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Process for synthesizing microporous titanium silicon fluorite ETS-10

A synthesis method, silicalite technology, applied in the direction of crystalline aluminosilicate zeolite, etc., to achieve the effect of simple method, simple synthesis system and high crystallinity

Inactive Publication Date: 2007-06-13
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are also studies reporting the use of Ti without the addition of fluoride ions, organic templates, and 2 (SO 4 ) 3 、TiCl 3 、TiO 2 ETS-10 is synthesized as a titanium source, but under this condition the product contains titanium dioxide impurities (Micopor.Mesopor.Mater., 2004, 67, 181; Micopor.Mesopor.Mater., 2004, 76, 113; Stud.Surf. Sci. Catal., 2004, 154, 770.)

Method used

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  • Process for synthesizing microporous titanium silicon fluorite ETS-10
  • Process for synthesizing microporous titanium silicon fluorite ETS-10

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Dissolve 6.00 grams of NaOH and 3.90 grams of KOH in 8.0 mL of distilled water, and then slowly add the resulting solution to 30.28 grams of sodium silicate solution (industrial water glass) to obtain a clear solution A; under vigorous stirring, 4.75 grams of TiCl 4 Slowly add 10.0mL of distilled water to prevent TiCl 4 The hydrolysis is too fast, and the temperature of the solution must be kept below 10°C with an ice-water bath, and a light yellow clear solution B is obtained. Under vigorous stirring, add solution B dropwise to solution A. After the addition, the pH value of the solution is about 11.5, and then adjust the pH value to 10.4-10.5 with concentrated hydrochloric acid, and transfer the obtained colloid into a polytetrafluoroethylene-lined hydrothermal In the kettle, crystallize at 230°C for 36 hours, cool naturally, filter the obtained product with suction, wash with distilled water, and dry at 100°C. BET measurement results product specific surface area 34...

Embodiment 2

[0021] Dissolve 6.40 g of NaOH and 4.20 g of KOH in 10.0 mL of distilled water, and then slowly add the resulting solution into 32.03 g of sodium silicate solution (water glass) to obtain a clear solution A; under vigorous stirring, 4.75 g of TiCl 4 Slowly add 8.0 mL of distilled water, and keep the temperature of the solution below 10°C with an ice-water bath during the addition, to obtain a pale yellow clear solution B. Under vigorous stirring, add solution B dropwise to solution A. After the addition, the pH value of the solution is about 11.5, and then adjust the pH value to 10.4-10.5 with concentrated hydrochloric acid, and transfer the obtained colloid into a polytetrafluoroethylene-lined hydrothermal In the kettle, crystallize at 200°C for 24 hours, cool naturally, filter the obtained product with suction, wash with distilled water, and dry at 100°C. BET measurement results product specific surface area 357.1m 2 / g, the pore volume is 0.172cm 3 / g.

Embodiment 3

[0023] Dissolve 6.40 g of NaOH and 4.20 g of KOH in 10.0 mL of distilled water, and then slowly add the resulting solution into 33.78 g of sodium silicate solution (water glass) to obtain a clear solution A; under vigorous stirring, 4.75 g of TiCl 4 Slowly add 10.0 mL of distilled water, and keep the temperature of the solution below 10°C with an ice-water bath during the addition, to obtain a light yellow clear solution B. Under vigorous stirring, add solution B dropwise to solution A. After the addition, the pH value of the solution is about 11.5, and then adjust the pH value to 10.4-10.5 with concentrated hydrochloric acid, and transfer the obtained colloid into a polytetrafluoroethylene-lined hydrothermal In the kettle, crystallize at 230°C for 36 hours, cool naturally, filter the obtained product with suction, wash with distilled water, and dry at 100°C. BET measurement results product specific surface area 364.8m 2 / g, the pore volume is 0.180cm 3 / g.

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Abstract

A process for synthesizing the milli-porous TiSi zeolite ETS-10 features that the inorganic Ti source and inorganic Si source take part in hydrothermal synthesis reaction in alkaline aqueous solution without organic template, F ions and crystal seeds.

Description

technical field [0001] The invention belongs to the technical field of inorganic molecular sieves, and in particular relates to a synthesis method of microporous titanium silicalite ETS-10. Background technique [0002] ETS-10 is a titanium silicalite with a unique microporous structure, the molecular formula is (NaK) 2 Si 5 TiO 13 . Kuznicki first reported the synthesis of this titanium silicalite in 1989 (US patent 4853202). Studies have shown that in this zeolite structure, there are two groups of one-dimensional long chains perpendicular to each other formed by the sharing of vertices of titanium-oxygen octahedra, and the long chains are wrapped in the pore structure composed of silicon-oxygen tetrahedrons. The framework of ETS-10 has three-membered, five-membered, seven-membered and twelve-membered rings, and the diameter of micropores composed of twelve-membered rings is about 7.6×4.9 Ȧ (Nature, 1994, 367, 347). Therefore, the structure of ETS-10 can be regarded a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/02
Inventor 岳斌周琰江磊闫世润贺鹤勇
Owner FUDAN UNIV
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