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Polyketone-grafted modified mesoporous silicon oxide material preparation method

A technology of mesoporous silica and graft modification, which is applied in the field of preparation of mesoporous silica materials, can solve problems such as difficulty in catalyst recovery and reactivation, and achieve the effect of mild polymerization conditions and simple process

Active Publication Date: 2014-01-08
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Carbon monoxide is very cheap, and the key lies in the catalyst. The recovery and reactivation of current catalysts are very difficult, and it is even more difficult to graft polyketones into mesoporous materials under the premise of synthesizing polyketones.

Method used

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  • Polyketone-grafted modified mesoporous silicon oxide material preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment 1, comparative example 1, 2

[0051] (1) The preparation of the sample of Example 1 is carried out according to the following steps:

[0052] Step 1: Weigh mesoporous silica SBA15 (2.4g, pore diameter about 7.2nm, Langmuir specific surface area 556m2 / g), add methanol 40mL, ultrasonically disperse and wash at room temperature 25°C for 1 hour, and then centrifuge ( 9000rpm, 10min), repeat washing three times; add 40mL acetone, ultrasonically disperse at room temperature 25°C for 1 hour, centrifuge, and dry the washed product in a vacuum oven to powder.

[0053] Step 2: Transfer the powdered SBA15 to a 100mL clean schlenk bottle, add a magnetic stirrer, stopper the bottle with a rubber stopper, seal it with parafilm, vacuumize while heating, and continuously vacuum-dry at 250°C for 24 hours. Slowly open the nitrogen gas, cool the SBA15 to room temperature under nitrogen protection, and inject 50 mL of anhydrous CH 2 Cl 2 , ultrasonically disperse at room temp...

Embodiment 2

[0086] Embodiment 2, comparative example 1,2,4

[0087] 1. Sample preparation

[0088] (1) The preparation of the sample of Example 2 is carried out according to the following steps:

[0089] Step 1: Weigh mesoporous silica SBA15 (2.4g, pore diameter about 7.2nm, Langmuir specific surface area 556m2 / g), add methanol 40mL, ultrasonically disperse and wash at room temperature 25°C for 1 hour, and then centrifuge ( 9000rpm, 10min), repeat washing three times; add 40mL acetone, ultrasonically disperse at room temperature 25°C for 1 hour, centrifuge, and dry the washed product in a vacuum oven to powder.

[0090] Step 2: Transfer the powdered SBA15 to a 100mL clean schlenk bottle, add a magnetic stirrer, stopper the bottle with a rubber stopper, seal it with parafilm, vacuumize while heating, and continuously vacuum-dry at 250°C for 24 hours. Slowly open the nitrogen gas, cool the SBA15 to room temperature under nitrogen protection, and inject 50 mL of anhydrous CH 2 Cl 2 , ult...

Embodiment 3

[0115] Example 3, Comparative Examples 1-2,4

[0116] 1. Sample preparation

[0117] (1) The sample preparation of Example 3 is carried out according to the following steps:

[0118] Step 1: Weigh mesoporous silica SBA15 (2.4g, pore diameter about 7.2nm, Langmuir specific surface area 556m2 / g), add methanol 40mL, ultrasonically disperse and wash at room temperature 25°C for 1 hour, and then centrifuge ( 9000rpm, 10min), repeat washing three times; add 40mL acetone, ultrasonically disperse for 1 hour, centrifuge, and dry the washed product in a vacuum oven to powder.

[0119] Step 2: Transfer the powdered SBA15 to a 100mL clean schlenk bottle, add a magnetic stirrer, stopper the bottle with a rubber stopper, seal with parafilm, vacuumize while heating, and continuously vacuum-dry at 250°C for 24 hours. Slowly open the nitrogen gas, cool the SBA15 to room temperature under nitrogen protection, and inject 50 mL of anhydrous CH 2 Cl 2 , ultrasonically disperse at room temperat...

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Abstract

The invention relates to a polyketone-grafted modified mesoporous silicon oxide material preparation method comprising the steps that: (1) mesoporous silicon oxide is subjected to pretreatment, such that clean mesoporous silicon oxide is obtained; (2) the mesoporous silicon oxide obtained in the step (1) is subjected to a reaction with a coupling agent 3-acryloyloxy propyl trichlorosilane, such that coupling-agent-loaded mesoporous silicon oxide is obtained; (3) the coupling-agent-loaded mesoporous silicon oxide is subjected to a reaction with a late transition metal catalyst Pd-alpha-diimine, such that catalyst-loaded mesoporous silicon oxide is obtained; and (4) the catalyst-loaded mesoporous silicon oxide is added into a reaction vessel; 2,2'-bipyridine and 4-tert-butyl styrene (TBS) are added under an atmosphere of carbon monoxide, such that a polymerization reaction is carried out; the obtained reaction mixture is subjected to separation and purification, such that the polyketone-grafted modified mesoporous silicon oxide material is obtained. The method provided by the invention has the advantages of simple process and mild polymerization conditions. With the method, polyketone is grafted on the surface of mesoporous silicon oxide with a covalent bond form, such that the material is more stable than that of other methods.

Description

technical field [0001] The invention relates to a mesoporous silicon oxide pore grafting technology, in particular to a preparation method of a polyketone graft-modified mesoporous silicon oxide material. Background technique [0002] Mesoporous silica is the largest mesoporous molecular sieve so far. This material belongs to mesoporous material. Its pore size is 4.6-30nm, adjustable, and has a large specific surface area, which can reach 600-1000m2 / g. [0003] In recent years, mesoporous silica has been a research hotspot because of its large specific surface area, good hydrothermal stability and biocompatibility. The pore size of SBA15 is adjustable, and the surface can be easily functionalized to be hydrophobic or hydrophilic; the large pore size is conducive to the transport of reactants in the channel, and SBA15, which has been modified to a certain extent, is a suitable chromatographic column packing, which can achieve different sizes of biological Molecules are separ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G67/02C08K9/12C08K9/06C08K3/36C08L73/00C03C4/00
Inventor 徐立新叶誉贤钟明强
Owner ZHEJIANG UNIV OF TECH
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