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The method for synthesizing tnu-9 molecular sieve

A TNU-9, molecular sieve technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of side reactions of synthetic templates, ineffective consumption of reaction raw materials, incompleteness, etc., and achieve crystallinity. High, the effect of overcoming incomplete reaction of raw materials, avoiding waste and ineffective consumption

Active Publication Date: 2021-04-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, under the strong alkaline environment of synthetic molecular sieves and in the whole reaction mixture system, side reactions or incomplete reactions will inevitably occur in the raw materials of synthetic templates, thereby causing ineffective consumption and waste of reaction raw materials, resulting in undesirable result

Method used

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  • The method for synthesizing tnu-9 molecular sieve
  • The method for synthesizing tnu-9 molecular sieve
  • The method for synthesizing tnu-9 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Under stirring conditions, mix 29.32g of 1-methylpyrrolidine and 36mL of absolute ethanol, and then add 33.05g of 1,4-dibromobutane dropwise to the above mixture at a rate of 5 drops / second. Pre-react for 8 hours to obtain the pre-reaction product A1. The molar ratio of 1,4-dibromobutane, 1-methylpyrrolidine and solvent ethanol is 1:2.25:4.12.

[0060] The pre-reaction product A1, 15g Al(NO 3 ) 3 9H 2 O. Dissolve 29.2g of NaOH solution in an appropriate amount of deionized water, mix well, and slowly add 61.9g of white carbon black under stirring conditions to make a milky white colloidal mixture whose molar composition is SiO 2 :Al 2 o 3 : Na 2 O:A1:H 2 O=100:2:36.7:15:4000, continue to stir for 1h, transfer to a 1L autoclave with mechanical stirring, stir at 160°C for hydrothermal crystallization for 14 days, stop the crystallization reaction, wash and filter the product Finally, dry at 80°C for 12 hours to obtain molecular sieve powder B1.

[0061] Carry out ...

Embodiment 2

[0063] Synthesize TNU-9 molecular sieve according to the method of Example 1, the difference is that under stirring conditions, 29.32g of 1-methylpyrrolidine and 43mL of ether are mixed, and then 33.05g of 1,4-dibromobutane is mixed with 10 drops / second Add it dropwise to the above mixture, and pre-react at 35°C for 16 hours to obtain the pre-reaction product A2. The molar ratio of 1,4-dibromobutane, 1-methylpyrrolidine and solvent ether is 1:2.0:2.76 . The molecular sieve raw powder B2 was obtained by replacing A1 with the pre-reaction product A2. Its XRD spectrum was consistent with that of Example 1. The relative crystallinity and synthesis cost were calculated and listed in Table 1.

Embodiment 3

[0065] TNU-9 molecular sieves were synthesized according to the method of Example 1, the difference being that, under stirring conditions, 27.37g of 1-methylpyrrolidine was mixed with 35mL of deionized water, and then 33.05g of 1,4-dibromobutane was added dropwise to The above mixed solution was pre-reacted at 60°C for 48 hours to obtain the pre-reaction product A3. The molar ratio of 1,4-dibromobutane, 1-methylpyrrolidine and solvent water was 1:2.1:12.96. The molecular sieve raw powder B3 was obtained by replacing A1 with the pre-reaction product A3. Its XRD spectrum was consistent with that of Example 1. The relative crystallinity and synthesis cost were calculated and listed in Table 1.

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Abstract

The disclosure relates to a method for synthesizing TNU‑9 molecular sieves, the method comprising the following steps: a. Mixing 1,4-dibromobutane and 1-methylpyrrolidine with a solvent, and pre-reacting at 15-90°C for 0.5- 96h, to obtain the pre-reaction product, the molar ratio of the 1,4-dibromobutane, 1-methylpyrrolidine and solvent is 1: (1.8~3): (1~20); b. The obtained pre-reaction product, inorganic base, aluminum source, silicon source and water are mixed to obtain a mixture to be crystallized, and the mixture to be crystallized is subjected to hydrothermal crystallization treatment to recover a solid product. The disclosed method eliminates the cumbersome processes such as high-cost separation and purification that are necessary for the conventional synthesis of TNU-9 molecular sieve templates, avoids a lot of time consumption, energy consumption and material consumption, and has an obvious cost reduction effect.

Description

technical field [0001] The present disclosure relates to a method for synthesizing TNU-9 molecular sieves. Background technique [0002] TNU-9 is a new type of molecular sieve with a three-dimensional ten-membered ring cross structure synthesized by Hong et al. in 2007. TNU-9 has two sets of ten-membered ring channels (0.52×0.6 and 0.51×0.55nm). Where the distance between the two sets of ten-membered ring channels is relatively narrow, they are connected to each other through another set of ten-membered ring channels (0.54×0.55nm). In addition, there is a larger cage structure inside the channel of TNU-9. TNU-9 molecular sieve has very good hydrothermal stability, and has shown good activity and shape selectivity in some reactions, such as: in toluene disproportionation reaction, TNU-9 showed high initial activity , and from the perspective of product distribution, TNU-9 also exhibited certain shape selectivity; in the reforming reaction of m-xylene, TNU-9 also exhibited h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/48
CPCC01B39/48C01P2002/72
Inventor 孙敏贾晓梅余少兵慕旭宏
Owner CHINA PETROLEUM & CHEM CORP
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