JP5767978B2 - 同形置換されたケイ酸塩 - Google Patents
同形置換されたケイ酸塩 Download PDFInfo
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Description
同形置換されたRUB−36層状ケイ酸塩の製造方法であって、
(1)シリカ、好ましくは非晶質シリカ、及び/又は少なくとも一種のシリカ前駆体と、水と、ジエチルジメチルアンモニウム化合物、トリエチルメチルアンモニウム化合物、およびジエチルジメチルアンモニウムとトリエチルメチルアンモニウム化合物との混合物からなる群から選ばれる少なくとも一種のテトラアルキルアンモニウム化合物と、必要に応じて少なくとも一種の塩基とを含む混合物を供給する工程、
(2)(1)で得られる混合物を水熱条件下で加熱して、RUB−36ケイ酸塩を含む懸濁液を与える工程、
(3)(2)により得られる懸濁液からRUB−36ケイ酸塩を分離し、必要に応じて(4)洗浄及び/又は(5)乾燥する工程
を含み、且つ
(a)(1)の混合物が、ケイ酸塩中のSi原子の少なくとも一部を同形置換するのに好適な少なくとも一種の元素の少なくとも一種の供給源を含み、及び/又は
(b)(3)において分離された、また必要に応じて洗浄及び/又は乾燥されたRUB−36ケイ酸塩)を後処理し、ケイ酸塩中のSi原子の少なくとも一部を少なくとも一種の好適な元素で同形置換することを特徴とする製造方法に関する。
(4)洗浄
及び/又は
(5)乾燥する上述の方法に関する。
(4)分離されたケイ酸塩を好ましくは6.5〜7.5の範囲のpHまで洗浄し、及び/又は
(5)分離され必要に応じて洗浄されたケイ酸塩を、好ましくは75〜125℃の範囲の温度で乾燥することからなる上述の方法に関する。
(6)(3)または(4)または(5)で得られるケイ酸塩を、好ましくは300〜700℃の範囲の、より好ましくは400〜600℃の範囲の温度で焼成する上述の方法に関する。
(II)該混合物を混練し、
(III)混練混合物を成型して、少なくとも一種の成型物を与え、
(IV)該少なくとも一種の成型物を乾燥させ、
(V)該少なくとも一種の乾燥成型物を焼成する。
349.8gのジエチルジメチルアンモニウムヒドロキシド(20.62重量%)水溶液を評量してビーカーに入れ、そこに72.7gの非晶質シリカ(アエロジル(R))を少しずつ加え、混合物を30分間攪拌した。次いで、3.6gのRUB−36を種結晶として加え、混合物を1時間攪拌した。
実施例1で得られたTi−RUB−36材料を大気下で焼成した。焼成温度は500℃であり、このケイ酸塩を1℃/分の速度で加熱してこの温度まで調整した。500℃の温度に5時間維持した。
5.434gのジエチルジメチルアンモニウムヒドロキシド(21.9重量%)水溶液を評量してビーカーに入れ、そこに1.2gのヒュームドシリカを少しずつ添加し、混合物を30分間攪拌した。0.036gのRUB−36を種結晶として添加し、混合物を1時間攪拌し、その後0.024gのホウ酸をこの混合物に加えた。得られた懸濁液を圧力消化容器に移し、この中で140℃の水熱条件下で8日間(192時間)加熱した。
Claims (29)
- 同形置換されたRUB−36層状ケイ酸塩の製造方法であって、
(1)シリカ、及び/又は少なくとも一種のシリカ前駆体と、水と、
ジエチルジメチルアンモニウム化合物、トリエチルメチルアンモニウム化合物、およびジエチルジメチルアンモニウムとトリエチルメチルアンモニウム化合物との混合物からなる群から選ばれる少なくとも一種のテトラアルキルアンモニウム化合物と、必要に応じて少なくとも一種の塩基とを含む混合物を供給する工程、
(2)(1)で得られる混合物を水熱条件下で加熱して、RUB−36ケイ酸塩を含む懸濁液を与える工程、
(3)(2)により得られる懸濁液からRUB−36ケイ酸塩を分離し、必要に応じて
(4)洗浄及び/又は(5)乾燥する工程
を含み、且つ
(a)(1)の混合物が、ケイ酸塩中のSi原子の少なくとも一部を同形置換するのに好適な少なくとも一種の元素の少なくとも一種の供給源を含むことを特徴とする製造方法。 - (b)(3)において分離された、また必要に応じて洗浄及び/又は乾燥されたRUB−36ケイ酸塩を、後処理が行われる工程に付し、ケイ酸塩中のSi原子の少なくとも一部を同形置換するのに好適な少なくとも一種の元素で同形置換する請求項1に記載の方法。
- 前記同形置換に好適な少なくとも一種の元素が、Al、B、Fe、Ti、Sn、Ga、Ge、Zr、V、Nb、およびこれらの二種以上の混合物からなる群から選ばれる請求項1または2に記載の方法。
- (1)の水混合物が、ジエチルジメチルアンモニウムヒドロキシド、トリエチルメチルアンモニウムヒドロキシド、またはジエチルジメチルアンモニウムヒドロキシドとトリエチルメチルアンモニウムヒドロキシドの混合物を含む請求項1〜3のいずれか1項に記載
の方法。 - 非晶質シリカが(1)で使用される請求項1〜4のいずれか一項に記載の方法。
- (1)により得られる混合物が、SiO2またはSiO2として計算されるシリカ前駆体、少なくとも一種のテトラアルキルアンモニウム化合物、及び水を、SiO2:テトラアルキルアンモニウム化合物:水のモル比で1:(0.45〜0.55):(0.5〜20)で含む請求項1〜5のいずれか一項に記載の方法。
- (1)により得られる混合物が、少なくとも一種の適当な種結晶材料を含む請求項1〜6のいずれか一項に記載の方法。
- (1)により得られる混合物が、SiO2及び/又はSiO2として計算されるシリカ前駆体と種結晶材料とを、質量比で1:(0.01〜0.2)で含む請求項7に記載の方法。
- (2)の混合物を1〜18日間の範囲の期間加熱する請求項1〜8のいずれか一項に記載の方法。
- (2)の混合物を135〜145℃の範囲の温度に加熱する請求項1〜9のいずれか一項に記載の方法。
- さらに、
(4)当該分離されたケイ酸塩を洗浄し、及び/又は
(5)当該分離され、必要に応じて洗浄されたケイ酸塩を乾燥する請求項1〜10のいずれか一項に記載の方法。 - (1)の反応混合物中のSiO2及び/又はSiO2として計算されるシリカ前駆体と同形置換に好適な少なくとも一種の元素(1)のモル比が、1:(0.0001〜0.1)である請求項1〜11のいずれか一項に記載の方法。
- (1)において用いられる水混合物がさらに過酸化水素を含む請求項12に記載の方法。
- 前記同形置換に好適な少なくとも一種の元素がTiであり、少なくとも一つのTi:過酸化水素のモル比が0.005〜0.01の範囲にある請求項13に記載の方法。
- Tiの供給源が、テトラアルキルオルソチタネートまたは2つ以上のテトラアルキルオルソチタネートの混合物である請求項14記載の方法。
- 前記後処理が、分離の直後に、または必要に応じて洗浄及び/又は乾燥の直後に行われる請求項2〜15のいずれか一項に記載の方法。
- (6)(3)または(4)または(5)で得られるケイ酸塩を焼成する工程を更に含む請求項1〜16のいずれか一項に記載の方法。
- 請求項1〜16のいずれか一項に記載の方法により得られる同形置換されたRUB−36ケイ酸塩。
- ケイ酸塩中のSi原子の少なくとも一部が少なくとも一種の適当な元素で同形置換されたRUB−36ケイ酸塩。
- 前記少なくとも一種の適当な元素が、Al、B、Fe、Ti、Sn、Ga、Ge、Zr、V、Nb、およびこれらの二種以上の混合物からなる群から選ばれる請求項18または19に記載のケイ酸塩。
- 前記層状ケイ酸塩中のSi:適当な元素の原子比が、1:(0.0001〜0.1)の範囲である請求項18〜20のいずれか一項に記載のRUB−36ケイ酸塩。
- 請求項17に記載の方法によって得られる同形置換されたRUB−37ケイ酸塩。
- ケイ酸塩中のSi原子の少なくとも一部が少なくとも一種の適当な元素で同形置換されたRUB−37ケイ酸塩。
- 層状ケイ酸塩中のSi:適当な元素の原子比が、1:(0.0001〜0.1)の範囲である請求項23〜24のいずれか一項に記載のRUB−37ケイ酸塩。
- DIN66135により求めたBET表面積が、150〜500m2/gの範囲にある請求項23〜26のいずれか一項に記載のケイ酸塩。
- 成型物中に含まれる請求項18〜27のいずれか一項に記載のケイ酸塩。
- 請求項18〜28のいずれか一項に記載のケイ酸塩の、モレキュラーシーブ、触媒、触媒支持体またはそのバインダー、吸着剤、顔料、洗剤の添加物、建材の添加物としての、塗装用ペーストや仕上げ剤にチキソトロピー性を与えるための外部および内部潤滑剤としての、難燃剤、紙状物の助剤や充填材としての、殺菌及び/又は殺真菌及び/又は除草剤組成物中での、イオン交換のための、セラミックスの製造のための、ポリマー中での、電気的、光学的または電気光学的部品や開閉素子またはセンサーとしての使用方法。
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PCT/EP2010/052699 WO2010100193A2 (en) | 2009-03-03 | 2010-03-03 | Isomorphously substituted silicate |
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PL2512667T3 (pl) | 2009-12-18 | 2018-04-30 | Basf Se | Zawierający żelazo zeolit, sposób wytwarzania zawierających żelazo zeolitów i sposób katalitycznej redukcji tlenków azotu |
US10850265B2 (en) | 2014-06-18 | 2020-12-01 | Basf Corporation | Molecular sieve catalyst compositions, catalytic composites, systems, and methods |
US9764313B2 (en) | 2014-06-18 | 2017-09-19 | Basf Corporation | Molecular sieve catalyst compositions, catalyst composites, systems, and methods |
US9889437B2 (en) | 2015-04-15 | 2018-02-13 | Basf Corporation | Isomorphously substituted catalyst |
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