Method for synthesizing dihydroxy dimethyl terephthalate by using oxygen catalytic oxidation method

A technology of dimethyl dihydroxyterephthalate and dimethyl hydroxyterephthalate, which is applied in the field of organic chemical synthesis, can solve the problems of three-waste discharge, high cost, low yield and the like, and achieves reduction of three-waste discharge and production The effect of simplifying the process and reducing by-products

Pending Publication Date: 2022-05-13
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In a word, the above-mentioned methods have the disadvantages of low yield, high cost, and serious discharge of three wastes.

Method used

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  • Method for synthesizing dihydroxy dimethyl terephthalate by using oxygen catalytic oxidation method
  • Method for synthesizing dihydroxy dimethyl terephthalate by using oxygen catalytic oxidation method
  • Method for synthesizing dihydroxy dimethyl terephthalate by using oxygen catalytic oxidation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: Co / N-C preparation

[0030] (1) Mix 2g of cobalt acetate tetrahydrate, 15g of glucose, 4g of urea, and 3g of water, and mix well to dissolve the cobalt acetate to obtain a red viscous liquid;

[0031] (2) Place the prepared red viscous liquid in a tube furnace and feed NH 3 , the temperature was raised to 800°C at a rate of 1°C / min, and maintained at 800°C for 2 hours, then the temperature was naturally lowered to 40°C, and the material was taken out to obtain 5.2g of Co / N-C catalytic material.

[0032] The BET specific surface area is 98㎡ / g and the pore volume is 0.32ml / g as determined by liquid nitrogen adsorption method. The content of surface elements Co: 10.1%, N: 6.3% was analyzed by scanning electron microscope surface energy spectroscopy (SEM-EDS).

Embodiment 2

[0033] Embodiment 2: Cu / N-C preparation

[0034] (1) Fully mix 3g of copper chloride dihydrate, 15g of glucose, 5g of urea, and 4g of water to dissolve the copper chloride to obtain a green viscous liquid.

[0035] (2) The prepared green viscous liquid is placed in a tube furnace and fed with NH 3 , the temperature was raised to 700°C at a rate of 3°C / min, and maintained at 700°C for 4 hours, then the temperature was naturally lowered to 40°C, and the material was taken out to obtain 5.8g of Cu / N-C catalytic material.

[0036] The BET specific surface area is 79㎡ / g and the pore volume is 0.29ml / g as determined by liquid nitrogen adsorption method. Surface element content Cu: 18.6%, N: 4.4% were analyzed by scanning electron microscope surface energy spectroscopy (SEM-EDS).

Embodiment 3

[0037] Embodiment 3: Ni / N-C preparation

[0038] (1) Fully mix 4g of nickel nitrate hexahydrate, 15g of glucose, 6g of urea, and 4g of water to dissolve the nickel nitrate to obtain a green viscous liquid.

[0039] (2) The prepared green viscous liquid is placed in a tube furnace and fed with NH 3 , the temperature was raised to 850°C at a rate of 5°C / min, and maintained at 850°C for 3 hours, then the temperature was naturally lowered to 35°C, and the material was taken out to obtain 5.4g of Ni / N-C catalytic material.

[0040] The BET specific surface area is 116㎡ / g and the pore volume is 0.35ml / g as determined by liquid nitrogen adsorption method. Surface element content Ni: 14.7%, N: 4.7% were analyzed by scanning electron microscope surface energy spectroscopy (SEM-EDS).

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Abstract

The invention relates to the technical field of organic chemical synthesis, in particular to a method for synthesizing dihydroxy dimethyl terephthalate by using an oxygen catalytic oxidation method. According to the technical scheme, oxygen (O2) is used as an oxidizing agent, a metal component (M) is Co, Ni, Cr, Mn, Fe, Cu and other elements under the action of a catalyst M / N-C, and DMSS is oxidized to generate DHTA in a proper solvent by controlling proper conditions. Oxygen is used as an oxidizing agent, the process is simplified, and the production cost is reduced. The by-product is a small amount of H2O, the emission of three wastes is greatly reduced, and the production process is clean and environment-friendly.

Description

technical field [0001] The invention relates to the technical field of organic chemical synthesis, in particular to the catalytic oxidation of 1,4-cyclohexanedione-2,5-dicarboxylate (DMSS) with oxygen to synthesize 2,5-dihydroxy dimethyl terephthalate (DHTA) catalysts and methods of application. Background technique [0002] Dimethyl 2,5-dihydroxyterephthalate (DHTA) plays an important role in the synthesis of functional materials and drugs, especially polymer modified materials (such as organic light-emitting materials and high-performance fibers PBO, M5, PBX, etc.). play a key role. In particular, M5, a new type of liquid crystal aromatic heterocyclic polymer fiber, has high strength, high modulus, excellent flame retardancy and compressive strength, and is widely used in various cutting-edge fields. DHTA has the properties of both terephthalic acid and salicylic acid, so the performance of this type of compound shows a broad market prospect. [0003] The main method of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/31C07C69/84B01J27/24
CPCC07C67/31B01J27/24C07C69/84
Inventor 单玉华方慧赵世丽刘平蔡志祥刘玮胡林玲王碟李焱叶
Owner CHANGZHOU UNIV
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