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Method for synthesizing NU-88 molecular sieve

A NU-88, molecular sieve technology, applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of energy consumption and material consumption, high cost of biquaternary ammonium salt template agent, and large time consumption, Achieve the effect of avoiding waste and ineffective consumption, overcoming incomplete reaction of raw materials, and avoiding time consumption

Active Publication Date: 2019-11-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, the method of synthesizing NU-88 molecular sieve is costly, which restricts its wide application
The high cost of the double quaternary ammonium salt template for the synthesis of NU-88 molecular sieve is one of the main reasons for the high cost of NU-88 molecular sieve
[0006] Synthetic double quaternary ammonium template agent 1, the method for 6-bis(N-methylpyrrolidine) hexane bromide (1,6-MPH) generally needs two kinds of raw materials 1-methylpyrrolidine (1-MP) and 1,6-Dibromohexane (1,6-DBH) reacts in a certain proportion in an appropriate solvent, and crystallization and multiple recrystallization methods are required to obtain relatively pure 1,6-MPH, while in crystallization, In the process of multiple recrystallizations, tedious operations such as freezing, filtering, washing with organic reagents, drying, adding appropriate organic solvents to dissolve, adding appropriate organic solvents to precipitate, filtering, washing, and drying, etc., consume a lot of time and Generate a lot of energy and material consumption

Method used

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  • Method for synthesizing NU-88 molecular sieve
  • Method for synthesizing NU-88 molecular sieve
  • Method for synthesizing NU-88 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Under stirring conditions, mix 21.093g of 1-methylpyrrolidine and 23mL of absolute ethanol, and then add 26.88g of 1,6-dibromohexane dropwise to the above mixture at a rate of 3 drops / second. The pre-reaction was performed for 4 hours to obtain the pre-reaction product A1. The molar ratio of 1,6-dibromohexane, 1-methylpyrrolidine and solvent ethanol was 1:2.25:3.66.

[0062] The pre-reaction product A1, 16.115g NaAlO 2 solution, 14.8g of 30% by weight NaOH solution was dissolved in an appropriate amount of deionized water, mixed uniformly, and under stirring conditions, 40g of white carbon black was slowly added to make a milky white colloidal mixture to be crystallized, and its molar composition was SiO 2 :Al 2 o 3 : Na 2 O:A1:H 2 O=100:3.3:16.7:16.7:5000, continue to stir for 1h, transfer to a 1L autoclave with mechanical stirring, stir at 160°C for hydrothermal crystallization for 13 days, stop the crystallization reaction, wash and filter the product Finally, d...

Embodiment 2

[0065] Synthesize NU-88 molecular sieve according to the method of Example 1, the difference is that under stirring conditions, 18.75g of 1-methylpyrrolidine and 32mL of ether were mixed, and then 26.875g of 1,6-dibromohexane was mixed with 5 drops / second Add it dropwise to the above mixture at a high speed, and pre-react at 35°C for 12 hours to obtain the pre-reaction product A2. The molar ratio of 1,6-dibromohexane, 1-methylpyrrolidine and solvent ether is 1:2:2.85 . 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

[0067] Synthesize NU-88 molecular sieve according to the method of Example 1, the difference is that, under stirring conditions, 19.69g of 1-methylpyrrolidine was mixed with 27mL of deionized water, and then 26.875g of 1,6-dibromohexane was mixed with 4 drops / Add it dropwise into the above mixture at a speed of 1 second, and pre-react at 60°C for 48 hours to obtain the pre-reaction product A3. The molar ratio of 1,6-dibromohexane, 1-methylpyrrolidine and solvent water is 1:2.1 : 13.89. 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 invention relates to a method for synthesizing an NU-88 molecular sieve. The method comprises the following steps that a, 1,6-dibromohexane, 1-methylpyrrolidine and a solvent are mixed for pre-reaction for 0.5-96 h at 15-90 DEG C, thus a pre-reaction product is obtained, wherein the molar ratio of the 1,6-dibromohexane to the 1-methylpyrrolidine to the solvent is 1:(1.8-3):(1-20); and b, the pre-reaction product obtained in the step a, an inorganic base, an aluminum source, a silicon source and water are mixed to obtain a to-be-crystallized mixture, the to-be-crystallized mixture is subjected to hydrothermal crystallization treatment, and a solid product is recovered. According to the method, the necessary cumbersome processes of high-cost separation, purification and the like necessary for conventional synthesis of a NU-88 molecular sieve template agent are omitted, a large amount of time consumption, energy consumption and material consumption are avoided, the cost is lowered, and the effect is obvious.

Description

technical field [0001] The present disclosure relates to a method of synthesizing NU-88 molecular sieves. Background technique [0002] NU-88 molecular sieve is a new type of molecular sieve first disclosed by patent USP60277707. The method uses bis(N-methylpyrrolidine) alkylene bromide as a template, wherein the alkylene group has 4 to 6 carbons, and dynamic crystallization is required for 9 to 22 days at a reaction temperature of 160°C. Obtain NU-88 molecular sieve. The molecular sieve structure of NU-88 has not been fully analyzed. According to the existing characterization and reaction evaluation results, it is speculated that it may belong to the BET family and has a three-dimensional twelve-membered ring channel structure. [0003] Lee S B reported a method for synthesizing NU-88 molecular sieve in Journal of catalysis, 2003, 215: 151-170. The template used in this method is 1,6-bis(N-methylpyrrolidine) hexane bromide, and NU-88 molecular sieve can only be used in n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04C01B39/48
CPCC01B39/04C01B39/48C01P2002/72
Inventor 孙敏余少兵贾晓梅慕旭宏
Owner CHINA PETROLEUM & CHEM CORP
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