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Preparation method of electronic grade hydrogenated pyromellitic dianhydride

A technology of pyromellitic dianhydride and pyromellitic acid, which is applied in the field of preparation of electronic-grade hydrogenated pyromellitic dianhydride, can solve problems such as insufficient temperature resistance, low dielectric constant, and small molecular weight, and achieve shortening Dehydration time, shorten the reaction process, save the effect of solvent

Active Publication Date: 2014-08-20
CHANGZHOU SUNLIGHT PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) Fully aromatic structure products (i.e. all diamine and dianhydride monomers use aromatic monomers): typically, all diamine and dianhydride monomers use fluorine-containing monomers. The biggest feature of this type of film is High temperature resistance and low dielectric constant, but fluorine-containing monomers are expensive
[0005] (2) Products with full alicyclic structure (i.e. diamine and dianhydride monomers all use alicyclic monomers): this type of product has the highest light transmittance, generally exceeding 90%, cut-off wavelength less than 250nm, and yellow index Y.I less than 3; However, because the main chain of the molecule is all alicyclic structure, the temperature resistance of the product is not enough. Generally, the Tg is 200-220 ° C, which cannot meet the high temperature resistance requirements of the product
[0006] (3) The dianhydride is an aromatic monomer, and the diamine is an alicyclic monomer: because the diamine monomer of this type of product is an alicyclic monomer, the amino group has a strong basicity, and is generally an aromatic diamine amino base Sexual 10 5 ~10 6 This will lead to the formation of polyamic acid salt immediately when the two monomers are polymerized in the solvent, which will form a precipitate in the polymerization solvent, and finally make the molecular weight of the product too small, the mechanical strength of the film is too low, and the product is useless. value
The purity of the 1,2,4,5-cyclohexanetetracarboxylic acid obtained by this method is only 98.2%~99.1%, and the purity of the obtained 1,2,4,5-cyclohexanetetracarboxylic anhydride is only 99.0%~ 99.4%, and the single metal ion content in the product is not mentioned, so the hydrogenated pyromellitic anhydride obtained by this method cannot be widely used in high-tech fields such as optoelectronics and microelectronics

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0022] The preparation method of the electronic-grade hydrogenated pyromellitic dianhydride of the present embodiment has the following steps:

[0023] ① Add 34.3g of commercially available pyromellitic dianhydride (98.2% in GC analysis purity) into a 500mL autoclave, add 250mL of deionized water and 2.5g of 5wt% Pd-C catalyst as a noble metal catalyst at the same time, to Hydrogen was introduced into the autoclave and the hydrogen pressure was controlled at 2MPa, the temperature was controlled at 33°C±1°C, and the reaction was carried out for 2h.

[0024] Then cool to room temperature (15°C-25°C, the same below) and filter the material, and the filter cake separates the Pd-C catalyst, which can be recovered and used in the next batch of catalytic hydrogenation reaction after being placed in the air overnight. After the filtrate was distilled to remove water, hydrogenated pyromellitic acid was precipitated; filtered again, the filter cake was decolorized and refined with deion...

Embodiment 2～ Embodiment 3）

[0029] Each embodiment is basically the same as Embodiment 1, and the differences are shown in Table 1.

[0030] Table 1

[0031] Example 1 Example 2 Example 3 noble metal catalyst 2.5g of 5wt% Pd-C catalyst 2g of 5wt% Ru-C catalyst 3g of 5wt% Pt-C catalyst Simultaneous hydrolysis and catalytic hydrogenation reaction temperature 33℃±1℃ 35℃±1℃ 31℃±1℃ Simultaneous hydrolysis and catalytic hydrogenation reaction pressure 2 MPa 1MPa 4MPa Simultaneous hydrolysis and catalytic hydrogenation reaction time 2h 2.5h 0.5h Hydrogenated pyromellitic acid Weight 39.2g, yield 97.1%, purity 99.50% Weight 39.4g, yield 97.6%, purity 99.46% Weight 39.3g, yield 97.3%, purity 99.48% Acetic anhydride 120g 100g 110g Dehydration reaction time 1h 1h 1h Hydrogenated pyromellitic dianhydride Weight 32.8g, yield 97.5%, purity 99.90% Weight 33.2g, yield 98.2%, purity 99.85% Weight 32.4g, yield 96.1%, purity 99.88% ...

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Abstract

The invention discloses a preparation method of electronic grade hydrogenated pyromellitic dianhydride. The method comprises the following steps: adding commercially available pyromellitic dianhydride with the purity greater than or equal to 98.0%, deionized water and a noble metal catalyst into an autoclave; feeding hydrogen into the autoclave and simultaneously carrying out a hydrolysis reaction and a catalytic hydrogenation reaction; carrying out aftertreatment after the reactions so as to obtain crude hydrogenated pyromellitic dianhydride; decoloring and refining crude hydrogenated pyromellitic dianhydride with deionized water and activated carbon so as to obtain hydrogenated pyromellitic dianhydride with the purity greater than or equal to 99.5%; finally, carrying out a dehydration reaction on hydrogenated pyromellitic dianhydride by using acetic anhydride so as to obtain electronic grade hydrogenated pyromellitic dianhydride with the purity greater than or equal to 99.85%. According to the method, the purity of prepared hydrogenated pyromellitic dianhydride can reach above 99.85%, and the content of single metal ions (such as sodium, potassium, calcium, iron, copper, aluminum and the like) in prepared hydrogenated pyromellitic dianhydride is respectively less than 1ppm. Thus, electronic grade hydrogenated pyromellitic dianhydride can be widely applied to the field of photoelectronics, micro-electronics and other high and new technologies.

Description

technical field [0001] The invention relates to a preparation method of an alicyclic dianhydride monomer, in particular to a preparation method of electronic-grade hydrogenated pyromellitic dianhydride. Background technique [0002] Colorless and transparent polyimide can be widely used in high-tech fields such as optoelectronics and microelectronics. For example, in the field of liquid crystal display, it is used as plastic substrate material, alignment film material, negative compensation film, etc. for flexible organic electroluminescent display OLED to replace glass; in the field of optical communication, it is used as passive or active waveguide material, optical switch Materials, optical filters, optical fibers, optoelectronic packaging materials, second-order nonlinear optical materials, photorefractive materials, photosensitive materials, and other related optoelectronic materials; used as substrate materials for solar cell arrays and antenna reflectors in the aerosp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 胡国宜吴建华闵雪锋周国平
Owner CHANGZHOU SUNLIGHT PHARMA
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