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Method for preparing 2,2-bi[3-(4-carboxylphthalimide)-4-hydroxyphenyl] hexafluoropropane

A phthalimide-based and hydroxyphenyl-based technology, which is applied in the field of preparation of aromatic organic compounds, can solve problems such as no patents or published literature reports, and achieve simple operation, low production cost, and reduced production cost Effect

Inactive Publication Date: 2010-06-02
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Regarding the preparation method of 2,2-bis[3-(4-carboxyphthalimido)-4-hydroxyphenyl]hexafluoropropane, there are no patents or published literature reports so far

Method used

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  • Method for preparing 2,2-bi[3-(4-carboxylphthalimide)-4-hydroxyphenyl] hexafluoropropane
  • Method for preparing 2,2-bi[3-(4-carboxylphthalimide)-4-hydroxyphenyl] hexafluoropropane
  • Method for preparing 2,2-bi[3-(4-carboxylphthalimide)-4-hydroxyphenyl] hexafluoropropane

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Experimental program
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Effect test

Embodiment 1

[0025] Add 18.3 grams (0.05 moles) of 2,2-bis(3-amino-4-hydroxyphenyl) hexafluoropropane (BAHPFP) and 140 milliliters of N-methyl-2-pyrrolidone (NMP) into the reaction kettle together, at room temperature After stirring and dissolving evenly, add 19.2 grams (0.1 moles) of trimellitic anhydride (TMA), after the stirring reaction becomes homogeneous, add 60 milliliters of xylene, nitrogen atmosphere, stir, heat up to reflux at 85°C to 210°C, and azeotrope After the dehydration imidization reaction for 12 hours, recover the azeotropic dehydrating agent xylene and part of the strong polar aprotic organic solvent N-methyl-2-pyrrolidone (NMP), turn off the heating system, stir, naturally cool to room temperature, add water, The solid product was precipitated, filtered, rinsed twice with an appropriate amount of cold NMP solvent, and dried to obtain 33.2 grams of 2,2-bis[3-(4-carboxyphthalimido)-4-hydroxyphenyl]hexafluoropropane (Theoretical amount is 35.7 grams), with a purity of 99...

Embodiment 2

[0027] 18.3 g (0.05 mol) of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (BAHPFP) and 80 ml of N,N-dimethylacetamide (DMAc) were added to the reaction kettle together, After stirring and dissolving evenly at room temperature, add 19.2 g (0.1 mole) of trimellitic anhydride (TMA), and stir to form a homogeneous reaction, then add 800 ml of toluene, stir in a nitrogen atmosphere, heat up to reflux at 85°C to 210°C, and azeotrope After the dehydration imidization reaction for 18 hours, reclaim the azeotropic dehydrating agent toluene and part of the strong polar aprotic organic solvent N,N-dimethylacetamide (DMAc), turn off the heating system, stir, naturally cool to room temperature, add water, The solid product was separated out, filtered, rinsed twice with an appropriate amount of cold N,N-dimethylacetamide (DMAc) solvent, and dried to obtain 34.5 grams of 2,2-bis[3-(4-carboxyphthalimide) )-4-hydroxyphenyl] hexafluoropropane (theoretical amount is 35.7 grams), purity 99.5%...

Embodiment 3

[0029] Add 18.3 grams (0.05 moles) of 2,2-bis(3-amino-4-hydroxyphenyl) hexafluoropropane (BAHPFP) and 100 milliliters of N-methyl-2-pyrrolidone (NMP) into the reaction kettle together, at room temperature After stirring and dissolving evenly, add 21.3 grams (0.11 moles) of trimellitic anhydride (TMA), after the stirring reaction becomes homogeneous, add 60 milliliters of xylene, nitrogen atmosphere, stir, 85 ℃ ~ 210 ℃ heating and reflux, azeotropic After 18 hours of dehydration imidization reaction, recover the azeotropic dehydrating agent xylene and part of the strong polar aprotic organic solvent N-methyl-2-pyrrolidone (NMP), turn off the heating system, stir, naturally cool to room temperature, add water, The solid product was separated out, filtered, rinsed twice with an appropriate amount of cold NMP solvent, and dried to obtain 34.8 grams of 2,2-bis[3-(4-carboxyphthalimido)-4-hydroxyphenyl]hexafluoropropane , purity 99.0%, according to the charging amount of 2,2-bis(3-am...

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Abstract

The invention relates to a method for preparing 2, 2-bis [3-(4- carboxyl phthalimide)-4-hydroxyphenyl] BAHPFP, which includes the following steps: 2, 2-bis (3-amido-4-hydroxyphenyl) BAHPFP with mol ratio of 1.00:2.00-2.22 and TMA are mixed for reaction in strongly polar aprotic organic solvent in inertia atmosphere and room temperature. After becoming homogeneous solution, they are added with azeotropic dehydrating agent for 2-18h azeotropic dehydrating reaction. And then, azeotropic dehydrating agent and strongly polar aprotic organic solvent are collected, and the reaction solution is cooledto the room temperature. At last, water is added to separate the product out, which is filtered, washed, and dried. Characterized with simple operation, friendly operating environment, high yield rate and high purity of the product, and repeated recycling of solvent, the invention is suitable for industrialized production.

Description

technical field [0001] The invention belongs to the field of preparation of aromatic organic compounds, in particular to a preparation method of 2,2-bis[3-(4-carboxyphthalimido)-4-hydroxyphenyl]hexafluoropropane. Background technique [0002] 2,2-bis[3-(4-carboxyphthalimide)-4-hydroxyphenyl]hexafluoropropane is one of the important raw materials for preparing polyamide-imide resin and polyester-imide resin. , is also a good heat-resistant modifier or curing agent for epoxy resin. [0003] Regarding the preparation method of 2,2-bis[3-(4-carboxyphthalimido)-4-hydroxyphenyl]hexafluoropropane, there are no patents or published literature reports so far. Contents of the invention [0004] The purpose of this invention is to provide a kind of 2, the preparation method of 2-bis[3-(4-carboxyphthalimido)-4-hydroxyphenyl] hexafluoropropane, the method process is simple, low in cost and environmentally friendly Friendly, high yield and purity, suitable for industrial production. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/48
Inventor 虞鑫海
Owner DONGHUA UNIV