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Preparation methods of 1,4,7,10-tetraazacyclododecane and nanofiltration membrane

A technology for tetraazacyclododecane, which is applied in the preparation of polyamide nanofiltration membranes and 1,4,7,10-tetraazacyclododecane, can solve complex processes, yield and purity low problems, to achieve the effect of high purity, good retention effect and good oxidation resistance

Inactive Publication Date: 2015-03-04
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the above-mentioned technical problems in the prior art, the present invention provides a kind of preparation method of 1,4,7,10-tetraazacyclododecane and nanofiltration membrane thereof, said 1,4,7 , The preparation method of 10-tetraazacyclododecane and its nanofiltration membrane should solve the complex process, yield and purity of 1,4,7,10-tetraazacyclododecane in the prior art. low technical issues

Method used

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  • Preparation methods of 1,4,7,10-tetraazacyclododecane and nanofiltration membrane
  • Preparation methods of 1,4,7,10-tetraazacyclododecane and nanofiltration membrane
  • Preparation methods of 1,4,7,10-tetraazacyclododecane and nanofiltration membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) In a three-neck flask equipped with a stirrer and a thermometer, add 86g of TETA, 130mL of solvent toluene, and 20g of water, stir, and cool to below 10°C, white crystals are precipitated, filtered by suction, and dried in a vacuum desiccator to obtain White crystals, 98.1 g of TETA hydrated crystals.

[0027] (2) Add 98.1g of TETA hydrated crystals into a three-necked flask with a water separator, add an appropriate amount of toluene, and heat to reflux to separate water. When the temperature of the liquid rose to 122°C, the water separation was stopped, and the TETA toluene solution in the reaction bottle was dried with anhydrous potassium carbonate. After standing still for 5 hours (so that potassium carbonate can fully absorb water and precipitate), filter potassium carbonate, evaporate toluene under reduced pressure, and obtain 58.9 g of linear TETA.

[0028] (3) Add TETA58.9g, DMF-DMA96.09g, and solvent toluene 200mL into a four-necked flask equipped with a r...

Embodiment 2

[0032] (1) In a three-neck flask equipped with a stirrer and a thermometer, add 64.8g of TETA, 98mL of solvent toluene, and 15.1g of water, stir, and cool to below 10°C, white crystals are precipitated, filtered by suction, and dried in a vacuum desiccator , to obtain white crystals, that is, 81.3 g of TETA hydrated crystals.

[0033] (2) Add 81.3g of TETA hydrated crystals into a three-necked flask with a water separator, add an appropriate amount of toluene, and heat to reflux to separate water. When the temperature of the liquid rose to 123°C, the water separation was stopped, and the TETA toluene solution in the reaction bottle was dried with anhydrous potassium carbonate. After standing still for 4.5h, potassium carbonate was filtered, and the toluene was evaporated under reduced pressure to obtain 50.2g of linear TETA.

[0034] (3) In a four-necked flask equipped with a reflux condenser, a thermometer, and a stirrer, add 50.2g of TETA, 80.7g of DMF-DMA, and 195mL of tol...

Embodiment 3

[0038] (1) In a three-necked flask equipped with a stirrer and a thermometer, add 110g of TETA, 166mL of solvent toluene, and 31.3g of water, stir, and cool to below 10°C, white crystals are precipitated, filtered by suction, and dried in a vacuum desiccator. Obtained white crystals, namely 129 g of TETA hydrated crystals.

[0039] (2) Add 129g of TETA hydrated crystals into a three-necked flask with a water separator, add an appropriate amount of toluene, and heat to reflux to separate water. When the temperature of the liquid rose to 125°C, the water separation was stopped, and the TETA toluene solution in the reaction bottle was dried with anhydrous potassium carbonate. After standing for 5 hours, potassium carbonate was filtered, and the toluene was evaporated under reduced pressure to obtain 81.9 g of linear TETA.

[0040] (3) Add TETA81.9g, DMF-DMA135.7g, and solvent toluene 300mL into a four-necked flask equipped with a reflux condenser, a thermometer, and a stirrer. U...

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Abstract

The invention discloses a preparation method of 1,4,7,10-tetraazacyclododecane. The method comprises the following steps: adopting triethylene tetramine, methyl benzene and water to obtain a triethylene tetramine hydrated crystal substance; heating the triethylene tetramine hydrated crystal substance and the methyl benzene to react to obtain a triethylene tetramine-methyl benzene solution, and obtaining linear triethylene tetramine through drying, filtration and reduced pressure distillation; enabling the linear triethylene tetramine, N,N-dimethylformamide dimethylacetal and methyl benzene to react, and crystallizing to obtain clear crystal bis-imidazoline; enabling potassium carbonate, solvent acetonitrile, bis-imidazoline and 1,2-ethylene dibromide to react, and conducting reduced pressure distillation, washing and drying to obtain bromine; under the protection of nitrogen, adding a potassium hydroxide water solution, heating to a back flow state, dropwise adding a bromine salt water solution, and conducting filtration, precipitation, condensation, cooling and crystallization to obtain the 1,4,7,10-tetraazacyclododecane. The invention also provides a preparation method of a polyamide nanofiltration membrane. According to the invention, the purity of 1,4,7,10-tetraazacyclododecane is improved.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a 1,4,7,10-tetraazacyclododecane, specifically a preparation of a 1,4,7,10-tetraazacyclododecane The method and the method for preparing polyamide nanofiltration membrane by using 1,4,7,10-tetraazacyclododecane. Background technique [0002] Macrocyclic polyamines refer to macrocyclic compounds containing multiple amino groups. Macrocyclic polyamines are a very important class of main molecules in supramolecular chemistry. They have strong coordination capabilities for metal ions. The formed metal complexes It is also a class of compounds with unique structures and properties. Due to the wide application of macrocyclic polyamine compounds and their complexes, their research has become one of the emerging topics in the new research field in recent years. They are not only widely used in transition metal complexes, but also have important application value in molecular r...

Claims

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Application Information

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IPC IPC(8): C07D257/02C08J7/16B01D71/56B01D69/12B01D67/00B01D61/02
CPCB01D61/027B01D67/0093B01D69/125B01D71/56B01D2311/00C07D257/02C08J7/16
Inventor 陈桂娥刘延军许振良管方方孙丽黄会红陆晓孝徐孙杰朱维纬
Owner SHANGHAI INST OF TECH
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