Method for directly synthesizing mesoporous material coated heteropolyacid functionalized MOF material

A technology of mesoporous materials and heteropolyacids, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, production of bulk chemicals, etc., to achieve high reaction yields, mild reaction conditions, and synthetic methods easy effect

Inactive Publication Date: 2015-02-11
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The use of mesoporous materials to coat heteropolyacid-modif

Method used

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  • Method for directly synthesizing mesoporous material coated heteropolyacid functionalized MOF material
  • Method for directly synthesizing mesoporous material coated heteropolyacid functionalized MOF material
  • Method for directly synthesizing mesoporous material coated heteropolyacid functionalized MOF material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 0.180g SBA-15, 0.1062g H 4 PMo 11 VO 40 19H 2 O(0.05mmol), 0.240gCu(NO 3 ) 2 ·3H 2 O (1 mmol), 0.105 g of 1,3,5-trimesic acid (0.5 mmol), 0.09 g of tetramethylammonium hydroxide (1 mmol) were dissolved in 10 mL of deionized water, and the pH was adjusted to 2.5 with 2M NaOH. The solution was transferred to a 23mL autoclave, the temperature was programmed to rise at 5°C / h, and then raised to 160°C for 48h. After slowly cooling down to room temperature, the target material was precipitated from the reaction solution in the form of crystals. The obtained material was washed with water, and its structure was determined by XRD single crystal diffraction (the specific structure is as follows: figure 1 Shown), the mass yield of the heteropolyacid material with dual active centers is 35% by calculating the mass.

[0021] Using the obtained catalytic material for benzene hydroxylation reaction, 0.025mmol catalyst, 0.78g benzene (10mmol), 6.8mL acetonitrile, 0.9g ascorbic ...

Embodiment 2

[0023] 0.20g SBA-15, 0.2123g H 4 PMo 11 VO 40 19H 2 O(0.1mmol), 0.120gCu(NO 3 ) 2 ·3H 2 O (0.5 mmol), 0.105 g of 1,3,5-trimesic acid (0.5 mmol), 0.045 g of tetramethylammonium hydroxide (0.5 mmol) were dissolved in 10 mL of deionized water, and the pH was adjusted to 7.8 using 2M NaOH. The solution was transferred to a 23mL autoclave, the temperature was programmed to rise at 50°C / h, and then raised to 120°C for 72h. After slowly cooling down to room temperature, the target material was precipitated from the reaction solution in the form of crystals. The obtained material was washed with water, and its structure was determined by XRD single crystal diffraction (the specific structure is as follows: figure 1 shown), the mass yield of the heteropolyacid material with dual active centers is 25% by calculating the mass.

[0024] Using the obtained catalytic material for benzene hydroxylation reaction, 0.10g catalyst, 0.78g benzene (10mmol), 6.8mL acetonitrile, 0.9g ascorbic...

Embodiment 3

[0026] 0.16g SBA-15, 0.2123g H 4 PMo 11 VO 40 19H 2 O(0.1mmol),0.240gCu(NO 3 ) 2 ·3H 2 O (1 mmol), 0.105 g of 1,3,5-trimesic acid (0.5 mmol), 0.18 g of tetramethylammonium hydroxide (2 mmol) were dissolved in 10 mL of deionized water, and the pH was adjusted to 4.8 using 2M NaOH. The solution was transferred to a 46mL autoclave, the temperature was programmed to rise at 20°C / h, and then raised to 240°C for 16h. After slowly cooling down to room temperature, the target material was precipitated from the reaction solution in the form of crystals. The obtained material was washed with water, and its structure was determined by XRD single crystal diffraction (the specific structure is as follows: figure 1 Shown), the mass yield of the heteropolyacid material with dual active centers is 42% by calculating the mass.

[0027] Using the obtained catalytic material for benzene hydroxylation reaction, 0.20g catalyst, 0.78g benzene (10mmol), 6.8mL acetonitrile, 0.9g ascorbic acid, 2...

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Abstract

The invention discloses a method for directly synthesizing a mesoporous material coated heteropolyacid functionalized MOF material, and relates to a method for a mesoporous material coated polyacid modified metal organic framework material, wherein a mesoporous molecular sieve, phosphorus molybdenum heteropoly acid, tetramethylammonium hydroxide, 1,3,5-trimesic acid, and Cu(NO3)2.3H2O are adopted as raw materials, a hydrothermal synthesis method is adopted, and water is adopted as a solvent to carry out one step synthesis at a temperature of 90-230 DEG C to obtain the target material. The catalysis material synthesized by the method is applied in the benzene hydroxylation reaction, wherein the good stability performance of the material is presented under the mild reaction conditions.

Description

technical field [0001] The present invention relates to a kind of mesoporous SBA-15, phosphomolybdenum heteropoly acid, tetramethylammonium hydroxide, 1,3,5-trimellitic acid, Cu(NO 3 ) 2 ·3H 2 O is used as a raw material, and the target material is synthesized in one step by hydrothermal synthesis at a reaction temperature of 90°C-230°C, using water as a solvent. Background technique [0002] Heteropolyacids (POMs) are a class of polymetallic oxygen cluster compounds composed of pre-transition metals, whose structure can be regulated at the molecular or atomic level. application. Heteropolyacids are a class of excellent homogeneous catalytic materials, which are difficult to separate from liquid reaction media. Therefore, scholars have been paying attention to the heterogeneous work with heteropolyacids. Technologies such as reaction-controlled phase transfer and reaction-induced self-separation, as well as a series of supports such as zeolite, silica gel, silica, perio...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C39/04C07C37/58
CPCY02P20/52
Inventor 高爽杨华王连月李军吕迎
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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