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Study on the Treatment of High Concentrations of Caprolactam Organic Wastewater with Chemical Method

Author: LiYanChun
Tutor: DuanZhengKang
School: Xiangtan University
Course: Chemical processes
Keywords: Caprolactam liquid waste Azeotropic distillation Cyclohexane carboxylic acid sulfonate Comprehensive management
CLC: X703
Type: Master's thesis
Year: 2009
Downloads: 113
Quote: 1
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Abstract


Caprolactam is an important organic chemical raw materials, the main purpose to generate polyamide slice through the polymerization of nylon-6 (often called slices) With the the nylon industrial demand is increasing, consumer demand for caprolactam has also increased rapidly. In caprolactam production process also generates a lot of brown-black, sticky, there is a strong pungent odor of organic wastewater, wastewater composition is complex, the main component of cyclohexane sulfonate, ammonium sulfate, toluene, cyclohexane carboxylic acid, benzoic acid, hexahydro benzoic acid, cyclohexane, cyclohexanone amide, caprolactam and other countries as one of the eight major categories of special wastewater, and are biodegradable high concentration organic wastewater containing ammonia nitrogen. In this paper comes from Shijiazhuang Chemical Fiber Co., Ltd. toluene production of caprolactam organic wastewater comprehensive analysis and processing. The first is the analysis of the traits and composition of the waste water, potassium dichromate calibration wastewater chemical oxygen demand (CODcr) for 516000mg / L; titration method for the determination of ammonia (NH3-N) to 121.8mg / L. Depending on the nature of the substances in the analysis system, the establishment the reverse ion chromatography (HPLC) analysis of the wastewater composition analysis conditions: column Shim-pack VP-ODSΦ4.6 x 250mm; mobile phase of methanol / water = 37.5 / 62.5 (v / v), the ion pair reagent tetrabutylammonium bromide concentration of 10 mmol / L, the buffer potassium dihydrogen phosphate concentration of 25mmol / L, the pH value of 2.5 to 3.5; detection wavelength 230nm; flow rate of 1.0mL/min. Major component of its content (mass fraction): water 53%, 11.93% cyclohexane carboxylic acid ammonium salt (sulfo Vice), cyclohexane carboxylic acid (CCA) 1.7%, caprolactam (CPL) 0.8%. Wastewater trait analysis method and analysis of oriented topics, as well as provide the basis for proposed wastewater treatment program. This paper focuses on the use of chemical caprolactam wastewater treatment, is committed to identify the best experimental program caprolactam wastewater treatment, to find the optimal experimental parameters. Ultimately determine the processing method is: Select toluene - benzene as mixed azeotropic agent, and the quality of materials ratio of 1:1:2, about 79 ℃ using an azeotropic distillation method, the effluent was removed about 53% of water, oil-water separator, the azeotropic agent recycle; using methanol as extraction detergent, a constant temperature of 42 to 44 ° C and stirred for 1.5h extract was washed three times, separation of organic and sulfonation byproducts about 61 ° C, recovery of methanol by distillation. The present processing method is very good wastewater is separated into water, salts, mixed organics concentrated solution (oil phase). Finally, treatment products qualitative and quantitative analysis, the comprehensive utilization of research products. Azeotropic water CODcr: 2800mg / l NH 3 -N: 15.1 mg of / l, reaching the requirements of the existing treatment system, treatment and discharge standards; salts in the main ingredient used after purification UV-visible spectrophotometry (UV-Vis), Fourier transform infrared (FT-IR) and nuclear magnetic resonance spectroscopy ( 1 the H and 13 C) spectroscopic analysis of qualitative analysis, Finally reverse ion quantitative liquid chromatography (HPLC), the identification of the final products obtained in the main component is cyclohexane carboxylic acid, sulfonic acid ammonium salt, the content was 96.5%, and further research and development of new uses; organics concentrated liquid The heat of combustion of 2.84 × 10 7 J / kg, and bituminous coal, alcohol, coke combustion value close to deployment, use as fuel.

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CLC: > Environmental science, safety science > Processing and comprehensive utilization of waste > General issues > Wastewater treatment and utilization
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