JP2020513399A - ベンジル基を含む構造誘導物質を用いたゼオライトの製造方法及びそれから製造されたゼオライト - Google Patents
ベンジル基を含む構造誘導物質を用いたゼオライトの製造方法及びそれから製造されたゼオライト Download PDFInfo
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- zeolite
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- 239000010457 zeolite Substances 0.000 title claims abstract description 203
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 192
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 189
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 76
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 title claims abstract description 39
- 239000000411 inducer Substances 0.000 title claims description 23
- 239000000126 substance Substances 0.000 claims abstract description 44
- 230000001939 inductive effect Effects 0.000 claims abstract description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010335 hydrothermal treatment Methods 0.000 claims description 34
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 30
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 24
- 150000001768 cations Chemical class 0.000 claims description 22
- -1 benzyltrimethylammonium ion Chemical class 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 238000010531 catalytic reduction reaction Methods 0.000 claims description 6
- 150000004820 halides Chemical class 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical group [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 5
- 239000007858 starting material Substances 0.000 claims description 4
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 3
- VBQDSLGFSUGBBE-UHFFFAOYSA-N benzyl(triethyl)azanium Chemical compound CC[N+](CC)(CC)CC1=CC=CC=C1 VBQDSLGFSUGBBE-UHFFFAOYSA-N 0.000 claims description 3
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 150000004679 hydroxides Chemical class 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 238000010586 diagram Methods 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 39
- 239000010949 copper Substances 0.000 description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 17
- 229910052802 copper Inorganic materials 0.000 description 17
- 239000000243 solution Substances 0.000 description 15
- 101150111792 sda1 gene Proteins 0.000 description 11
- 238000002441 X-ray diffraction Methods 0.000 description 9
- NDKBVBUGCNGSJJ-UHFFFAOYSA-M benzyltrimethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)CC1=CC=CC=C1 NDKBVBUGCNGSJJ-UHFFFAOYSA-M 0.000 description 9
- 238000001027 hydrothermal synthesis Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 8
- 239000011259 mixed solution Substances 0.000 description 6
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 5
- HTZCNXWZYVXIMZ-UHFFFAOYSA-M benzyl(triethyl)azanium;chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC1=CC=CC=C1 HTZCNXWZYVXIMZ-UHFFFAOYSA-M 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical group C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000005341 cation exchange Methods 0.000 description 3
- QDYLMAYUEZBUFO-UHFFFAOYSA-N cetalkonium chloride Chemical compound CCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 QDYLMAYUEZBUFO-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005342 ion exchange Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- ANHXKSXTBQIUAZ-UHFFFAOYSA-M benzyl(tributyl)azanium;hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CC1=CC=CC=C1 ANHXKSXTBQIUAZ-UHFFFAOYSA-M 0.000 description 2
- FKPSBYZGRQJIMO-UHFFFAOYSA-M benzyl(triethyl)azanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC1=CC=CC=C1 FKPSBYZGRQJIMO-UHFFFAOYSA-M 0.000 description 2
- KXHPPCXNWTUNSB-UHFFFAOYSA-M benzyl(trimethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC1=CC=CC=C1 KXHPPCXNWTUNSB-UHFFFAOYSA-M 0.000 description 2
- QEABVDWVSDSQRO-UHFFFAOYSA-M benzyl(tripropyl)azanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CC1=CC=CC=C1 QEABVDWVSDSQRO-UHFFFAOYSA-M 0.000 description 2
- 229960000228 cetalkonium chloride Drugs 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 2
- 238000004904 shortening Methods 0.000 description 2
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 230000002730 additional effect Effects 0.000 description 1
- 229910001579 aluminosilicate mineral Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/46—Other types characterised by their X-ray diffraction pattern and their defined composition
- C01B39/48—Other types characterised by their X-ray diffraction pattern and their defined composition using at least one organic template directing agent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/7007—Zeolite Beta
-
- 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
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic 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
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
- B01D53/9418—Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/7015—CHA-type, e.g. Chabazite, LZ-218
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
- B01J29/76—Iron group metals or copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
- B01J29/76—Iron group metals or copper
- B01J29/7615—Zeolite Beta
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/026—After-treatment
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/18—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control
- F01N3/20—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control specially adapted for catalytic conversion ; Methods of operation or control of catalytic converters
- F01N3/2066—Selective catalytic reduction [SCR]
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Abstract
Description
ベンジル基を含む第1構造誘導物質、ゼオライトの原料結晶、塩基性物質、及び蒸留水を含む水和ゲルを準備するステップ;並びに
前記水和ゲルを水熱合成するステップ
を含み、
前記ゼオライトの原料結晶は、アルミニウム酸化物及びシリカを含み、
前記ベンジル基を含む第1構造誘導物質は、ベンジルトリメチルアンモニウムイオン、ベンジルトリエチルアンモニウムイオン、ベンジルトリプロピルアンモニウムイオン及びベンジルトリブチルアンモニウムイオンを陽イオンとする水酸化物、ハロゲン化物、炭酸塩、及び硫酸塩からなる群より選択される少なくとも1種を含む、ベンジル基を含む構造誘導物質を用いる。
蒸留水にNaOHを溶解させた後、アルミニウム酸化物及びシリカを含むゼオライトUSY(このとき、SiO2/Al2O3のモル比=30)を添加し、均一溶液になるまで混合して混合溶液を調製した。ベンジルトリメチルアンモニウムヒドロキシド(SDA1)を前記混合溶液に添加した後、均一溶液になるまで混合して、次のようなモル比の組成を有する水和ゲルを製造した。
SiO2:NaOH:SDA1:H2O=1:0.2:0.2:22.62
蒸留水にNaOHを溶解させた後、アルミニウム酸化物及びシリカを含むゼオライトUSY(このとき、SiO2/Al2O3のモル比=30)を添加し、均一溶液になるまで混合して混合溶液を調製した。ベンジルトリメチルアンモニウムクロライド(SDA2)を前記混合溶液に添加した後、均一溶液になるまで混合して、次のようなモル比の組成を有する水和ゲルを製造した。
SiO2:NaOH:SDA2:H2O=1:0.4:0.4:22.62
蒸留水にNaOHを溶解させた後、アルミニウム酸化物及びシリカを含むゼオライトUSY(このとき、SiO2/Al2O3のモル比=30)を添加し、均一溶液になるまで混合して混合溶液を調製した。ベンジルトリエチルアンモニウムクロライド(SDA3)を前記混合溶液に添加した後、均一溶液になるまで混合して、次のようなモル比の組成を有する水和ゲルを製造した。
SiO2:NaOH:SDA3:H2O=1:0.4:0.4:22.62
蒸留水にNaOHを溶解させた後、アルミニウム酸化物及びシリカを含むゼオライトUSY(このとき、SiO2/Al2O3のモル比=30)を添加し、均一溶液になるまで混合して混合溶液を調製した。ベンジルトリメチルアンモニウムヒドロキシド(SDA1)及びベンジルジメチルヘキサデシルアンモニウムクロライド(SDA4)を前記混合溶液に添加した後、均一溶液になるまで混合して、次のようなモル比の組成を有する水和ゲルを製造した。
SiO2:NaOH:SDA1:SDA4:H2O
=1:0.2:0.2:0.01:22.62
蒸留水にNaOHを溶解させた後、アルミニウム酸化物及びシリカを含むゼオライトUSY(このとき、SiO2/Al2O3のモル比=30)を添加し、均一溶液になるまで混合して混合溶液を調製した。ベンジルトリメチルアンモニウムヒドロキシド(SDA1)及びNa2SO4を前記混合溶液に添加した後、均一溶液になるまで混合して、次のようなモル比の組成を有する水和ゲルを製造した。
SiO2:NaOH:SDA1:H2O:Na2SO4
=1:0.2:0.2:22.62:0.1
蒸留水にNaOHを溶解させた後、アルミニウム酸化物及びシリカを含むゼオライトUSY(このとき、SiO2/Al2O3のモル比=500)を添加し、均一溶液になるまで混合して混合溶液を調製した。ベンジルトリメチルアンモニウムヒドロキシド(SDA1)を前記混合溶液に添加した後、均一溶液になるまで混合して、次のようなモル比の組成を有する水和ゲルを製造した。
SiO2:NaOH:SDA1:H2O=1:0.3:0.2:22.62
常用化されたSSZ−13形態のゼオライトとして、N,N,N−トリアルキルアダマンタンアンモニウム水酸化物を含んだ水和ゲルを、水熱合成して製造した。
Claims (13)
- ゼオライトの製造方法において、
ベンジル基を含む第1構造誘導物質、ゼオライトの原料結晶、塩基性物質、及び蒸留水を含む水和ゲルを準備するステップ;並びに
前記水和ゲルを水熱合成するステップ
を含み、
前記ゼオライトの原料結晶は、アルミニウム酸化物及びシリカを含み、
前記ベンジル基を含む第1構造誘導物質は、ベンジルトリメチルアンモニウムイオン、ベンジルトリエチルアンモニウムイオン、ベンジルトリプロピルアンモニウムイオン及びベンジルトリブチルアンモニウムイオンを陽イオンとする水酸化物、ハロゲン化物、炭酸塩、及び硫酸塩からなる群より選択される少なくとも1種を含む
ことを特徴とする、ベンジル基を含む構造誘導物質を用いたゼオライトの製造方法。 - 前記水和ゲルは、第2構造誘導物質をさらに含み、
前記第2構造誘導物質は、下記化学式で表されるイオンを陽イオンとする水酸化物、ハロゲン化物、炭酸塩、及び硫酸塩からなる群より選択される少なくとも1種を含み、
- 製造されたゼオライトの平均粒子直径が、0.2μm〜1.0μmであることを特徴とする、請求項2に記載のベンジル基を含む構造誘導物質を用いたゼオライトの製造方法。
- 前記ゼオライトの原料結晶は、SiO2/Al2O3のモル比が5〜600であることを特徴とする、請求項1に記載のベンジル基を含む構造誘導物質を用いたゼオライトの製造方法。
- 製造されたゼオライトが、SSZ−13(Standard Oil Synthetic Zeolite−13)形態であることを特徴とする、請求項2に記載のベンジル基を含む構造誘導物質を用いたゼオライトの製造方法。
- 前記ゼオライトの原料結晶は、SiO2/Al2O3のモル比が490〜510のBEA(Zeolite Beta)形態であることを特徴とする、請求項4に記載のベンジル基を含む構造誘導物質を用いたゼオライトの製造方法。
- 前記水和ゲルは、硫酸イオンを含む化合物をさらに含むことを特徴とする、請求項1に記載のベンジル基を含む構造誘導物質を用いたゼオライトの製造方法。
- Si/Alのモル比が10〜100であり、
750℃〜950℃の温度範囲で水熱処理した後もゼオライトの構造が維持される、ゼオライト。 - 850℃〜950℃の温度範囲で水熱処理した後もゼオライトの構造が維持されることを特徴とする、請求項8に記載のゼオライト。
- 前記水熱処理した後も比表面積が500m2/g以上、600m2/g以下であることを特徴とする、請求項8に記載のゼオライト。
- 前記ゼオライトの構造は、ゼオライトの格子当たりAl原子が0〜4個含まれ、
Cu/Alのモル比が0.2〜0.4であることを特徴とする、請求項8に記載のゼオライト。 - 前記水熱処理した後に250℃〜500℃の温度範囲で選択的触媒還元反応が行われるとき、NOx転換率が50%以上、80%以下であることを特徴とする、請求項11に記載のゼオライト。
- 請求項1〜7のいずれか1つに記載の製造方法によって製造されるゼオライト。
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