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A kind of tetraphenylphenyl graft polysiloxane and its preparation method and application

A technology of tetraphenylphenyl and polysiloxane, which is applied in chemical instruments and methods, and other chemical processes, can solve the problems of loss of stationary phase and lack of high selectivity, and achieve low column loss and excellent separation selectivity , the effect of novel structure

Inactive Publication Date: 2011-12-28
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are many GC stationary phases available today, there is still a lack of high selectivity and low bleed stationary phases

Method used

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  • A kind of tetraphenylphenyl graft polysiloxane and its preparation method and application
  • A kind of tetraphenylphenyl graft polysiloxane and its preparation method and application
  • A kind of tetraphenylphenyl graft polysiloxane and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Example 1 Preparation of tetraphenylphenyl graft polysiloxane, the preparation method is as follows:

[0024] (1) Synthesis of tetraphenylcyclopentadienone: add 7.0g benzil and 7.0g dibenzyl ketone into a 100ml three-necked round-bottom flask, then add 50ml hot ethanol; nitrogen protection, heating and stirring, in When the solution was close to boiling, slowly add dropwise the ethanol solution of 5.0ml potassium hydroxide in the solution, the concentration of potassium hydroxide is 0.2g / ml (1.0g potassium hydroxide is dissolved in 5.0ml ethanol), and continue to reflux for 15 Stop the reaction after a few minutes, cool and filter with suction to obtain a black powder which is tetraphenylcyclopentadienone; recrystallize it in a mixed solvent of ethanol:toluene=1:1, dry it in the air, and set aside.

[0025] (2) Preparation of methylvinyl silicone raw rubber: add 31.0g octamethylcyclotetrasiloxane and 4.0g tetramethyltetravinylcyclotetrasiloxane to a 250ml four-necked ro...

Embodiment 2

[0028] Embodiment 2 prepares tetraphenylphenyl graft polysiloxane, and preparation method is as follows:

[0029] (1) Synthesis of tetraphenylcyclopentadienone: add 7.0g benzil and 7.0g dibenzyl ketone into a 100ml three-necked round-bottom flask, then add 50ml hot ethanol; nitrogen protection, heating and stirring, in When the solution is close to boiling, slowly add dropwise the ethanol solution of 5.0ml potassium hydroxide in the solution, the concentration of potassium hydroxide is 0.2g / ml (1.0g potassium hydroxide is dissolved in 5.0ml ethanol), continue to reflux for 20 Stop the reaction after a few minutes, cool and filter with suction to obtain a black powder which is tetraphenylcyclopentadienone; recrystallize it in a mixed solvent of ethanol:toluene=1:1, dry it in the air, and set aside.

[0030] (2) Preparation of methylvinyl silicone raw rubber: add 31.0g octamethylcyclotetrasiloxane and 4.0g tetramethyltetravinylcyclotetrasiloxane to a 250ml four-necked round-bott...

Embodiment 3

[0032] Embodiment 3 prepares tetraphenylphenyl graft polysiloxane, and preparation method is as follows:

[0033] (1) Synthesis of tetraphenylcyclopentadienone: add 7.0g benzil and 7.0g dibenzyl ketone into a 100ml three-necked round-bottom flask, then add 50ml hot ethanol; nitrogen protection, heating and stirring, in When the solution is close to boiling, slowly add 5.0ml of potassium hydroxide ethanol solution dropwise to the solution, the concentration of potassium hydroxide is 0.2g / ml (1.0g of potassium hydroxide is dissolved in 5.0ml of ethanol), and continue to reflux for 16 Stop the reaction after a few minutes, cool and filter with suction to obtain a black powder which is tetraphenylcyclopentadienone; then recrystallize it in a mixed solvent of ethanol:toluene=1:1, dry it in the air, and set aside.

[0034] (2) Preparation of methylvinyl silicone raw rubber: add 31.0g octamethylcyclotetrasiloxane and 4.0g tetramethyltetravinylcyclotetrasiloxane to a 250ml four-necked...

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Abstract

The invention discloses a tetraphenylphenyl graft polysiloxane, the structural formula is as shown in the attached drawing of the abstract, and the molecular weight is 85,000-100,000. The invention also discloses its preparation method: mixing tetraphenylcyclopentadienone, anhydrous diphenyl ether, and methyl vinyl silicon raw rubber, and grafting to methyl vinyl silicon raw rubber through Diels-Alder reaction Just go up. The invention also discloses the use of tetraphenylphenyl-grafted polysiloxane, which can be used as a stationary phase of gas chromatography, relying on its strong inductive action and dispersion force, in addition to separating general hydrocarbon substances , It has excellent separation selectivity for substituted isomers of benzene, fused ring aromatics, aza, oxa, thia condensed ring aromatics, polycyclic aromatic hydrocarbons and other environmental pollutants.

Description

technical field [0001] The invention relates to a tetraphenylphenyl grafted polysiloxane, a preparation method thereof and an application as a gas chromatography stationary phase. Background technique [0002] Capillary gas chromatography is characterized by high resolution and is widely used in petrochemical, organic synthesis, physiological and biochemical, medical and health fields. To make the capillary chromatographic column have good performances such as high column efficiency, low activity and high stability, it is necessary to synthesize a chromatographic stationary phase with excellent performance. In gas chromatography, polysiloxane is the most widely used stationary phase, and this type of stationary phase is also an important research content of chromatographers in recent years. Bernhard X.Mayer etc. synthesized 50% n-octylmethyl, 50% diphenyl polysiloxane (Analyst, 2003, 128, 1238-1242) and 75% diphenyl, 25% dimethyl polysiloxane Alkanes (J.Sep.Sci., 2002, 25,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/38C08G77/20B01J20/285
Inventor 吴波滕爽赵军栾维东李建平
Owner SHANDONG UNIV