Process for preparing biphthalimide

A bisphthalimide and primary amine technology, which is applied in the field of preparation of organic compounds, can solve problems such as no published literature or patent reports, and achieve simple operation, no environmental pollution, high product yield and purity Effect

Inactive Publication Date: 2007-08-01
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Bisphthalimide compounds have good application prospects in electronic components due to their excellent resistance to alternating cold and heat, but there are no published literature or patent reports on the preparation of bisphthalimides

Method used

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  • Process for preparing biphthalimide
  • Process for preparing biphthalimide
  • Process for preparing biphthalimide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 60 grams (1.0 moles) of ethylenediamine (EDA) and 2000 milliliters of N-methyl-2-pyrrolidone (NMP) were added together in the reaction kettle, after stirring at room temperature, the ice-water bath was cooled to keep the temperature in the reaction system at Within the temperature range of 0°C to 10°C, add phthalic anhydride (PA) in batches, totaling 370 g (2.5 moles), stir and react at 0°C to 10°C for 5 hours, add 800 ml of xylene, and stir , heated up to 140°C, refluxed water separation reaction for 10 hours, turned off the heating system, stirred, naturally cooled to room temperature, and precipitated a white solid product, filtered, rinsed twice with an appropriate amount of cold NMP solvent, and dried to obtain 313.6 grams ( Yield: 98%) white crystals of N,N'-(1,2-ethylene)bisphthalimide with a purity of 99.8%.

Embodiment 2

[0034]74 grams (1.0 moles) of 1,3-propanediamine (13PDA) and 2000 milliliters of N,N-dimethylacetamide (DMAc) were added to the reaction kettle together, after stirring at room temperature, the ice-water bath was cooled to make the reaction The temperature in the system was maintained within the temperature range of 0°C to 10°C, and phthalic anhydride (PA) was added in batches, totaling 325.6 grams (2.2 moles). After stirring and reacting at 0°C to 10°C for 3 hours, 2000 Milliliter of toluene, stirred, heated up to 120 ° C, refluxed water separation reaction for 8 hours, turned off the heating system, stirred, naturally cooled to room temperature, a white solid product was precipitated, filtered, rinsed twice with an appropriate amount of cold DMAc solvent, and dried. 317.3 g (95% yield) of white N,N'-(1,3-propylene)bisphthalimide crystals were obtained with a purity of 99.6%.

Embodiment 3

[0036] Add 23.8 g (0.1 mol) of 3,3'-dimethyl-4,4'-diaminodicyclohexylmethane (DMDACM) and 300 ml of N,N-dimethylformamide (DMF) into the reaction kettle together , after stirring evenly at room temperature, cooling in an ice-water bath to maintain the temperature in the reaction system within the temperature range of 0°C to 10°C, adding phthalic anhydride (PA) in batches, a total of 32.6 grams (0.22 moles), at 0 After stirring and reacting at ℃~10℃ for 1 hour, add 600 ml of toluene, stir, heat up to 110℃, reflux and water separation reaction for 10 hours, turn off the heating system, stir, and naturally cool to room temperature, a white solid product is precipitated, filtered, Rinse twice with an appropriate amount of cold DMF solvent, and dry to obtain 47.8 grams (96% yield) of white N, N'-[4-methylene-bis(3-methylcyclohexyl)]bisphthaloimide Amine crystals with a purity of 99.2%.

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PUM

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Abstract

The invention relates to a method for preparing biphthalimide, comprising following steps: (1) putting binary primary amine and ortho-phthalic anhydride with the molar ratio being 1.0: 2.0-2.5 in strong polar non-polar organic solvent, reacting for 1-5 hours at 0- 10 Deg. C and getting clean, transparent and homogeneous solution; (2) adding azeotropic anhydrating agent, heating to 110- 150 Deg. C, refluxing imination catalyst and reacting for 1- 10 hours, cooling, crystallizing, filtering, washing and drying, getting biphthalimide, and volume ratio between strong non-polar organic solvent and azeotropic anhydrating agent is 1.0: 0.1- 10. The invention is characterized by high productivity, high purity of above 99%, reusable solvent, simple operation, environment-friendly and suitability for industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of organic compounds, in particular to a preparation method of bisphthalimide. Background technique [0002] The imide ring organic compound has very high thermal stability (that is, its molecular structure is stable and does not undergo chemical changes after repeated cycles of hot melting, cooling and solidification), solvent resistance, radiation resistance and flame retardancy. Therefore, it can be used as a heat-resistant modifier or heat-resistant curing agent for various resin systems (such as epoxy resin, phenolic resin, polyurethane resin, polyester resin, polyamide resin and silicone resin, etc.), and can also be used as a synthetic polymer Raw material intermediate of imide resin. [0003] Polyimide resin is a kind of polymer with excellent comprehensive performance, which has excellent heat resistance, low temperature resistance, solvent resistance, self-lubrication, radiation resistance an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/48
Inventor 虞鑫海徐永芬赵炯心
Owner DONGHUA UNIV
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