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Adamantane functionalized polyether carbonate material as well as preparation method and application thereof

A polyether carbonate and functionalized technology is applied in the field of gas chromatography to achieve the effects of high yield, low cost of raw materials, obvious separation advantages and application value

Active Publication Date: 2022-05-13
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Polyether carbonate diol has the advantages of both polyether and polyester. It is often used in leather resin, water-based polyurethane, surface treatment and other fields. It has not been reported in the field of chromatographic analysis.

Method used

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  • Adamantane functionalized polyether carbonate material as well as preparation method and application thereof
  • Adamantane functionalized polyether carbonate material as well as preparation method and application thereof
  • Adamantane functionalized polyether carbonate material as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] A kind of preparation method of adamantane functionalized polyether carbonate material, concrete preparation steps are as follows:

[0035] (1) 1-adamantanecarbonyl chloride is dissolved in anhydrous dichloromethane to obtain the anhydrous dichloromethane solution of 1-adamantanecarbonyl chloride; under nitrogen protection, the number average molecular weight M n =2000 polyether carbonate diol (PPCD) and triethylamine are dissolved in anhydrous dichloromethane (DCM) at a molar ratio of 1:4, and 1-adamantanecarbonyl chloride is slowly added to it under stirring at 0°C. In water dichloromethane solution, the molar ratio of PPCD to 1-adamantanecarbonyl chloride is 1:7.2. After the dropwise addition, stir and react at 30°C for 24 hours. Wash with dilute hydrochloric acid, distilled water, and saturated brine, dry the organic layer with anhydrous magnesium sulfate, and filter, and use the eluent (V 二氯甲烷 :V 甲醇 =40: 1) Separating and purifying on a silica gel column to obtai...

Embodiment 2

[0041] The APPC chromatographic column prepared in Example 1 is used for the separation and determination of octane isomers composed of isooctane, 2,2-dimethylhexane, 3-methylheptane and n-octane:

[0042] The chromatographic parameters are as follows: nitrogen with a purity of 99.99% is the carrier gas, the flow rate is 0.4 mL / min, the column temperature is 30°C, the injection port temperature is 250°C, and the detector temperature is 300°C.

[0043] Separation result as figure 2 As shown, the chromatographic peak numbers 1 to 4 in the figure represent isooctane, 2,2-dimethylhexane, 3-methylheptane and n-octane in turn. Depend on figure 2It can be seen that the octane isomers can be separated by using the APPC chromatographic column and the chromatographic peaks have good symmetry, which shows that the APPC chromatographic column has high selectivity for non-polar alkane isomers and meets the requirements for chromatographic analysis and determination of sample components....

Embodiment 3

[0045] The APPC chromatographic column prepared in Example 1 is used to separate and measure butanediol isomers composed of 2,3-butanediol, 1,3-butanediol and 1,4-butanediol:

[0046] The chromatographic parameters are as follows: nitrogen with a purity of 99.99% is the carrier gas, the flow rate is 1mL / min, the temperature program is 100°C to 160°C (the temperature rise rate is 10°C / min), the inlet temperature is 250°C, and the detector temperature is 300°C .

[0047] Separation result as image 3 As shown, the chromatographic peak numbers 1 to 3 in the figure represent 2,3-butanediol, 1,3-butanediol and 1,4-butanediol in turn. Depend on image 3 It can be seen that the APPC chromatographic column can baseline-separate easily adsorbed butanediol isomers and the chromatographic peaks have good symmetry, indicating that the APPC chromatographic column has high selectivity and good inertness to alcohol isomers, which meets the requirements of sample component chromatographic a...

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Abstract

The invention relates to an adamantane functionalized polyether carbonate material as well as a preparation method and application thereof, and belongs to the technical field of gas chromatography. The material is formed by bonding an adamantane unit and a chain polyether carbonate structure. The method comprises the following steps: dissolving polyether carbonate diol and an alkaline reagent in an organic solvent under the protection of protective gas, dropwise adding a 1-adamantane formyl chloride solution while stirring at the temperature of-4 DEG C to 0 DEG C, reacting after dropwise adding to obtain a crude product, and separating and purifying to obtain the material. When the material is used as a gas chromatography stationary phase, various isomers with different types and properties can be efficiently separated.

Description

technical field [0001] The invention relates to an adamantane functionalized polyether carbonate material, a preparation method and an application thereof, and belongs to the technical field of gas chromatography. Background technique [0002] Gas chromatography (GC) has been widely used in the analysis and determination of sample components in many fields. In GC analysis, the selectivity and inertness of the stationary phase are the main factors that determine the resolution of component chromatographic peaks, and the resolution directly affects the qualitative / quantitative analysis results of components. At present, the most commonly used GC stationary phases are polysiloxanes and polyethylene glycols, which are suitable for the separation of near-polar components to the stationary phase, which affects the separation, analysis and determination of complex sample components to a certain extent. For example, the polar polyethylene glycol stationary phase is mainly suitable ...

Claims

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Application Information

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IPC IPC(8): C08G64/42B01J20/26B01J20/281B01J20/30
CPCC08G64/42B01J20/281B01J20/265
Inventor 齐美玲孙子琦
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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