A kind of modified im-5 molecular sieve and its preparation method and application and the method of toluene methanol alkylation reaction

A technology of IM-5 and molecular sieve, which is applied in molecular sieve catalysts, chemical instruments and methods, organic chemistry, etc., can solve the problems of poor stability, low conversion rate of toluene, decreased conversion rate of toluene, etc., and achieve long service life and high catalytic efficiency , high catalytic activity and stability

Active Publication Date: 2020-08-18
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

The results show that although the selectivity of xylene and p-xylene in the toluene-methanol alkylation reaction of the IM-5 molecular sieve after hydrothermal treatment is improved, the activity decreases, and the conversion rate of toluene decreases with the prolongation of the reaction time
[0010] Although the above-mentioned modified IM-5 molecular sieve has improved xylene selectivity to a certain extent in toluene-methanol alkylation reaction, either there is a defect that the conversion rate of toluene is low, or there is a defect that the stability is poor, and the stability play a vital role in whether it can be industrialized

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  • A kind of modified im-5 molecular sieve and its preparation method and application and the method of toluene methanol alkylation reaction
  • A kind of modified im-5 molecular sieve and its preparation method and application and the method of toluene methanol alkylation reaction
  • A kind of modified im-5 molecular sieve and its preparation method and application and the method of toluene methanol alkylation reaction

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preparation example Construction

[0024] The preparation method of the H-IM-5 molecular sieve can be prepared according to conventional techniques, such as generally prepared according to the following steps:

[0025] The Na-type IM-5 molecular sieve (NaIM-5 molecular sieve) was subjected to ammonium exchange, then dried and calcined.

[0026] In the preparation process of the H-IM-5 molecular sieve, the ammonium exchange process may include: contacting the Na-type IM-5 molecular sieve with an ammonium nitrate solution. In the ammonium exchange process, the solid-to-liquid ratio (g / mL) of the Na-type IM-5 molecular sieve to the ammonium nitrate solution may be 1:(5-10). The concentration of the ammonium nitrate solution used may be 0.1-0.5 mol / L. Preferably, the ammonium exchange is performed multiple times, for example, 2-4 times, most preferably 3 times. Moreover, each ammonium exchange may be performed for 0.5-5 hours, preferably 1-3 hours, most preferably 2 hours.

[0027] During the preparation process...

Embodiment approach

[0040] The purpose of the present invention can be achieved as long as the above modifier solution is used to modify the H-IM-5 molecular sieve, and the types of the quaternary ammonium cations and quaternary phosphonium cations are not particularly limited. For example, the quaternary ammonium cation can be provided by a quaternary ammonium salt and / or a quaternary ammonium base, and the quaternary ammonium salt and the quaternary ammonium base can contain one quaternary ammonium cation, two quaternary ammonium cations, three quaternary ammonium cations or more, preferably containing One or two quaternary ammonium cations; the quaternary phosphonium cations can be provided by quaternary phosphonium salts and / or quaternary phosphonium bases, which can contain one quaternary phosphonium cation, two quaternary phosphonium cations, three quaternary phosphonium cations or more, preferably containing a quaternary phosphonium cation. The quaternary ammonium salts, quaternary ammoniu...

preparation example 1

[0079] SiO 2 / Al 2 o 3 The NaIM-5 molecular sieve with a molar ratio of 38 was ion-exchanged three times with ammonium nitrate solution with a concentration of 0.5mol / L at 80°C, the solid-liquid ratio (g / mL) was 1:8, and the time for each ion exchange was 2 hours. The molecular sieve obtained after the exchange was washed with deionized water, dried at 90°C for 10 hours, and calcined at 550°C for 5 hours to obtain H-IM-5 molecular sieve P-Z 1 (Na 2 O content is less than 0.1% by mass), and the physical and chemical parameters are shown in Table 1.

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Abstract

The invention relates to the field of molecular sieve preparation, particularly to a modified IM-5 molecular sieve, a preparation method and applications thereof, and a toluene methanol alkylation reaction method. The preparation method of the modified IM-5 molecular sieve comprises: making a modifier solution and an H-IM-5 molecular sieve contact, and roasting the solid material obtained throughthe contacting, wherein the modifier solution contains quaternary ammonium cation and quaternary phosphonium cation, and is alkaline, and the contacting temperature is 100-200 DEG C. According to thepresent invention, the micro-pore area of the modified IM-5 molecular sieve is more than 300 m<2> / g, the micro-pore volume of the modified IM-5 molecular sieve is more than 0.13 cm<3> / g, and the phosphorus content is 0.1-15 wt% (calculated as P2O5) by using the total amount of the modified IM-5 molecular sieve as the reference; and with the application of the modified IM-5 molecular sieve in the toluene methanol alkylation reaction, the high catalytic activity and the high stability are high.

Description

technical field [0001] The invention relates to the field of molecular sieve preparation, in particular to a modified IM-5 molecular sieve, a method for preparing a modified IM-5 molecular sieve, a modified IM-5 molecular sieve obtained by the preparation method, and a modified IM-5 molecular sieve in The application in the alkylation reaction of toluene and methanol and a method for the alkylation reaction of toluene and methanol. Background technique [0002] IM-5 molecular sieves were first synthesized by Suk Bong Hong et al. (USP6136290) using pyrrolidine bisquaternary ammonium salt templates. Pore, its pore structure is similar to ZSM-5 molecular sieve, and the molecular sieve also has a 12-membered ring cage structure, which is different from ZSM-5. That The amount of acid and Lewis acid is close to that of TUN structure molecular sieve, The ratio of acid to Lewis acid (B / L) is close to that of ZSM-5 molecular sieve. [0003] IM-5 molecular sieves have shown good...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/70C07C2/86C07C15/08C01B39/02
CPCY02P20/52
Inventor 孙敏陈俊文王永睿贾晓梅余少兵慕旭宏舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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