JP2021526118A - Zsm‐5系ゼオライトの製造方法 - Google Patents
Zsm‐5系ゼオライトの製造方法 Download PDFInfo
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- 239000010457 zeolite Substances 0.000 title claims abstract description 75
- 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 68
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 64
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 70
- 239000012452 mother liquor Substances 0.000 claims abstract description 61
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 150000003839 salts Chemical class 0.000 claims abstract description 25
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 23
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 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
- 239000011734 sodium Substances 0.000 claims description 12
- 238000002425 crystallisation Methods 0.000 claims description 8
- 230000008025 crystallization Effects 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000004215 Carbon black (E152) Substances 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 229930195733 hydrocarbon Natural products 0.000 claims description 4
- 150000002430 hydrocarbons Chemical class 0.000 claims description 4
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 4
- 150000002894 organic compounds Chemical class 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 3
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 9
- 230000003472 neutralizing effect Effects 0.000 abstract description 9
- 239000000243 solution Substances 0.000 description 61
- 238000003786 synthesis reaction Methods 0.000 description 34
- 230000015572 biosynthetic process Effects 0.000 description 33
- 239000013078 crystal Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 11
- 238000002347 injection Methods 0.000 description 11
- 239000007924 injection Substances 0.000 description 11
- 230000003287 optical effect Effects 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 238000011084 recovery Methods 0.000 description 8
- 229910004298 SiO 2 Inorganic materials 0.000 description 7
- 239000000499 gel Substances 0.000 description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 235000019353 potassium silicate Nutrition 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 229910000323 aluminium silicate Inorganic materials 0.000 description 3
- 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 3
- 239000002245 particle Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 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 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000010669 acid-base reaction Methods 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000007848 Bronsted acid Substances 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052680 mordenite Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000012066 reaction slurry Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- -1 specifically Chemical compound 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C01B39/36—Pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11
- C01B39/38—Type ZSM-5
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Abstract
Description
[式1]
0.20≦Wa/Wb≦0.40
前記式1中、Waは前記反応母液内の塩の含有量であり、Wbは前記反応母液内のシリカの含有量である。
[式2]
0.22≦Wa/Wb≦0.32
前記式1中、Waは前記反応母液内の塩の含有量であり、Wbは前記反応母液内のシリカの含有量である。
0.20≦Wa/Wb≦0.40
0.20≦Wa/Wb≦0.40
0.22≦Wa/Wb≦0.32
(ステップ1)シリカ源である水ガラス(SiO2=20wt%、Na2O=6wt%)29kgに蒸留水23kgを添加して30分間撹拌した後、結晶性ZSM‐5核を0.4kgを添加した溶液に、アルミニウム塩(Al2O3=8wt%)3.1kg、硫酸0.9kgおよび蒸留水23kgを30分間撹拌して混合した溶液を添加し、1時間維持して第1溶液を製造した。この際、前記第1溶液のゲル化を防ぐために、第1溶液を60℃に加熱して水溶液状態に製造した。
実施例1のステップ2で第1溶液50kgに第2溶液50kgを添加した以外は、実施例1と同じ方法でゼオライトを製造した。
実施例1のステップ2で第1溶液60kgに第2溶液40kgを添加した以外は、実施例1と同じ方法でゼオライトを製造した。
実施例1のステップ2で第1溶液5kgに第2溶液95kgを添加した以外は、実施例1と同じ方法でゼオライトを製造した。
実施例1のステップ2で第1溶液10kgに第2溶液90kgを添加した以外は、実施例1と同じ方法でゼオライトを製造した。
実施例1のステップ2で第1溶液20kgに第2溶液80kgを添加した以外は、実施例1と同じ方法でゼオライトを製造した。
実施例1のステップ2で第1溶液70kgに第2溶液30kgを添加した以外は、実施例1と同じ方法でゼオライトを製造した。
実施例1のステップ2で第1溶液80kgに第2溶液20kgを添加した以外は、実施例1と同じ方法でゼオライトを製造した。
実施例1のステップ2で残りの液を添加することなく、第1溶液100kgを使用した以外は、実施例1と同じ方法でゼオライトを製造した。
Claims (11)
- シリカ源、アルミナ源、中和剤、および結晶性ZSM‐5核を含む混合物を加熱し、溶液状態の第1溶液を製造するステップと、
前記第1溶液に塩を含む第2溶液を混合し、反応母液を製造するステップと、
前記反応母液を水熱合成反応器に連続して供給し、連続結晶化するステップとを含み、
下記式1を満たす、ZSM‐5系ゼオライトの製造方法。
[式1]
0.20≦Wa/Wb≦0.40
(前記式1中、Waは、前記反応母液内の塩の含有量であり、Wbは、前記反応母液内のシリカの含有量である。) - 前記第1溶液を製造するステップにおける加熱温度は30〜60℃であり、加熱時間は1〜3時間である、請求項1に記載のZSM‐5系ゼオライトの製造方法。
- 前記塩は、硫酸ナトリウム(Na2SO4)、硝酸ナトリウム(NaNO3)、トリナトリウムホスフェート(Na3PO4)、またはこれらの組み合わせを含む、請求項1に記載のZSM‐5系ゼオライトの製造方法。
- 前記水熱合成反応器は、連続撹拌槽型反応器(Continuous Stirred‐Tank Reactor、CSTR)、またはプラグフロー反応器(Plug Flow Reactor、PFR)である、請求項1に記載のZSM‐5系ゼオライトの製造方法。
- 前記第2溶液は、前記水熱合成反応器の未反応の残りの液である、請求項1に記載のZSM‐5系ゼオライトの製造方法。
- 前記反応母液を製造するステップにおいて、前記第2溶液が前記水熱合成反応器の前端に再循環し、前記第1溶液と混合される、請求項5に記載のZSM‐5系ゼオライトの製造方法。
- 前記連続結晶化するステップにおける反応温度は150〜200℃である、請求項1に記載のZSM‐5系ゼオライトの製造方法。
- 前記反応母液の粘度は1000〜2700cPである、請求項1に記載のZSM‐5系ゼオライトの製造方法。
- 前記式1は、下記式2を満たす、請求項1に記載のZSM‐5系ゼオライトの製造方法。
[式2]
0.22≦Wa/Wb≦0.32
(前記式1中、Waは、前記反応母液内の塩の含有量であり、Wbは、前記反応母液内のシリカの含有量である。) - 請求項1に記載の製造方法により製造されたZSM‐5系ゼオライト。
- 請求項10に記載のZSM‐5系ゼオライトを用いて、炭化水素、酸素含有有機化合物、またはこれらの混合物から軽質オレフィンを製造する方法。
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