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Method for preparing diphenic acid

A technology of biphenylformic acid and glacial acetic acid, which is applied in the direction of carboxylate preparation, organic compound preparation, oxidative preparation of carboxylic acid, etc., can solve the problems of not obtaining reference documents, etc., and achieve simple method, high yield and good impact resistance performance effect

Inactive Publication Date: 2006-02-15
COUNCIL OF SCI & IND RES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Based on literature research and patent data, the prior art of bibenzoic acid preparation was searched, but no corresponding references were obtained

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 25 grams of phenanthrene and 253 grams of glacial acetic acid were added to the reactor and heated to 85°C. 100 ml of 30% hydrogen peroxide solution was added dropwise to the reaction mixture over 40 minutes. After the hydrogen peroxide solution was added dropwise, the temperature was maintained at 85° C. for 6 hours. The resulting mixture was distilled under reduced pressure to reduce its volume by half and the mass was cooled. During cooling, a large amount of biphenylcarboxylic acid crystallized out. The cooled mixture was filtered, and after adding 10% sodium carbonate solution and activated carbon (for decolorization), the resulting residue was boiled at 100°C and filtered, after which the residue was discarded, and the filtrate was acidified with hydrochloric acid to keep the pH at 4.5 And cooled, biphenylformic acid crystallized out from it. This process was repeated several times until pure diphenylcarboxylic acid with a melting point of 228°C was obtained. ...

Embodiment 2

[0038] 25 grams of phenanthrene and 253 grams of glacial acetic acid were added to the reactor and heated to 85°C. 200 ml of 30% hydrogen peroxide solution was added dropwise to the reaction mixture over 40 minutes. After the hydrogen peroxide solution was added dropwise, the temperature was maintained at 85° C. for 6 hours. The resulting mixture was distilled under reduced pressure to reduce its volume by half and the mass was cooled. During cooling, a large amount of biphenylcarboxylic acid crystallized out. The cooled mixture was filtered, and after adding 10% sodium carbonate solution and activated carbon (for decolorization), the resulting residue was boiled at 100°C and filtered, after which the residue was discarded, and the filtrate was acidified with hydrochloric acid to keep the pH at 4.5 And cooled, biphenylformic acid crystallized out from it. This process was repeated several times until pure diphenylcarboxylic acid with a melting point of 229°C was obtained. ...

Embodiment 3

[0040] 25 grams of phenanthrene and 253 grams of glacial acetic acid were added to the reactor and heated to 85°C. 88 ml of 30% hydrogen peroxide solution were added dropwise to the reaction mixture over 30 minutes. After the hydrogen peroxide solution was added dropwise, the temperature was maintained at 80°C for 3.5 hours. The resulting mixture was distilled under reduced pressure to reduce its volume by half and the mass was cooled. During cooling, a large amount of biphenylcarboxylic acid crystallized out. The cooled mixture was filtered, and after adding 10% sodium carbonate solution and activated carbon (for decolorization), the resulting residue was boiled at 100°C and filtered, after which the residue was discarded, and the filtrate was acidified with hydrochloric acid to keep the pH at 4.5 And cooled, biphenylformic acid crystallized out from it. This process was repeated several times until pure diphenylcarboxylic acid with a melting point of 229°C was obtained. ...

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Abstract

The present invention provides a process for the preparation of diphenic acid from phenanthrene which comprises heating phenanthrene and glacial acetic acid, adding dropwise a pre-determined amount of 30 % hydrogen peroxide, heating the resulting mixture after completion of drop wise addition of hydrogen peroxide, distilling the resulting mixture under reduced pressure to make the volume half, cooling the mixture till diphenic acid crystalises out, filtering the cooled mixture and boiling the residue after adding 10 % solution of sodium carbonate and activated charcoal, filtering and discarding the residue; acidifying the filtrate with hydrogen chloride; cooling the resultant mixture till more diphenic acid crystallises out; repeating filtration till pure diphenic acid is obtained.

Description

technical field [0001] The present invention relates to the synthetic method of biphenylformic acid. More specifically, the present invention relates to a method for the synthesis of biphenylcarboxylic acid from phenanthrene. The invention can be used to produce high-temperature heat-resistant resins, engineering plastics, liquid crystal macromolecules, pharmaceutical preparations, agricultural chemical industrial products and the like. This method produces a suitable sufficiently thermally stable poly(amide-imide) resin that has good impact resistance, tensile strength or elongation properties and can be drawn into long fibers. Diphenylcarboxylic acid residues act as chain terminators for reactions with aromatic diamines. Background technique [0002] After naphthalene, phenanthrene is the second major component of high-temperature coal tar. It is concentrated in the anthracene oil fraction (300-360°C) of the coal tar distillation process. It constitutes 30-40% of the c...

Claims

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Application Information

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IPC IPC(8): C07C51/285C07C63/331C07C51/31
CPCC07C51/31C07C63/331
Inventor 考沙尔·基肖尔·蒂瓦里库马尔斯·钱德拉·比特桑贾伊·库马尔·塔库尔卡姆莱什·库马尔·米什拉苏库鲁·罗摩克里希纳·拉奥
Owner COUNCIL OF SCI & IND RES
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