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Method for synthesizing EMM-23 molecular sieve

A technology of EMM-23 and molecular sieve, which is applied in molecular sieves and alkali 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

Pending Publication Date: 2020-12-01
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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  • Method for synthesizing EMM-23 molecular sieve
  • Method for synthesizing EMM-23 molecular sieve
  • Method for synthesizing EMM-23 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Under stirring conditions, mix 70.92g of N,N,N',N'-tetramethyl-1,6-hexanediamine and 70mL of absolute ethanol, and then add 77.45g of 1,4-dibromobutane with 3 drops / Add it dropwise to the above mixture at a speed of 2 seconds, and pre-react at 50°C for 8 hours to obtain the pre-reaction product A1. 1,4-dibromobutane, N,N,N',N'-tetramethyl-1, The molar ratio of 6-hexanediamine to solvent ethanol is 1:1.15:3.43.

[0068] The pre-reaction product A1, 17.51gNaAlO 2 solution, 109.72g of 30% by weight NaOH solution was dissolved in an appropriate amount of deionized water, mixed uniformly, and under stirring conditions, 150g of solid silica gel was slowly added to make a milky white colloidal mixture whose molar composition was SiO 2 :Al 2 o 3 : Na 2 O:A1:H 2 O=100:1:20:15:1000, continue to stir for 1h, transfer to a 1L autoclave with mechanical stirring, perform the first stage of hydrothermal crystallization at 120°C for 1 day, then raise the temperature to 165°C for ...

Embodiment 2

[0071] Synthesize EMM-23 molecular sieve according to the method of Example 1, the difference is that under stirring conditions, 77.09gN,N,N',N'-tetramethyl-1,6-hexamethylenediamine and 90mL diethyl ether were mixed, and then Add 77.45g of 1,4-dibromobutane dropwise to the above mixture at a rate of 10 drops / second, and pre-react at 35°C for 16 hours to obtain the pre-reaction product A2. 1,4-dibromobutane, N,N , The molar ratio of N',N'-tetramethyl-1,6-hexanediamine to solvent ether is 1:1.25:2.47. The pre-reaction product A2 was used instead of A1 for hydrothermal crystallization treatment to obtain molecular sieve powder B2, whose XRD spectrum was consistent with that of Example 1, and its relative crystallinity and synthesis cost were calculated and listed in Table 1.

Embodiment 3

[0073] Synthesize EMM-23 molecular sieve according to the method of Example 1, the difference is that 55.51g of N,N,N',N'-tetramethyl-1,6-hexamethylenediamine was mixed with 75mL of deionized water under stirring conditions , and then 77.45g of 1,4-dibromobutane was added dropwise to the above mixture at a rate of 5 drops / second, and pre-reacted at 60°C for 48 hours to obtain the pre-reaction product A3. 1,4-Dibromobutane, The molar ratio of N,N,N',N'-tetramethyl-1,6-hexanediamine to solvent water is 1:0.9:11.8. The pre-reaction product A3 was used instead of A1 for hydrothermal crystallization treatment to obtain molecular sieve powder B3, whose XRD spectrum was consistent with that of Example 1, and its 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 EMM-23 molecular sieve. The method comprises the following steps: a, 1, 4-dibromobutane, N, N, N ', N'-tetramethyl-1, 6-hexamethylenediamine and asolvent are mixed and subjected to a pre-reaction at 15-90 DEG C for 0.5-96 h, a pre-reaction product is obtained, and the molar ratio of 1, 4-dibromobutane, N, N, N ', N'-tetramethyl-1, 6-hexamethylenediamine to the solvent is 1: (0.8-1.5): (1-20); and b, mixing the pre-reaction product obtained in the step a, inorganic alkali, an aluminum source, a silicon source and water to obtain a mixture to be crystallized, carrying out hydrothermal crystallization treatment on the mixture to be crystallized, and recovering a solid product. According to the method, the tedious processes of high-cost separation, purification and the like which are necessary for conventional synthesis of the EMM-23 molecular sieve template agent are omitted, a large amount of time consumption, energy consumption andmaterial consumption are avoided, and the effect of reducing the cost is obvious.

Description

technical field [0001] The present disclosure relates to a method of synthesizing EMM-23 molecular sieves. Background technique [0002] EMM-23 molecular sieve is a new type of silica-alumina molecular sieve first synthesized by ExxonMobil in 2012. In 2014, its structure was analyzed as a three-dimensional channel system composed of a one-dimensional 21-membered ring channel and a two-dimensional 10-membered ring channel. On April 2, 2015, it was recognized by the International Molecular Sieve Association (IZA), and its topology code was approved as EWT. The molecular sieve is the world's first silica-alumina molecular sieve with super large pores and stable structure. The molecular sieve still has a high specific surface area and thermal stability after being calcined at 540°C. US20140336394A1 discloses that the template for synthesizing EMM-23 molecular sieves is bis(N-propylpyrrolidinium)pentane cation or bis(N-propylpyrrolidinium)hexane diocation. CN107311190A disclo...

Claims

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Application Information

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IPC IPC(8): C01B39/48
CPCC01B39/48
Inventor 孙敏余少兵贾晓梅王永睿罗一斌
Owner CHINA PETROLEUM & CHEM CORP
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