US20050037226A1 - Alkali resistant refractories - Google Patents
Alkali resistant refractories Download PDFInfo
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- US20050037226A1 US20050037226A1 US10/639,791 US63979103A US2005037226A1 US 20050037226 A1 US20050037226 A1 US 20050037226A1 US 63979103 A US63979103 A US 63979103A US 2005037226 A1 US2005037226 A1 US 2005037226A1
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- Prior art keywords
- lithium
- accordance
- refractory
- alkali
- surface layer
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- 239000011819 refractory material Substances 0.000 title claims abstract description 35
- 239000003513 alkali Substances 0.000 title claims abstract description 22
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 40
- 239000002344 surface layer Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 18
- 239000010410 layer Substances 0.000 claims description 17
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 14
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 14
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 14
- 239000008207 working material Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 230000001464 adherent effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims 1
- 238000000151 deposition Methods 0.000 claims 1
- YQNQTEBHHUSESQ-UHFFFAOYSA-N lithium aluminate Chemical compound [Li+].[O-][Al]=O YQNQTEBHHUSESQ-UHFFFAOYSA-N 0.000 claims 1
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 claims 1
- 229910052912 lithium silicate Inorganic materials 0.000 claims 1
- 230000008569 process Effects 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 238000002309 gasification Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 4
- 229910052863 mullite Inorganic materials 0.000 description 4
- 241001062472 Stokellia anisodon Species 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910052681 coesite Inorganic materials 0.000 description 3
- 239000013068 control sample Substances 0.000 description 3
- 229910052906 cristobalite Inorganic materials 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 229910052682 stishovite Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910052905 tridymite Inorganic materials 0.000 description 3
- 150000001447 alkali salts Chemical class 0.000 description 2
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 2
- -1 lithium aluminates Chemical class 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 229910000873 Beta-alumina solid electrolyte Inorganic materials 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910010092 LiAlO2 Inorganic materials 0.000 description 1
- 241001417490 Sillaginidae Species 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 239000002551 biofuel Substances 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 229910000174 eucryptite Inorganic materials 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002642 lithium compounds Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- 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
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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
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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 .
- Gasification of black liquor produced at paper mills during the pulping process is an attractive process of recovering inorganic materials while generating electrical power/steam/biofuels/hydrogen from the waste stream.
- the process has been delayed in development due to poor resistance of containment materials to alkali attack during long-term operations.
- Degradation of refractory and metallic containment materials in pilot-scale and demonstration-scale gasifiers presents a serious obstacle to the commercialization of black liquor gasifiers.
- Gasification vessel refractory linings degrade rapidly (6 months to a year), requiring replacement.
- Alkali resistant containment materials could extend the lifetime of refractory liners, making black liquor gasification a more attractive alternative to recovery boilers.
- 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.
- 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 lithium-containing material; and heating the refractory material to a sufficient temperature so that the lithium-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 700° C. to 1300° C. to produce an adherent, lithium-rich surface layer.
- 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.
- Li 2 CO 3 An approximately 2 mm 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 ) and LiAlO 2 .
- 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 .
- 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.
- degradation of the refractory is retarded.
- 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 2 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.
- 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 -infused 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 lithium-containing composition could be applied to the refractory lining and heated in place to form lithium compounds on the surface.
- 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 2 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.
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Abstract
Description
- The United States Government has rights in this invention pursuant to contract no. DE-AC05-00OR22725 between the United States Department of Energy and UT-Battelle, LLC.
- 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 Na2CO3.
- Gasification of black liquor produced at paper mills during the pulping process is an attractive process of recovering inorganic materials while generating electrical power/steam/biofuels/hydrogen from the waste stream. The process has been delayed in development due to poor resistance of containment materials to alkali attack during long-term operations. Degradation of refractory and metallic containment materials in pilot-scale and demonstration-scale gasifiers presents a serious obstacle to the commercialization of black liquor gasifiers. Gasification vessel refractory linings degrade rapidly (6 months to a year), requiring replacement. Alkali resistant containment materials could extend the lifetime of refractory liners, making black liquor gasification a more attractive alternative to recovery boilers.
- Accordingly, 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.
- 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.
- In accordance with another aspect of the present invention, a method of making an alkali-resistant material includes the steps of: applying to a refractory material at least one lithium-containing material; and heating the refractory material to a sufficient temperature so that the lithium-containing material forms an alkali-resistant surface layer on the refractory material.
- In accordance with a further aspect of the present invention, 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. - For a better understanding of the present invention, together with other and further objects, advantages and capabilities thereof, reference is made to the following disclosure and appended claims in connection with the above-described drawings.
- Any lithium-containing composition having a low melting point (less than 1300° C.), for example, LiOH and Li2CO3, is applied, either as a powder or as a paste formed from a mixture of powder and fluid, to the surface of alumina and alumino-silicate refractories. The lithium-containing composition is subsequently reacted at a temperature in the range of 700° C. to 1300° C. to produce an adherent, lithium-rich surface layer. 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 Na2CO3/Na2S. 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.
- An approximately 2 mm thick layer of dry Li2CO3 was applied to the surfaces of mullite/SiO2 refractory materials. The refractory and Li2CO3 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 (Li2Al2SiO6) and LiAlO2.
- 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 Na2CO3 and Na2S. 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 inFIG. 2 . - Other refractory materials such as: alumina, mixed α-β-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. As the lithium reacts with the alumina and/or silica minerals present in the refractory it forms a lithium-rich layer. On immersion in molten alkali salts, degradation of the refractory is retarded.
- 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.
- In other embodiments of the present invention, a solution containing Li2CO3, 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. Moreover, molten Li2CO3 or LiOH can be infused into the refractory with the subsequent formation of a lithium-rich layer.
- A solution containing Li2CO3 is applied to the surface of a mullite/SiO2 refractory material and allowed to infuse thereinto. The Li2CO3-infused 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.
- Moreover, a slurry of Li2CO3 and/or LiOH or a lithium-containing composition could be applied to the refractory lining and heated in place to form lithium compounds on the surface.
- An aqueous slurry of Li2CO3 is sprayed onto the surface of a mullite/SiO2 refractory material. The Li2CO3-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.
- Moreover, Li2CO3 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.
- Li2CO3 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. In the gasifier, the Li2CO3 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.
Claims (16)
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
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US10/639,791 US20050037226A1 (en) | 2003-08-12 | 2003-08-12 | Alkali resistant refractories |
PCT/US2004/026166 WO2005016846A1 (en) | 2003-08-12 | 2004-08-12 | Alkali resistant refractories |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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US10/639,791 US20050037226A1 (en) | 2003-08-12 | 2003-08-12 | Alkali resistant refractories |
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US20050037226A1 true US20050037226A1 (en) | 2005-02-17 |
Family
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Family Applications (1)
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US10/639,791 Abandoned US20050037226A1 (en) | 2003-08-12 | 2003-08-12 | Alkali resistant refractories |
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WO (1) | WO2005016846A1 (en) |
Cited By (3)
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CN105199784A (en) * | 2015-10-30 | 2015-12-30 | 新奥科技发展有限公司 | Fluidized bed gasifying furnace and manufacture method of furnace lining of fluidized bed gasifying furnace |
CN105219444A (en) * | 2015-10-30 | 2016-01-06 | 新奥科技发展有限公司 | The making method of a kind of fluidized-bed gasification furnace and furnace lining thereof |
CN116444281A (en) * | 2023-06-13 | 2023-07-18 | 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) | Sodium sulfate refractory material |
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