JP2015507591A - 高活性大結晶zsm−5の合成 - Google Patents
高活性大結晶zsm−5の合成 Download PDFInfo
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- JP2015507591A JP2015507591A JP2014544807A JP2014544807A JP2015507591A JP 2015507591 A JP2015507591 A JP 2015507591A JP 2014544807 A JP2014544807 A JP 2014544807A JP 2014544807 A JP2014544807 A JP 2014544807A JP 2015507591 A JP2015507591 A JP 2015507591A
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- zsm
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- 239000013078 crystal Substances 0.000 title claims abstract description 49
- 238000003786 synthesis reaction Methods 0.000 title claims description 14
- 230000015572 biosynthetic process Effects 0.000 title claims description 13
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- 239000000203 mixture Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000011541 reaction mixture Substances 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 20
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000010457 zeolite Substances 0.000 claims abstract description 14
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 13
- 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 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 8
- 230000008025 crystallization Effects 0.000 claims abstract description 8
- RGHNJXZEOKUKBD-SQOUGZDYSA-N Gluconic acid Natural products OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims abstract description 7
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims abstract description 5
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- 238000007323 disproportionation reaction Methods 0.000 claims description 9
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- 238000001354 calcination Methods 0.000 description 4
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
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- HTDJPCNNEPUOOQ-UHFFFAOYSA-N hexamethylcyclotrisiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O1 HTDJPCNNEPUOOQ-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
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- 239000011738 major mineral Substances 0.000 description 1
- 235000011963 major mineral Nutrition 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 229910052605 nesosilicate Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 150000004762 orthosilicates Chemical class 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 125000000286 phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
- 150000003058 platinum compounds Chemical class 0.000 description 1
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920001921 poly-methyl-phenyl-siloxane Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000012254 powdered material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 239000012855 volatile organic compound Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
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- 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
- B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
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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
- C01B39/36—Pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11
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Abstract
Description
を特徴とすることができるシロキサンを挙げることができるが、これらに限定されるものではない。R1基およびR2基中の炭化水素置換基は、一般にそれぞれ1〜10個の炭素原子を含有することができる(たとえば、ある実施形態においてはメチル、エチル、および/またはフェニルを含有する基が好ましくなりうる)。使用されるシロキサンの(数平均)分子量は、一般に約80g/mol〜約20,000g/mol(たとえば約150g/mol〜約10,000g/mol)であり得る。代表的なシロキサンとしては、ジメチルシリコーン、ジエチルシリコーン、フェニルメチルシリコーン、メチル水素シリコーン、エチル水素シリコーン、フェニル水素シリコーン、メチルエチルシリコーン、フェニルエチルシリコーン、ジフェニルシリコーン、メチルトリフルオロプロピルシリコーン、エチルトリフルオロプロピルシリコーン、ポリジメチルシリコーン、テトラクロロフェニルメチルシリコーン、テトラクロロフェニルエチルシリコーン、テトラクロロフェニル水素シリコーン、テトラクロロフェニルフェニルシリコーン、メチルビニルシリコーン、エチルビニルシリコーンなど、ならびにそれらの組み合わせおよび/またはコポリマーを挙げることができるが、これらに限定されるものではない。シロキサン化合物は、直鎖である必要はなく、分岐および/または環状(たとえば、ヘキサメチルシクロトリシロキサン、オクタメチルシクロテトラシロキサン、ヘキサフェニルシクロトリシロキサン、オクタフェニルシクロテトラシロキサンなど、およびそれらの組み合わせ)であってよい。これに加えて、またはこれと交代にこれらの化合物の混合物を使用することができ、他の官能基を有するシロキサン/シリコーンを使用することもできる。
以下のモル組成を得るのに十分な量のSipernat(登録商標)−320シリカ、硫酸アルミニウム、NaOH、および脱イオン水を含む反応混合物からZSM−5結晶を合成した:
SiO2/Al2O3:約40
H2O/SiO2:約13.9
OH−/SiO2:約0.27
約950グラムの水、それぞれ約270グラムのSipernat(登録商標)−120または−350、約40グラムのアルミン酸ナトリウム溶液(水中45%)、および69グラムの50%水酸化ナトリウム水溶液から混合物を調製した。次に約9グラムのZSM−5シードを混合物に加えた。得られた混合物は以下のモル組成を示した:
SiO2/Al2O3:約40
H2O/SiO2:約13.9
OH−/SiO2:約0.27
約950グラムの水、約273グラムのSipernat(登録商標)−120、約45グラムのアルミン酸ナトリウム溶液(水中45%)、約89グラムのトリエタノールアミン(TEA)溶液(98%)、および約69グラムの50%水酸化ナトリウム水溶液混合物を調製した。次に約9グラムのZSM−5シードを混合物に加えた。得られた混合物は以下のモル組成を示した:
SiO2/Al2O3:約36
H2O/SiO2:約13.9
OH−/SiO2:約0.29
Na+/SiO2:約0.29
約950グラムの水、約270グラムのSipernat(登録商標)−120、約40グラムのアルミン酸ナトリウム溶液(水中45%)、約43グラムのd−グルコン酸一ナトリウム塩、および約69グラムの50%水酸化ナトリウム水溶液から混合物を調製した。次に約9グラムのZSM−5シードを混合物に加えた。得られた混合物は以下のモル組成を示した:
SiO2/Al2O3:約40
H2O/SiO2:約13.9
OH−/SiO2:約0.27
約9.5kgの水、約2.7kgのSipernat(登録商標)−120、約400グラムのアルミン酸ナトリウム溶液(水中45%)、約430グラムのd−グルコン酸一ナトリウム塩、および約690グラムの50%水酸化ナトリウム水溶液から混合物を調製した。次に約20グラムのZSM−5シードを混合物に加えた。得られた混合物は以下のモル組成を示した:
SiO2/Al2O3:約40
H2O/SiO2:約13.9
OH−/SiO2:約0.27
約955グラムの水、約273グラムのSipernat(登録商標)−120、約40グラムのアルミン酸ナトリウム溶液(水中45%)、約89グラムのトリエタノールアミン(TEA)溶液(98%)、および約75グラムの50%水酸化ナトリウム水溶液から混合物を調製した。次に約9グラムのZSM−5シードを混合物に加えた。得られた混合物は以下のモル組成を示した:
SiO2/Al2O3:約40
H2O/SiO2:約13.9
OH−/SiO2:約0.2
Na+/SiO2:約0.27
約65部(約538℃で焼成したものに基づく)の実施例5のZSM−5結晶を約35部の通常のUltrasil(商標)コロイダルシリカ混合物とLancasterミキサー中で混合した。十分な水を加えて、約2インチのBonnot押出機上で押出可能なペーストを形成した。実施例5のZSM−5、シリカ、および水を含有するペーストの混合物を押し出し、ホットパックオーブン中約121℃で終夜(約8〜16時間)乾燥させた。得られた押出物の圧壊強度を観測すると約125ポンド/インチであった。乾燥させた押出物を窒素中約538℃で焼成して、生成物を焼成Na型に変換した。N2焼成押出物を飽和空気で加湿し、約1N硝酸アンモニウム水溶液で交換して、ナトリウムを約500ppm未満のレベルまで除去した。硝酸アンモニウム交換の後、乾燥する前に、押出物を脱イオン水で洗浄して残留硝酸イオンを除去した。アンモニウム交換した押出物を約121℃で終夜(約8〜16時間)乾燥させ、空気中約538℃で焼成した。空気焼成後、得られたH型押出物は、約620のアルファ値を示した。
Claims (10)
- テンプレートの非存在下での高活性大結晶ZSM−5型ゼオライトの製造方法であって:
(a)水、150m2/g未満の表面積を有するシリカ源、アルミナ源、シード、アルカリ金属酸化物の供給源M及び、グルコン酸またはその塩の供給源Qを含む反応混合物を調製するステップであって、前記混合物が、40以下のSiO2/Al2O3モル比を有するステップ;
(b)前記反応混合物を約100℃〜200℃の結晶化温度で、ZSM−5の結晶を形成するために十分な時間加熱するステップ;
(c)前記反応混合物から、40以下のSiO2/Al2O3モル比を有するZSM−5の結晶を回収するステップであって、前記結晶の大部分は、少なくとも約2μmの少なくとも1つの結晶寸法を有するステップを含む、製造方法。 - 前記シリカ源が、125m2/g未満の比表面積を有する、請求項1に記載の方法。
- 前記反応混合物が:
SiO2/Al2O3:最大約40/1;
H2O/SiO2:約5〜約50;
OH−/SiO2:約0.05〜約0.5
M/SiO2;約0.05〜約0.5;および
Q/SiO2:約0.05〜約1.0
の量のモル組成を有する、請求項1または2に記載の方法。 - 前記反応混合物が、約15/1〜約40/1のSiO2/Al2O3モル比を有する、請求項1〜3のいずれかに記載の方法。
- 加熱ステップ(b)が、約2時間〜約100時間の時間で行われる、請求項1〜4のいずれかに記載の方法。
- 前記反応混合物が、前の合成で得たZSM−5シードを含有する、請求項1〜5のいずれかに記載の方法。
- 前記反応混合物が、25℃において1000cP未満の粘度を有する、請求項1〜6のいずれかに記載の方法。
- ステップ(c)で回収される前記ZSM−5が、35以下のSiO2/Al2O3モル比を有する、請求項1〜7のいずれかに記載の方法。
- 請求項1〜8のいずれかに記載の製造方法によって製造されたZSM−5。
- 転化条件下、トルエン供給材料を、請求項1〜8のいずれかに記載の製造方法によって製造された活性およびケイ素選択化型のZSM−5と接触させるステップを含む、トルエンからパラキシレンへの選択的不均化方法。
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JP2022545768A (ja) * | 2019-07-23 | 2022-10-31 | 盧敬泰 | 新規構造及びかせ状モルフォロジーを有するアルミノシリケート構造体、これの製造方法及びこれを固定相で充填したhplcカラム |
JP7204043B2 (ja) | 2019-07-23 | 2023-01-13 | 盧敬泰 | 新規構造及びかせ状モルフォロジーを有するアルミノシリケート構造体、これの製造方法及びこれを固定相で充填したhplcカラム |
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KR101858310B1 (ko) | 2018-05-15 |
JP5990594B2 (ja) | 2016-09-14 |
SG11201402190SA (en) | 2014-09-26 |
EP2785645A1 (en) | 2014-10-08 |
US8900547B2 (en) | 2014-12-02 |
WO2013081994A1 (en) | 2013-06-06 |
US20130144100A1 (en) | 2013-06-06 |
KR20140108665A (ko) | 2014-09-12 |
CN103958411B (zh) | 2016-08-24 |
CA2855875A1 (en) | 2013-06-06 |
CN103958411A (zh) | 2014-07-30 |
BR112014012577A2 (pt) | 2017-06-06 |
EP2785645B1 (en) | 2017-06-14 |
CA2855875C (en) | 2018-08-14 |
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