Refining method for isophthalic acid

A technology of isophthalic acid and its refining method, which is applied in the field of isophthalic acid refining, can solve problems such as high energy consumption and cost, high reaction temperature, and waste water generation, and achieve low production cost, low energy consumption, and product purity high effect

Pending Publication Date: 2019-02-22
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to overcome the defects of high reaction temperature, waste water, high energy consumption and cost, and insufficient product purity in the existing refining method of isophthalic acid, and provide a refining method for isophthalic acid. method

Method used

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  • Refining method for isophthalic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Embodiment 1: the mensuration of isophthalic acid yield and purity

[0054] Isophthalic acid yield and purity are analyzed and tested by high performance liquid chromatography, and the specific instruments and test conditions are as follows:

[0055] 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.

[0056] Chromatographic conditions:

[0057] 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

[0061] Embodiment 2: the preparation of isophthalic acid crude product

[0062] References (Wu Xingan, He Binhong, Wang Yanhui, etc. [J]. Modern Chemicals, 2005(25), 1).

[0063] The experimental device adopts a 1000mL volume high-temperature-resistant titanium reaction kettle. The kettle uses a double paddle stirrer, and the upper paddle is a flat-blade disc turbine stirring paddle, which effectively ensures the high turbulence of the liquid phase and the shearing and breaking of bubbles to promote fluid circulation. The lower paddle is a propulsive stirring paddle, which forms an upflow circulation in the reactor to realize the vigorous mixing and stirring of gas and liquid.

[0064] The reaction temperature of the experiment is 177 ° C ~ 193 ° C, air is introduced, the reaction pressure is 1.1 MPa, the solvent ratio (acetic acid: m-xylene, mass ratio) = 3:1, the catalyst ratio Co / Mn / Br = 2:1:3 (mass ratio, the initial cobalt content is 1200ppm), the air feed rate is 120ml / ...

Embodiment 3

[0065] Embodiment 3: the preparation of isophthalic acid crude product

[0066] 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), the m-xylene conversion rate is 98% after the reaction finishes, and the isophthalic acid yield is 96%, and the purity of isophthalic acid is 98.34%, and the m-toluic acid content is 2%, and m-toluene Formic acid content is 1.64% (g / g), 3-CBA content is 160ppm (10 -6 g / g).

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Abstract

The invention discloses a refining method for isophthalic acid. The refining method comprises the following step: washing an isophthalic acid crude product with a solvent to obtain an isophthalic acidfine product, wherein the solvent is a nitrile solvent or a mixed solvent of the nitrile solvent and water and the 3-CBA content in the isophthalic acid crude product is not smaller than 25 ppm. Therefining method disclosed by the invention is mild in reaction condition and high in product purity. The content of the impurity 3-CBA is smaller than 25 ppm. The refining method is superior to a catalytic hydrogenation refining method and is low in energy consumption and cost, and less wastewater is generated.

Description

technical field [0001] The invention relates to a method for refining 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 cation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/43C07C51/47C07C63/24
CPCC07C51/43C07C51/47C07C63/24
Inventor 孙伟振吕全明赵玲
Owner EAST CHINA UNIV OF SCI & TECH
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