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A kind of selective laser sintering polyimide powder and its preparation method

A technology of laser sintering molding and polyimide powder, which is applied in the direction of additive processing, etc., can solve the problems of not reaching the fineness of SLS material molding, the price is difficult to promote and use on a large scale, and the particle size of materials is large, so as to meet the selection requirements The effect of precise laser sintering molding process requirements, broadening the solvent system, and uniform particle size distribution

Active Publication Date: 2018-06-15
JIANGHAN UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The only high-grade heat-resistant material that has been developed so far is polyetheretherketone (PEEK), and because of the high price of polyetheretherketone (PEEK), although PEEK has good performance in some application fields, it is hindered by the high price. Difficult to popularize and utilize on a large scale (Shi Yusheng, Yan Chunze, Wei Qingsong, etc. Polymer composite materials for selective laser sintering 3D printing. Chinese Science: Information Science, 2015,45:204)
[0005] Therefore, many researchers are devoting themselves to adopting various methods to prepare heat-resistant polymer materials applicable to the SLS mode. However, the existing polyimide powders have the following defects: (1) The method of making powders is cryogenic ball milling , the particle size of the prepared material is relatively large, which cannot meet the requirements of SLS material molding fineness; (2) in the current general polyimide preparation method, the slurry is a polyamic acid prepolymer, and the slurry The prepared powder is polyamic acid, which requires further imidization to meet the high-temperature use requirements of the material; (3) Even if chemical imidization is used to prepare polyimide slurry, the synthesis process uses a large amount of acetic anhydride, pyridine, triethyl Reagents such as amines, the processing pollution is relatively large, and the cost is high. This method is rarely used in industry

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  • A kind of selective laser sintering polyimide powder and its preparation method
  • A kind of selective laser sintering polyimide powder and its preparation method
  • A kind of selective laser sintering polyimide powder and its preparation method

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Embodiment 1

[0042] A preparation method for selective laser sintering molding polyimide powder, comprising the steps of:

[0043] 1) Under the protection of nitrogen or argon, add 1.0814g (10mmol) of p-phenylenediamine into 23g of 1-butyl-3-methylimidazolium bromide solvent (15% solid content), heat up to 50°C and stir to fully dissolve it Afterwards, cool to room temperature for subsequent use;

[0044] 2) Add 2.9422g (10mmol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride to the solution obtained in step 1) in batches, the interval between each batch is 30min, and then gradually raise the temperature to 180°C In the process of gradually heating up, firstly, the temperature is raised from normal temperature to 100°C at a rate of 20°C / min, and then the temperature is kept at 20°C for 20 minutes until the temperature reaches 180°C. After 8 hours of continuous reaction, it is washed and dried in turn. During the drying process, first add an appropriate amount of methanol and deionized wa...

Embodiment 2

[0046] A preparation method for selective laser sintering molding polyimide powder, comprising the steps of:

[0047] 1) Under the protection of nitrogen or argon, add 2.1628g (20mmol) of p-phenylenediamine into 45g of 1-butyl-3-methylimidazolium bromide solvent (solid content 5%), raise the temperature to 50°C and stir to fully dissolve it Afterwards, cool to room temperature for subsequent use;

[0048] 2) Add 5.8844g (20mmol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride to the solution obtained in step 1) in batches, the interval between each batch is 20min, and then gradually raise the temperature to 180°C In the process of gradually heating up, firstly, the temperature is raised from normal temperature to 100°C at a rate of 20°C / min, and then the temperature is kept at 20°C for 20 minutes until the temperature reaches 180°C. After 8 hours of continuous reaction, it is washed and dried in turn. During the drying process, first add an appropriate amount of methanol and...

Embodiment 3

[0050] A preparation method for selective laser sintering molding polyimide powder, comprising the steps of:

[0051] 1) Under nitrogen or argon protection, add 1.2415g (5mmol) 3,4'-diaminodiphenylsulfone and 1.2415g (5mmol) 4,4'-diaminodiphenylsulfone to 25.2977g 1-butyl-3 -In the methylimidazolium bromide solvent (solid content 15%), heat up to 50°C and stir to make it fully dissolved, then cool to normal temperature for later use;

[0052] 2) Add 1.9813g (10mmol) of butane-1,2,3,4-tetracarboxylic dianhydride into the solution obtained in step 1) in batches, the interval between each batch is 40min, and then gradually raise the temperature to 180°C, In the process of gradually heating up, firstly, the temperature is raised from normal temperature to 100°C at a rate of 20°C / min, and then the temperature is kept at 20°C for 20 minutes until the temperature reaches 180°C. After 12 hours of continuous reaction, it is washed and dried in turn. During the treatment process, first...

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Abstract

The invention discloses a selective laser sintering polyimide powder and a preparation method thereof. The preparation method comprises the following steps: 1) under the protection of nitrogen or argon, diamine is added into an ionic solvent, and the temperature is raised to 25- Stir at 60°C to make it fully dissolve, then cool to room temperature for later use; 2) Add the dianhydride to the solution obtained in step 1) in batches, the interval between each batch is 20-40min, and then gradually raise the temperature to 120-260°C, and continue After reacting for 2 to 24 hours, it is washed and dried in sequence to obtain the polyimide powder which can be selectively laser sintered and molded. In the present invention, diamine is imidized in one step in an ionic solvent, and the prepared polyimide powder not only has a high degree of imidization and high heat resistance stability, but also its particle size distribution, apparent density, shape and other parameters meet the selected requirements. Laser sintering molding process requirements.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a selective laser sintering polyimide powder and a preparation method thereof. Background technique [0002] Polyimide is a kind of rigid chain polymer with imide ring in the main chain and relatively regular chemical structure. As the highest heat-resistant resin developed in the early 1960s, it is widely used in aerospace, microelectronics, liquid crystal, laser and other fields. [0003] The performance of polyimide powder is not only related to the molecular structure of the reaction monomer, but also closely related to the reaction solvent system and polymerization process. In order to obtain polyimide powder with high imidization degree and high heat resistance grade, it is often prepared in a high-temperature one-step method in an aprotic polar solvent (N,N-dimethylformamide, N-methylpyrrolidone), However, the low stability of the solvent itself, high toxicity,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/10B33Y70/00
CPCC08G73/1032C08G73/1039C08G73/1064C08G73/1067C08G73/1071C08G73/1078C08G73/1082C08G73/1085
Inventor 尤庆亮付华刘继延于洁阮敏刘学清陈妤红张玲
Owner JIANGHAN UNIVERSITY