JP2015221746A - シリカゲル系触媒担体 - Google Patents
シリカゲル系触媒担体 Download PDFInfo
- Publication number
- JP2015221746A JP2015221746A JP2015121907A JP2015121907A JP2015221746A JP 2015221746 A JP2015221746 A JP 2015221746A JP 2015121907 A JP2015121907 A JP 2015121907A JP 2015121907 A JP2015121907 A JP 2015121907A JP 2015221746 A JP2015221746 A JP 2015221746A
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- bead
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- metal
- spherical beads
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000003054 catalyst Substances 0.000 title claims abstract description 21
- 239000000741 silica gel Substances 0.000 title description 16
- 229910002027 silica gel Inorganic materials 0.000 title description 16
- 239000011324 bead Substances 0.000 claims abstract description 109
- 229910052751 metal Inorganic materials 0.000 claims abstract description 37
- 239000002184 metal Substances 0.000 claims abstract description 37
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 239000011148 porous material Substances 0.000 claims abstract description 14
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- 239000002253 acid Substances 0.000 claims description 29
- 229910052752 metalloid Inorganic materials 0.000 claims description 28
- 150000002738 metalloids Chemical class 0.000 claims description 28
- 239000003960 organic solvent Substances 0.000 claims description 22
- 150000001875 compounds Chemical class 0.000 claims description 20
- 239000002243 precursor Substances 0.000 claims description 18
- 239000012074 organic phase Substances 0.000 claims description 14
- 239000008346 aqueous phase Substances 0.000 claims description 13
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 10
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 235000019353 potassium silicate Nutrition 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 6
- 239000004115 Sodium Silicate Substances 0.000 claims description 5
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052910 alkali metal silicate Inorganic materials 0.000 claims description 4
- 239000004111 Potassium silicate Substances 0.000 claims description 3
- 229910052915 alkaline earth metal silicate Inorganic materials 0.000 claims description 3
- 239000008119 colloidal silica Substances 0.000 claims description 3
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 3
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 2
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims 1
- 229910052906 cristobalite Inorganic materials 0.000 claims 1
- 229910052682 stishovite Inorganic materials 0.000 claims 1
- 229910052905 tridymite Inorganic materials 0.000 claims 1
- 239000000969 carrier Substances 0.000 abstract 1
- 239000002685 polymerization catalyst Substances 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 22
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 15
- 239000002245 particle Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 239000012798 spherical particle Substances 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000010908 decantation Methods 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- -1 polypropylene Polymers 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 3
- 239000007809 chemical reaction catalyst Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- 235000011054 acetic acid Nutrition 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000011260 aqueous acid Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 239000000017 hydrogel Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 235000019260 propionic acid Nutrition 0.000 description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000008399 tap water Substances 0.000 description 2
- 235000020679 tap water Nutrition 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 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
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000012644 addition polymerization Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000004375 physisorption Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
Description
(A)少なくとも一種の少なくとも部分的に水混和性の有機溶媒と水と少なくとも一種の金属及び/又は半金属酸化物の少なくとも一種の前駆化合物とを含む混合物を、混合物Aとして提供する工程と、
(B)少なくとも一種の少なくとも部分的に水混和性の有機溶媒と水と少なくとも一種の酸とを含む混合物を、混合物Bとして提供する工程と、
(C)該混合物AとBとを混合して、上記少なくとも一種の金属及び/又は半金属酸化物の少なくとも一種の前駆化合物を上記少なくとも一種の酸と反応させて、球状ビーズを含む水相と有機相とを含む混合物Cを得る工程と、
(D)工程Cで得られる混合物Cから有機相を分離して球状ビーズを含む水相を得る工程と、
(E)必要に応じて、工程(D)で得られる球状ビーズを少なくとも一種の酸で処理する工程と、
(F)(F)工程(D)または(E)で得られる球状ビーズを乾燥する工程とからなる本発明の球状ビーズの製造方法により達成されることを見出した。
工程(A)は、少なくとも一種の少なくとも部分的に水混和性の有機溶媒と水と少なくとも一種の少なくとも一種の金属及び/又は半金属酸化物の前駆化合物とからなる混合物を、混合物Aとして供給することからなる。
蒸留水の使用が好ましい。
本発明の方法のある好ましい実施様態においては、この少なくとも一種の金属及び/又は半金属酸化物の少なくとも一種の前駆化合物が、ケイ酸カリウム及び/又はケイ酸ナトリウムなどおのアルカリ金属ケイ酸塩、アルカリ土類金属ケイ酸塩、コロイダルシリカ、およびこれらの混合物からなる群から選ばれる。
本発明の方法の工程(B)は、少なくとも一種の少なくとも部分的に水混和性の有機溶媒と水と少なくとも一種の酸を含む混合物を、混合物Bとして与えることからなる。
工程(C)は、混合物AとBとを混合し、その少なくとも一種の金属及び/又は半金属酸化物の少なくとも一種の前駆化合物に少なくとも一種の酸を反応させて、球状ビーズを含む水相と有機相とからなる混合物Cを得ることからなる。
xNa2O・ySiO2+H2SO4(aq.)→SiO2+Na2SO4+H2O
工程(D)は、工程(C)で得られた混合物Cから有機相を分離し、球状ビーズを含む水相を得ることからなる。
本発明の方法の任意の工程(E)は、工程(D)で得られる球状ビーズを少なくとも一種の酸で処理することからなる。
本発明の方法の工程(F)は、工程(D)または(E)で得られる球状ビーズを乾燥することからなる。
− 二台のブッデベルグ社製のPLR−11T型の防爆型圧縮空気攪拌器
− 二台のビスコジェット120mm攪拌装置
− 二台の冷却水と保護ガス供給口とを持つ10リットルのジャケット付きガラス反応器
− 上記の二台のジャケット付きガラス反応器に初めに投入される物質の混合用の二流路ぜん動ポンプ、
− 数個の10リットル受器
− 10リットルのガラス瓶
1. 2リットルの5.2%硫酸
2. 2リットルの水ガラス溶液(密度:1.269g/cm3)
3. 12リットルのn−ブタノール、工業グレード、水で飽和
4. 中和用の約40%の硫酸
5. 約10リットルの1%硫酸
沈澱化:
ジャケット付き反応器をそれぞれ6リットルのn−ブタノールで満たした後、攪拌器を約500rpmに調整する。次いで、上記希硫酸を一つの容器に投入し、水ガラス溶液を他の容器に投入する。添加と乳化が終了後、両方共に攪拌器速度を約300rpmに低下させる。ポンプを用いて、これらの得られたエマルジョンを、受器からチューブ中に取り出し、可動型の受器に移す。
中和後のシリカゲルを10リットルのガラス瓶に入れ、80℃の温水浴に約2.5時間移す。
シリカゲルの上の液体を吸引で除いた後、1%のH2SO4溶液(0.5〜15%を超える広い濃度範囲が可能)を添加する。1時間後、この上澄液をもう一度吸引除去し、シリカゲルをもう一度、1%のH2SO4溶液と混合する。この操作を5回繰り返し、最後にシリカゲルを水と混合する。この操作を繰り返す。
このシリカゲルを乾燥キャビネット中で170℃で乾燥させる。
球状粒子の化学組成(XRFを用いDIN51418により測定):
SiO2>98%
微量のAl、Na、Fe、硫酸、塩化物(それぞれ<0.01%)
色:白色
嵩密度:0.18kg/l(DIN8948/7.6により測定)
すべてのデータは、ふるい分けしていない非分級材料のものである:
D10=16μm
D50=55μm
D90=96μm
BET表面積(乾燥ヒドロゲル):550m2/g
乾燥ヒドロゲルの気孔体積:1.7cm3/g
(A)少なくとも一種の少なくとも部分的に水混和性の有機溶媒と水と少なくとも一種の金属及び/又は半金属酸化物の少なくとも一種の前駆化合物とを含む混合物を、混合物Aとして提供する工程と、
(B)少なくとも一種の少なくとも部分的に水混和性の有機溶媒と水と少なくとも一種の酸とを含む混合物を、混合物Bとして提供する工程と、
(C)該混合物AとBとを混合して、上記少なくとも一種の金属及び/又は半金属酸化物の少なくとも一種の前駆化合物を上記少なくとも一種の酸と反応させて、球状ビーズを含む水相と有機相とを含む混合物Cを得る工程と、
(D)工程Cで得られる混合物Cから有機相を分離して球状ビーズを含む水相を得る工程と、
(E)必要に応じて、工程(D)で得られる球状ビーズを少なくとも一種の酸で処理する工程と、
(F)(F)工程(D)または(E)で得られる球状ビーズを乾燥する工程と、
を含む本発明の球状ビーズの製造方法により達成されることを見出した。
Claims (10)
- 平均径が10〜120μmの範囲にあり、BET表面積が400〜800m2/gの範囲にあり、気孔体積が0.3〜3.0cm3/gの範囲にある、少なくとも一種の金属及び/又は半金属酸化物を含む球状ビーズであって、あるビーズのいずれの位置でのビーズ径も該ビーズの平均径から10%以上相違することがなく、該ビーズの表面が実質的に平滑であることを特徴とするビーズ。
- 上記少なくとも一種の金属及び/又は半金属酸化物がSiO2やAl2O3、TiO2、MgO、およびこれらの混合物からなる群から選ばれる請求項1に記載のビーズ。
- SiO2を少なくとも96重量%の量で含む請求項1または2に記載のビーズ。
- 上記少なくとも一種の金属及び/又は半金属酸化物が実質的に非晶質である請求項1〜3のいずれか一項に記載のビーズ。
- BET表面積が500〜600m2/gの範囲にある請求項1〜4のいずれか一項に記載のビーズ。
- 気孔体積が1.5〜2.5cm3/gの範囲にある請求項1〜5のいずれか一項に記載のビーズ。
- (A)少なくとも一種の少なくとも部分的に水混和性の有機溶媒と水と少なくとも一種の金属及び/又は半金属酸化物の少なくとも一種の前駆化合物とを含む混合物を、混合物Aとして提供する工程と、
(B)少なくとも一種の少なくとも部分的に水混和性の有機溶媒と水と少なくとも一種の酸とを含む混合物を、混合物Bとして提供する工程と、
(C)該混合物AとBとを混合して、上記少なくとも一種の金属及び/又は半金属酸化物の少なくとも一種の前駆化合物を上記少なくとも一種の酸と反応させて、球状ビーズを含む水相と有機相とを含む混合物Cを得る工程と、
(D)工程Cで得られる混合物Cから有機相を分離して球状ビーズを含む水相を得る工程と、
(E)必要に応じて、工程(D)で得られる球状ビーズを少なくとも一種の酸で処理する工程と、
(F)工程(D)または(E)で得られる球状ビーズを乾燥する工程とからなる請求項1〜6のいずれか一項に記載のビーズの製造方法。 - 前記少なくとも一種の金属及び/又は半金属酸化物の少なくとも一種の前駆化合物が、ケイ酸カリウム及び/又はケイ酸ナトリウムなどのアルカリ金属ケイ酸塩とアルカリ土類金属ケイ酸塩、コロイダルシリカゾル、およびこれらの混合物からなる群から選ばれる請求項7に記載の方法。
- 請求項1〜6のいずれか一項に記載の球状ビーズと少なくとも一種の触媒的に活性な金属とを含むことを特徴とする粒子状触媒。
- 請求項1〜6のいずれか一項に記載の球状ビーズの触媒または触媒担体としての利用。
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WO2019049839A1 (en) | 2017-09-05 | 2019-03-14 | Showa Denko K.K. | PROCESS FOR PRODUCING SILICA SUPPORT AND SILICA SUPPORT |
US10919836B2 (en) | 2017-09-05 | 2021-02-16 | Showa Denko K.K. | Production method of aliphatic carboxylic acid ester |
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CN103464216B (zh) * | 2013-09-26 | 2015-08-19 | 中国海洋石油总公司 | 醋酸与丁烯合成醋酸仲丁酯杂多酸催化剂硅胶载体的制法 |
US9745201B2 (en) | 2014-01-29 | 2017-08-29 | Mitsubishi Materials Corporation | Synthetic amorphous silica powder and process for manufacturing same |
JP6714989B2 (ja) | 2015-01-19 | 2020-07-01 | 国立大学法人秋田大学 | 排ガス浄化触媒用担体及び排ガス浄化触媒 |
FR3065649B1 (fr) * | 2017-04-28 | 2020-05-29 | IFP Energies Nouvelles | Monolithe poreux contenant du tio2 et son procede de preparation |
WO2023178116A1 (en) * | 2022-03-16 | 2023-09-21 | W. R. Grace & Co.-Conn | Silica-supported polyolefin catalyst system |
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WO2019049839A1 (en) | 2017-09-05 | 2019-03-14 | Showa Denko K.K. | PROCESS FOR PRODUCING SILICA SUPPORT AND SILICA SUPPORT |
US10919836B2 (en) | 2017-09-05 | 2021-02-16 | Showa Denko K.K. | Production method of aliphatic carboxylic acid ester |
US11890592B2 (en) | 2017-09-05 | 2024-02-06 | Resonac Corporation | Method for producing silica carrier, and silica carrier |
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US20130165608A1 (en) | 2013-06-27 |
EP2408554A1 (de) | 2012-01-25 |
WO2010105941A1 (de) | 2010-09-23 |
US8986642B2 (en) | 2015-03-24 |
RU2011141701A (ru) | 2013-04-27 |
RU2522595C2 (ru) | 2014-07-20 |
EP2408554B1 (de) | 2016-12-14 |
JP6035380B2 (ja) | 2016-11-30 |
CN102355946B (zh) | 2014-06-11 |
KR20110130450A (ko) | 2011-12-05 |
US20120010379A1 (en) | 2012-01-12 |
CA2755648A1 (en) | 2010-09-23 |
JP2012520236A (ja) | 2012-09-06 |
CN102355946A (zh) | 2012-02-15 |
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