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
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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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