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2-methyl-3,4-diphenyl phenyl-grafted polysiloxane and preparation method and application thereof

A technology of diphenylphenyl and polysiloxane, which is applied in the application field of gas chromatography stationary phase, can solve the problems of inability to meet the requirements of separation of complex mixture samples, and achieves excellent separation selectivity, excellent heat resistance and chromatographic properties. Separation of selective effects

Inactive Publication Date: 2011-08-31
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are a variety of reported and commercialized stationary phases, they still cannot meet the requirements for the separation of complex mixture samples. The stationary phases with good reproducibility, easy coating, high selectivity and good temperature resistance are still the most important. Important tasks for chromatographers

Method used

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  • 2-methyl-3,4-diphenyl phenyl-grafted polysiloxane and preparation method and application thereof
  • 2-methyl-3,4-diphenyl phenyl-grafted polysiloxane and preparation method and application thereof
  • 2-methyl-3,4-diphenyl phenyl-grafted polysiloxane and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 2-Methyl-3, the preparation of 4-diphenylphenyl grafted polysiloxane, the specific preparation method is as follows:

[0036] (1) Synthesis of 2-methyl-3,4-diphenylcyclopentadienone:

[0037] 1. 4-hydroxyl-2 (5)-methyl-3, the synthesis of 4-diphenyl-cyclopent-2-enone: add 21.0g (0.1mol) benzil in 500ml round bottom flask, 18.0ml ( 0.2mol) butanone, 1.3g potassium hydroxide and 250.0ml absolute absolute ethanol, and electromagnetically stirred at room temperature for 24h. The reaction solution was poured into a beaker containing 1000ml of water, stirred to disperse the product, left to stand for 2 hours, and filtered with suction to obtain a white powder. It was recrystallized in a mixed solution of ethanol / water and fully dried to obtain 4-hydroxy-2(5)-methyl-3,4-diphenyl-cyclopent-2-enone as white crystals.

[0038] ② Synthesis of 2-methyl-3,4-diphenylcyclopentadienone: 25.0g (0.095mol) 4-hydroxyl-2(5)-methyl-3,4-diphenyl-cyclopentadienone Put 2-enone into a dry 100...

Embodiment 2

[0045] 2-Methyl-3, the preparation of 4-diphenylphenyl grafted polysiloxane, the specific preparation method is as follows:

[0046] (1) Synthesis of 2-methyl-3,4-diphenylcyclopentadienone:

[0047] 1. 4-hydroxyl-2 (5)-methyl-3, the synthesis of 4-diphenyl-cyclopent-2-enone: add 21.0g (0.1mol) benzil in 500ml round bottom flask, 18.0ml ( 0.2mol) butanone, 1.3g potassium hydroxide and 250.0ml absolute absolute ethanol, and electromagnetically stirred at room temperature for 24h. The reaction solution was poured into a beaker containing 1000ml of water, stirred to disperse the product, left to stand for 2 hours, and filtered with suction to obtain a white powder. It was recrystallized in a mixed solution of ethanol / water and fully dried to obtain 4-hydroxy-2(5)-methyl-3,4-diphenyl-cyclopent-2-enone as white crystals.

[0048] ② Synthesis of 2-methyl-3,4-diphenylcyclopentadienone: 25.0g (0.095mol) 4-hydroxyl-2(5)-methyl-3,4-diphenyl-cyclopentadienone Put 2-enone into a dry 100...

Embodiment 3

[0054] 2-Methyl-3, the preparation of 4-diphenylphenyl grafted polysiloxane, the specific preparation method is as follows:

[0055] (1) Synthesis of 2-methyl-3,4-diphenylcyclopentadienone: ① 4-hydroxyl-2(5)-methyl-3,4-diphenyl-cyclopentadienone Synthesis: 21.0g (0.1mol) of benzil, 18.0ml (0.2mol) of butanone, 1.3g of potassium hydroxide and 250.0ml of absolute ethanol were added to a 500ml round bottom flask, and electromagnetically stirred at room temperature for 24h. The reaction solution was poured into a beaker containing 1000ml of water, stirred to disperse the product, left to stand for 2 hours, and filtered with suction to obtain a white powder. It was recrystallized in a mixed solution of ethanol / water and fully dried to obtain 4-hydroxy-2(5)-methyl-3,4-diphenyl-cyclopent-2-enone as white crystals.

[0056] ② Synthesis of 2-methyl-3,4-diphenylcyclopentadienone: 25.0g (0.095mol) 4-hydroxyl-2(5)-methyl-3,4-diphenyl-cyclopentadienone Put 2-enone into a dry 100ml round-...

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Abstract

The invention provides 2-methyl-3,4-diphenyl phenyl-grafted polysiloxane of which the structural general formula is shown in the drawing of the abstract, wherein m and n are positive integers; and the ratio of m to n is 9:1, and the molecular weight is 80,000-100,000. The invention also provides a preparation method of 2-methyl-3,4-diphenyl phenyl-grafted polysiloxane. The preparation method is as follows: 2-methyl-3,4-diphenylcyclopentadienone is grafted onto methyl vinyl silicone raw rubber through Diels-Alder reaction to prepare 2-methyl-3,4-diphenyl phenyl-grafted polysiloxane. The invention also provides an application of 2-methyl-3,4-diphenyl phenyl-grafted polysiloxane used as gas chromatographic stationary phase.

Description

technical field [0001] The invention relates to a 2-methyl-3,4-diphenylphenyl grafted polysiloxane, its preparation method and its application as a gas chromatography stationary phase. Background technique [0002] Since its invention in 1956, capillary chromatographic columns have been widely used in various industries due to their characteristics of fast, efficient, and high sensitivity. The chromatographic column is the most important part of gas chromatography, and the stationary phase in the capillary determines the separation performance of the chromatographic column. Polysiloxane has been widely used as a stationary phase in capillary gas chromatography due to its good temperature resistance and easy film formation (J.Sep.Sci., 2001, 24(6), 473-476). People such as M.L.Lee have done a lot of work (Journal of High Resolution Chromatography, 2005, 7 (2), 89-92. Journal of Microcolumn Separations, 2005, 1(3), 142-149). Although there are a variety of reported and comm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38C07C49/657C07C45/66B01J20/285B01D15/22
Inventor 吴波高尧华朱晨牛妍妍周阳
Owner SHANDONG UNIV
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