Method for synthesizing ITQ-13 molecular sieve

A technology of ITQ-13, synthesis method, applied in molecular sieve and alkali exchange compound, molecular sieve catalyst, molecular sieve characteristic polymorphic crystalline silicon, etc., can solve the problems of poor repeatability and cumbersome steps

Inactive Publication Date: 2008-10-01
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

[0007] The purpose of the present invention is to provide a simple and easy method for synthesizing pure silicon and silicon-aluminum ITQ-13 molecular sieves, which can overcome the shortcomings of previous synthesis methods that are difficult to directly synthesize silicon-aluminum ITQ-13 molecular sieves, and the steps are cumbersome and poor in repeatability.

Method used

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  • Method for synthesizing ITQ-13 molecular sieve

Examples

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Comparison scheme
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Embodiment 1

[0027] (1) Preparation of template solution

[0028] Add 36g of 1,6-dibromohexane (96wt%) and 80g of trimethylamine solution (31-35wt% ethanol solution) into a 500ml three-necked flask, and quickly add an appropriate amount of ethanol under magnetic stirring. Continuously stirred at room temperature for 48 hours and the reaction was complete, and the resulting white precipitate (hexylbisammonium dibromide, RBr 2 ) was filtered and washed well with ethyl acetate and diethyl ether solution to recover the solid, and the resulting white crystals were dried at room temperature for 12 hours.

[0029] Preparation of Dihydroxyhexanediammonium R(OH) by Ion Exchange Using Amberlite IRN-78 Resin as Hydroxide Source 2 , The resin is activated by acid washing and alkali washing before use, and washed to neutral with distilled water. RBr in distilled water 2 Dissolve to form a solution of about 0.05 mol / L, adjust the speed of the solution flowing through the resin exchange column to achiev...

Embodiment 2

[0039] In Example 1, solution F was replaced by 40wt% HF solution, slowly added dropwise to gel G, transferred to a 200ml stainless steel reaction kettle, and heated to 175°C in the same way, after 28 days of crystallization, the sample after roasting XRD see attached figure 1 c.

Embodiment 3

[0041] In Example 1, the gel G was transferred into a 200ml stainless steel reaction kettle with a polytetrafluoroethylene liner, and the temperature was raised to 175°C in the same way. After 28 days of crystallization, see the XRD of the sample after roasting. figure 1 d.

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Abstract

The invention relates to a method for synthesizing a pure silicon ITQ-13 molecular sieve and an aluminium silicon ITQ-13 molecular sieve. The synthesis of the pure silicon ITQ-13 molecular sieve is characterized in that white carbon black is taken as silicon source while the synthesis of the aluminium silicon ITQ-13 molecular sieve is characterized in that the white carbon black is taken as the silicon source, and aluminium isopropoxide or aluminium nitrate nona-hydrate is taken as aluminum source. The method of the invention overcomes the defects that the aluminium silicon ITQ-13 molecular sieve is difficult to be directly synthesized, the synthesis procedures are complex and the repeatability is poor by the previous synthesis method.

Description

technical field [0001] The invention provides a method for synthesizing pure silicon and silicon-aluminum ITQ-13 molecular sieve in a hydrothermal system, specifically a method using white carbon black as a silicon source, aluminum isopropoxide or aluminum nitrate nonahydrate as an aluminum source Method for synthesizing pure silicon and silicon aluminum ITQ-13 molecular sieves. Background technique [0002] ITQ-13 molecular sieve (USP 6,471,941) is a new type of molecular sieve invented by Mobil Corporation in 2002. It contains three sets of orthogonal channel systems intersecting each other. Its structural characteristics are: the first set of channels is parallel to the a axis and has 9 members Ring straight channel structure, the channel opening is The second set of channels is parallel to the b-axis and vertically intersects with the first set of channels. It is also a 10-member ring straight channel structure with an opening of The two sets of channels are connecte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/48C01B39/04C01B37/02B01J29/04
Inventor 徐龙伢许国梁朱向学刘盛林谢素娟
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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