Polyimide resin and preparation method thereof

A technology of polyimide resin and diamine monomer, which is applied in the field of polyimide resin and its preparation, can solve the problems of low strength and toughness, low dimensional control precision, insufficient thermal stability, etc., and achieve low viscosity and easy preparation Simple process and excellent performance

Active Publication Date: 2021-11-26
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The main purpose of the present invention is to provide a preparation method of polyimide oligomers for the problems and deficiencies in the prior art, effectively solving the problem of polyimide resin oligomers used in UV light curing additive manufacturing. Problems such as poor fluidity, low dimensional control accuracy, low strength and toughness, and insufficient thermal stability

Method used

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  • Polyimide resin and preparation method thereof
  • Polyimide resin and preparation method thereof
  • Polyimide resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] A kind of polyimide resin that is used for UV photocuring additive manufacturing, its preparation method comprises the steps:

[0062] 1) Under a nitrogen protection atmosphere at -2°C, mix 4.40g of 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (6FOHA) and 2.99g of 1,3-bis(3-aminopropyl ) Tetramethyldisiloxane (SiDA) was poured into a three-necked flask filled with 55ml N-methylpyrrolidone (NMP), stirred until it was completely dissolved, and then 8.88g 4,4'-(hexafluoroisopropylene) diphthalein was added Continue to stir the acid anhydride (6FDA) until it is completely dissolved; then add 1.5g of capping agent maleic anhydride, and stir for 3 hours at -2°C;

[0063] 2) Under a nitrogen protection atmosphere, the temperature was raised to 55°C, 100°C, and 200°C at a rate of 10°C / min in sequence, and the imidization reaction was carried out with stirring and heat preservation treatment for 2 hours respectively; then cooled to room temperature;

[0064] 3) Add 1.50g g...

Embodiment 2

[0067] A kind of polyimide resin that is used for UV photocuring additive manufacturing, its preparation method comprises the steps:

[0068] 1) Under nitrogen protection atmosphere at 2°C, mix 4.40g 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (6FOHA) and 2.99g 1,3-bis(3-aminopropyl) Pour tetramethyldisiloxane (SiDA) into a three-necked flask containing 20ml of tetrahydrofuran, stir until completely dissolved, then add 8.88g of pyromellitic dianhydride (PMDA) and continue stirring until completely dissolved; then add 1.5g of capped agent maleic anhydride, stirred at 2°C for 4 hours;

[0069] 2) Under a nitrogen protection atmosphere, the temperature was raised to 65°C, 110°C, and 210°C at a rate of 10°C / min in sequence, and the imidization reaction was carried out with stirring and heat preservation treatment for 2 hours respectively; then cooled to room temperature;

[0070] 3) Add 1.50 g of glycidyl methacrylate (GMA), 20 mg of triethylamine, 45 mg of tetraethylammoni...

Embodiment 3

[0078] A kind of polyimide resin for UV photocuring additive manufacturing, its synthesis route diagram sees figure 2 , the specific preparation method comprises the following steps:

[0079] 1) Under nitrogen protection atmosphere at 2°C, mix 2.40g 4,4'-diphenyl ether diamine (ODA) and 2.00g 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (6FOHA ) into a three-necked flask filled with 55ml of N-methylpyrrolidone (NMP), stirred until completely dissolved, then added 5.00g of pyromellitic dianhydride (PMDA) and continued to stir until completely dissolved; then added 1.00g of capping agent Toic anhydride, stirred at 2°C for 4h;

[0080] 2) Under a nitrogen protection atmosphere, the temperature was raised to 65°C, 110°C, and 210°C at a rate of 10°C / min in sequence, and the imidization reaction was carried out with stirring and heat preservation treatment for 2 hours respectively; then cooled to room temperature;

[0081] 3) Add 1.50 g of glycidyl methacrylate (GMA), 20 mg ...

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Abstract

The invention relates to polyimide resin, which comprises the following components in percentage by mass: 5 to 25 percent of a composite diamine monomer, 5 to 25 percent of a dianhydride monomer, 45 to 85 percent of an organic solvent, 0.01 to 0.5 percent of an antioxidant, 0.01 to 0.5 percent of a catalyst, 1 to 5 percent of an end-capping reagent and 1 to 5 percent of a photosensitive grafting component. According to the preparation method disclosed by the invention, three improvement means of trifluoromethyl diamine modification, chemical grafting modification and re-dissolution of precipitates in water are combined, and an imidization process is controlled before photocuring additive manufacturing, so that a polyimide resin system with low viscosity and good dispersity is prepared; the stability and the precision of photocuring forming are favorably promoted and improved, and the shrinkage rate of an obtained imidization product can be obviously reduced; and the product has a wide application prospect in the fields of stereo lithography additive manufacturing technologies and the like (such as DLP, SLA and the like).

Description

technical field [0001] The invention belongs to the technical field of functional materials, and in particular relates to a polyimide resin and a preparation method thereof. Background technique [0002] Polyimide (PI), as a class of polymers with imide rings on the main chain, has excellent comprehensive properties due to its highly symmetrical and stable structure, and is widely used in automotive, aerospace and other fields; but it also has poor solubility. , high melting point and other disadvantages, which in turn increases the molding cost and limits its molding shape. [0003] The emergence of additive manufacturing provides a new direction for the molding of polyimide. Photocuring-based additive manufacturing (e.g., SLA and DLP) is capable of generating highly complex 3D geometries from micrometer to mesoscale on a micrometer scale. In addition, due to the excellent fluidity of photosensitive liquid resins, through-hole structures can also be conveniently construct...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C08G73/10C08F283/04C08F222/14B33Y70/00
CPCC08G73/1075C08G73/106C08G73/1039C08G73/1014C08G73/105C08G73/1071C08G73/1042B33Y70/00C08F283/045C08F222/103Y02P10/25
Inventor罗国强刘之强李家劲宋非凡沈强张联盟
OwnerWUHAN UNIV OF TECH