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Preparation method of 1,4-bi(4-maleimide-2-trifluoromethylphenoxy) benzene

A technology based on trifluoromethylphenoxy and maleimide, which is applied in 1 field, can solve problems such as unseen problems, and achieve the effects of high product yield and purity, simple operation process, and low investment in reaction equipment

Inactive Publication Date: 2012-08-08
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] But, do not see relevant 1, the preparation method of 4-bis(4-maleimido-2-trifluoromethylphenoxy) benzene, only report it as a kind of bismaleimide resin Raw materials, application in the preparation of polyacrylimide foam materials

Method used

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  • Preparation method of 1,4-bi(4-maleimide-2-trifluoromethylphenoxy) benzene
  • Preparation method of 1,4-bi(4-maleimide-2-trifluoromethylphenoxy) benzene
  • Preparation method of 1,4-bi(4-maleimide-2-trifluoromethylphenoxy) benzene

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Embodiment 1

[0038]Add 42.8 grams (0.1 mole) of 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene (BAPB-2TF) and 190 milliliters of N-methyl-2-pyrrolidone into the reactor at room temperature Under stirring, after dissolving completely, add maleic anhydride solid in batches, make reaction temperature maintain at room temperature state, add maleic anhydride (MA) solid 20.5 grams (0.21 mol) altogether, stir reaction 1 hour at room temperature, obtain 1,4 - bis(4-carboxycrotonamido-2-trifluoromethylphenoxy)benzene (BAPB-2TF-BMA) solution; subsequently, add 1.0 g of anhydrous calcium chloride powder, 205 ml of toluene azeotropic dehydrating agent , 1.0 grams of N,N-dimethylaniline, stirred, heated up until reflux water separation, after 2 to 3 hours, distilled toluene azeotropic dehydrating agent (recycling and recycling), cooled to room temperature, added dropwise under high-speed stirring 214 milliliters of ethanol, the solid product was precipitated, filtered, the mother liquor was purified ...

Embodiment 2

[0047] 42.8 g (0.1 mol) of 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene (BAPB-2TF), 60 ml of N-methyl-2-pyrrolidone and 500 ml of N,N -Dimethylformamide is added in the reactor, stirred at room temperature, after dissolving completely, add maleic anhydride solid in batches, make reaction temperature maintain at room temperature state, add maleic anhydride (MA) solid 19.6 grams (0.2 mol) altogether , stirred at room temperature for 1 hour to obtain 1,4-bis(4-carboxybutenamido-2-trifluoromethylphenoxy)benzene (BAPB-2TF-BMA) solution; subsequently, add 1.0 g of anhydrous Calcium chloride powder, 98 milliliters of xylene azeotropic dehydrating agent, 0.5 gram of N, N-dimethylaniline, stir, heat up until reflux water separation, after 2 to 3 hours, distill out xylene azeotropic dehydrating agent (recovery 428 milliliters of ethanol was added dropwise under high-speed stirring, and the solid product was precipitated, filtered, mother liquor fractionated and purified for recyclin...

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Abstract

The invention disposes a preparation method of 1,4-bi(4-maleimide-2-trifluoromethylphenoxy) benzene, mainly comprising the following steps of: (1) reacting 1,4-bi(4-amino-2-trifluoromethylphenoxy) benzene and maleic anhydride which have the molar ratio of 1.0:2.0-2.1 in an organic solvent system at room temperature for 1 hour to obtain a 1,4-bi(4-carboxyl crotonamide-2-trifluoromethylphenoxy) benzene solution; (2) adding anhydrous calcium chloride solid powder, an azeotropic dehydrating agent and N,N-dimethylaniline, heating, refluxing and diverting water to react for 2-3 hours, then distilling to obtain the azeotropic dehydrating agent, cooling to room temperature, dripping ethanol under high-speed stirring, precipitating solid products, filtering, washing, and drying so as to obtain 1,4-bi(4-maleimide-2-trifluoromethylphenoxy) benzene powder. The invention has the advantages of simple operation process, high yield coefficient, little three wastes, environmental protection and suitability for industrialization production.

Description

technical field [0001] The invention relates to a preparation method of an organic compound, in particular to a preparation method of 1,4-bis(4-maleimido-2-trifluoromethylphenoxy)benzene. Background technique [0002] People synthesized bismaleimide resin (BMI) as early as the 1940s. As early as 1948, American Searle obtained a patent for BMI synthesis. Since then, Searle has synthesized various BMI monomers with different structures and properties on the basis of improving the synthesis method. By the end of the 1960s, the French Rhone-Poulenc company first developed M-33BMI resin and its composite materials. Early work focused on high-temperature-resistant fiberglass insulation. In the late 1970s, in order to solve the problem of poor moisture and heat resistance of epoxy, BMI began to be used as an advanced composite material (ACM) matrix and aerospace materials. In the past two decades, BMI resin has been developed rapidly and widely used. There are no less than 20 ki...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D207/452
Inventor 虞鑫海陈梅芳
Owner DONGHUA UNIV