JPWO2014013969A1 - Maz型ゼオライトの製造方法 - Google Patents
Maz型ゼオライトの製造方法 Download PDFInfo
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- 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 100
- 239000010457 zeolite Substances 0.000 title claims abstract description 95
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 94
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000013078 crystal Substances 0.000 claims abstract description 62
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000011541 reaction mixture Substances 0.000 claims abstract description 50
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 24
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 22
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 229910052593 corundum 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 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- 239000000126 substance Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- 239000011734 sodium Substances 0.000 description 11
- 238000002425 crystallisation Methods 0.000 description 10
- 230000008025 crystallization Effects 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 239000005416 organic matter Substances 0.000 description 7
- 229910001415 sodium ion Inorganic materials 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 229910001414 potassium ion Inorganic materials 0.000 description 6
- 229910001388 sodium aluminate Inorganic materials 0.000 description 6
- 230000032683 aging Effects 0.000 description 5
- 229910001413 alkali metal ion Inorganic materials 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 238000003795 desorption Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 4
- 229910000323 aluminium silicate Inorganic materials 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000011973 solid acid Substances 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 229910052680 mordenite Inorganic materials 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000001308 synthesis method Methods 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 239000008119 colloidal silica Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 239000013335 mesoporous material Substances 0.000 description 2
- 239000012229 microporous material Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- -1 tetramethylammonium ions Chemical class 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- 239000004111 Potassium silicate Substances 0.000 description 1
- 241000705939 Shortia uniflora Species 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- 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
- C01B39/34—Type ZSM-4
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
-
- 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
- B01J29/7011—MAZ-type, e.g. Mazzite, Omega, ZSM-4 or LZ-202
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/04—Mixing
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Description
SiO2/Al2O3=24〜60
(Na2O+K2O)/SiO2=0.25〜0.5
K2O/(Na2O+K2O)=0.1〜0.5
H2O/SiO2=5〜50
(2)SiO2/Al2O3比が5〜10であり、かつ平均粒子径が0.1μm以上である有機化合物を含まないMAZ型ゼオライトを種結晶として用い、これを、前記反応混合物中のシリカ成分に対して0.1〜30重量%の割合で該反応混合物に添加し、
(3)前記種結晶が添加された前記反応混合物を80〜200℃で密閉下に加熱することを特徴とするMAZ型ゼオライトの製造方法を提供するものである。
・(Na2O+K2O)/SiO2=0.25〜0.5
・K2O/(Na2O+K2O)=0.1〜0.5
・H2O/SiO2=5〜50
・SiO2/Al2O3=26〜55
・(Na2O+K2O)/SiO2=0.28〜0.45
・K2O/(Na2O+K2O)=0.15〜0.4
・H2O/SiO2=10〜30
走査型電子顕微鏡:(株)日立ハイテクノロジーズ社製、電界放出型走査電子顕微鏡 S−4800
組成分析装置:(株)バリアン製、ICP−AES LIBERTY SeriesII
窒素吸着特性測定装置:(株)カンタクローム インスツルメンツ社製、AUTOSORB−1
アンモニア昇温脱離(Temperature−Programmed Deosprtion、TPD)装置:日本ベル製、BEL−CAT
(1)種結晶の合成
テトラメチルアンモニウムヒドロキシドをOSDAとして用い、アルミン酸ナトリウムをアルミナ源、コロイダルシリカ(LUDOX、HS−40)をシリカ源、水酸化ナトリウムをアルカリ源とする従来公知の方法(非特許文献1)により反応混合物を調製した。この反応混合物を3日間室温で熟成した後、23ccのステンレス製密閉容器に入れて100℃で7日間、静置加熱を行ってゼオライトオメガ(MAZ型ゼオライト)の結晶を合成した。このゼオライトオメガを電気炉中で空気を流通しながら550℃で20時間焼成して、有機物を含まないゼオライトオメガの結晶を製造した。この結晶を走査型電子顕微鏡により観察した結果、平均粒子径は0.85μmであった。組成分析の結果、SiO2/Al2O3比は6.8であった。焼成した後のゼオライトオメガのX線回折図を図1に示す。この有機物を含まないゼオライトオメガの結晶を、以下に述べる実施例及び比較例において、種結晶として使用した。この種結晶をNH4 +イオンに交換し、焼成することによってH+型とした後、液体窒素温度において窒素吸脱着等温線(図4)を測定した。この等温線から細孔特性を評価した結果、ミクロ孔表面積:236m2/g、ミクロ孔容積:0.093cc/gであった。また、このH+型試料のアンモニアTPDの脱離曲線(図5(a))から求めた固体酸量は0.93mmol/gであった。
純水6.751gに、アルミン酸ナトリウム0.157gと50%水酸化カリウム0.490g及び36%水酸化ナトリウム溶液1.309gを溶解して水溶液を得た。この水溶液に粉末状シリカ(Cab−O−Sil、M5)1.316gを添加して均一に混合して表1に記載した組成のゲルを得た。この反応混合物を23ccのステンレス製密閉容器に入れて、撹拌することなしに140℃で5時間予備加熱した。その後、密閉容器を急冷した後、有機物を含まないゼオライトオメガの種結晶0.263gを反応混合物に添加して均一に混合した。次に密閉容器を再度140℃で24時間、自生圧力下で静置加熱した。密閉容器を冷却後、生成物をろ過、温水洗浄して白色粉末を得た。この生成物のX線回折測定の結果、この生成物は図2に示すように不純物を含まないMAZ型ゼオライトであることが確認された。
表1に示す条件を採用した以外は実施例1と同様にしてMAZ型ゼオライトを得た。ただし、表1に示すとおり、MAZ型ゼオライトに加えて副生成物としてゼオライトTの生成が観察される場合があった。MAZ型ゼオライトのみが生成した実施例3について測定したX線回折図を図3に示す。実施例3で得られた結晶をNH4 +イオンに交換し、焼成することによってH+型とした後、液体窒素温度において窒素吸脱着等温線(図4)を測定した。この等温線から細孔特性を評価した結果、ミクロ孔表面積:392m2/g、ミクロ孔容積:0.15cc/gであった。またこのH+型試料のアンモニアTPDの脱離曲線(図5(b))から求めた固体酸量は1.14mmol/gであった。
純水7.407gに、アルミン酸ナトリウム0.220gと50%水酸化カリウム0.312g及び36%水酸化ナトリウム溶液0.710gを溶解して水溶液を得た。この水溶液に粉末状シリカ(Cab−O−Sil、M5)1.352gと有機物を含まないゼオライトオメガの種結晶0.268gを添加して均一に混合して、表2に示す組成のゲルを得た。この反応混合物を23ccのステンレス製密閉容器に入れて、撹拌することなしに140℃で48時間、自生圧力下で静置加熱した。密閉容器を冷却後、生成物をろ過、温水洗浄して白色粉末を得た。この生成物のX線回折測定の結果、この生成物はモルデナイトであった。
表2に示す条件を採用した以外は比較例1と同様の操作を行った。比較例2及び3では、生成物が確認されたが、その同定はできなかった。比較例4ではアモルファス物質の生成が確認された。
Claims (3)
- (1)以下に示すモル比で表される組成の反応混合物となるように、シリカ源、アルミナ源、アルカリ源、及び水を混合し、
SiO2/Al2O3=24〜60
(Na2O+K2O)/SiO2=0.25〜0.5
K2O/(Na2O+K2O)=0.1〜0.5
H2O/SiO2=5〜50
(2)SiO2/Al2O3比が5〜10であり、かつ平均粒子径が0.1μm以上である有機化合物を含まないMAZ型ゼオライトを種結晶として用い、これを、前記反応混合物中のシリカ成分に対して0.1〜30重量%の割合で該反応混合物に添加し、
(3)前記種結晶が添加された前記反応混合物を80〜200℃で密閉下に加熱することを特徴とするMAZ型ゼオライトの製造方法。 - 種結晶を含まない反応混合物を密閉下に80〜200℃の温度で予備加熱した後、種結晶を該反応混合物に添加し、更に該反応混合物を80〜200℃の温度で密閉下に加熱する請求項1に記載の製造方法。
- 密閉下に加熱する工程で反応混合物を撹拌する請求項1又は2に記載の製造方法。
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JPH03237013A (ja) * | 1989-08-30 | 1991-10-22 | Soc Natl Elf Aquitaine <Snea> | マッツァイトの類からの新規なゼオライト、その合成方法、及びその触媒としての用途 |
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