Method for preparing vanillin molecular engram polymer

A technology of imprinting polymer and vanillin, which is applied in the separation/purification of carbonyl compounds, organic chemistry, etc., to simplify the production process, facilitate the separation effect, and facilitate the improvement of the effect.

Inactive Publication Date: 2007-12-12
NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Information on the separation of vanillin from complex systems by polymeric materials prepared by this method has not been reported

Method used

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  • Method for preparing vanillin molecular engram polymer
  • Method for preparing vanillin molecular engram polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 1mmol of vanillin and 2mmol, 3mmol, 4mmol, 5mmol, 6mmol, 7mmol of methacrylamide functional monomer and dissolve them in 20mL of dimethyl sulfoxide solvent. After ultrasonic mixing for 15min, add 20mmol of N,N-methylene Based bisacrylamide cross-linking agent, ultrasonically mixed for 5 minutes, the molar ratios of template molecule: functional monomer: cross-linking agent were 1:2:20, 1:3:20, 1:4:20, 1:5: 20, 6 reaction systems of 1:6:20, 1:7:20; then add 5mL of emulsifier Tween-80 to each reaction system, ultrasonically mix for 10min, then add 0.25mmol of initiator azobisisobutyl Nitrile, then add 80mL dimethyl sulfoxide; blow nitrogen for 10min, seal, stir and heat in a water bath at 50°C at 300 rpm, react for 14h, and obtain a polymer containing vanillin.

[0029] Soaking and washing the polymer with dimethyl sulfoxide solvent is repeated 2 to 3 times to completely clean the vanillin remaining on the surface of the polymer. Naturally air-dried to obtain a sol...

Embodiment 2-1

[0031] Embodiment 2-1 dehydrated alcohol example

[0032]Weigh 1mmol of vanillin and 2mmol, 3mmol, 4mmol, 5mmol, 6mmol, 7mmol of methacrylamide respectively and dissolve them in 20mL of absolute ethanol solvent. After ultrasonic mixing for 15min, add 20mmol of cross-linking agent N,N-methylene Bisacrylamide, ultrasonically mixed for 5 minutes, to obtain template molecules: functional monomers: crosslinking agent 1:2:20, 1:3:20, 1:4:20, 1:5:20, 1:6:20, 6 reaction systems of 1:7:20. Add 5mL emulsifier Tween-80 to each system, ultrasonically mix for 10min, then add 0.25mmol initiator azobisisobutyronitrile, and add 80mL absolute ethanol. Nitrogen for 10 minutes, sealed. In a water bath at 50°C, stir and heat at a low speed, and react for 14 hours to obtain a polymer containing vanillin.

[0033] Soaking and washing the polymer with anhydrous ethanol solvent is repeated 2 to 3 times to completely clean the vanillin remaining on the surface of the polymer. Naturally air-dried t...

Embodiment 2-2

[0034] Embodiment 2-2 toluene example

[0035] Weigh 1mmol of vanillin and dissolve them in 20mL of toluene solvent with 2mmol, 3mmol, 4mmol, 5mmol, 6mmol, and 7mmol of methacrylamide respectively, and add 20mmol of cross-linking agent N,N-methylenebispropene after ultrasonic mixing for 15min Amide, ultrasonically mixed for 5min to obtain template molecules: functional monomers: crosslinking agent 1:2:20, 1:3:20, 1:4:20, 1:5:20, 1:6:20, 1: 6 reaction systems of 7:20. Add 5mL of emulsifier Tween-80 to each system, ultrasonically mix for 10min, then add 0.25mmol of initiator azobisisobutyronitrile, and add 80mL of toluene. Nitrogen for 10 minutes, sealed. In a water bath at 50°C, stir and heat at a low speed, and react for 14 hours to obtain a polymer containing vanillin.

[0036] Soaking and washing the polymer with toluene solvent is repeated 2 to 3 times to completely clean the vanillin remaining on the surface of the polymer. Naturally air-dried to obtain a solid polymer...

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Abstract

The invention discloses a method for preparing vanillin molecular imprinting polymer by separating and extracting vanillin produced in industrial process, belonging to high- molecule polymerization field. It comprises following steps: dissolving vanillin module moledule and methacrylamide functional monomer into disslovant, adding crosslinking agent, emulsifying agent and initiator under supersonic condtion, water bathing and getting polymer containing imprinting molecule inside; washing polymer to remove vanillin molecule bond inside of polymer and getting final product. The maximum recovery rate for vanillin is 91%, which is far higher than that of 72% in current industrial separation method. There is no inorganic salt wastewater generation during vanillin separation process. The imprinting polymer is a kind of high- efficiency and clean environmental- protecting material, and the application prospect is quite good.

Description

technical field [0001] The invention belongs to the field of macromolecule polymerization, and specifically uses molecular imprinting technology to synthesize a separation material with a specific recognition ability for vanillin molecules, and the separation material can separate and purify vanillin products produced in industrial synthesis processes A method for preparing a vanillin molecularly imprinted polymer. technical background [0002] Vanillin, whose scientific name is 3-methoxy-4-hydroxybenzaldehyde, is a synthetic fragrance widely used in the world. In recent years, with the continuous expansion of the application field of vanillin, the global demand for vanillin is increasing Increased by 5% per year. At present, the industrialized production of vanillin in China mainly adopts chemical synthesis, and the guaiacol method is one of the most commonly used methods. In 2003, the research and test plant of Jihua Group Corporation built the first domestic production ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/44C08F2/22C08F4/04C08F20/56C08F20/06C08J9/26C07C47/575C07C45/79
Inventor 李鱼翦英红范宁伟张琛王晓丽李都峰
Owner NORTH CHINA ELECTRIC POWER UNIV (BAODING)
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