Method for synthesizing NU-88 molecular sieves

A NU-88 and molecular sieve technology, which is applied in the direction of molecular sieve compounds, molecular sieve characteristic silicates, molecular sieves and alkali exchange compounds, etc., can solve the problems of high cost, energy and material consumption, and large time consumption of double quaternary ammonium salt templates , to achieve the effect of overcoming incomplete reaction of raw materials, avoiding waste and ineffective consumption, and avoiding time consumption

Active Publication Date: 2019-11-05
CHINA PETROLEUM & CHEM CORP +1
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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-DB

Method used

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  • Method for synthesizing NU-88 molecular sieves

Examples

Experimental program
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Embodiment 1

[0067] Under stirring conditions, mix 25.2g of N-methyl-4-piperidone and 23mL of absolute ethanol, and then drop 20g of 1,3-dibromopropane into the above mixture at a rate of 5 drops / second. Pre-reaction at ℃ for 4 hours to obtain the pre-reaction product A1. The molar ratio of 1,3-dibromopropane, N-methyl-4-piperidone and solvent ethanol is 1:2.25:4.07.

[0068] The pre-reaction product A1, 12.086g NaAlO 2 solution, 27.229g of tetraethylammonium hydroxide solution (TEAOH), 10.19g of 30% by weight NaOH solution were dissolved in an appropriate amount of deionized water, mixed evenly, and under stirring conditions, 40g of white carbon black was slowly added to form a milky white colloid The mixture to be crystallized, its molar composition is SiO 2 :Al 2 o 3 : Na 2 O:TEAOH:A1:H 2 O=100:3.3:12:10:15:4000, continue to stir for 1h, transfer to a 1L high-pressure reactor with mechanical stirring, stir and crystallize at 120°C for 2 days, then raise the temperature to 160°C and...

Embodiment 2

[0071]Synthesize NU-88 molecular sieve according to the method of Example 1, the difference is that under stirring conditions, 22.4g of N-methyl-4-piperidone and 32mL of ether were mixed, and then 20g of 1,3-dibromopropane was mixed with 4 drops / Add it dropwise to the above mixed solution at a speed of 2 seconds, and pre-react at 35°C for 12 hours to obtain the pre-reaction product A2. The molar ratio of 1,3-dibromopropane, N-methyl-4-piperidone and solvent ether is 1:2:3.18. 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

[0073] Synthesize NU-88 molecular sieve according to the method of Example 1, the difference is that under stirring conditions, 23.52g of N-methyl-4-piperidone was mixed with 27mL of deionized water, and then 20g of 1,3-dibromopropane was mixed with 5 Add it dropwise to the above mixture at a rate of drop / second, and pre-react at 55°C for 48 hours to obtain the pre-reaction product A3. The moles of 1,3-dibromopropane, N-methyl-4-piperidone and solvent water The ratio is 1:2.1:15.5. 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 NU-88 molecular sieves. The method comprises the following steps of (1) mixing 1,3-dibromopropane, 1-methyl-4-piperidone and a solvent, and carryingout a pre-reaction at 15-60 DEG C for 0.5-96 h to obtain a pre-reaction product, wherein a molar ratio of the 1,3-dibromopropane to the 1-methyl-4-piperidone to the solvent is 1 to (1.8 to 3) to (1 to20); and (2) mixing the pre-reaction product obtained in the step (1), an organic alkali, an inorganic alkali, an aluminium source, a silicon source and water to obtain a to-be-crystallized mixture,conducting hydrothermal crystallization treatment on the to-be-crystallized mixture, and recovering a solid product. According to the disclosed method, necessary tedious processes, including high-costseparation and purification, of conventional synthesis of a NU-88 molecular sieve template are omitted, large time consumption, energy consumption and material consumption are avoided, and the cost reduction 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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IPC IPC(8): C01B39/48C01B37/00
CPCC01B37/005C01B39/48
Inventor 孙敏余少兵贾晓梅王永睿慕旭宏
Owner CHINA PETROLEUM & CHEM CORP
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