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Process for preparing m-phthalic acid

A technology for the preparation of isophthalic acid and its preparation process, applied in the field of preparation of isophthalic acid, can solve the problems of high energy consumption and cost, high greenhouse gas emissions, high reaction temperature, etc., and achieve reduction of production cost, energy consumption, and energy consumption The effect of low, high product purity

Inactive Publication Date: 2019-03-19
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The technical problem to be solved by the present invention is to overcome the problems of equipment corrosion, high greenhouse gas emissions and high reaction temperature in the oxidation process of the existing isophthalic acid preparation process, and further overcome the high reaction temperature in the refining process, the generation of waste water, and the energy consumption. And cost is high, the defect such as product purity is not high enough, and a kind of preparation technology of isophthalic acid is provided

Method used

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  • Process for preparing m-phthalic acid
  • Process for preparing m-phthalic acid
  • Process for preparing m-phthalic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment 1: the mensuration of isophthalic acid yield and purity

[0051] Isophthalic acid yield and purity are analyzed and tested by high performance liquid chromatography, and the specific instruments and test conditions are as follows:

[0052] The HPLC detection method adopts the American Agilent 1120 high performance liquid chromatograph, automatic sample injector, Agilent 1120 UV / Vis detector, Empower 2 data processing system.

[0053] Chromatographic conditions:

[0054] Chromatographic column: Agilent TC-C18 chromatographic column (4.6×250mm, 5μm); mobile phase A is 100% acetonitrile, mobile phase B is 17% methanol + 83% water; gradient elution conditions: A from 30% in 0 to 20min to 100%, B from 100% to 30% in 20~25min, B from 70% to 0% in 0~20min, B from 0% to 70% in 20~25min; flow rate: 1mL / min; column temperature: 30 ℃; detection wavelength: 260nm; injection volume: 20μL. Under this condition, the retention time of the main peak of isophthalic acid is ...

Embodiment 2

[0058] Embodiment 2: the preparation of isophthalic acid crude product

[0059] Add 10mL of m-xylene, 24mL of acetonitrile, and 16mL of water into a 100mL round-bottomed flask, keep the pH value at 4-4.5, stir with a six-blade impeller, and bubble ozone into the solution at a flow rate of 20ml / min to keep The pressure is normal pressure, the temperature is room temperature, the ultraviolet light is continuously irradiated for 20 hours, and the power of the ultraviolet lamp is 100W (200mW / cm 2 , 310nm), after the reaction finishes, the m-xylene conversion rate is 98%, and the isophthalic acid yield is 96%, and the m-toluic acid content is 2%, and the 3-CBA content is 160ppm (10 -6 g / g).

Embodiment 3

[0060] Embodiment 3: the preparation of isophthalic acid crude product

[0061] Add 25mL of m-xylene, 15mL of acetonitrile, and 10mL of water into a 100mL round-bottomed flask, keep the pH value at 4 to 4.5, stir with a six-blade impeller, and bubble ozone into the solution. The flow rate of ozone is 9mL / min, and keep The pressure is normal pressure, the temperature is 25°C, the ultraviolet light is continuously irradiated for 20 hours, and the power of the ultraviolet lamp is 100W (200mW / cm 2 , 310nm). After the reaction, the remaining amount of m-xylene was 0.006 mol, the content of isophthalic acid was 0.131 mol, the conversion rate of m-xylene was 97%, and the yield of isophthalic acid was 60%.

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Abstract

The invention discloses a process for preparing m-phthalic acid. The process comprises the following steps: (1) performing an oxidation reaction as shown in the specification on m-xylene in a solventunder the effect of oxidant, namely an ozone oxidant, and ultraviolet irradiation to obtain a m-phthalic acid crude product; and (2) washing the m-phthalic acid crude product prepared in the step (1)with a solvent to obtain a m-phthalic acid refined product, wherein the solvent is a nitrile solvent or mixed solvent of nitrile solvent and water. According to the process, application of a bromine catalyst with strong corrosion is avoided in the oxidizing process, and application of a noble metal Pd / C catalyst is avoided in the refining process, high-temperature reaction is not required, cost and energy consumption can be saved, massive waste water cannot be generated, and the content of 3-CBA is lower than 25ppm. The process is better than a catalytic hydrogenation refining method, and hashigh product purity.

Description

technical field [0001] The invention relates to a process for preparing isophthalic acid. Background technique [0002] Iso-phthalic acid (IPA) is a fast-growing organic chemical intermediate raw material, mainly used as a modified monomer of PET resin to improve the processing and product performance of PET resin, and replace phthalic anhydride to produce high-strength A chemically resistant unsaturated resin that replaces phthalic anhydride to produce high-performance, high-solids alkyd resins. In foreign countries, IPA is widely used and has a promising development prospect. Many large companies are preparing to expand production capacity and build new IPA devices. With the continuous expansion of device scale, its cost will continue to decrease, and its application fields and market share will continue to expand. The application of IPA in my country has a certain foundation. At present, it has been applied in the field of bottle-grade polyester resin and polyester cati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/34C07C63/24
CPCC07C51/34C07C63/24
Inventor 孙伟振吕全明赵玲
Owner EAST CHINA UNIV OF SCI & TECH
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