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Functionalized mid-pore silica material and preparation and application thereof

A mesoporous silica and functionalization technology, applied in the field of cyclohexane solution, can solve the problems of alkaline wastewater polluting the environment, high cost, corrosion equipment and yield

Inactive Publication Date: 2014-09-24
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the disadvantages of high cost, polluting the environment by generating a large amount of alkaline wastewater, corroding equipment and low yield.

Method used

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  • Functionalized mid-pore silica material and preparation and application thereof
  • Functionalized mid-pore silica material and preparation and application thereof
  • Functionalized mid-pore silica material and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment one: the preparation of catalyst A

[0022] Take 2.61g hexadecylamine and dissolve in 50ml water and 20ml ethanol to prepare solution 1. Take 8.32g tetraethyl orthosilicate (TEOS) to obtain solution 2. Take 0.2gVOSO 4 (Molar ratio Si / V=50) solution in 10ml of water to prepare solution 3. Under vigorous stirring, solutions 2 and 3 were slowly added to solution 1. Aging for 24 hours, suction filtration, washing the precipitate, and drying at 80°C. Baked at 550°C for 5 hours in a muffle furnace. Catalyst A was prepared.

Embodiment 2

[0023] Embodiment two: catalytic decomposition cyclohexyl hydroperoxide active determination

[0024] Add 0.02g of catalyst A to a 50ml stainless steel reaction kettle with electromagnetic stirring, and then add 10ml of about (7.8g) cyclohexane solution containing 6% (0.5029mmol / g) of cyclohexyl hydroperoxide. Replace the reactor with nitrogen first, then close the gas inlet and outlet valves, heat to 120°C while stirring, keep the temperature constant for 30 minutes, cool down, and take out the reaction product.

[0025] The content of cyclohexane hydrogen peroxide before and after the reaction was analyzed by iodine-sodium thiosulfate redox titration method, and the amount of cyclohexanol and cyclohexanone in the reaction solution and the generated solution before and after the reaction were analyzed by gas chromatography internal standard method. The test results are shown in Table 1.

Embodiment 3

[0026] Embodiment three: preparation and catalytic activity of catalyst B

[0027] Except that the type of transition metal is different, the catalyst preparation method is the same as that of Example 1. The transition metal source is Co(CH 3 COO) 2 . The method for testing the activity of the catalyst is the same as in Example 2, and the results are shown in Table 1.

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PUM

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Abstract

The invention discloses a functionalized hexagonal mid-pore silica (HMS) material used in decomposition reaction of cyclohexyl hydroperoxide, the surface of functionalized hexagonal mid-pore silica material is superficial immobilized with one or a plurality of metal elements with cyclohexyl hydroperoxide decomposition ability. The material can be synthesized at room temperature by the sol-gel method. At a relatively low temperature, the material can be used as a catalyst for the catalytic liquid phase decomposition of the cyclohexyl hydroperoxide, and the material has high catalytic activity. Compared with catalysts in the prior art, the catalyst used in the invention has the advantages of being high in efficiency, cheap, convenient to use and the like.

Description

technical field [0001] The invention relates to a cyclohexane solution containing cyclohexyl hydroperoxide, in which cyclohexyl hydroperoxide is converted into cyclohexyl alcohol and cyclohexane under the catalysis of mesoporous silica (HMS) carrying transition metals The keto approach. Background technique [0002] In 1992, Mobil scientists opened a new era of molecular sieve science for the synthesis of M41S (MCM-41, MCM-48, MCM-50) series silicon-based mesoporous materials. Compared with classical microporous molecular sieves, mesoporous materials not only have larger pore size, but also have larger specific surface area (about 1000m 2 / g) and wall thickness, which also has high chemical and thermodynamic stability. Therefore, once the material came out, it attracted great attention from researchers in the fields of heterogeneous catalysis, adsorption separation, and advanced inorganic materials. [0003] HMS is a new type of silicon-based mesoporous material developed...

Claims

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Application Information

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IPC IPC(8): B01J29/03C07C27/00C07C35/08C07C29/132C07C49/403C07C45/53
Inventor 徐杰郑玺孙志强王敏高进苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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