Method for simultaneously preparing pyromellitic acid and terephthalic acid with coal serving as raw material

A technology of pyromellitic acid and terephthalic acid, applied in chemical instruments and methods, preparation of carboxylic acid by ozone oxidation, preparation of carboxylate, etc. Social and economic benefits, the effect of broad application prospects

Inactive Publication Date: 2012-12-12
LIUPANSHUI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

my country's TPA is mainly used to produce polyester, but TPA production has long lagged behind the development of polyester production, resulting in a sharp increase in TPA imports

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The anthracite is crushed, shrunk and ground to 40 mesh according to the national standard, and the temperature is about 80 ℃, the vacuum degree is 10 -2 Bake at mmHg until the moisture is less than 1.0% as the oxidation test sample.

[0026] The equipment used in the experiment is the GSHA-1.5L autoclave produced by Shandong Penglai Luhao Chemical Machinery Co., Ltd. Oxidation test The weight of the anthracite coal put into the kettle is 10g, potassium hydroxide 50g, distilled water 180g, filled with O 2 To 6.0MPa, rise to 360°C under stirring, stop heating after constant temperature oxidation for 1h. After cooling, the oxidation product is removed from the autoclave and the insoluble residue (slag + minerals) is filtered off. The filtrate was acidified with concentrated sulfuric acid to pH=3, and then the humic acid was filtered off, and the filtrate was acidified with concentrated sulfuric acid to pH=1.5. Then the filtrate was extracted several times with butanone...

Embodiment 2

[0031] Aged bituminous coal is crushed, shrunk and ground to 80 meshes according to national standards, and is heated at a temperature of about 80°C and a vacuum of 10 -2 Bake at mmHg until the moisture is less than 1.0% as the oxidation test sample.

[0032] The equipment used in the experiment is the GSHA-1.5L autoclave produced by Shandong Penglai Luhao Chemical Machinery Co., Ltd. Oxidation test The weight of old bituminous coal put into the kettle is 20g, the mixture of calcium hydroxide and sodium methoxide is 200g, distilled water is 2.2g, filled with O 2 To 1MPa, rise to 100°C under stirring, stop heating after constant temperature oxidation for 0.5h. After cooling, the oxidation product is removed from the autoclave and the insoluble residue (slag + minerals) is filtered off. The filtrate was acidified with concentrated sulfuric acid to pH=2, and then humic acid was filtered out, and the filtrate was acidified with concentrated sulfuric acid to pH=1. Then the filtr...

Embodiment 3

[0037] The mixture of anthracite and aged bituminous coal is crushed, shrunk and ground to 60 meshes according to national standards, and is heated at a temperature of about 80°C and a vacuum of 10 -2 Bake at mmHg until the moisture is less than 1.0% as the oxidation test sample.

[0038] The equipment used in the experiment is the GSHA-1.5L autoclave produced by Shandong Penglai Luhao Chemical Machinery Co., Ltd. Alkali Oxygen Oxidation Test 100g of anthracite and aged bituminous coal mixture, 10g of ammonia water, 200g of distilled water, O 2 Pressurize to 10MPa, rise to 400°C under stirring, stop heating after constant temperature oxidation for 5h. After cooling, the oxidation product is removed from the autoclave and the insoluble residue (slag + minerals) is filtered off. The filtrate was acidified with concentrated sulfuric acid to pH=5, and then humic acid was filtered out, and the filtrate was acidified with concentrated sulfuric acid to pH=3. Then the filtrate was ...

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Abstract

Disclosed is a method for simultaneously preparing a pyromellitic acid and a terephthalic acid with coal serving as a raw material. The method includes firstly, adding potassium hydroxide, a coal sample and distilled water in a high pressure kettle to perform a reaction, cooling after the reaction to obtain an oxidation product, filtering and removing insoluble residues to obtain a filter liquor, acidizing the filter liquor by a concentrated sulfuric acid to enable a water soluble acid to be completely free, extracting a processed solution by butanone to obtain an extract liquor, subjecting the extract liquor to a vacuum evaporation to obtain a concentrate, recycling the butanone, subjecting the concentrate to a vacuum drying to obtain the water soluble acid, subjecting the water soluble acid to a selective decarboxylation in a mixed medium of an sulfuric acid, potassium acid sulfate and the distilled water to obtain the pyromellitic acid, adding coal acids and catalysts which remain after the preparation of the pyromellitic acid in a reacting kettle to perform a constant temperature isomerization reaction of the coal acids to obtain a filter liquor, cooling the filter liquor after the reaction, adjusting potential of hydrogen (pH) of the filter liquor by an diluted hydrochloric acid, precipitating the terephthalic acid in a sedimentation mode, filtering, washing and drying to obtain the refined terephthalic acid. By means of the method, the pyromellitic acid and the terephthalic acid can be simultaneously prepared, the reaction conditions are mild, conditions for devices are low, the terephthalic acid is a main product due to a high yield, and the pyromellitic acid is an auxiliary product.

Description

technical field [0001] The invention belongs to the technical field of coal chemical processing, in particular to a method for simultaneously preparing pyromellitic acid and terephthalic acid by using coal as a raw material. Background technique [0002] my country is rich in coal resources, far larger than oil reserves. Coal will not only continue to be the main source of energy for my country's economic development, but also a reliable source of important chemical raw materials. But coal is an inefficient and highly polluting energy source. In our country, the utilization rate is very low, and the environmental pollution is becoming more and more serious. Therefore, the chemical conversion and product development of coal are becoming more and more important. In recent years, the rapid development of the synthesis of high-performance aromatic polymer materials has led to an increasing demand for aromatic compounds, which provides an excellent opportunity for the developm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/313C07C63/26C07C51/38C07C51/353C07C51/15C07C51/21
Inventor 杜琨范志芳李琳缪应菊
Owner LIUPANSHUI NORMAL UNIV
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