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The method for synthesizing im-5 molecular sieve

A technology of IM-5 and molecular sieve, which is applied in the direction of molecular sieves and base exchange compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of ineffective consumption, waste, and incompleteness of reaction raw materials, so as to overcome the incomplete reaction of raw materials and avoid Waste and ineffective consumption, avoiding the effect of time consumption

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

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Problems solved by technology

However, this method does not provide a specific recycling method for template raw materials. If the unreacted raw materials cannot be effectively recovered, it will inevitably cause waste.
In addition, under the strong alkaline environment of the synthetic molecular sieve and in the whole reaction mixture system, the raw materials of the synthetic template will inevitably undergo side reactions or incomplete reactions, resulting in ineffective consumption and waste of the reaction raw materials, resulting in undesirable result

Method used

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  • The method for synthesizing im-5 molecular sieve
  • The method for synthesizing im-5 molecular sieve
  • The method for synthesizing im-5 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Under stirring conditions, mix 35g of 1-methylpyrrolidine and 37mL of absolute ethanol, then add 43.97g of 1,5-dibromopentane dropwise to the above mixture at a rate of 3 drops / second, and pre- After reacting for 8 hours, the pre-reaction product A1 was obtained. The molar ratio of 1,5-dibromopentane, 1-methylpyrrolidine and solvent ethanol was 1:2.15:3.39.

[0065] The pre-reaction product A1, 43.78gNaAlO 2 solution, 53.46mL of 30% by weight NaOH solution was dissolved in an appropriate amount of deionized water, mixed evenly, and under stirring conditions, 150g of solid silica gel was slowly added to make a milky white colloidal mixture to be crystallized, the molar composition of which was SiO 2 :Al 2 o 3 : Na 2 O:A1:H 2 O=100:2.5:17.5:8:900, continue to stir for 1h, transfer to a 1L autoclave with mechanical stirring, carry out the first stage of hydrothermal crystallization at 140°C for 2 days, then raise the temperature to 172°C for the second stage The secon...

Embodiment 2

[0068] Synthesize IM-5 molecular sieve according to the method of Example 1, the difference is that, under stirring conditions, 33.22g of 1-methylpyrrolidine and 48mL of ether are mixed, and then 43.97g of 1,5-dibromopentane is mixed with 10 drops / second Add it dropwise to the above mixed solution at a high speed, and pre-react at 35°C for 16 hours to obtain the pre-reaction product A2. The molar ratio of 1,5-dibromopentane, 1-methylpyrrolidine and solvent ether is 1:2.04:2.47 . 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

[0070]Synthesize IM-5 molecular sieves according to the method of Example 1, the difference is that, under stirring conditions, 34.19g of 1-methylpyrrolidine was mixed with 40mL of deionized water, and then 43.97g of 1,5-dibromopentane was mixed with 5 drops / Add it dropwise to 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 1,5-dibromopentane, 1-methylpyrrolidine and solvent water is 1:2.1 : 11.8. 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 IM‑5 molecular sieves, the method comprising the following steps: a. Mixing 1,5-dibromopentane 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 1,5-dibromopentane, 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 omits the cumbersome processes such as high-cost separation and purification that are necessary for the conventional synthesis of IM-5 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 of synthesizing IM-5 molecular sieves. Background technique [0002] IM-5 is a new molecular sieve. In 1997, Benazzi et al reported the synthesis method of IM-5 molecular sieve for the first time, and the template agent used was a kind of diquaternary ammonium salt—1,5-bis(N-methylpyrrolidine)pentane bromide (MPPBr 2 ). IM-5 molecular sieve has a distinctive two-dimensional ten-membered ring channel system, and its structure is composed of a two-dimensional ten-membered ring channel system and some three-dimensional characteristic holes, so it not only has the long-range ordered binary structure of ordinary microporous materials. At the same time, the existence of holes can play a positive role in the contact between reactants and active centers, promoting the diffusion of products and reducing the formation of carbon deposits. IM-5 also has better thermal stability and hydrothermal stability than ZSM-5, wh...

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 孙敏贾晓梅余少兵王永睿慕旭宏
Owner CHINA PETROLEUM & CHEM CORP
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