KR100405512B1 - HIGH EFFICIENCY ELECTRODE PLATING METHOD FOR THE GENERATION OF NaOCL - Google Patents

HIGH EFFICIENCY ELECTRODE PLATING METHOD FOR THE GENERATION OF NaOCL Download PDF

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KR100405512B1
KR100405512B1 KR10-1998-0056032A KR19980056032A KR100405512B1 KR 100405512 B1 KR100405512 B1 KR 100405512B1 KR 19980056032 A KR19980056032 A KR 19980056032A KR 100405512 B1 KR100405512 B1 KR 100405512B1
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plating
plating thickness
sodium hypochlorite
electrode
composition ratio
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KR10-1998-0056032A
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KR20000040399A (en
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김흥락
김동수
김광일
강성건
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주식회사 포스코
재단법인 포항산업과학연구원
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/12—Process control or regulation
    • C25D21/14—Controlled addition of electrolyte components
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/24—Halogens or compounds thereof
    • C25B1/26—Chlorine; Compounds thereof
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • C25B11/097—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds comprising two or more noble metals or noble metal alloys
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/50—Electroplating: Baths therefor from solutions of platinum group metals
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/04—Electroplating with moving electrodes
    • C25D5/06—Brush or pad plating
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C25D5/50—After-treatment of electroplated surfaces by heat-treatment

Abstract

본 발명은 고효율 하이포아염소산소듐 발생용 전극을 도금하는 방법에 관한 것으로서, 모재인 Ti 표면에 브러싱(Brushing)법으로 도금두께를 일정하게 하고 Pt계 금속인 Pt, Ru 및 Ir 조성물의 첨가 비율을 변화시켜가면서, 도금밀착성 및 하이포아염소산소듐의 발생효율을 측정분석하여 Pt와 Ru 및 Ir 조성물의 최적의 조성비를 결정하는 조성물의 조성비결정단계와; 상기 조성물의 조성비결정단계에서 결정된 조성비의 조건하에서 전극의 도금두께를 변화시켜가면서 도금밀착성 및 하이포아염소산소듐의 발생효율을 측정분석하여 도금두께를 결정하는 도금두께결정단계와; 모재인 Ti 표면에 상기 도금두께결정단계에서 결정된 도금두께로 도금되도록 브러싱법으로 도금두께를 조정하면서 400∼600℃에서 1시간동안 열처리하는 브러싱 및 열처리단계로 형성한 도금전극을 고효율 하이포아염소산소듐의 발생에 이용, 도수관 속의 생물들의 고착을 효율적으로 방지할 수 있는 장점이 있다.The present invention relates to a method of plating an electrode for generating high efficiency sodium hypochlorite, the plating thickness of which is constant on the surface of Ti as a base material by brushing, and the addition ratio of Pt, Ru and Ir compositions, which are Pt-based metals, to be added. A composition ratio determining step of determining the optimum composition ratio of the Pt, Ru, and Ir compositions by measuring and analyzing plating adhesion and generation efficiency of sodium hypochlorite; A plating thickness determining step of determining the plating thickness by measuring and analyzing the plating adhesion and the generation efficiency of sodium hypochlorite while changing the plating thickness of the electrode under the conditions of the composition ratio determined in the composition ratio determining step of the composition; High-efficiency sodium hypochlorite plated electrode formed by the brushing and heat treatment step of heat treatment at 400-600 ° C. for 1 hour while adjusting the plating thickness to be plated by the plating thickness determined in the plating thickness determination step on the base Ti surface Used in the generation of, there is an advantage that can effectively prevent the settling of the organisms in the water pipe.

Description

고효율 하이포아염소산소듐 발생용 전극도금방법{HIGH EFFICIENCY ELECTRODE PLATING METHOD FOR THE GENERATION OF NaOCL}High-efficiency hypochlorite generation electrode plating method {HIGH EFFICIENCY ELECTRODE PLATING METHOD FOR THE GENERATION OF NaOCL}

본 발명은 고효율 하이포아염소산소듐 발생용 전극을 도금하는 방법에 관한 것으로서, 특히 해수를 냉각수로 사용하는 대규모 임해공장이나 제철소 또는 발전소에서 해수를 자연상태 그대로 사용할 경우에 도수관 내부에 번식하는 해초류 및 조개류의 번식을 억제할 목적으로 강 알카리성인 하이포아염소산소듐을 전기적으로 발생시켜 이를 해수속에 ppm 단위로 첨가하여 사용함으로써 도수관 속의 생물들의 고착을 방지하기 위한 고효율 하이포아염소산소듐 발생용 전극도금방법에 관한 것이다.The present invention relates to a method for plating an electrode for generating high-efficiency hypochlorite, particularly seaweeds and shellfish that propagate inside water pipes when the seawater is used as it is in a large-scale coastal plant, steel mill or power plant using seawater as cooling water. Highly alkaline sodium hypochlorite for the purpose of suppressing propagation of chlorine, and it is added to the seawater in ppm unit to use for high efficiency sodium plating method for electrodeposition of sodium hypochlorite will be.

일반적으로 해초류 및 조개류가 도수관내에 고착하는 것을 방지하기 위한 종래의 방법으로는 염소가스나 염산을 도수관 입구에 취입하여 사용하였으나, 이는 가스 노출의 위험성 때문에 현재는 대부분 해수를 전기분해하여 하이포아염소산소듐을 투입하고 있는 실정에 있다. 해수를 전기분해하는 방법은 전기분해를 위해 사용하는 전극으로 초기에는 탄소(C)를 이용하는 방법에서 Ti, 그리고 Ti+Pt로 계속하여 발전하여 현재는 모재인 Ti 표면에 백금계 혼합물질을 도포하여 사용하고 있으며, 도금전극의 구조는 해수전해설비 설치상 단극(Unipolar)형과 양극(Bipolar) 형으로 구분된다.In general, chlorine gas or hydrochloric acid is blown into the inlet of the water pipe as a conventional method for preventing seaweeds and shellfish from sticking to the water pipe. However, due to the risk of gas exposure, most sodium hypochlorite is electrolyzed at present. It is in the situation of investing. Electrolysis of seawater is an electrode used for electrolysis. Initially, carbon (C) is used to continuously develop Ti and Ti + Pt. The structure of the plated electrode is divided into unipolar type and bipolar type when installing seawater electrolysis equipment.

도금전극의 모재로 사용되는 Ti의 상태가 하이포아염소산소듐 발생에 중요한 변수로 작용하는데, 이것은 모재 자체의 표면이 불균일하거나 미세 요철의 변화에 따라 도금전극의 상태가 결정되기 때문이다. Ti 표면은 적당한 요철이 있어야만 도금박막을 도포할 경우에 도금박막과 Ti와의 표면 흡착력이 증가되어 최종적으로 도금전극의 수명이 향상되는 효과가 있고, 도금박막을 도포하기 위해서는 진공증착법, 전기도금법, 그리고 브러싱(Brushing)법이 있다.The state of Ti, which is used as the base material of the plated electrode, acts as an important variable in the generation of sodium hypochlorite, because the surface of the base material itself is uneven or the state of the plated electrode is determined by the change of fine irregularities. The surface of Ti must have proper irregularities to increase the surface adsorption force between the plating thin film and Ti when the plating thin film is applied. Finally, the life of the plating electrode can be improved. There is a brushing method.

본 발명은 상기한 실정을 감안하여 생산가격이 저렴하고 두께제어가 가장 쉬우면서도 연속되는 브러싱 작업에서도 상대적으로 요철이 없는 Ti 표면보다 요철이 있는 경우에 균일도가 향상되는 도금박막을 얻을 수 있는 브러싱(Brushing)법을 이용하여 하이포아염소산소듐 발생을 향상시킬 수 있는 고효율 하이포아염소산소듐 발생용 전극도금방법을 제공함에 그 목적이 있다.In view of the above-described circumstances, the present invention provides a plated thin film having improved uniformity when the production price is low and the thickness control is most easy, and even in the continuous brushing operation, the irregularities are higher than the Ti surface which is relatively uneven. An object of the present invention is to provide an electrode plating method for generating sodium hypochlorite, which can improve the generation of sodium hypochlorite by using a brushing method.

도 1a,1b는 도금전극의 조성성분별 하이포아염소산소듐 발생효율 및 도금밀착성을 나타낸 도면,1a and 1b are diagrams showing the generation efficiency and plating adhesion of sodium hypochlorite for each composition component of the plating electrode;

도 2a,2b는 도금전극의 도금두께별 하이포아염소산소듐 발생효율 및 도금밀착성을 나타낸 도면이다.2A and 2B are diagrams showing the generation efficiency and plating adhesion of sodium hypochlorite according to the plating thickness of the plating electrode.

상기한 목적을 달성하기 위한 본 발명 고효율 하이포아염소산소듐 발생용 전극도금방법은 모재인 Ti 표면에 브러싱(Brushing)법으로 도금두께를 일정하게 하고 Pt계 금속인 Pt, Ru 및 Ir 조성물의 첨가 비율을 변화시켜가면서, 도금밀착성 및 하이포아염소산소듐의 발생효율을 측정분석하여 Pt, Ru 및 Ir 조성물의 최적의 조성비를 결정하는 조성물의 조성비결정단계와; 상기 조성물의 조성비결정단계에서 결정된 조성비의 조건하에서 전극의 도금두께를 변화시켜가면서 도금밀착성 및 하이포아염소산소듐의 발생효율을 측정분석하여 도금두께를 결정하는 도금두께결정단계와; 모재인 Ti 표면에 상기 도금두께결정단계에서 결정된 도금두께로 도금되도록 브러싱법으로 도금두께를 조정하면서 400∼600℃에서 1∼5시간 열처리하는 브러싱 및 열처리단계로 이루어지는 것을 특징으로 한다.Electrode plating method for generating high efficiency sodium hypochlorite in accordance with the present invention for achieving the above object is to make the plating thickness constant by brushing (Brushing) on the surface of Ti as a base material and the addition ratio of Pt, Ru and Ir composition of Pt-based metal A composition ratio determining step of determining the optimum composition ratio of the Pt, Ru, and Ir compositions by measuring and analyzing plating adhesion and generation efficiency of sodium hypochlorite; A plating thickness determining step of determining the plating thickness by measuring and analyzing the plating adhesion and the generation efficiency of sodium hypochlorite while changing the plating thickness of the electrode under the conditions of the composition ratio determined in the composition ratio determining step of the composition; It is characterized in that it comprises a brushing and heat treatment step of heat treatment at 400 ~ 600 ℃ 1 to 5 hours while adjusting the plating thickness to be plated with the plating thickness determined in the plating thickness determination step on the base surface Ti.

상기 조성물의 조성비결정단계에서 결정된 조성물의 조성비는 Pt 30∼70%, Ru 15∼45%, Ir 15∼45%이며, 도금두께결정단계에서 결정된 도금두께는 3∼10㎛이다.The composition ratio of the composition determined in the composition ratio determining step of the composition is Pt 30 ~ 70%, Ru 15 ~ 45%, Ir 15 ~ 45%, the plating thickness determined in the plating thickness determination step is 3 ~ 10㎛.

본 발명은 브러싱방법을 이용한 것으로서, 브러싱작업 사이에 전개되는 열처리과정은 상대적으로 도금박막을 도포할 경우에 도금물질의 상호 유동성 및 접착성 향상을 위해서 사용되는 용액의 증발을 위한 것이며, 또한 도금박막의 모재 표면과의 흡착력 강화, 도금박막의 굳기를 향상시키기 위한 것이다.The present invention uses a brushing method, and the heat treatment process developed between brushing operations is for evaporation of a solution used to improve the mutual fluidity and adhesion of the plating material when the plating film is relatively coated. It is to enhance the adsorption power with the surface of the base metal and the hardness of the plated thin film.

이하 첨부도면을 참조하여 본 발명 고효율 하이포아염소산소듐 발생용 전극도금방법을 상세하게 설명한다.Hereinafter, the electrode plating method for generating high efficiency sodium hypochlorite of the present invention will be described in detail with reference to the accompanying drawings.

본 발명은 먼저 해수전해를 위한 도금전극의 기본 조건인 하이포아염소산소듐의 발생효율과 함께 전극수명에 관련된 도금박막의 도금밀착성을 향상시키는데, 필요한 도금두께 및 도금성분을 변화하여 각각에 대응하는 측정값들을 비교하여 최선의 전극도금방법을 제공하는 것이다.The present invention first improves the plating adhesion of the plated thin film related to the electrode life together with the generation efficiency of sodium hypochlorite, which is a basic condition of the plated electrode for seawater electrolysis, and changes the required plating thickness and the plated component so that the corresponding measurement is performed. Compare the values to provide the best electrode plating method.

따라서 본 발명은 도금성분을 모재인 Ti 표면에 브러싱법으로 전극의 도금두께를 일정하게 조정한 다음, 도금물질로서 사용된 Pt계 금속인 Pt, Ru 및 Ir의 조성비를 다르게 하여 도금밀착성 및 하이포아염소산소듐의 발생효율을 측정분석하여 도금성분에 관한 조건을 확보하며, 도금성분에 대한 조건이 결정된 다음 이 조건 하에서 도금두께를 변화하면서 도금밀착성 및 하이포아염소산소듐의 발생효율을 관찰하여 도금두께에 대한 조건을 확보한다.Therefore, in the present invention, the plating thickness of the electrode is uniformly adjusted by brushing on the surface of Ti, which is a base material, and then the plating adhesion and hypoaity are varied by varying the composition ratio of Pt-based metals, Pt, Ru and Ir, which are used as plating materials. Measure and analyze the generation efficiency of sodium chlorine to secure the conditions for the plating components, determine the conditions for the plating components, and then change the plating thickness under these conditions to observe the plating adhesion and the generation efficiency of sodium hypochlorite. Secure the conditions for

이러한 도금물질의 조성비 및 도금두께를 결정하는 방법을 보면, 먼저 도금박막에 대한 하이포아염소산소듐의 발생효율을 관찰하기 위해서 도금전극을 3%, 식염수 400ml에 넣어 전극판을 (+)전극으로 하고, 전극봉을 (-)전극으로 하여 전원을 인가한다. 이때 인가하는 전원의 전류는 4.8A로 시간은 3분으로 통일하고 하이포아염소산소듐의 발생을 시험하였다. 발생된 하이포아염소산소듐이 포함된 식염수를 색중화법으로 발생량을 검증하기 위해서 요오드화칼륨(Potassium Iodide)과 Na2S2O3를 이용하여 발생량을 계산하여 도 1a 및 1b에 도금성분비에 따른 하이포아염소산소듐의 발생량으로 나타냈다. 도금밀착성은 1/2인치 Sud를 에폭시를 이용하여 도금전극 표면에 고착시킨 후, 온도를 150℃로 하여 2시간 베이킹하고, 자연상태에서 50시간 방치하여 충분히 도금전극과 Sud를 고착시킨후 도금밀착력 시험기로 인장시험을 하였다. 도금밀착력은 약 1400PSI 이상을 확보한 것으로 관찰되었고, 발생효율은 Pt(30∼70%), Ir 및 Ru(15∼45%)에서 하이포아염소산소듐의 발생량이 이론치인 0.317g의 90% 인 0.285g 이상으로 나타났다. 도 2a 및 2b는 도금두께의 변화에 따른 하이포아염소산소듐의 발생량을 나타낸 것으로서, 도금두께가 3㎛ 이상 10㎛ 이하에서 가장 좋은 발생량과 함께 도금밀착력 1400PSI 이상의 도금밀착성을 나타냄을 알 수 있었다.In the method of determining the composition ratio and plating thickness of the plating material, first, in order to observe the generation efficiency of sodium hypochlorite in the plating film, the electrode plate was made into (+) electrode in 3% and 400 ml of saline solution. Apply power using electrode as (-) electrode. At this time, the current of the power supply applied was 4.8 A, the time was unified to 3 minutes, and the generation of sodium hypochlorite was tested. In order to verify the amount of generated sodium saline containing sodium hypochlorite by the color neutralization method, the amount generated using potassium iodide (Potassium Iodide) and Na 2 S 2 O 3 was calculated, and the hypochlorite according to the plating component ratio in FIGS. 1A and 1B. It was shown by the generation amount of sodium chlorate. Plating adhesion property is that 1/2 inch sud is fixed on the surface of the plating electrode using epoxy, then baked for 2 hours at a temperature of 150 ° C, and left for 50 hours in a natural state to sufficiently fix the plating electrode and sud. Tensile tests were performed with a tester. Plating adhesion was observed to secure about 1400 PSI or more, and the generation efficiency was 0.285, which is 90% of 0.317g of theoretical hypochlorite at Pt (30-70%), Ir and Ru (15-45%). more than g. 2A and 2B show the generation amount of sodium hypochlorite according to the change of the plating thickness, and it can be seen that the plating thickness shows the plating adhesion strength of 1400PSI or more with the best generation amount at 3 µm or more and 10 µm or less.

본 발명 고효율 하이포아염소산소듐 발생용 전극도금방법으로 도금된 도금전극을 도수관에 사용하면 고효율 하이포아염소산소듐의 발생으로 도수관 속의 생물들의 고착을 효율적으로 방지할 수 있는 장점이 있다.When the plating electrode plated by the electrode plating method for generating high efficiency sodium hypochlorite is used in a water pipe, the present invention has the advantage of effectively preventing the adhesion of organisms in the water pipe due to the generation of high efficiency sodium hypochlorite.

Claims (2)

모재인 Ti 표면에 브러싱(Brushing)법으로 도금두께를 일정하게 하고 Pt계 금속인 Pt, Ru 및 Ir 조성물의 첨가 비율을 변화시켜가면서 도금밀착성 및 하이포아염소산소듐의 발생효율을 측정분석하여 Pt, Ru 및 Ir 조성물의 최적의 조성비를 결정하는 조성물의 조성비결정단계와; 상기 조성물의 조성비결정단계에서 결정된 조성비의 조건하에서 전극의 도금두께를 변화시켜가면서 도금밀착성 및 하이포아염소산소듐의 발생효율을 측정분석하여 도금두께를 결정하는 도금두께결정단계와; 모재인 Ti 표면에 상기 도금두께결정단계에서 결정된 도금두께로 도금되도록 브러싱법으로 도금두께를 조정하면서 400∼600℃에서 1시간 열처리하는 브러싱 및 열처리단계로 이루어지고, 상기 조성물의 조성비결정단계에서 결정된 조성물의 최적의 조성비가 Pt 30∼70％, Ru 15∼45％, Ir 15∼45％인 것을 특징으로 하는 고효율 하이포아염소산소듐 발생용 전극도금방법.The plating thickness was fixed on the surface of the base Ti by brushing, and the Pt, Ru, and Ir compositions of Pt-based metals were changed, and the plating adhesion and the generation efficiency of sodium hypochlorite were measured and analyzed. A composition ratio determining step of the composition for determining an optimal composition ratio of the Ru and Ir compositions; A plating thickness determining step of determining the plating thickness by measuring and analyzing the plating adhesion and the generation efficiency of sodium hypochlorite while changing the plating thickness of the electrode under the conditions of the composition ratio determined in the composition ratio determining step of the composition; It is composed of a brushing and heat treatment step of heat treatment at 400 ~ 600 ℃ for 1 hour while adjusting the plating thickness to be plated to the plating thickness determined in the plating thickness determination step on the base surface Ti, and determined in the composition ratio determination step of the composition An optimum plating ratio of the composition is 30 to 70% of Pt, 15 to 45% of Ru, and 15 to 45% of Ir. The electrode plating method for generating high sodium hypochlorite. 제 1항에 있어서, 상기 도금두께결정단계에서 결정된 도금두께가 3∼10㎛인 것을 특징으로 하는 고효율 하이포아염소산소듐 발생용 전극도금방법.The electrode plating method of claim 1, wherein the plating thickness determined in the plating thickness determination step is 3 to 10 µm.
KR10-1998-0056032A 1998-12-18 1998-12-18 HIGH EFFICIENCY ELECTRODE PLATING METHOD FOR THE GENERATION OF NaOCL KR100405512B1 (en)

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KR100812990B1 (en) 2006-11-08 2008-03-13 고등기술연구원연구조합 Manufacturing method of mono-polar electrode

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KR100383269B1 (en) * 2000-12-26 2003-05-12 주식회사 포스코 Pt complex Electrode for seawater electrolysis

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JPS5550479A (en) * 1978-10-09 1980-04-12 Tdk Corp Electrode for electrolysis of dilute salt water
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JPS5518503A (en) * 1978-07-21 1980-02-08 Japan Carlit Co Ltd:The Electrode for electrolytic manufacturing hypochlorite
JPS5550479A (en) * 1978-10-09 1980-04-12 Tdk Corp Electrode for electrolysis of dilute salt water
JPS5925988A (en) * 1982-08-04 1984-02-10 Japan Carlit Co Ltd:The Electrode for electrolyzing sea water
JPS63121688A (en) * 1986-11-11 1988-05-25 Permelec Electrode Ltd Electrode for electrolysis and its production
JPH0277394A (en) * 1988-09-13 1990-03-16 Masaaki Murotani Insoluble electrode for electromagnetic propulsion ship

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100812990B1 (en) 2006-11-08 2008-03-13 고등기술연구원연구조합 Manufacturing method of mono-polar electrode

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