KR100417516B1 - Method and apparatus for measurement of acid concentration using impedance spectrum in cold rolling pickling line - Google Patents
Method and apparatus for measurement of acid concentration using impedance spectrum in cold rolling pickling line Download PDFInfo
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- KR100417516B1 KR100417516B1 KR10-1999-0063408A KR19990063408A KR100417516B1 KR 100417516 B1 KR100417516 B1 KR 100417516B1 KR 19990063408 A KR19990063408 A KR 19990063408A KR 100417516 B1 KR100417516 B1 KR 100417516B1
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- acid concentration
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- 239000002253 acid Substances 0.000 title claims abstract description 101
- 238000005554 pickling Methods 0.000 title claims abstract description 36
- 238000005259 measurement Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000001453 impedance spectrum Methods 0.000 title claims abstract description 12
- 238000005097 cold rolling Methods 0.000 title abstract description 4
- 238000011084 recovery Methods 0.000 claims abstract description 11
- 238000001228 spectrum Methods 0.000 claims 1
- 238000005098 hot rolling Methods 0.000 abstract description 6
- 229910000831 Steel Inorganic materials 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 239000010959 steel Substances 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 239000000523 sample Substances 0.000 description 7
- 230000005684 electric field Effects 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000005855 radiation Effects 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- 239000003930 superacid Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/021—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance before and after chemical transformation of the material
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- G01N33/0078—
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- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
본 발명은 산농도 측정 방법 및 장치에 관한 것으로서, 특히 냉연공장 산세라인(Pickling Line)에서 열연강판의 미산세 및 과산세를 방지하기 위해 산회수라인에 임피던스 스펙트럼를 이용한 산농도 측정 방법 및 장치에 관한 것이다.The present invention relates to a method and apparatus for measuring acid concentration, and more particularly, to a method and apparatus for measuring acid concentration using an impedance spectrum in an acid recovery line in order to prevent pickling and over-pickling of a hot rolled steel sheet in a pickling line of a cold rolling mill. will be.
본 발명은 열간압연으로 인해 생성된 스트립 표면의 스케일, 보관 및 이송과정에서 생성된 불순물을 HCl용액 탱크에 스트립을 통과시켜 제거하기 위한 산세처리과정에서 산탱크의 산농도를 측정하기 위해 산회수 라인에 별도의 산농도 측정배관을 설치하고, 전극을 측정배관에 삽입하여 전극에 교류전원의 주파수를 달리하면서 교류임피던스의 변화를 측정하므로써 광범위한 주파수 영역에서의 임피던스 특성을 이용하여 산용액의 농도를 측정하는 방법 및 장치를 제공한다.The present invention is an acid recovery line for measuring the acid concentration of the acid tank in the pickling process to remove the impurities generated during the scaling, storage and transport of the strip surface generated by hot rolling through the strip through the HCl solution tank A separate acid concentration measurement pipe is installed in the pipe, and the electrode is inserted into the measurement pipe to measure the concentration of the acid solution using impedance characteristics in a wide frequency range by measuring the change in AC impedance while varying the frequency of the AC power supply to the electrode. It provides a method and apparatus.
Description
본 발명은 냉연 산세라인(Pickling Line)에서 열연공정후의 열연코일을 산세하는 과정에서 산농도에 따라 발생되는 미산세 및 과산세의 직접적 원인이 되는 산탱크의 산농도를 임피던스 스펙트럼(Impedance Spectrum)를 이용하여 검사하므로써 산농도를 일정하게 유지하기 위한 중요한 변수가 되는 산농도를 측정하는 방법 및 장치에 관한 것이다.According to the present invention, the acid concentration of an acid tank which is a direct cause of unpickling and peroxidation in the process of pickling a hot rolled coil after a hot rolling process in a pickling line is measured by an impedance spectrum. The present invention relates to a method and apparatus for measuring acid concentration, which is an important variable for maintaining a constant acid concentration by inspection.
산세라인 산탱크의 산농도는 열연코일의 산세후에 발생되는 미산세 및 과산세등의 영향에 의해 냉연코일의 품질에 중요한 영향을 주는 요소이다.Pickling Line The acid concentration of pickling tank is an important factor that affects the quality of cold rolled coils due to the effects of premature pickling and superacid pickling generated after pickling of hot rolled coil.
냉연공정에서의 산세목적은 열연코일표면의 산화막을 제거하기 위한 것이다. 고온으로 열간압연 작업시 코일표면에서 철과 산소가 반응하여 생성되는 스케일은 갈철광, 자철광, 적철광등의 산화물로 형성된다, 이 중 갈철광이 스케일의 95퍼센트를 차지하고 있다. 산세액은 황산, 염산, 질산, 인산등이 있으나 산세용액으로는 황산이 대표적이나 최근 염산이 주로 사용되고 있는데 염산이 황산에 비해 약 1.5배의 산세력이 좋다. 산세처리과정에서 생성된 폐산은 산재생설비인 산회수 설비로 공급되어 재생산되어 산세탱크에 이르게 되는데 각 탱크에 유입되는 스케일에 대한 최적의 반응을 시킬 수 있는 염산 용액을 공급하기 위해서는 산세탱크의 정확한 산농도 측정이 필요로 한다.The purpose of pickling in the cold rolling process is to remove the oxide film on the hot rolled coil surface. In the hot rolling operation at high temperature, the scale produced by the reaction of iron and oxygen on the coil surface is formed of oxides such as iron ore, magnetite and hematite, among which 95% of the scale is ore. Acid pickling solutions include sulfuric acid, hydrochloric acid, nitric acid, and phosphoric acid. However, sulfuric acid is the most typical pickling solution, but hydrochloric acid is used mainly. The waste acid generated during the pickling process is supplied to the acid recovery facility, which is an acid regeneration facility, and is regenerated to reach the pickling tank.In order to supply the hydrochloric acid solution that can optimally react to the scale flowing into each tank, Acid concentration measurement is required.
냉연공정의 산세라인공정후에 발생되는 미산세는 기준 산농도보다 산탱크의 산농도가 부족할 때 발생되는 현상으로 스케일이 제거되지 않아 후공정에서의 냉연 제품품질의 표면형상에 영향을 준다. 그리고 과산세는 기준 산농도보다 산탱크의 산농도가 높을 경우에 발생되며 코일의 표면이 검게되어 냉연제품의 표면 광택에 영향을 주게된다.The pickling after the pickling line process of the cold rolling process is a phenomenon that occurs when the acid concentration of the acid tank is less than the standard acid concentration. In addition, the superacid tax is generated when the acid concentration of the acid tank is higher than the standard acid concentration, and the surface of the coil becomes black, which affects the surface gloss of the cold rolled product.
기존의 산농도 검사방식은 다음과 같다.The existing acid concentration test method is as follows.
첫째, 방사선 밀도계에 의한 측정방식이 있다. 밀도계의 방사선 흡수는 측정성분의 흡수계수에 의존한다. 측정성분에 대해 방사선 동위원소 Am, Cs 각각에 의한 측정성분의 광흡수 계수차에 의해 산농도를 측정하고 있으나 측정성분의 광흡수계수가 밀도에 따라 차별화되지 않기 때문에 산농도 측정이 정확히 이루어지지 않는다. 또한 방사선에 의해 발생되는 피폭등의 위험성을 가지고 있어 관리에 문제가 되고 있다.First, there is a measurement method by a radiation density meter. The radiation absorption of the density meter depends on the absorption coefficient of the measurement component. The acid concentration is measured by the light absorption coefficient difference of the measurement component by the radioisotope Am and Cs, respectively, but the measurement of the acid concentration is not accurate because the light absorption coefficient of the measurement component is not differentiated according to the density. . In addition, there is a risk of exposure caused by radiation, which is a problem in management.
둘째, 비중전도도계에 의한 측정방식이 있다. 산용액의 비중과 전도도에 따른 산농도값을 테이블화하여 산농도값을 도출하고 있지만 온도등의 변수에 영향을 받아 정확한 측정이 이루어지지 않고 있다.Second, there is a measurement method using a specific gravity conductivity meter. Acid concentration values are derived by tabulating acid concentration values according to specific gravity and conductivity of acid solution, but accurate measurements are not made due to the influence of variables such as temperature.
상기한 종래의 문제점을 해결하기 위해 안출된 본 발명은 냉연 산세라인에서 열연공정후의 열연코일을 공급받아 열간압연으로 인해 생성된 스트립표면의 스케일의 미산세 및 과산세를 방지하고 측정정확도를 높이기 위하여 임피던스 스펙트럼을 이용한 온라인 산농도 측정 방법 및 장치를 제공하는 데 그 목적이 있다.The present invention devised to solve the above-mentioned problems is to receive the hot rolled coil after the hot rolling process in the cold rolled pickling line to prevent fine pickling and over-pickling of the scale of the strip surface generated by hot rolling and to increase the measurement accuracy. An object of the present invention is to provide a method and apparatus for measuring online acid concentration using an impedance spectrum.
도 1은 본 발명을 구현하는 시스템의 블록 구성도1 is a block diagram of a system implementing the present invention.
도 2는 주파수변화에 따른 임피던스의 크기 변화도2 is a change in the magnitude of the impedance according to the frequency change
도 3은 산용액 샘플에 따른 산농도 그래프Figure 3 is a graph of acid concentration according to the acid solution sample
도 4는 주파수가 10Hz일 때의 산용액 샘플에 따른 임피던스 크기 변화도4 is a change in impedance magnitude according to an acid solution sample when the frequency is 10 Hz
도 5는 임피던스의 크기가 수렴하는 영역에서의 각 샘플용액의 임피던스 크기를 보여주는 그래프5 is a graph showing the magnitude of impedance of each sample solution in the region where the magnitude of impedance converges.
* 도면의 주요부분에 대한 부호의 설명 *Explanation of symbols on the main parts of the drawings
1 : 산회수 탱크 2 : 산농도 측정배관1: Acid recovery tank 2: Acid concentration measurement piping
3 : 전극 4 : 주파수 가변 교류전원 장치3: electrode 4: frequency variable AC power supply
5 : 임피던스 스펙트럼 측정부 6 : 모니터5: impedance spectrum measuring unit 6: monitor
7 : 산용액 샘플 A 8 : 산용액 샘플 B7: Acid solution sample A 8: Acid solution sample B
9 : 산용액 샘플 C9: acid solution sample C
상기한 목적을 달성하기 위한 본 발명은 냉연 산세라인의 산농도를 온라인으로 검사하기 위해 산회수탱크의 산농도측정배관에 전극을 삽입하고 인가교류전원의 주파수를 달리하면서 광범위한 주파수영역에서의 임피던스 특성으로 산용액의 산농도를 측정한다.In order to achieve the above object, the present invention provides an impedance characteristic in a wide range of frequencies while inserting an electrode into an acid concentration measurement pipe of an acid recovery tank and varying the frequency of an applied AC power source to check the acid concentration of a cold rolled pickling line online. Measure the acid concentration of the acid solution.
본 발명의 방 측정대상물질인 산용액에 전기장을 인가하면 산용액을 구성하고 있는 물질의 이온이나 원자는 이에 응답하게 되고 그 결과는 임피던스의 변화로 측정된다. 즉, 전기장에 의한 측정대상 물질의 임피던스 변화는 그 물질의 성분변화에 따라 달라지므로 이에 대한 특성을 통해 산농도를 측정하는 것이다.When an electric field is applied to the acid solution, which is the material to be measured, the ions or atoms of the material constituting the acid solution respond to this, and the result is measured as a change in impedance. In other words, the impedance change of the material to be measured by the electric field depends on the change in the composition of the material, so the acid concentration is measured through the characteristics thereof.
이하, 첨부도면을 참조하여 본 발명의 실시예를 설명하면 다음과 같다.Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings.
도 1은 상기의 본 발명에 따른 산용액의 산농도 측정방법을 구현하는 장치의 구성도이다.1 is a block diagram of a device for implementing a method for measuring the acid concentration of the acid solution according to the present invention.
도면에서 보듯이 본 발명의 냉연 산세라인의 산농도 측정장치는, 산회수 탱크(1)의 산농도를 측정하기 위해 산회수 라인에 별도로 설치되는 산농도 측정배관(2); 상기 산농도 측정배관(2)에 삽입되는 전극(3); 상기 전극(3)에 교류전원을 인가하는 주파수 가변 교류전원 장치(4); 상기 주파수 가변 교류전원장치(4)에서 상기 전극(3)에 교류전원을 인가함에 따라 변화되는 상기 산농도 측정 배관(2)내 산용액의 교류임피던스를 측정하는 임피던스 스텍트럼 측정부(5); 및 상기 임피던스 스펙트럼 측정부의 산농도측정 결과를 사용자에게 보여주는 모니터(6)로 구성된다.As shown in the drawings, the acid concentration measuring apparatus of the cold rolled pickling line of the present invention includes: an acid concentration measuring pipe 2 installed separately in the acid recovery line to measure the acid concentration of the acid recovery tank 1; An electrode 3 inserted into the acid concentration measurement pipe 2; A frequency variable AC power supply device (4) for applying AC power to the electrode (3); An impedance spectrum measuring unit (5) for measuring an AC impedance of an acid solution in the acid concentration measuring pipe (2) which is changed by applying AC power to the electrode (3) in the frequency variable AC power supply device (4); And a monitor 6 showing the acid concentration measurement results of the impedance spectrum measuring unit to the user.
이와 같이 구성되는 산농도 측정 장치를 이용한 산농도 측정 방법은 다음과 같다.The acid concentration measuring method using the acid concentration measuring apparatus configured as described above is as follows.
산세처리 과정에서 생성된 폐산을 재생하기 위한 산회수 탱크(1)에 설친된 산농도측정배관(2)내에 설치된 전극(3)에 주파수 가변 교류전원장치(4)에서 교류전원을 인가한다. 그리고 전기장 인가에 따른 양 전극(3)에서의 임피던스변화를 임피던스 스펙트럼 측정부(5)에서 분석하여 산농도를 측정하고, 그 측정 결과를 조업실의 모니터(6)로 전송하여 사용자가 인식할 수 있도록 한다. 사용자는 모니터(6)에 표시되는 산농도 측정결과를 이용하여 산탱크의 산용액 농도를 산세과정에서 요구되는 최적농도로 조절할 수 있게 된다.AC power is supplied from the variable frequency AC power supply 4 to the electrode 3 installed in the acid concentration measuring pipe 2 installed in the acid recovery tank 1 for regenerating the waste acid generated in the pickling process. The impedance change at the positive electrode 3 according to the electric field is analyzed by the impedance spectrum measuring unit 5 to measure the acid concentration, and the measurement result is transmitted to the monitor 6 of the operating room to be recognized by the user. Make sure The user can adjust the acid solution concentration of the acid tank to the optimum concentration required in the pickling process by using the acid concentration measurement result displayed on the monitor 6.
도 2는 전극에 인가되는 전계를 정전계 대신 전계가 시간적으로 변화하는 교류전계를 인가해서 주파수에 따른 임피던스 변화를 측정한 그래프이다. 인가주파수의 범위는 10Hz에서 13MHz까지의 영역으로 광범위한 시간변화에 대한 산용액의 분포된 성분의 농도를 측정하므로서 측정정도를 향상시킬 수 있다.FIG. 2 is a graph measuring an impedance change according to frequency by applying an alternating electric field in which an electric field changes in time instead of an electrostatic field. The frequency range of the applied frequency ranges from 10Hz to 13MHz, which improves the measurement accuracy by measuring the concentration of distributed components of the acid solution over a wide range of time changes.
도 2는 전극의 인가전원 주파수를 10Hz에서 10MHz까지 변화시켰을 경우의 각샘플 산용액의 임피던스를 측정한 그래프이다. 주파수가 증가함에 따라 │Z(f)│의 크기가 감소하다가 일정한 값으로 접근하고 있다. 이값은 산용액의 실제저항 값을 반영하고 있다.Fig. 2 is a graph measuring the impedance of each sample acid solution when the applied power supply frequency of the electrode is changed from 10 Hz to 10 MHz. As the frequency increases, the magnitude of Z (f) decreases and approaches a constant value. This value reflects the actual resistance of the acid solution.
도 3은 각 샘플 산용액의 산농도값을 나타낸 것이고, 도 4는 주파수가 10Hz일 때 시편종류에 따른 임피던스의 변화를 나타낸 것인데 산농도가 증가할수록 임피던스가 감소함을 알 수 있다.Figure 3 shows the acid concentration value of each sample acid solution, Figure 4 shows the change in impedance according to the specimen type when the frequency is 10Hz, it can be seen that the impedance decreases as the acid concentration increases.
도 5는 주파수가 증가함에 따라 임피던스의 크기가 일정한 값으로 수렴할 때의 임피던스 값을 보여주고 있으며, 산농도와 임피던스의 크기가 반비례함을 알 수 있다.5 shows an impedance value when the magnitude of the impedance converges to a constant value as the frequency increases, and it can be seen that the acid concentration and the magnitude of the impedance are inversely proportional to each other.
이상에서 본 발명에 대한 기술사상을 첨부도면과 함께 서술하였지만 이는 본 발명의 바람직한 실시예를 예시적으로 설명한 것이지 본 발명을 한정하는 것은 아니다. 또한, 이 기술분야의 통상의 지식을 가진 자라면 누구나 본 발명의 기술사상의 범주를 이탈하지 않는 범위 내에서 다양한 변형 및 모방이 가능함은 명백한 사실이다.The technical spirit of the present invention has been described above with reference to the accompanying drawings, but this is by way of example only and not intended to limit the present invention. In addition, it is obvious that any person skilled in the art can make various modifications and imitations without departing from the scope of the technical idea of the present invention.
상술한 바와 같은 본 발명은 냉연 산세라인에서 열연공정후의 열연코일을 산세하는 과정에서 산농도에 따라 발생되는 미산세 및 과산세의 직접적 원인이 되는 산탱크의 산농도를 임피던스 스펙트럼에 의하여 정확하게 측정하므로써 산농도의측정 신뢰도를 향상시키고, 산농도 관리 및 제어의 최적화가 가능하여 미산세 및 과산세를 방지할 수 있어 냉연제품품질을 향상시킬 수 있다.The present invention as described above by accurately measuring the acid concentration of the acid tank which is a direct cause of the pickling and peracid generated by the acid concentration in the process of pickling the hot rolled coil after the hot rolling process in the cold-roll pickling line by the impedance spectrum It is possible to improve the reliability of measurement of acid concentration and to optimize acid concentration management and control to prevent fine pickling and over pickling, thereby improving cold rolled product quality.
또한 염산가스의 대기방출에 의한 환경오염을 방지하는 효과도 있다.In addition, there is an effect to prevent environmental pollution by air emissions of hydrochloric acid gas.
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