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Method for synthesizing trimellitic acid

A trimellitic acid and synthesis method technology, applied in the field of trimellitic acid synthesis, can solve the problems of difficult reaction monitoring, harsh reaction conditions, incomplete reaction, etc., achieve cheap and easy reagents, reduce reaction time, and easy monitoring Effect

Active Publication Date: 2018-11-06
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the problems existing in the prior art: harsh reaction conditions, expensive reagents, incomplete reaction, difficult reaction monitoring, etc.

Method used

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  • Method for synthesizing trimellitic acid
  • Method for synthesizing trimellitic acid
  • Method for synthesizing trimellitic acid

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Embodiment 1

[0024] Synthesis of Trimethyl 1,2,4-Benzenetricarboxylate

[0025] Add trimellitic anhydride (100.0 g (gram), 520.48 mmol (mmol)) to a 1 L (liter) round bottom flask, then add 500 mL of methanol to dissolve it, add 16 mL of concentrated sulfuric acid with a mass fraction of 98% dropwise, and heat at 70° C. Refluxing reaction, after 48h (hours), detected by TLC (thin layer chromatography), the reaction is over. Spin off methanol under reduced pressure at 50°C, add 200mL of water, extract with dichloromethane (30mL×10), combine the organic phases, wash with saturated sodium bicarbonate (100mL×3), wash with saturated brine (100mL×3), and finally After drying with anhydrous sodium sulfate and spin-drying, 118.4 g of colorless oily substance 1,2,4-benzenetricarboxylate trimethyl was obtained, with a yield of 90.20%.

[0026] 1 H NMR (400MHz, CDCl 3 )δ: 8.43(s, 1H), 8.21(d, J=8.0Hz, 1H), 7.76(d, J=8.0Hz, 1H), 3.96(s, 3H), 3.94(s, 6H); 13 C NMR (300MHz, CDCl3) δ: 167.63, 166.83, ...

Embodiment 2

[0031] In step (1), the mass volume ratio of trimellitic anhydride, methanol, and concentrated sulfuric acid is 1:4.5:0.15, the reaction temperature is 75°C, and the reaction time is 50 hours. The yield of trimethyl 1,2,4-benzenetricarboxylate is 89.88%.

[0032] The mass volume ratio of 1,2,4-benzenetricarboxylic acid trimethyl ester, methanol and sodium hydroxide in step (2): 1:4.5:3.0, the reaction temperature is 75°C, the reaction time is 40h, the yield of trimellitic acid: 90.02%.

Embodiment 3

[0034] In step (1), the mass volume ratio of trimellitic anhydride, methanol, and concentrated sulfuric acid is 1:5.5:0.18, the reaction temperature is 68°C, the reaction time is 65 hours, and the yield of trimethyl 1,2,4-benzenetricarboxylate is 89.92%.

[0035] Mass volume ratio of 1,2,4-benzenetricarboxylate, methanol and sodium hydroxide in step (2): 1:5.5:3.5, reaction temperature 68°C, reaction time 45h, yield of trimellitic acid: 89.78%.

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Abstract

The invention belongs to the technical field of organic chemical industry and in particular relates to a method for synthesizing trimellitic acid. The method comprises the following steps: taking trimellitic anhydride as an initial raw material, carrying out an esterification reaction to produce 1,2,4-trimethyl benzene tricarboxylate, and carrying out a hydrolysis reaction on 1,2,4-trimethyl benzene tricarboxylate, thereby obtaining the trimellitic acid. The method disclosed by the invention is simple in operation, the reaction conditions are mild, the used reagents are cheap and readily available, the after-treatment is simple, column chromatography is not needed, the reaction endpoint is easily monitored, the yield is high, and industrial production can be realized.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, in particular to a method for synthesizing trimellitic acid. Background technique [0002] Trimellitic acid is a white crystalline compound, easily soluble in ethanol and dimethylformamide, soluble in acetone, slightly soluble in water and ethyl acetate, almost insoluble in benzene, chloroform and carbon disulfide, and its structural formula is as follows: [0003] [0004] It is mainly used in the preparation of trimellitic anhydride and trimellitic ester, used in resins, plasticizers, dyes, adhesives, etc., and has broad application prospects. In the existing synthetic method of trimellitic acid, there are problems such as harsh reaction conditions, expensive reagents, incomplete reaction, and difficult reaction monitoring. [0005] Patent CN106187739A discloses a continuous production method of trimellitic acid, the method includes premixing, oxidation, coarse crystalliza...

Claims

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Application Information

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IPC IPC(8): C07C27/02C07C63/307
CPCC07C51/09C07C67/08C07C63/307C07C69/76
Inventor 胡昆闫雪龙任杰
Owner CHANGZHOU UNIV
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