WO2005016846A1 - Materiaux refractaires resistant a l'alcali - Google Patents

Materiaux refractaires resistant a l'alcali Download PDF

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Publication number
WO2005016846A1
WO2005016846A1 PCT/US2004/026166 US2004026166W WO2005016846A1 WO 2005016846 A1 WO2005016846 A1 WO 2005016846A1 US 2004026166 W US2004026166 W US 2004026166W WO 2005016846 A1 WO2005016846 A1 WO 2005016846A1
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WO
WIPO (PCT)
Prior art keywords
lithium
accordance
refractory
alkali
surface layer
Prior art date
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PCT/US2004/026166
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English (en)
Inventor
Roberta A. Peascoe Meisner
Camden R. Hubbard
James R. Keiser
Peter J Gorog
Original Assignee
Ut-Battelle, Llc
University Of Tennessee Research Foundation
Weyerhaeuser Company
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Application filed by Ut-Battelle, Llc, University Of Tennessee Research Foundation, Weyerhaeuser Company filed Critical Ut-Battelle, Llc
Publication of WO2005016846A1 publication Critical patent/WO2005016846A1/fr

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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/185—Mullite 3Al2O3-2SiO2
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/19—Alkali metal aluminosilicates, e.g. spodumene
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5024—Silicates
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
    • C04B41/5031—Alumina
    • C04B41/5032—Aluminates
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
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    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/87—Ceramics
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J3/00—Production of combustible gases containing carbon monoxide from solid carbonaceous fuels
    • C10J3/72—Other features
    • C10J3/74—Construction of shells or jackets
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
    • C04B2235/3203—Lithium oxide or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
    • C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427—Silicates other than clay, e.g. water glass
    • C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
    • C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/80—Phases present in the sintered or melt-cast ceramic products other than the main phase
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
    • C04B2235/9692—Acid, alkali or halogen resistance
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10J—PRODUCTION OF PRODUCER GAS, WATER-GAS, SYNTHESIS GAS FROM SOLID CARBONACEOUS MATERIAL, OR MIXTURES CONTAINING THESE GASES; CARBURETTING AIR OR OTHER GASES
    • C10J2300/00—Details of gasification processes
    • C10J2300/09—Details of the feed, e.g. feeding of spent catalyst, inert gas or halogens
    • C10J2300/0983—Additives
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12736—Al-base component
    • Y10T428/12743—Next to refractory [Group IVB, VB, or VIB] metal-base component

Definitions

  • the present invention relates to refractory materials that are resistant to alkali attack, and more particularly to refractory materials having a lithium rich surface treatment that retards degradation of refractories upon exposure to alkali-rich molten salts particularly molten Na 2 CO 3 .
  • objectives of the present invention include provision of alkali resistant refractory containment materials for high-temperature vessels, and especially for black liquor gasification processes in order to make such processes more feasible. Further and other objects of the present invention will become apparent from the description contained herein. SUMMARY OF THE INVENTION In accordance with one aspect of the present invention, the foregoing and other objects are achieved by an article that includes a refractory material having a surface layer characterized by a greater concentration of lithium than the refractory material.
  • a method of making an alkali-resistant material includes the steps of: applying to a refractory material at least one litWum-containing material; and heating the refractory material to a sufficient temperature so that the lilMum-containing material forms an alkali-resistant surface layer on the refractory material.
  • a method of forming an alkali-resistant layer on a refractory vessel liner includes the steps of: providing a working material including lithium; and heating the working material in the vessel to a sufficient temperature so that the lithium forms an alkali-resistant surface layer on the vessel liner.
  • FIG. 1 is a photograph of a test sample, after immersion testing in molten high alkali smelt, of refractory material having a lithium-rich layer in accordance with the present invention.
  • Fig. 2 is a photograph of a control sample, after immersion testing in molten high alkali smelt, of refractory material as received from the manufacturer and without a lithium-rich layer.
  • the lithium-containing composition is subsequently reacted at a temperature in the range of
  • the surface layer is generally characterized as having a higher concentration of lithium than the bulk refractory.
  • the surface layer is resistant to chemical attack by alkaline species, and protects the underlying bulk refractory material from chemical attack by alkaline species.
  • the surface layer retards the degradation of refractory materials exposed to alkali-rich molten smelts, for example, molten Na 2 CO 3 /Na 2 S.
  • the surface layer generally comprises crystalline and/or glassy phases which may include at least one of the following classes of compounds: lithium aluminates, lithium silicates, and lithium alumina silicates, depending on composition of the starting refractory material.
  • the surface layer can be altered during molten smelt exposure to form a layer material that appears to further retard sodium ion penetration.
  • EXAMPLE I An approximately 2mm thick layer of dry Li 2 CO 3 was applied to the surfaces of mullite/SiO 2 refractory materials. The refractory and Li 2 CO 3 layer was heated in air to a temperature of 900°C for one hour to affect the desired reaction and formation of a lithium-rich surface layer on the refractory material. Subsequent x- ray examination of the surface revealed the formation of crystalline eucryptite (Li 2 Al 2 SiO 6 ) andLiAlO 2 .
  • EXAMPLE H A sample of refractory material prepared in accordance with Example I and an untreated control sample were immersed for 50 hours at 1000°C in high alkali molten salt containing Na 2 CO 3 and Na 2 S. Cross sections were subsequently cut from the samples. An improvement in alkali resistance was observed for the sample having a lithium-rich surface layer, shown in Fig. 1, compared to the untreated control sample, shown in Fig. 2.
  • Other refractory materials such as: alumina, mixed ⁇ - ⁇ -alumina, and magnesium- alumina-spinel based refractories have shown some improved resistance to molten alkali salts after a lithium treatment though not to the extent observed for mullite-based refractories.
  • the lithium reacts with the alumina and/or silica minerals present in the refractory it forms a lithium-rich layer.
  • the present invention can be used to coat individual firebricks and/or high- temperature vessel liners. A damaged or worn lithium-rich layer can be repaired by re- application thereof by any of the processes described herein.
  • the present invention can significantly extend the life of refractory materials.
  • a solution containing Li CO 3 , LiOH and/or other lithium composition(s) can be infused via capillary action into the refractory body prior to heating between 700° and 1300°C and subsequent formation of lithium-rich layer.
  • molten Li 2 CO 3 or LiOH can be infused into the refractory with the subsequent formation of a lithium-rich layer.
  • EXAMPLE ⁇ i A solution containing Li 2 CO 3 is applied to the surface of a mullite/SiO 2 refractory material and allowed to infuse thereinto. The Li 2 CO 3 -infi ⁇ sed refractory is heated in air to a temperature of 900°C for one hour to affect the desired reaction and formation of a lithium-rich layer on the refractory material.
  • a slurry of Li 2 CO 3 and/or LiOH or a litliium-containing composition could be applied to the refractory lining and heated in place to form lithium compounds on the surface.
  • EXAMPLE IV An aqueous slurry of Li 2 CO 3 is sprayed onto the surface of a mullite/SiO 2 refractory material.
  • the Li 2 CO 3 -coated refractory is heated in air to a temperature of 900°C for one hour to affect the desired reaction and formation of a lithium-rich layer on the refractory material.
  • Li 2 CO 3 and/or LiOH or a lithium-containing composition can be added to working material, for example, black liquor and/or biomass, and injected into the gasifier therewith so that during gasification, the formation (new, maintenance, and/or repair) of a lithium-rich layer occurs on the refractory liner during the biogasification process.
  • Li 2 CO 3 is added to a batch of black liquor prior to injection into a gasification vessel.
  • the black liquor is then injected into the gasifier and the biogasification process is carried out therein.
  • the Li CO 3 is deposited on the refractory liner where it reacts with the refractory liner material, forming a lithium- rich layer thereon.
  • Refractory materials made in accordance with the present invention are suitable for use as containment materials or as containment liners for applications where high levels of alkali molten salts are present, for example, biogasification processes. While there has been shown and described what are at present considered the preferred embodiments of the invention, it will be obvious to those skilled in the art that various changes and modifications can be prepared therein without departing from the scope of the inventions defined by the appended claims.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Combustion & Propulsion (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Furnace Housings, Linings, Walls, And Ceilings (AREA)

Abstract

L'invention concerne un matériau réfractaire résistant à l'alcali pourvu d'une couche de surface qui se caractérise par une concentration en lithium plus élevée que celle du matériau réfractaire volumineux.
PCT/US2004/026166 2003-08-12 2004-08-12 Materiaux refractaires resistant a l'alcali WO2005016846A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US10/639,791 2003-08-12
US10/639,791 US20050037226A1 (en) 2003-08-12 2003-08-12 Alkali resistant refractories

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WO2005016846A1 true WO2005016846A1 (fr) 2005-02-24

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CN105199784B (zh) * 2015-10-30 2018-09-18 新奥科技发展有限公司 一种流化床气化炉及其炉衬的制作方法
CN105219444B (zh) * 2015-10-30 2018-09-18 新奥科技发展有限公司 一种流化床气化炉及其炉衬的制作方法
CN116444281B (zh) * 2023-06-13 2023-09-26 内蒙古建筑职业技术学院(内蒙古自治区建筑职工培训中心) 一种硫酸钠耐火材料

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