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Method for preparing electronic grade hydrogenated trimellitic anhydride

A technology for trimellitic anhydride and trimellitic acid, which is applied in the field of preparation of electronic grade hydrogenated trimellitic anhydride, can solve the problems of low purity of hydrogenated trimellitic anhydride and cannot meet electronic grade requirements, etc., achieves purity and metal ion content to help, reduces production costs, and improves conversion rate effect

Active Publication Date: 2011-11-23
CHANGZHOU SUNLIGHT PHARMA
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

The purity of hydrogenated trimellitic anhydride obtained by this method is low (only 98.6%), and the content of individual metal ions in the product is not mentioned, which obviously cannot meet the requirements of electronic grade

Method used

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  • Method for preparing electronic grade hydrogenated trimellitic anhydride

Examples

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Embodiment 1）

[0019] The preparation method of the electronic grade hydrogenated trimellitic anhydride of the present embodiment has the following steps:

[0020] ① Hydrolysis of acid anhydride into acid reaction. Add 35g of commercially available trimellitic anhydride (standard GB / T 23967-2009 "Industrial Trimellitic anhydride", trimellitic anhydride content is 95wt%) and 350mL of deionized water into a 500mL three-necked bottle, and reflux to generate trimellitic acid , reflux reaction for 4 hours, then cooled to ambient temperature (25°C in this example), white crystals precipitated, filtered, decolorized and refined the filter cake with activated carbon to obtain 37g of white trimellitic acid, the yield was 96.7%, The purity by GC analysis was 99.6%.

[0021] ② Catalytic hydrogenation reaction. In the autoclave of 500mL, add the 37g trimellitic acid that step ① makes, add simultaneously the mixed solvent that is made up of the ethanol of 120mL and the deionized water of 120mL and the ...

Embodiment 2～ Embodiment 5）

[0024] The steps of each embodiment 1. are the same as Example 1, the difference is that step 2. catalytic hydrogenation reaction and step 3. dehydration into anhydride reaction, the specific differences of catalytic hydrogenation reaction are shown in Table 1, dehydration into anhydride reaction See Table 2 for specific differences.

[0025] Table 1

[0026] Example 1 Example 2 Example 3 Example 4 Example 5 mixed solvent 120mL of ethanol and 120mL of deionized water 120mL methanol and 120mL deionized water 120mL THF and 120mL deionized water 120mL DMF and 120mL deionized water 120 mL of isopropanol and 120 mL of deionized water noble metal catalyst 3.5g of 5wt% Pd-C catalyst 2.0g of 10wt% Rh-C catalyst 3.5g of 5wt% Ru-C catalyst 1.0g of 5wt% Pt-C catalyst 3.0g of 10wt% Rh-C catalyst hydrogen pressure 2 MPa 3 MPa 4MPa 2 MPa 1 MPa temperature 80℃～85℃ 60℃～65℃ 95℃～100℃ 40℃～65℃ 75℃～80℃ time 3h 4h 7h ...

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Abstract

The invention discloses a method for preparing electronic grade hydrogenated trimellitic anhydride, which comprises the following steps of: 1. hydrolyzing trimellitic anhydride which is used as a raw material with deionized water, and decolorizing and refining with active carbon; 2. adding trimellitic acid, a mixed solvent and a noble metal catalyst into an autoclave; introducing hydrogen into the autoclave for carrying out a catalytic hydrogenation reaction; preparing a crude hydrogenated trimellitic acid by post treatment after complete reaction; decolorizing and refining the crude hydrogenated trimellitic acid with deionized water and active carbon, wherein the weight of the noble metal catalyst is 0.5%-10% of the weight of the trimellitic acid; and 3. dehydrating the hydrogenated trimellitic acid in an organic solvent with acetic anhydride to obtain the electronic grade hydrogenated trimellitic anhydride of which the purity is greater than or equal to 99.95%,. The purity of the hydrogenated trimellitic anhydride prepared by the method can reach above 99.95%, and the content of metal ions (such as sodium, kalium, calcium, ferrum, copper, aluminum and like) is less than 1ppm.

Description

technical field [0001] The invention relates to a method for preparing electronic-grade chemical raw materials, in particular to a method for preparing electronic-grade hydrogenated trimellitic anhydride. Background technique [0002] Ordinary hydrogenated trimellitic anhydride is usually used as a curing agent for high-power blue LED epoxy resin packaging materials. If it is to be used in the field of microelectronics, it can be used as an alicyclic polyamide-imide with high light transmittance and low dielectric constant. The monomer must meet the requirements of product purity ≥ 99.9% and single metal ion content in the product ≤ 1ppm. [0003] Chinese patent document CN1428324A discloses a method for preparing hydrogenated aromatic polycarboxylic acid and a method for preparing hydrogenated aromatic polycarboxylic acid anhydride. It specifically discloses a method for preparing 1,2,4-cyclohexanetricarboxylic acid (i.e., hydrogenated trimellitic acid) from trimellitic ac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/89
Inventor 胡国宜李玉玲吴建华
Owner CHANGZHOU SUNLIGHT PHARMA
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