KR100764838B1 - Apparatus for ingredient analysis of wastewater containing purity terephtalic acid and method of ingredient analysis using the same - Google Patents

Abstract

An apparatus for analyzing the wastewater containing terephthalic acid of high purity, and its method are provided to measure the concentration of terephthalic acid, acetic acid, benzoic acid and p-toluene acid contained in the wastewater generated in the manufacturing process of terephthalic acid simultaneously. An apparatus for analyzing the wastewater containing terephthalic acid comprises a pretreatment device(120) which removes the float of the wastewater obtained in the manufacturing process of terephthalic acid; a spray pump(140) which transfers the pretreated wastewater; a spectrophotometer(160) which measures the absorbance of the transferred wastewater; a PC(180) which stores the transmitted data of the absorbance of the wastewater and calculates the concentration of the wastewater by using the measured data; and a control and signal transmission unit(200) which transmits the concentration of the wastewater to a dispersion control system.

Description

Apparatus for ingredient analysis of wastewater containing purity terephtalic acid and method of ingredient analysis using the same}

1 is a process flow chart of a property analysis device of high purity terephthalic acid wastewater according to the present invention.

<Description of the symbols for the main parts of the drawings>

Process Flow Chart for Appearance Analysis Apparatus of High Purity Terephthalic Acid Wastewater

120 Pretreatment ...

160 ... Spectrophotometer 180 ... PC for device control

200 ... control and signal transmission unit

The present invention relates to a constellation analysis device and a constellation analysis method using the same, more specifically, terephthalic acid, acetic acid, benzoic acid, and paratoluic acid components of wastewater generated in a terephthalic acid manufacturing process can be measured simultaneously using a spectrophotometer. The present invention relates to an improved constellation analysis apparatus for high purity terephthalic acid wastewater and a constellation analysis method using the same, which enables simple pretreatment and analysis of wastewater samples and automated analysis.

In general, an important factor that affects the treatment efficiency in the operation of anaerobic treatment processes for treating wastewater from terephthalic acid manufacturing is the concentration of various pollutants contained in the wastewater.

The main components of these pollutants are terephthalic acid, acetic acid, benzoic acid, and para-toluic acid. The pollutants are decomposed by anaerobic microorganisms growing in the anaerobic treatment process and finally converted to methane and carbon dioxide.

On the other hand, analysis of wastewater generated in the terephthalic acid manufacturing process includes sampling, sample transfer, sample fractionation, weight basis, injection into a container, solution preparation, solution injection, dissolution, filtering, sample solution fractionation, insertion of analyser, analysis, result calculation, and It is analyzed through the same steps as the result notification.

The pretreatment stage for instrument analysis may be from sample collection to sample solution fractionation, and the instrument analysis stage may be from insertion to analysis of the analyzer, and the post-treatment stage after instrument analysis may be divided into calculation of results and notification of results.

On the other hand, the technique used in the existing instrumental analysis step was using a chromatogram using a liquid mobile phase and a gas mobile phase, and analysis of terephthalic acid, benzoic acid, and paratoluic acid was performed using High Performance Liquid Chromatograph (HPLC). For the analysis of acetic acid, instrumental analysis using gas chromatography (GC) was used.

However, it was not possible to measure the concentration of each pollutant in the wastewater that changes in real time because it requires a lot of manpower and time in the pretreatment stage and a lot of time for the mobile phase to pass through the packed column and separate in the instrument analysis stage.

In addition, in terms of equipment configuration, various equipments such as injectors, pumps, columns, and detectors are complicated and require many additional factors such as gas supply for maintenance and detection of liquid and gas mobile phase materials. Difficulties were encountered in automating the analysis and making it unattended.

Therefore, real-time automatic analysis of the wastewater of terephthalic acid manufacturing process is made possible by supplementing the disadvantages of the analysis method using the chromatogram as described above, thereby enabling stable operation of the anaerobic wastewater treatment process, thereby improving the operation of an eco-friendly plant. Apparatus for analyzing the properties of high-purity terephthalic acid wastewater and its method are urgently needed.

The present invention was created in order to solve the above problems, by establishing a constellation analysis device of high-purity terephthalic acid wastewater and a constellation analysis method using the same to perform the real-time automatic analysis of wastewater concentration of terephthalic acid manufacturing process and through this stable stable anaerobic wastewater treatment process The purpose of the present invention is to provide an improved constellation analysis device for high purity terephthalic acid wastewater and a constellation analysis method using the same.

It is still another object of the present invention to simultaneously measure the terephthalic acid, acetic acid, benzoic acid, and paratoluic acid components of wastewater generated in a terephthalic acid manufacturing process using a spectrophotometer, thereby simplifying and automating the analysis of wastewater samples and real-time online monitoring. can do.

Other objects and advantages of the invention will be described below and will be appreciated by the embodiments of the invention. In addition, the objects and advantages of the invention may be realized by the means and combinations indicated in the claims.

In order to achieve the above object, the high purity terephthalic acid wastewater property analysis apparatus of the present invention includes a pretreatment apparatus for removing suspended matter in the wastewater of the terephthalic acid manufacturing process; An injection pump for transferring the wastewater sample pretreated in the pretreatment device; A spectrophotometer for measuring the absorbance of the wastewater sample conveyed by the injection pump; A device control PC (personal computer) for receiving and storing the measurement data of the wastewater sample absorbance measured by the spectrophotometer and calculating the concentration value of the wastewater using the measured data; And a control and signal transmission unit for transmitting the concentration value of the wastewater to a distributed control system, thereby providing a property analysis device for high purity terephthalic acid wastewater.

Property analysis method of high purity terephthalic acid wastewater of the present invention, the pretreatment step of removing the suspended matter in the wastewater of the terephthalic acid manufacturing process; A transfer step of transferring the wastewater sample pretreated in the pretreatment step by a injection pump; An absorbance measuring step of measuring absorbance of the wastewater sample transferred by the injection pump by a spectrophotometer; A wastewater concentration value calculating step of receiving and storing measurement data of the wastewater sample absorbance measured by a device control PC, and calculating the concentration value of the wastewater using the measured data; And a transmission step of transmitting the concentration value of the wastewater to a distributed control system by a control and signal transmission unit.

The concentration value calculating step may include measuring ultraviolet (Ultra violet; UV) -near-infrared (NIR) spectra of a wastewater sample; Analyzing the wastewater sample by high performance liquid chromatography and gas chromatography to determine the concentration; Determining a correlation between the measured spectral value and the concentration value; And measuring the concentration of wastewater using the determined correlation.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.

Prior to this, terms or words used in the present specification and claims should not be construed as being limited to the common or dictionary meanings, and the inventors should properly explain the concept of terms in order to explain their invention in the best way. Based on the principle that can be defined, it should be interpreted as meaning and concept corresponding to the technical idea of the present invention.

Therefore, the embodiments described in the specification and the drawings shown in the drawings are only the most preferred embodiment of the present invention and do not represent all of the technical idea of the present invention, various modifications that can be replaced at the time of the present application It should be understood that there may be equivalents and variations.

1 is a process flow diagram 100 for a property analysis apparatus for high purity terephthalic acid wastewater according to the present invention. As shown, it includes a pretreatment device 120, injection pump 140, spectrophotometer 160, a personal computer (PC) 180 for controlling the device and a control and signal transmission unit 200.

The pretreatment device 120, in order to accurately measure the concentration of contaminants in the wastewater of the terephthalic acid manufacturing process using the absorbance spectrum of UV-VIS-NIR, scatters light in the wastewater sample to prevent suspended solids from interfering with the accurate absorbance measurement. Automatically removed and pretreated wastewater is transferred to the property analyzer of the present invention to analyze the concentration of the wastewater.

The injection pump 140 transfers the pretreated wastewater sample to a flow cell inside the spectrophotometer 160 which will be described later. On the other hand, since the influence of the characteristic peak region of the solvent water in the NIR region should be minimized, the higher the concentration of the substance present in the sample, the more accurate. Therefore, the best pretreatment method is to remove unsustained wastewater by loading the undiluted wastewater into the analyzer, thereby preventing errors in absorbance measurement in the near infrared ray (NIR) region and simplifying the pretreatment process. To this end, the dilution with water of the wastewater sample is not performed.

On the other hand, the flow cell (flow cell), acts as a holder for holding the sample in the spectroscopic method for measuring the absorbance when light passes through the waste water sample and has an inlet and an outlet to enable continuous measurement, the material is It is formed of quartz.

In addition, the absorbance measurement of the wastewater sample is measured at the detector after passing the light from the light source for absorbance measurement while the wastewater sample is contained in the flow cell. In this case, the flow cell preferably has a distance of 1 mm from the light source passing through the sample to minimize the influence of water as a solvent. The distance passed within the sample by the light from the light source is not limited to this because it is determined by the design of the flow cell containing the sample.

The spectrophotometer 160 measures the absorbance of the wastewater sample transported by the injection pump 140, and is controlled by a device control PC 180 to be described later to sequentially display ultraviolet-visible-near-infrared rays. Measure the absorbance.

The device control PC 180 receives the absorbance measurement data measured by the spectrophotometer 160 and stores the measured data in the PC 180. When the absorbance scan of one wastewater sample is completed, the absorbance of the wastewater sample is completed. The spectra are obtained and the stored data are simultaneously calculated by the program of the PC using the mathematical model to determine the concentrations of terephthalic acid, acetic acid, benzoic acid, and paratoluic acid.

The control and signal transmission unit 200 is a distributed control system with a signal of 4-20 mA using a digital / analog converter D / A converter; To DCS}.

It describes a method for analyzing the properties of high purity terephthalic acid wastewater according to the present invention.

First, the property analysis method of the high purity terephthalic acid wastewater includes a pretreatment step, a transfer step, an absorbance measurement step, a concentration value calculation step and a transfer step of the wastewater.

First, in the pretreatment step, the suspended matter in the wastewater of the terephthalic acid manufacturing process is removed, and in the transfer step, the wastewater sample pretreated in the pretreatment step is transferred by the injection pump 140.

Next, in the absorbance measurement step, the wastewater sample transferred by the injection pump 140 is supplied into the flow cell, and then ultraviolet (Ultra violet; UV) -visible light (Visible; VIS) using the spectrophotometer 160. }-Absorbance of Near Infrared Ray (NIR) is measured.

Meanwhile, in the case of the conventional method using high performance liquid chromatography (HPLC), the absorbance of single wavelength light in the UV region was calculated to detect the concentration of each component separated through the column. . However, the present invention measures the absorbance spectrum over the UV-VIS-NIR region after the sample is loaded into the flow cell.

In the step of calculating the concentration value of the wastewater, the measurement data of the wastewater sample absorbance measured by the device control PC 180 is received and stored, and the concentration value of the wastewater is calculated using the measured data. More specifically, terephthalic acid, acetic acid, benzoic acid and terephthalic acid, acetic acid, benzoic acid and terephthalic acid, acetic acid, benzoic acid and paratoluic acid were measured using the PLS (partial least square) model. Calculate the concentration of paratoluic acid.

Here, the PLS model for calculating the concentration of terephthalic acid, acetic acid, benzoic acid and paratoluic acid in wastewater from the UV-VIS-NIR spectrum is generalized through the following procedure.

First, the ultraviolet-visible-near-infrared spectrum of the same wastewater sample is measured, and the wastewater sample is analyzed by high performance liquid chromatography (HPLC) and gas chromatography (Gas chromatography; GC). The concentrations of terephthalic acid, acetic acid, benzoic acid and paratoluic acid are measured.

Next, the correlation between the measured spectral value and the concentration value is determined. More specifically, the spectral database measured for samples of various concentration ranges is X data, and the measured angles are determined by HPLC and GC instrumental analysis. The correlation between X and Y databases is determined using the PLS model based on Principal Component Analysis (PCA), which is one of the multivariate statistical techniques, using Y data as the concentration database for each substance.

Finally, in the transmission step, the control and signal transmission unit 200 transmits the concentration value of the wastewater to the distributed control system.

As mentioned above, although this invention was demonstrated by the limited embodiment and drawing, this invention is not limited to this and it is described by the person of ordinary skill in the art to this invention, and below. Various modifications and variations are possible without departing from the scope of the appended claims.

As described above, the apparatus for analyzing properties of high purity terephthalic acid wastewater of the present invention and the method for analyzing properties using the same have the following effects.

First, the pretreatment and analysis process of the wastewater sample is simple and real-time online monitoring is possible by automating the analysis process.

Second, the wastewater concentration measurement and monitoring can be performed more conveniently without directly measuring the concentration of the wastewater.

Third, the terephthalic acid, acetic acid, benzoic acid, and paratoluic acid components of the wastewater generated in the terephthalic acid manufacturing process can be measured simultaneously using a spectrophotometer.

Fourth, the real-time automatic analysis of wastewater concentration of terephthalic acid manufacturing process enables stable operation of anaerobic wastewater treatment process to promote eco-friendly plant operation.

Claims (3)

A pretreatment apparatus for removing suspended matter in wastewater of a terephthalic acid manufacturing process; An injection pump for transferring the wastewater sample pretreated in the pretreatment device; A spectrophotometer for measuring the absorbance of the wastewater sample conveyed by the injection pump; A device control PC (personal computer) for receiving and storing the measurement data of the wastewater sample absorbance measured by the spectrophotometer and calculating the concentration value of the wastewater using the measured data; And Apparatus for analyzing properties of high purity terephthalic acid wastewater comprising a control and signal transmission unit for transmitting the concentration value of the wastewater to a distributed control system. A pretreatment step of removing the suspended matter in the wastewater of the terephthalic acid manufacturing process; A transfer step of transferring the wastewater sample pretreated in the pretreatment step by a injection pump; An absorbance measuring step of measuring absorbance of the wastewater sample transferred by the injection pump by a spectrophotometer; A wastewater concentration value calculating step of receiving and storing measurement data of wastewater sample absorbance measured by a device control PC, and calculating the concentration value of the wastewater using the measured data; And And a transmission step of transmitting the concentration value of the wastewater to a distributed control system by a control and signal transmission unit. The method of claim 2, The concentration value calculation step, Measuring an ultraviolet-visible-near infrared spectrum of the wastewater sample; Analyzing the wastewater sample by high performance liquid chromatography and gas chromatography to determine the concentration; Determining a correlation between the measured spectral value and the concentration value; And Characterization method of the high purity terephthalic acid wastewater comprising the step of measuring the concentration of wastewater using the determined correlation.

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