is higher, typically about 8.
  • the equilibrium for the overall reactions (5) and (10) is strongly shifted to the right; the free energy G is -13.4 kcal/mole and -44.5 kcal/mole for (5) and (10), respectively, while the equilibrium constant log K at
  • 25°C is 10.9 and 32.-8, respectively.
  • the calcium sulphate formed is sparingly soluble and crystallizes at the conditions normally used as the dihydrate, i.e. gypsum.
  • the likewise sparingly soluble calcium sulphite gives soft and spongy deposits while the gypsum deposits are hard.
  • the pH of the scrubber solution determines the nature of the final product. Below pH about 6 there is mainly produced bisulphite HS0 3 , above pH about 6.5 mainly sulphite SO-.
  • the bisulphite ions produced are oxidized at a relatively low pH to sulphate ions:
  • reaction (17) which best proceeds at about pH 6.
  • An important side reaction will be reaction (17) shown hereinbefore.
  • the used scrubber liquid is pumped to a regeneration vessel in which the active sulphite is re-formed by the addition of, e.g., calcium hydroxide (e.g. as milk of lime) :
  • This according to the invention is obtained by oxidation in aqueous medium of sulphite or bisulphite to sulphate at pH 6.5-9.5, preferably about 8.6 and at a temperature below 50 C, preferably 25-30 C by catalysis with a sulphite-oxidizing enzyme.
  • a bacterial sulphite oxidase is used, e.g. originating from species of the genus Thiobacillus, e.g. Thiobacillus thioparus or Thiobacillus novellus.
  • a sulphite oxidase has its optimum pH at about 8.0 and to a high degree looses its activity at temperatures above 55 C (cf. Lyric and Suzuki, Can. J. Biochem. _48_, pp. 334-343 (1970)).
  • a sulphite oxidase originating from liver of vertebrates, especially mammals or birds.
  • a sulphite oxidase originating from liver from oxen, calves or chicks can be used advantageously.
  • Such an enzyme has been known for a long time, cf. Cohen and Fridovich, J. Biological Chemistry, no. 2, January 1972, pp. 359-366 and 367-373. It has its optimum pH and hence its highest activity at pH 8.6 and is irreversibly inactivated at about pH 5. It is irreversibly inactivated at temperatures above 50 C and has the highest activity at 25-30°C. S0 4 ions have a protecting effect on the enzyme. It is commercially available in a purified form.
  • hepatic sulphite oxidase it is not necessary to use in a highly purified form; it can according to the invention as well be used in an isolated, more or less purified form. It is not necessary for the sulphite oxidase to have been isolated from cells and organelles; when used it may be bonded in cells or parts of cells. According to the invention it can be preferably used as mitochondria from liver cells.
  • the immobilization of the sulphite oxidase can be conducted in various ways well-known in the technology using enzymes on an industrial scale. Bonding to an ion exchanger matrix or covalently to a carrier material, e.g. using glutaraldehyde, are examples thereof. If the enzyme in its bonded state has a relatively high molecular weight, it can be suitable to have it present in a gel matrix, in particular if it is desired to use the enzyme in the form of mitochondria or while present in cell fragments. It is important to ensure that the sulphate produced in the oxidation does not precipitate in the immediate surroundings of the enzyme because thereby its activity could be reduced. On the other hand the sulphate must be removed currently to ensure a complete oxidation of SO..
  • An appropriate method for ensuring this according to the invention is to use the enzyme in a state in which it is bonded to or in particles (e.g. of a gel matrix of a hydrocolloid such as carrageenan, an alginate or polyacrylamide) which is suspended in the oxidation reactor for * sulphite/bisulphite together with particles of an ion exchanger for the exchange of sulphate ions with hydroxyl ions, the ion exchanger particles being removed continuously from the reaction as they are loaded with sulphate, whereupon the loaded ion exchanger particles are regenerated and recycled to the oxidation reactor.
  • particles e.g. of a gel matrix of a hydrocolloid such as carrageenan, an alginate or polyacrylamide
  • the sulphite is oxidized enzymatically to sulphate and the sulphate ion is ion exchanged with another ion, e.g. OH on a strongly basic anion exchanger, e.g. one of those commercially availabe under the name "Amberlite , ⁇ ⁇ being quaternary ammonium compounds.
  • another ion e.g. OH on a strongly basic anion exchanger, e.g. one of those commercially availabe under the name "Amberlite , ⁇ ⁇ being quaternary ammonium compounds.
  • Another advantageous method for the immobilization of the sulphite oxidase is to encapsulate it, either in in the form of free enzyme or, e.g., mitochondria, into microcapsules the walls of which are semipermeable and which are produced by polymerization of a suitable organic material.
  • This method can be advantageously combined with the former such that the microcapsules are suspended in the water in the oxidation reactor together with ion exchanger particles.
  • the enzyme according to the invention is immobilized in microcapsules having a semipermeable wall and together with buffer substances, e.g. ampholines having such a molecular weight that they cannot pass the semipermeable wall and which keep pH in the water in the microcapsules on or close to the optimum value of 8.6.
  • Fig. 1 schematically as an example shows a plant - for desulphurization of flue gas by the double alkali method and utilizing the principles of the invention.
  • Fig. 2 schematically and in larger scale shows an oxidation reactor being a part of a preferred embodiment of the plant according to fig. 1, and Fig. 3 schematically in very large scale shows a microcapsule containing the sulphite oxidizing enzyme, usable in the reactor shown in Fig. 2.
  • the flue gas which has been cooled (e.g. by being coupled to a district heating system) and freed from floating dust particles and other possible contents but still contains largely the whole amount of S0rada, is passed through a conduit 10 to a scrubber tower 12 (absorption vessel) which at the top has a demister 14 and at the bottom water containing a basic substance, in the present case sodium hydroxide and/or sodium carbonate, the plant being adapted to utilize the double alkali method.
  • a basic substance in the present case sodium hydroxide and/or sodium carbonate
  • the reactions explained above take place, from the top of the tower the gaseous components are led to the atmosphere through a conduit 15, and from the lower portion of the tower an aqueous solution containing sodium sulphite and sulphite and bisulphite ions are extracted through a conduit 16 via a filter 18 to an oxidation reactor 20 containing the sulphite oxidizing enzyme in immobilized form together with an ion exchanger, both of which in the suspended state.
  • the " liquid is kept at about pH 8.6, at least in the immediate vicinity of the enzyme or the particles in which the enzyme is immobilized.
  • An inlet 19 from a buffer tank 22 is connected to conduit 16, the buffer tank being fed from a conduit 24 that via a filter 25 is fed from the upper portion of the oxidation vessel 20 and is adjusted to increase the pH value to about 9 with sodium hydroxide, so that the sulphite solution in conduit 16 enters the oxidation reactor 20 at a pH of about 8-9.
  • a return pipe 26 leads to scrubber tower 12 for the pH adjustment of the scrubber water.
  • Oxygen usually in the form of air, is passed to the oxidation tank through a pipe 28.
  • two types of particles are present in suspension in reactor 20, viz. firstly particles with immobilized enzyme and secondly ion exchanger particles on which the sulphate is precipitated which has been produced by the oxidation of sulphite and bisulphite under the influence of the enzyme. This causes an increase of the density of these particles and thus, as indicated in the figure, they settle in the lower portion of the oxiation reactor 20.
  • a pipe 30 From there they are passed through a pipe 30 to a tank 32, in which the loaded ion exchanger particles are regenerated as the sulphate ions are eluted from the ion exchanger particles.
  • Regenerated ion exchanger particles are passed through a pipe 34 from the bottom of tank 32 via a washing system 35 back to reactor 20.
  • the elution of sulphate ions in the tank 32 is effected, e.g., with strong sodium hydroxide so as to form sodium sulphate.
  • the sodium sulphate is passed as a solution in water through a pipe 36 to a vessel 38.
  • the sodium hydroxide is passed through a pipe 37 back to vessel 32 and the gypsum precipitated in vessel 38 is passed through a pipe 40 to a centrifuge in which it is dewatered and is removed for deposition or use, the separated water being returned to vessel 38.
  • the above conduit 37 extends from the precipitation tank 38 so that sodium ions are returned to tank 32, in which there is optionally supplemented with fresh sodium hydroxide.
  • Fig. 2 in a larger scale shows the oxidation reactor 20. It is indicated that suspended herein there are present particles (e) (shown in highly exaggerated enlargement) with immobilized ⁇ enzyme and particles ⁇ with ion exchanger particles binding SO. and hence obtaining a higher density and sinking to the bottom of reactor 20, from where they are removed through conduit 30.
  • the water containing dissolved sulphite enters through the pipe 16; its pH is if required adjusted to about 8 with, e.g., NaOH or KOH.
  • the scrubber water freed from sulphite and sulphate as mentioned is drained off through pipe 24 to the buffer tank.
  • a separator 42 is arranged to withhold the enzyme containing particles and ion exchanger particles.
  • Fig. 3 in extremely large scale schematically shows how enzyme can be encapsulated in microcapsules together with a buffer substance - in this case one or more ampholines - keeping pH near the optimum ' pH - value of 8.6.
  • the microcapsules have semipermeable walls that can ⁇ not be passed by the ampholine and the enzyme, but can be passed by sulphite and sulphate ions as intimated.
  • Fig. 3 E stands for enzyme and A for ampholine, but it is to be understood that there is aimed at molecules or minor aggregations thereof, not a further immobilization within the microcapsules which themselves constitute the immobilization.
  • the invention is notably expected to be of importance in the desulphurization of flue gases and roast gases.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Organic Chemistry (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Molecular Biology (AREA)
  • Geology (AREA)
  • Treating Waste Gases (AREA)

Abstract

L'oxydation catalytique en milieu aqueux de sulfite ou de bisulfite s'effectue à un pH compris entre 6,5 et 9,5 mais se situant de préférence autour de 8,6, et à une température inférieure à 50°C, comprise de préférence entre 25 et 30°C, par catalyse au moyen d'une enzyme d'oxydation de sulfite. Une oxydase de sulfite provenant du foie de boeuf, de veau ou de poussin est particulièrement appropriée. Elle peut être utilisée sous la forme d'organelles ou de fragments cellulaires, tels que notamment les mitochondries, ou sous une forme isolée plus ou moins purifiée. Elle peut en particulier être immobilisée, par exemple dans des microcapsules comportant une paroi semi-perméable et en association avec des substancse tampon, ainsi qu'avec des particules échangeuses d'ions servant à recueillir les ions de sulfate. Ledit procédé est particulièrement utile pour l'oxydation de sulfite obtenu dans la purification de gaz de fumée ou de grillage avec des composés basiques de métaux alcalins, de métaux alcalino-terreux ou d'ammonium, par exemple dans le procédé à l'alcali double.
PCT/DK1988/000042 1987-03-13 1988-03-11 Procede de transformation de sulfite et/ou de bisulfite en sulfate par oxydation catalytique au milieu aqueux WO1988007023A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DK1305/87 1987-03-13
DK130587A DK130587A (da) 1987-03-13 1987-03-13 Fremgangsmaade til afsvovling af roeggasser

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0505642A1 (fr) * 1991-03-28 1992-09-30 Nakano Vinegar Co., Ltd. Capteur biologique de S02
EP1277508A2 (fr) * 2001-07-18 2003-01-22 Herr Klaus Grote Procédé et dispositif pour éliminer polluants contenus dans un gaz déchappement
WO2004088032A2 (fr) * 2003-04-03 2004-10-14 Kemira Oyj Procede permettant de recycler du soufre dans un processus de production de pate a papier
WO2009052775A1 (fr) 2007-10-23 2009-04-30 Babcock Noell Gmbh Installation et procédé de purification de gaz de fumée
EP2486969A1 (fr) * 2011-02-10 2012-08-15 Alstom Technology Ltd Procédé et dispositif pour traiter l'eau de mer effluente d'un épurateur d'eau de mer
EP2578544A1 (fr) * 2011-10-07 2013-04-10 Alstom Technology Ltd Procédé et système pour contrôler le traitement des effluents issus d'un épurateur de gaz de fumée à l'aide d'eau de mer
EP3069781A1 (fr) * 2015-03-20 2016-09-21 General Electric Technology GmbH Système pour l'élimination du soufre d'un gaz de combustion
US9630864B2 (en) 2015-06-17 2017-04-25 General Electric Technology Gmbh Seawater plant with inclined aeration and mixed auto recovery

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2070580A (en) * 1980-03-04 1981-09-09 Apv Co Ltd Oxidation of organic wastes

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2070580A (en) * 1980-03-04 1981-09-09 Apv Co Ltd Oxidation of organic wastes

Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0505642A1 (fr) * 1991-03-28 1992-09-30 Nakano Vinegar Co., Ltd. Capteur biologique de S02
EP1277508A2 (fr) * 2001-07-18 2003-01-22 Herr Klaus Grote Procédé et dispositif pour éliminer polluants contenus dans un gaz déchappement
EP1277508A3 (fr) * 2001-07-18 2004-01-02 Herr Klaus Grote Procédé et dispositif pour éliminer polluants contenus dans un gaz déchappement
WO2004088032A2 (fr) * 2003-04-03 2004-10-14 Kemira Oyj Procede permettant de recycler du soufre dans un processus de production de pate a papier
WO2004088033A2 (fr) * 2003-04-03 2004-10-14 Kemira Oyj Recyclage de soufre dans un procede de production de pate a papier
WO2004088032A3 (fr) * 2003-04-03 2004-11-25 Kemira Oyj Procede permettant de recycler du soufre dans un processus de production de pate a papier
WO2004088033A3 (fr) * 2003-04-03 2005-01-06 Kemira Oyj Recyclage de soufre dans un procede de production de pate a papier
US8337790B2 (en) 2007-10-23 2012-12-25 Babcock Noell Gmbh System and method for purification of flue gases
WO2009052775A1 (fr) 2007-10-23 2009-04-30 Babcock Noell Gmbh Installation et procédé de purification de gaz de fumée
US9327230B2 (en) 2011-02-10 2016-05-03 Alstom Technology Ltd Method and a device for treating effluent seawater from a seawater scrubber
EP2486969A1 (fr) * 2011-02-10 2012-08-15 Alstom Technology Ltd Procédé et dispositif pour traiter l'eau de mer effluente d'un épurateur d'eau de mer
CN107010710A (zh) * 2011-02-10 2017-08-04 通用电器技术有限公司 处理来自海水洗涤器的排出海水的方法和装置
TWI564067B (zh) * 2011-02-10 2017-01-01 通用電器技術有限公司 用於處理自海水洗滌塔排出的海水之方法及裝置
CN103347590A (zh) * 2011-02-10 2013-10-09 阿尔斯通技术有限公司 处理来自海水洗涤器的排出海水的方法和装置
JP2014509257A (ja) * 2011-02-10 2014-04-17 アルストム テクノロジー リミテッド 海水スクラバーからの排出海水を処理するための方法及び装置
WO2012107817A1 (fr) * 2011-02-10 2012-08-16 Alstom Technology Ltd Procédé et dispositif de traitement d'effluent d'eau de mer provenant d'un épurateur d'eau de mer
KR101536608B1 (ko) * 2011-02-10 2015-07-14 알스톰 테크놀러지 리미티드 해수 스크러버로부터 폐수 해수를 처리하기 위한 방법 및 디바이스
JP2014531315A (ja) * 2011-10-07 2014-11-27 アルストム テクノロジー リミテッドＡＬＳＴＯＭ Ｔｅｃｈｎｏｌｏｇｙ Ｌｔｄ 燃焼排ガス海水清浄器からの排水の処理制御方法およびシステム
CN103958419A (zh) * 2011-10-07 2014-07-30 阿尔斯通技术有限公司 控制来自海水烟道气体洗涤器的流出物的处理的方法及系统
CN103958419B (zh) * 2011-10-07 2016-08-17 通用电器技术有限公司 控制来自海水烟道气体洗涤器的流出物的处理的方法及系统
WO2013050988A1 (fr) * 2011-10-07 2013-04-11 Alstom Technology Ltd Procédé et système de commande de traitement d'effluent d'épurateur de gaz de combustion à eau de mer
EP2578544A1 (fr) * 2011-10-07 2013-04-10 Alstom Technology Ltd Procédé et système pour contrôler le traitement des effluents issus d'un épurateur de gaz de fumée à l'aide d'eau de mer
EP3069781A1 (fr) * 2015-03-20 2016-09-21 General Electric Technology GmbH Système pour l'élimination du soufre d'un gaz de combustion
WO2016150801A1 (fr) * 2015-03-20 2016-09-29 Alstom Technology Ltd Système pour l'élimination de soufre d'un gaz de carneau
US10040024B2 (en) 2015-03-20 2018-08-07 General Electric Technology Gmbh System for sulphur removal from a flue gas
US9630864B2 (en) 2015-06-17 2017-04-25 General Electric Technology Gmbh Seawater plant with inclined aeration and mixed auto recovery

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Publication number Publication date
DK130587D0 (da) 1987-03-13
DK130587A (da) 1988-09-14

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