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Halogen-free phosphorus-containing flame-retardant polyimide resin composition and preparation method thereof

A technology of polyimide resin and composition, applied in the direction of chemical instruments and methods, layered products, metal layered products, etc., can solve the problems of reducing the brittleness of cured products, achieve improved toughness, excellent heat and humidity resistance, and storage Highly stable effect

Active Publication Date: 2011-12-14
INNOTEK TECH CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent application 201010270929 discloses a method of preparing flame retardant resin by reacting DOPO with BMI and allyl compounds, which has good flame retardant effect but also reduces the brittleness of the cured product

Method used

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  • Halogen-free phosphorus-containing flame-retardant polyimide resin composition and preparation method thereof
  • Halogen-free phosphorus-containing flame-retardant polyimide resin composition and preparation method thereof
  • Halogen-free phosphorus-containing flame-retardant polyimide resin composition and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Add 180g of BMI-1000, 90g of BBA, 10g of BE-188EL, and 49.1g of FP-100 into the reaction kettle, and react at 120°C for 5 hours to obtain a polyimide resin composition. The obtained polyimide resin The phosphorus content in the composition is 2.00%.

[0049] Production of copper foil substrate:

[0050] Dilute the resin composition prepared in the above example 1 with methyl ethyl ketone to a solid content of 55%, stir for 3 hours at a stirring speed of 120 rpm, and impregnate 7628 glass fiber cloth on an impregnation machine to make 7628 The glass fiber cloth is impregnated with a resin composition of 43% relative to the weight of the glass fiber cloth, and baked at 210°C for 4 minutes to make a film; stack 6 films, put copper foil on both sides and then press them together , the pressing temperature is 240° C., the pressing time is 3 hours, and the pressing pressure is 400 psi to make a copper foil substrate.

Embodiment 2

[0052] Add 160g of BMI-8000, 100g of DBS, 20g of BE-188EL, and 28.7g of FRPAA into the reaction kettle, and react at 125°C for 4 hours to obtain a polyimide resin composition. The obtained polyimide resin composition The phosphorus content in is 1.60%.

[0053] Production of copper foil substrate:

[0054] Dilute the resin composition prepared in the above example 2 with methyl ethyl ketone to a solid content of 40%, stir for 5 hours at a stirring speed of 50 rpm, and impregnate 7628 glass fiber cloth on an impregnation machine to make 7628 The glass fiber cloth is impregnated with a resin composition of 40% relative to the weight of the glass fiber cloth, and baked at 170°C for 5 minutes to make a film; stack 6 films, put copper foil on both sides and then press them , the pressing temperature is 220° C., the pressing time is 4 hours, and the pressing pressure is 200 psi to make a copper foil substrate.

Embodiment 3

[0056] Add 150g of BMI-6000, 110g of BBA, 15g of BE-188EL, and 27g of FP-100 into the reaction kettle, and react at 130°C for 3 hours to obtain a polyimide resin composition. The obtained polyimide resin composition The phosphorus content in the product is 1.20%.

[0057] Production of copper foil substrate:

[0058] Dilute the resin composition prepared in the above example 3 with methyl ethyl ketone to a solid content of 50%, stir for 4 hours at a stirring speed of 100 rpm, and impregnate 7628 glass fiber cloth on an impregnation machine to make 7628 The glass fiber cloth is impregnated with a resin composition that is 50% of the weight of the glass fiber cloth, and baked at 200°C for 4 minutes to make a film; stack 8 films, put copper foil on both sides and then press them together , the pressing temperature is 230° C., the pressing time is 4 hours, and the pressing pressure is 300 psi to make a copper foil substrate.

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Abstract

The invention relates to a halogen-free phosphorus-containing flame retardant polyimide resin composite, which is characterized by comprising the following components in part by weight: 150 to 180 parts of bismaleimide, 90 to 110 parts of allyl compound, 10 to 20 parts of bisphenol A epoxy resin and 10 to 50 parts of phosphorus-containing compound. The invention also relates to a preparation method for the halogen-free phosphorus-containing flame retardant polyimide resin composite. The method comprises the following steps of: adding the bismaleimide, the allyl compound, the bisphenol A epoxyresin and the phosphorus-containing compound into a reaction kettle, and reacting at the temperature of between 120 and 140 DEG C for 3 to 5 hours to obtain the halogen-free phosphorus-containing flame retardant polyimide resin composite. The halogen-free phosphorus-containing flame retardant polyimide resin composite is synthesized in one step and does not contain halogens and has high flame retardant performance; according to UL94 V0 flame retardant grade tests, the toughness of the cured composite is improved; and the moist heat resistant performance of the composite is high, and the composite meets the requirements of flame retardance and processing in the process of processing copper-clad plates and has high the storage stability.

Description

technical field [0001] The invention relates to a polyimide resin composition used for copper foil substrates or copper-clad boards, in particular to a halogen-free and phosphorus-containing flame-retardant polyimide resin composition and a preparation method thereof. Background technique [0002] Bismaleimide (BMI) is a kind of compound with dual active end groups, which can be cross-linked and cured under the action of heating or catalyst, and has good heat resistance, excellent mechanical properties, moisture resistance and chemical resistance ; And the processing performance is good, the molding process is flexible, the source of raw materials is wide, and the cost is low. It is an ideal matrix resin for advanced composite materials. It has been widely used in aerospace, mechanical electronics, transportation and other departments. However, general-purpose bismaleimide resins have a high melting point and require high-temperature curing, and the cured product has a high ...

Claims

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Application Information

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IPC IPC(8): C08G73/12C08F283/04C08L63/02C08L79/08C08L51/08C08K5/5399C08K5/5313B32B15/08B32B15/20B32B17/04
Inventor 林学佐陈欣宏陈冠青钟迪克
Owner INNOTEK TECH CHINA
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