Allylation hyperbranched polyphenyl ether modified bismaleimide resin and preparation method thereof

A technology of bismaleimide resin and bismaleimide, applied in the field of allylated hyperbranched polyphenylene ether modified bismaleimide resin and its preparation, can solve the unfavorable large-scale industrial Problems such as chemicalization and low product yield, to achieve the effect of excellent manufacturability, abundant raw materials, and outstanding toughness

Inactive Publication Date: 2010-11-10
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Before the present invention was made, the Chinese invention patent "An Allylated Hyperbranched Polyphenylene Ether and Its Preparation Method" (CN101717503A) disclosed a method of preparing allyl-terminated hyperbranched polyphenylene ether with an aqueous alkali metal hydroxide solution as a solvent. The method of polyphenylene ether has the characteristics of green and environmental protection, but the yield of the product prepared by this method is low, which is not conducive to large-scale industrialization
There is no report on the application of allylated hyperbranched polyphenylene ether in BMI modification

Method used

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  • Allylation hyperbranched polyphenyl ether modified bismaleimide resin and preparation method thereof
  • Allylation hyperbranched polyphenyl ether modified bismaleimide resin and preparation method thereof
  • Allylation hyperbranched polyphenyl ether modified bismaleimide resin and preparation method thereof

Examples

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Embodiment 1

[0020] (1) Preparation of hyperbranched polyphenylene ether

[0021] In a nitrogen atmosphere, 2.41g (6.82mmol) 4-bromo-4',4"-dihydroxytriphenylmethane, 1.08g (7.81mmol) anhydrous K 2 CO 3 And 25.0ml of toluene were added to 98ml of dimethyl sulfoxide (DMSO) successively. After heating and refluxing for dehydration for 3 hours, the reaction system was cooled to 45°C, 13.5mg (0.14mmol) of catalyst CuCl was added, and the temperature was raised to 170°C and kept constant React for 40 hours. After the mixture was cooled to room temperature, it was acidified with hydrochloric acid, and after stirring for 0.5 hours, it was dropped into a solution of methanol and water (volume ratio 1:8) for precipitation, filtered, and dried under vacuum at 60°C. The crude product was dissolved in a small amount of tetrahydrofuran (THF), filtered, the filtrate was precipitated with cyclohexane, then filtered, washed with cyclohexane, and dried under vacuum at 90°C to obtain hyperbranched polyphenylene...

Embodiment 2

[0032] Preparation of allylated hyperbranched polyphenylene ether

[0033] Under argon atmosphere, at room temperature, 100g of the hyperbranched polyphenylene ether prepared in step (1) of Example 1, 10g of potassium hydroxide, 100g of dimethylformamide (DMF) and 1g of tetrabutyl bromide Ammonium was put into a three-necked flask. The temperature was raised to 70°C and stirred for 1 hour. After the temperature was lowered to 40°C, 10g of 3-bromopropene was added dropwise, and the dropping was completed within 0.5 hours; then the temperature was raised to 60°C, kept refluxed for 3 hours, then 70°C was raised, kept refluxed for 2 hours. After the completion of the reaction, it was cooled to room temperature, stirred and dropped into a solution of methanol and water (volume ratio 1:3), and filtered. After the filter cake was vacuum-dried at 50°C, it was dissolved in tetrahydrofuran, added dropwise to cyclohexane while stirring, filtered, and the filter cake was dried in vacuum at...

Embodiment 3

[0037] Preparation of allylated hyperbranched polyphenylene ether

[0038] Under a nitrogen atmosphere, at room temperature, 100g of the hyperbranched polyphenylene ether prepared in step (1) of Example 1, 1.5g of sodium hydroxide, 150g of dimethylacetamide (DMAc) and 2g of benzyltriethyl chloride The ammonium hydroxide was put into a three-necked flask. The temperature was raised to 60°C and stirred for 0.5 hour. After the temperature was lowered to 50°C, 20 g of 3-chloropropene was added dropwise, and the dropping was completed in 2.5 hours. Then the temperature was raised to 60°C, kept refluxed for 2 hours, and then raised to 80°C, kept refluxed for 2 hours. After the reaction is completed, cool to room temperature, stir and drop into a solution of methanol and water (volume ratio 1:2), and filter. After the filter cake was vacuum-dried at 60°C, it was dissolved in tetrahydrofuran, added dropwise to cyclohexane while stirring, filtered, and the filter cake was dried in vacu...

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Abstract

The invention discloses an allylation hyperbranched polyphenyl ether modified bismaleimide resin and a preparation method thereof. The method for preparing the resin comprises the following steps of: according to the molar ratio, stirring 100 parts of bismaleimide and 30 to 85 parts of diallylphenyl compound at the temperature of between 110 and 140 DEG C until the mixture is transparent; adding 1 to 55 parts of allylation hyperbranched polyphenyl ether into the mixture; and reacting for 20 to 100 minutes at the temperature of between 110 and 140 DEG C and cooling so as to obtain the allylation hyperbranched polyphenyl ether modified bismaleimide resin. The method for synthesizing the allylation hyperbranched polyphenyl ether by adopting dimethyl sulfoxide and other weak polar solvents has the advantages of simple process, rich raw materials, high yield, and the capacity of meeting the requirement on mass production. The prepared modified bismaleimide resin has the advantages of excellent toughness, heat resistance, wet resistance and higher dielectrical property (low dielectric constant and dielectric loss). The preparation method for the modified bismaleimide resin also has the characteristics of simple process and easy control.

Description

Technical field [0001] The invention relates to an allylated hyperbranched polyphenylene ether modified bismaleimide resin and a preparation method thereof, belonging to the field of polymer materials. Background technique [0002] Bismaleimide (BMI) resin has excellent heat resistance, heat and humidity resistance, dielectric properties, good mechanical properties and dimensional stability, so it is widely used as high-performance adhesives, advanced composite resin matrix, insulating paint, etc. Used in many high-tech fields such as aerospace, electronics and electrical appliances, and transportation. However, BMI cured products are brittle. Since the 1970s, the toughening modification of BMI has been the research focus of high-performance resins. The use of high-performance thermoplastic resins to modify thermosetting resins is the main way to toughen thermosetting resins. At present, polyethersulfone, polyaryletherketone, polyhydantoin, polyarylether, polyimide and polybenzi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F290/06C08F222/40C08G65/48
Inventor 顾嫒娟黄萍珍梁国正袁莉
Owner SUZHOU UNIV
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