Preparation method for diether diphthalimide

A technology of diphthalimide and phthalimide, which is applied in the field of preparation of diether diphthalimide, can solve problems such as uneven heating, high boiling point, solvent residue, etc. Simple, waste water reduction effect

Active Publication Date: 2019-05-10
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN1634904A, US4017511A, US4247464A etc. have all reported in aprotic polar solvents such as dimethylsulfoxide (DMSO), N,N'-dimethylformamide (DMF), N,N'-dimethylacetamide ( In DMAC), diether diphthalimides are prepared by reacting phenoxides with phthalimide compounds substituted by benzene rings. Although such solvents can accelerate the nucleophilic substitution reaction on carbon atoms, they have high boiling points and poor thermal stability. , volatile, and miscible with water and organic phases, making it difficult to separate the product
In additi

Method used

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  • Preparation method for diether diphthalimide
  • Preparation method for diether diphthalimide
  • Preparation method for diether diphthalimide

Examples

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Effect test

Embodiment 1

[0047] Add 150 mL of o-xylene in a 500 mL three-necked flask, start stirring, feed nitrogen, then add bisphenol A (22.8 g, 0.1 mol) and sodium hydroxide (8.8 g, 0.22 mol) in sequence, start heating, and the temperature of the system rises to After 100°C, continue to keep warm for 2 hours, then raise the temperature to the reflux of the system (about 143°C), divide the water for 2-3 hours until there is no drop of water in the water separator, and then add 1-butyl-3-methylimidazole hexafluorophosphate ( [BMIM][PF 6 ], 1.42g, 5mmol, purchased from Hubei Yuancheng Saichuang Technology), N-methyl-4-nitrophthalimide (4-NPI, 41.2g, 0.2mol), add 37mL of phthalimide Toluene, heated to 140°C, reacted for 8h, then cooled to normal temperature, poured into 200mL water, heated to 70°C, and kept stirring for 30min, then left to separate layers, took the upper o-xylene layer, repeatedly added water to wash three times, collected organic layer, evaporated to dryness to obtain 52.3g of dieth...

Embodiment 2

[0049] Add 150 mL of o-xylene in a 500 mL three-necked flask, start stirring, feed nitrogen, then add bisphenol A (22.8 g, 0.1 mol) and sodium hydroxide (8.8 g, 0.22 mol) in sequence, start heating, and the temperature of the system rises to After 100°C, continue to keep warm for 2 hours, then raise the temperature to reflux of the system (about 143°C), separate the water for 2-3 hours until there is no drop of water in the water separator, and then add 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIM][BF 4 ]), 1.13g, 5mmol, purchased from Bailingwei Technology Co., Ltd.), N-methyl-4-nitrophthalimide (4-NPI, 41.2g, 0.2mol), add 37mL o-xylene , heated to 140°C, reacted for 8h, then cooled to room temperature, poured into 200mL water, heated to 70°C, and kept stirring for 30min, then stood to separate layers, took the upper o-xylene layer, repeatedly added water to wash three times, and collected the organic layer and evaporated to dryness to obtain 51.8 g of diether diphth...

Embodiment 3

[0051] Add 300mL of toluene into a 1000mL three-necked flask, start the stirring, blow in nitrogen, then add bisphenol S (50.0g, 0.2mol) and potassium hydroxide (23.5g, 0.42mol) in sequence, turn on the heating, and the temperature of the system rises to 100°C Afterwards, continue to keep warm for 2 hours, then raise the temperature to the reflux of the system (about 110°C), separate the water for 3 to 4 hours until there is no drop of water in the water separator, and then add 1-butyl-3-methylimidazolium hexafluorophosphate ([BMIM ][PF 6 ], 4.5g, 16mmol), N-methyl-4-nitrophthalimide (4-NPI, 82.4g, 0.4mol), add 75mL of toluene, heat up to 110°C, react for 6h, then Cool to room temperature, pour into 400mL water, heat to 70°C, and keep stirring for 30min, then let stand to separate layers, take the upper toluene layer, add water to wash three times, collect the organic layer, and evaporate to dryness to obtain diether diphthalimide 107.1 g, yield 94.2%.

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Abstract

The invention discloses a method for preparing diether diphthalimide. The method comprises the following steps: step (A): in a reaction kettle, enabling a diphenol raw material to react with one or more of strong base and strong alkali and weak acid salt in a non-polar solvent, such as methylbenzene or o-xylene, under an inert atmosphere; and step (B): enabling a reaction product of the step (A) to react with phthalimide in the presence of an ionic liquid catalyst, to obtain the diether diphthalimide. The method is capable of performing a nucleophilic reaction in the non-polar solvent, addingionic liquid as a phase transfer catalyst, and improving a reaction yield. After ending the reaction, impurities are removed through a water extraction method, and wastewater generation is greatly reduced. The diether diphthalimide is obtained by reducing a pressure and evaporating an organic layer, a process is simple, and an obtained product is high in purity.

Description

technical field [0001] The invention relates to a preparation method of a diether diphthalimide, in particular to a preparation method of a bisphenol A type diether diphthalimide. Background technique [0002] Diether dianhydride is an important monomer for the synthesis of polyetherimide (PEI), and diether diphthalimide is an important intermediate for the synthesis of bisether dianhydride. The traditional method for preparing diether diphthalimide is to first prepare phenoxide in a non-polar solvent, and then synthesize diether diphthalimide by nucleophilic reaction in a polar aprotic solvent. CN1634904A, US4017511A, US4247464A etc. have all reported in aprotic polar solvents such as dimethylsulfoxide (DMSO), N,N'-dimethylformamide (DMF), N,N'-dimethylacetamide ( In DMAC), diether diphthalimides are prepared by reacting phenoxides with phthalimide compounds substituted by benzene rings. Although such solvents can accelerate the nucleophilic substitution reaction on carbon...

Claims

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Application Information

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IPC IPC(8): C07D209/48
Inventor 屈亚青郗朕捷李旭峰张鑫陈海波
Owner WANHUA CHEM GRP CO LTD
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