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Method for Co-SBA-16 mesoporous molecule sieve for direct hydroxylation synthesis for phenol

A mesoporous molecular sieve, co-sba-16 technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of harsh synthesis conditions, low catalytic activity, difficult to control, etc., to achieve simple operation, High catalytic activity and easy handling

Inactive Publication Date: 2015-06-03
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to solve the problems that the existing cobalt-loaded SBA-16 mesoporous silicon molecular sieves have harsh synthesis conditions, difficult to control, long cycle and low catalytic activity, and provide a method for synthesizing Co-SBA-16 mesoporous silicon molecular sieves

Method used

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  • Method for Co-SBA-16 mesoporous molecule sieve for direct hydroxylation synthesis for phenol
  • Method for Co-SBA-16 mesoporous molecule sieve for direct hydroxylation synthesis for phenol
  • Method for Co-SBA-16 mesoporous molecule sieve for direct hydroxylation synthesis for phenol

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specific Embodiment approach 1

[0017] Specific embodiment one: the synthesis method of Co-SBA-16 mesoporous molecular sieve in this embodiment is realized according to the following steps:

[0018] 1. In bottle A, weigh 0.1429 mmol of triblock polymer F127, add 0.4356 mol of absolute ethanol, sonicate for 20-30 minutes, then place in a water bath at 25-35°C and stir for 1.5-2.5 hours;

[0019] 2. In bottle B, weigh 0.7089~2.127mmol of cobalt nitrate, add 0.2401mol of absolute ethanol, then add 17.73mmol of ethyl orthosilicate drop by drop under stirring conditions, and then add 1.5~2.5ml to a concentration of 0.03M HCl, ultrasonic for 10-20min, then placed in a water bath at 25-35°C and stirred for 1.5-2.5h;

[0020] 3. Add 0.5~1.5ml of 0.1M HCl to the stirred solution in bottle A, stir for 10~20min, then add 1.248~1.664mmol of 1,3,5-trimethylbenzene into bottle A, and place Stir in a 25-35°C water bath for 1.5-2.5 hours;

[0021] 4. After stirring the solution in bottle B for 1.5-2.5 hours, raise the tem...

specific Embodiment approach 2

[0024] Embodiment 2: The difference between this embodiment and Embodiment 1 is that in Step 1, ultrasound is performed for 25 minutes, and then placed in a water bath at 30°C and stirred for 2 hours. Other steps and parameters are the same as those in Embodiment 1.

specific Embodiment approach 3

[0025] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that in step 2, 2ml of HCl with a concentration of 0.03M is added, ultrasonicated for 15 minutes, and then placed in a 30°C water bath and stirred for 2 hours. Other steps and parameters are the same as those in Embodiment 1 or Embodiment 2.

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Abstract

The invention provides a Co-SBA-16 mesoporous molecule sieve synthesis method, and relates to a Co-SBA-16 synthesis method. A purpose of the present invention is to mainly solve problems of harsh synthesis conditions, difficult control, long period and low catalysis activity of the existing cobalt-loaded SBA-16 type mesoporous silicon molecule sieve. The method comprises: 1, adding F127 and anhydrous ethanol to a bottle A, and sequentially carrying out an ultrasound treatment and stirring; 2, adding cobalt nitrate, anhydrous ethanol, tetraethyl orthosilicate and HCl to a bottle B, and sequentially carrying out an ultrasound treatment and stirring; 3, adding HCl to the stirred solution in the bottle A, stirring, adding 1,3,5-trimethylbenzene, and stirring; 4, after stirring in the bottle B, heating, and continuously stirring; and 5, completely transferring the solution in the bottle A to the bottle B, stirring, placing in a baking oven, pouring to a watch glass, evaporating the solvent, taking the solid substance, and baking to obtain the finished product. The synthesis method has characteristics of simple conditions, easy operation, good repeatability, and short experimental period, wherein the obtained Co-SBA-16 mesoporous molecule sieve has high catalysis activity.

Description

technical field [0001] The invention relates to a method for synthesizing Co-SBA-16. Background technique [0002] Supported cobalt catalyst is an important catalyst. Compared with other silica carrier materials, SBA-16 mesoporous silicon molecular sieve has the advantages of high specific surface area, large pore volume, uniform pore size distribution, high hydrothermal stability, etc., which make it very good in the field of catalytic carriers. Application prospects. However, it is prepared under strongly acidic conditions, and under strongly acidic synthesis conditions, the added metal ions will mainly exist in the form of cations, and it is difficult to form metal-oxygen bonds-silicon bonds. Therefore, it is very difficult to directly introduce metals into mesoporous silicon materials during the synthesis process, thus limiting their applications in catalysis. In order to obtain acids, bases and redox centers, metals are mainly introduced through hydrothermal synthesi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/035C07C39/04C07C37/60
CPCY02P20/52
Inventor 朱宇君湛鑫琳袁福龙董永利付宏刚
Owner HEILONGJIANG UNIV
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