JP6347528B2 - ホウケイ酸塩ton−骨格型分子篩の合成 - Google Patents
ホウケイ酸塩ton−骨格型分子篩の合成 Download PDFInfo
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- 239000002808 molecular sieve Substances 0.000 title claims description 57
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims description 57
- 230000015572 biosynthetic process Effects 0.000 title description 6
- 238000003786 synthesis reaction Methods 0.000 title description 6
- 239000011541 reaction mixture Substances 0.000 claims description 27
- -1 hydroxide ions Chemical class 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 14
- 238000002425 crystallisation Methods 0.000 claims description 13
- 230000008025 crystallization Effects 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 230000000737 periodic effect Effects 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 10
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 8
- MMOXROMROKIYTR-UHFFFAOYSA-O CCCC.C[N+]1=CNC=C1 Chemical compound CCCC.C[N+]1=CNC=C1 MMOXROMROKIYTR-UHFFFAOYSA-O 0.000 claims description 7
- 229910052796 boron Inorganic materials 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 3
- MCTWTZJPVLRJOU-UHFFFAOYSA-O 1-methylimidazole Chemical compound CN1C=C[NH+]=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-O 0.000 claims 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 150000001450 anions Chemical class 0.000 description 4
- 239000000499 gel Substances 0.000 description 4
- 239000010457 zeolite Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000002178 crystalline material Substances 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 230000001627 detrimental effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 125000005842 heteroatom Chemical group 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000005216 hydrothermal crystallization Methods 0.000 description 2
- 230000001404 mediated effect Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 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 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- CDMADVZSLOHIFP-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane;decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 CDMADVZSLOHIFP-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical class [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B37/00—Compounds having molecular sieve properties but not having base-exchange properties
- C01B37/007—Borosilicates
-
- 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
- C01B39/06—Preparation of isomorphous zeolites characterised by measures to replace the aluminium or silicon atoms in the lattice framework by atoms of other elements, i.e. by direct or secondary synthesis
- C01B39/12—Preparation of isomorphous zeolites characterised by measures to replace the aluminium or silicon atoms in the lattice framework by atoms of other elements, i.e. by direct or secondary synthesis the replacing atoms being at least boron atoms
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Catalysts (AREA)
Description
一態様では、結晶化条件下で、(1)少なくとも1つのケイ素の供給源と、(2)少なくとも1つのホウ素の供給源と、(3)水酸化物イオンと、(4)1,3−ジメチルイミダゾリウムカチオン及び1,4−ビス(N−メチルイミダゾリウム)ブタンジカチオンからなる群から選択される構造規定剤とを接触させることによる、ホウケイ酸塩TON−骨格型分子篩の調製法を提供する。
(a) (1)少なくとも1つのケイ素の供給源と、(2)少なくとも1つのホウ素の供給源と、(3)周期表の1族及び2族から選択される元素の少なくとも1種の供給源と、(4)水酸化物イオンと、(5)1,3−ジメチルイミダゾリウムカチオン及び1,4−ビス(N−メチルイミダゾリウム)ブタンジカチオンからなる群から選択される構造規定剤と、(6)水とを含有する反応混合物を調製することと、
(b) 前記反応混合物を分子篩の結晶を形成するのに十分な結晶化条件下に維持すること
によりホウケイ酸塩TON−骨格型分子篩を調製する方法を提供する。
表中、Qは、1,3−ジメチルイミダゾリウムカチオン及び1,4−ビス(N−メチルイミダゾリウム)ブタンジカチオンからなる群から選択される構造規定剤であり、そして、Mは、周期表の1族及び2族の元素からなる群から選択される。
以下の用語を、明細書を通じて使用し、特に断りのない限り、以下の意味を有するものとする。
一般に、ホウケイ酸塩TON−骨格型分子篩を、
(a) (1)少なくとも1つのケイ素の供給源と、(2)少なくとも1つのホウ素の供給源と、(3)周期表の1族及び2族から選択される元素の少なくとも1種の供給源と、(4)水酸化物イオンと、(5)1,3−ジメチルイミダゾリウムカチオン及び1,4−ビス(N−メチルイミダゾリウム)ブタンジカチオンからなる群から選択される構造規定剤と、(6)水とを含有する反応混合物を調製することと、
(b) 前記反応混合物を分子篩の結晶を形成するのに十分な結晶化条件下に維持すること
によって調製する。
実際、分子篩は、(a)上記した通りに反応混合物を調製すること、及び(b)前記反応混合物を、分子篩の結晶を形成するのに十分な結晶化条件下に維持すること、により調製される。
本明細書に記載の方法により作製されたホウケイ酸塩TON−骨格型分子篩は、合成したままで且つ無水状態で、表2に(モル比換算で)記載されたような組成を有し、組成変数Q及びMは、本明細書に上記した通りである。
結晶性材料を、モル比換算で、以下の表3に示す組成を有するゲル組成物(即ち、反応混合物)を調製することにより合成した。ケイ素の供給源は、オルトケイ酸テトラエチルであった。ホウ素の供給源は、四ホウ酸ナトリウム10水和物であった。得られたゲルをParrオートクレーブに入れ、そしてオーブン中で150から160℃にて加熱した。オートクレーブを43rpmにて4から7日回転させた。その後、オートクレーブを取出し、そして室温まで冷却させた。その後、固体をろ過により回収し、そして脱イオン水で十分に洗浄した。得られた生成物を粉末X線回折により分析した。
Claims (3)
- (a)(1)少なくとも1種のケイ素の供給源と、(2)少なくとも1種のホウ素の供給源と、(3)周期表の1族及び2族から選択される元素(M)の少なくとも1種の供給源と、(4)水酸化物イオンと、(5)1,4−ビス(N−メチルイミダゾリウム)ブタンジカチオンの構造規定剤(Q)と、及び(6)水とを含有する反応混合物を調製することと、
(b)前記反応混合物を、分子篩の結晶を形成するのに十分な結晶化条件下に維持することを含む、
ホウケイ酸塩TON−骨格型分子篩を調製する方法であって、
前記分子篩が、モル比換算で、以下のものを含む前記反応混合物から調製される、方法。
表中、
(1)Mは、周期表の1族及び2族の元素からなる群から選択され、そして
(2)Qは、1,4−ビス(N−メチルイミダゾリウム)ブタンジカチオンの構造規定剤である。 - 前記分子篩が、モル比換算で、以下のものを含む反応混合物から調製される、請求項1に記載の方法。
- 前記分子篩が、合成したままで且つ無水状態にて、モル比換算で、以下のような組成を有する、請求項1に記載の方法:
表中、
(1)Qは、1,4−ビス(N−メチルイミダゾリウム)ブタンジカチオンの構造規定剤であり、そして
(2)Mは、周期表の1族及び2族の元素からなる群から選択される。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US14/051,178 US9266744B2 (en) | 2013-10-10 | 2013-10-10 | Synthesis of borosilicate ton-framework type molecular sieves |
US14/051,178 | 2013-10-10 | ||
PCT/US2014/038961 WO2015053822A1 (en) | 2013-10-10 | 2014-05-21 | Synthesis of borosilicate ton-framework type molecular sieves |
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JP2016534961A JP2016534961A (ja) | 2016-11-10 |
JP2016534961A5 JP2016534961A5 (ja) | 2017-06-29 |
JP6347528B2 true JP6347528B2 (ja) | 2018-06-27 |
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Country Status (6)
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US (1) | US9266744B2 (ja) |
EP (1) | EP3055251B1 (ja) |
JP (1) | JP6347528B2 (ja) |
CN (1) | CN105636905B (ja) |
SG (1) | SG11201602757WA (ja) |
WO (1) | WO2015053822A1 (ja) |
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US9266744B2 (en) * | 2013-10-10 | 2016-02-23 | Chevron U.S.A. Inc. | Synthesis of borosilicate ton-framework type molecular sieves |
CN110662716B (zh) * | 2017-06-05 | 2022-11-04 | 雪佛龙美国公司 | Sfe骨架型分子筛的合成 |
JP7097950B2 (ja) * | 2018-02-20 | 2022-07-08 | シェブロン ユー.エス.エー. インコーポレイテッド | 分子ふるいssz-113、その合成および使用 |
JP7119128B2 (ja) * | 2018-06-07 | 2022-08-16 | シェブロン ユー.エス.エー. インコーポレイテッド | モレキュラーシーブssz-109の合成 |
KR102689243B1 (ko) * | 2018-08-27 | 2024-07-30 | 셰브런 유.에스.에이.인크. | 분자체 ssz-56의 합성 |
CN111422881B (zh) * | 2020-04-10 | 2021-11-05 | 吉林大学 | 一种ton型沸石分子筛及其制备方法 |
CN115475655B (zh) * | 2021-05-31 | 2024-04-05 | 中国石油化工股份有限公司 | 含硼Silicate-1分子筛催化剂及其制备方法和制备己内酰胺的方法 |
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2013
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EP3055251B1 (en) | 2018-07-11 |
EP3055251A1 (en) | 2016-08-17 |
CN105636905B (zh) | 2018-01-05 |
US9266744B2 (en) | 2016-02-23 |
CN105636905A (zh) | 2016-06-01 |
SG11201602757WA (en) | 2016-05-30 |
US20150104378A1 (en) | 2015-04-16 |
WO2015053822A1 (en) | 2015-04-16 |
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