鈦基體增強(qiáng)摻硼金剛石電極電催化過程動力學(xué)研究
發(fā)布時間：2018-07-28 10:15
【摘要】：水環(huán)境中存在的有機(jī)污染物直接關(guān)乎人類身體健康,同時與社會發(fā)展有著至關(guān)重要的聯(lián)系,去除水體中難降解有機(jī)污染物已成為水環(huán)境保護(hù)的迫切要求。電催化氧化技術(shù)以電極表面電化學(xué)產(chǎn)生強(qiáng)氧化性活性物質(zhì)為媒介直接或間接氧化有機(jī)物,被環(huán)保工作者廣泛的應(yīng)用到有機(jī)物去除領(lǐng)域。摻硼金剛石(BDD)電極被認(rèn)作為電催化氧化領(lǐng)域最為理想高效的電極材料,而具體的有機(jī)物電催化氧化過程、機(jī)理及動力學(xué)增強(qiáng)機(jī)制有待進(jìn)一步研究。本論文以BDD電極電催化有機(jī)污染物為基礎(chǔ),重點(diǎn)圍繞高效BDD電極的構(gòu)筑及其在有機(jī)污染物的礦化過程,探索BDD電極電催化氧化有機(jī)污染物的機(jī)理、降解過程和鈦基體結(jié)構(gòu)與電催化之間的聯(lián)系;同時針對電極/溶液界面的電催化機(jī)理及動力學(xué)過程,設(shè)計實現(xiàn)增強(qiáng)電催化氧化過程動力學(xué)的具體途徑和方式。具體的主要研究成果如下:(1)基于提高BDD電極電催化活性的目的,在多孔鈦基體上通過熱絲化學(xué)氣相沉積方法制備了三維多孔鈦基摻硼金剛石(3D-Ti/BDD)薄膜,SEM、XRD和Raman測試表明多孔Ti/BDD薄膜保持了與二維BDD薄膜近似的質(zhì)量、晶型及相成分。在保持BDD電極自身高析氧電位特點(diǎn)的前提下,基體結(jié)構(gòu)由二維到多孔鈦的改變使薄膜呈現(xiàn)三維多孔結(jié)構(gòu),增加了BDD薄膜電極的表面積,多孔鈦/BDD電極的有效電化學(xué)面積由二維BDD電極的2.62 cm2 cm-2增加到8.37 cm2cm-2;循環(huán)伏安測試及電化學(xué)阻抗測試表明多孔鈦BDD對鐵氰化鉀氧化還原對具有更高的電催化活性和更快的電荷轉(zhuǎn)移速率,電荷轉(zhuǎn)移電阻由128.3Ωcm2降低到31.3Ωcm2。同時bdd薄膜沉積過程的操作參數(shù)也發(fā)揮著重要的作用,碳源濃度、硼摻雜濃度及反應(yīng)器壓力等通過影響沉積過程中金剛石顆粒的成核和生長速率,直接影響bdd晶粒的表面形貌及質(zhì)量,通過操作參數(shù)的控制能夠?qū)崿F(xiàn)微米及納米級多孔bdd薄膜的可控制備。(2)抗炎藥物在三維bdd電極上的降解過程及動力學(xué)研究�？寡姿幬镆殉蔀楫�(dāng)前水環(huán)境中出現(xiàn)的新型有機(jī)污染物,選取撲熱息痛為模擬污染有機(jī)物,研究其在bdd電極上的降解過程及動力學(xué)。撲熱息痛在循環(huán)伏安曲線的0.90v附近出現(xiàn)明顯的氧化峰,證明在撲熱息痛在bdd電極上的電催化過程存在電子轉(zhuǎn)移反應(yīng),并且其在對應(yīng)電位下的響應(yīng)電流與有機(jī)物濃度呈現(xiàn)良好的線性關(guān)系。不同電流密度下的有機(jī)物降解過程表明,隨著電流密度的升高,用于有機(jī)物電催化過程的電流逐漸增加,加快了撲熱息痛的整體礦化速率;但高電流密度也加劇了電極表面析氧副反應(yīng)的進(jìn)行,造成電流效率逐漸下降。撲熱息痛在bdd電極上的降解動力學(xué)符合準(zhǔn)一級反應(yīng)動力學(xué),在二維及多孔bdd電極上對應(yīng)的表觀速率常數(shù)分別為0.208、0.344h-1。多孔bdd電極擁有更大的比表面積,為撲熱息痛在bdd電極上的直接電子轉(zhuǎn)移過程提供更多的反應(yīng)活性位點(diǎn),促進(jìn)間接電催化氧化撲熱息痛過程中強(qiáng)氧化活性羥基自由基的電生成,最終表現(xiàn)出更快的電化學(xué)反應(yīng)動力學(xué)速率。最后,根據(jù)撲熱息痛電催化降解過程的存在的中間產(chǎn)物,提出了其在bdd電極上的機(jī)理及降解途徑。(3)對苯二酚在不同電極材料上的電催化礦化過程表明電極的電催化氧化活性與電極析氧電位及表面產(chǎn)生羥基自由基能力有著重要的聯(lián)系;不同取代基團(tuán)的對位取代酚類化合物在bdd電極上的電化學(xué)降解實驗顯示電催化反應(yīng)的活性受取代官能團(tuán)自身的電子效應(yīng)制約,有機(jī)物礦化過程中取代基脫離苯環(huán)成為整個電催化反應(yīng)過程的決速步驟,且電催化反應(yīng)速率與取代基特征hammett常數(shù)σ呈近似線性關(guān)系。bdd電催化氧化機(jī)理主要以電產(chǎn)生強(qiáng)氧化活性羥基自由基為媒介,多孔bdd電極自身多孔結(jié)構(gòu)的存在使多孔bdd電極表面產(chǎn)生羥基自由基的量約為二維電極的2.7倍,多孔bdd電極對于不同種類有機(jī)物的階躍電流為二維電極的2倍,表現(xiàn)出更高的間接電催化氧化能力。電催化氧化不同種類有機(jī)物的降解結(jié)果表明,多孔bdd電極能夠?qū)崿F(xiàn)更快的去除速率和電流效率,但多孔電極內(nèi)部不規(guī)則的孔道結(jié)構(gòu)造成有機(jī)物在多孔電極內(nèi)部的傳質(zhì)過程變得困難,成為整個降解過程的限制步驟,造成了多孔電極羥基自由基利用率只有50~60%,這在一定程度削弱了多孔BDD電極高催化氧化能力的優(yōu)勢。(4)針對于上述多孔電極孔洞內(nèi)部傳質(zhì)受限的問題,進(jìn)一步設(shè)計用于增強(qiáng)電極/溶液界面?zhèn)髻|(zhì)過程的三維網(wǎng)絡(luò)BDD電極。以三維網(wǎng)絡(luò)鈦作為沉積基體制備得到具有表面微結(jié)構(gòu)的三維網(wǎng)絡(luò)BDD電極。電極微結(jié)構(gòu)表面為電催化氧化反應(yīng)提供更多的活性位點(diǎn),有效電化學(xué)表面積為二維BDD電極的1.6倍。由于表面積的增強(qiáng)作用及天然的網(wǎng)絡(luò)結(jié)構(gòu),三維網(wǎng)絡(luò)BDD電極在鐵氰化鉀氧化還原對溶液中的相關(guān)電化學(xué)測試中表現(xiàn)出更高的電催化活性和較低的傳質(zhì)電阻;表面疏水性的增強(qiáng)作用使電極表面產(chǎn)生的羥基自由基更容易脫離電極表面進(jìn)入本體溶液與有機(jī)物進(jìn)行電化學(xué)氧化作用,增加了羥基自由基的利用效率;三維網(wǎng)絡(luò)結(jié)構(gòu)增強(qiáng)有機(jī)物在電極表面的傳質(zhì)過程使有機(jī)物在電極表面具有更快的傳質(zhì)系數(shù),削弱了傳質(zhì)過程控制的限制,以上因素使三維網(wǎng)絡(luò)BDD電極相在具體的不同種類有機(jī)物的礦化實驗中表現(xiàn)出更快的去除速率及動力學(xué)過程。此外,將三維網(wǎng)絡(luò)鈦基體還可擴(kuò)展到其他用于水處理的網(wǎng)絡(luò)鈦基體和活性涂層,制備得到的網(wǎng)絡(luò)PbO2電極表現(xiàn)出比擬于BDD電極的優(yōu)異電催化氧化性能,驗證了此類網(wǎng)絡(luò)電極的適用性和高效性。
[Abstract]:Organic pollutants in water environment are directly related to human health and have a vital relationship with social development. It has become an urgent requirement for water environmental protection to remove the difficult degradation of organic pollutants in water bodies. The electrocatalytic oxidation technology produces strong oxidizing active substances from the electrode surface electrochemistry as the direct or indirect oxygen. Organic compounds are widely used by environmentalists in the field of organic matter removal. Boron doped diamond (BDD) electrode is considered as the most ideal and efficient electrode material in the field of electrocatalytic oxidation. The mechanism and kinetics enhancement mechanism of the specific organic electrocatalytic oxidation process need further study. This paper uses BDD electrode to electrocatalysis organic pollution. On the basis of the dye, focusing on the construction of high efficiency BDD electrode and the mineralization process of organic pollutants, the mechanism of electrocatalytic oxidation of organic pollutants by BDD electrode, the relationship between the degradation process and the titanium matrix structure and electrocatalysis are explored. At the same time, the electro catalytic mechanism and the kinetic process of the electrode / solution interface are designed to enhance the electrical stimulation. The concrete main research results are as follows: (1) based on the purpose of improving the electrocatalytic activity of BDD electrode, a three-dimensional porous titanium based boron doped diamond (3D-Ti/BDD) film was prepared on porous titanium substrate by hot wire chemical vapor deposition. The SEM, XRD and Raman tests showed that the porous Ti/BDD film was preserved. On the premise of maintaining the high oxygen evolution potential of the BDD electrode, the matrix structure from the change of two-dimensional to porous titanium makes the thin film three-dimensional porous structure, increases the surface area of the BDD film electrode, and the effective electrochemical area of the porous titanium /BDD electrode is 2.62 from the two-dimensional BDD electrode, on the premise of maintaining the high oxygen evolution potential of the BDD electrode. Cm2 cm-2 increases to 8.37 cm2cm-2; cyclic voltammetry and electrochemical impedance tests indicate that porous titanium BDD has higher electrocatalytic activity and faster charge transfer rate for potassium ferricyanide redox, and the operation parameters of the charge transfer resistance from 128.3 Omega cm2 to 31.3 Omega cm2. and the BDD film deposition process are also important. The surface morphology and quality of BDD grains are directly affected by the influence of carbon source concentration, boron doping concentration and reactor pressure on the nucleation and growth rate of the diamond particles in the deposition process. The controllable preparation of micrometer and nanoscale porous BDD films can be achieved through the control of operating parameters. (2) the degradation of anti-inflammatory drugs on the three-dimensional BDD electrode Study of process and dynamics. Anti inflammatory drugs have become a new organic pollutant in the current water environment. The degradation process and kinetics of paracetamol on the BDD electrode are studied. Paracetamol appears obvious oxidation peak near the 0.90v of cyclic voltammetry curve. It is proved that paracetamol is on the BDD electrode. There is an electron transfer reaction in the electrocatalysis process, and the response current at the corresponding potential has a good linear relationship with the concentration of organic matter. The degradation process of organic matter under different current density shows that the current increase in the electrocatalytic process of organic matter increases with the increase of current density, accelerating the overall mineralization of acetaminophen. However, the high current density also aggravates the oxidation side reaction of the electrode surface, resulting in the gradual decrease of the current efficiency. The degradation kinetics of acetaminophen on the BDD electrode conforms to the quasi first order reaction kinetics, and the apparent rate constant on the two-dimensional and porous BDD electrode has a larger comparison table for the 0.208,0.344h-1. porous BDD electrode, respectively. The area provides more reactive sites for the direct electron transfer of paracetamol on the BDD electrode, promoting the electroformation of the strongly oxidized active hydroxyl radical in the process of indirect electrocatalytic oxidation acetaminophen, and eventually showing a faster electrochemical reaction kinetic rate. The mechanism and degradation pathway on the BDD electrode are proposed. (3) the electrocatalytic mineralization of hydroquinone on different electrode materials shows that the electrocatalytic oxidation activity of the electrode has an important relation with the electrode oxygen evolution potential and the surface generation of hydroxyl radical. The substituent phenols of different substituent groups are in the BD The electrochemical degradation experiments on the D electrode show that the activity of the electrocatalytic reaction is restricted by the electronic effect of the substituent functional group itself. The substituent is separated from the benzene ring in the mineralization process and becomes the quick step of the whole electrocatalytic reaction process, and the electrocatalytic reaction rate is approximately linear with the Hammett constant of the substituent group, which has an approximate linear relationship with the electrocatalytic oxygen (.Bdd). The mechanism mainly produces the strong oxidation active hydroxyl radical as the medium, and the existence of porous structure of porous BDD electrode makes the amount of hydroxyl radical produced on the surface of the porous BDD electrode is about 2.7 times that of the two-dimensional electrode, and the step current of the porous BDD electrode is 2 times that of the two dimensional electrode for different kinds of organic matter, showing a higher indirect electrical stimulation. The degradation of different kinds of organic compounds by electrocatalytic oxidation shows that the porous BDD electrode can achieve faster removal rate and current efficiency. However, the irregular pore structure inside the porous electrode leads to the difficulty in the mass transfer process of organic matter in the porous electrode, which is a limiting step for the whole degradation process and causes much more. The utilization rate of hydroxyl radical of hole electrode is only 50~60%, which weakens the advantage of high catalytic oxidation ability of porous BDD electrode. (4) to further design the three dimension network BDD electrode for enhancing the mass transfer process of electrode / solution interface for the problem of the internal mass transfer in the porous electrode hole. A three-dimensional network BDD electrode with surface microstructures is prepared. The electrode microstructural surface provides more active sites for the electrocatalytic oxidation reaction, and the effective electrochemical surface area is 1.6 times as high as that of the two-dimensional BDD electrode. Due to the enhancement of surface area and the natural network structure, the three-dimensional network BDD electrode redox to the solution of the solution of the potassium ferricyanide Higher electrocatalytic activity and lower mass transfer resistance were shown in the related electrochemical tests, and the enhancement of surface hydrophobicity made the hydroxyl radicals produced on the surface of the electrode more easily detached from the surface of the electrode to enter the bulk solution and the organic matter to be electrochemical oxidation, and increased the efficiency of the hydroxyl radical. The mass transfer process of organics on the electrode surface makes the organic matter have a faster mass transfer coefficient on the surface of the electrode and weakens the restriction of the mass transfer process control. The above factors make the three-dimensional network BDD electrode show a faster removal rate and dynamic process in the mineralizing experiment of different kinds of organic matter. In addition, the three-dimensional network is used. The complex titanium matrix can also be extended to other network titanium and active coatings for water treatment. The obtained network PbO2 electrode shows excellent electrocatalytic oxidation performance compared to the BDD electrode, and the applicability and efficiency of this kind of network electrode have been verified.
【學(xué)位授予單位】：吉林大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2017
【分類號】：O646.5;O643.3
本文編號：2149766
[Abstract]:Organic pollutants in water environment are directly related to human health and have a vital relationship with social development. It has become an urgent requirement for water environmental protection to remove the difficult degradation of organic pollutants in water bodies. The electrocatalytic oxidation technology produces strong oxidizing active substances from the electrode surface electrochemistry as the direct or indirect oxygen. Organic compounds are widely used by environmentalists in the field of organic matter removal. Boron doped diamond (BDD) electrode is considered as the most ideal and efficient electrode material in the field of electrocatalytic oxidation. The mechanism and kinetics enhancement mechanism of the specific organic electrocatalytic oxidation process need further study. This paper uses BDD electrode to electrocatalysis organic pollution. On the basis of the dye, focusing on the construction of high efficiency BDD electrode and the mineralization process of organic pollutants, the mechanism of electrocatalytic oxidation of organic pollutants by BDD electrode, the relationship between the degradation process and the titanium matrix structure and electrocatalysis are explored. At the same time, the electro catalytic mechanism and the kinetic process of the electrode / solution interface are designed to enhance the electrical stimulation. The concrete main research results are as follows: (1) based on the purpose of improving the electrocatalytic activity of BDD electrode, a three-dimensional porous titanium based boron doped diamond (3D-Ti/BDD) film was prepared on porous titanium substrate by hot wire chemical vapor deposition. The SEM, XRD and Raman tests showed that the porous Ti/BDD film was preserved. On the premise of maintaining the high oxygen evolution potential of the BDD electrode, the matrix structure from the change of two-dimensional to porous titanium makes the thin film three-dimensional porous structure, increases the surface area of the BDD film electrode, and the effective electrochemical area of the porous titanium /BDD electrode is 2.62 from the two-dimensional BDD electrode, on the premise of maintaining the high oxygen evolution potential of the BDD electrode. Cm2 cm-2 increases to 8.37 cm2cm-2; cyclic voltammetry and electrochemical impedance tests indicate that porous titanium BDD has higher electrocatalytic activity and faster charge transfer rate for potassium ferricyanide redox, and the operation parameters of the charge transfer resistance from 128.3 Omega cm2 to 31.3 Omega cm2. and the BDD film deposition process are also important. The surface morphology and quality of BDD grains are directly affected by the influence of carbon source concentration, boron doping concentration and reactor pressure on the nucleation and growth rate of the diamond particles in the deposition process. The controllable preparation of micrometer and nanoscale porous BDD films can be achieved through the control of operating parameters. (2) the degradation of anti-inflammatory drugs on the three-dimensional BDD electrode Study of process and dynamics. Anti inflammatory drugs have become a new organic pollutant in the current water environment. The degradation process and kinetics of paracetamol on the BDD electrode are studied. Paracetamol appears obvious oxidation peak near the 0.90v of cyclic voltammetry curve. It is proved that paracetamol is on the BDD electrode. There is an electron transfer reaction in the electrocatalysis process, and the response current at the corresponding potential has a good linear relationship with the concentration of organic matter. The degradation process of organic matter under different current density shows that the current increase in the electrocatalytic process of organic matter increases with the increase of current density, accelerating the overall mineralization of acetaminophen. However, the high current density also aggravates the oxidation side reaction of the electrode surface, resulting in the gradual decrease of the current efficiency. The degradation kinetics of acetaminophen on the BDD electrode conforms to the quasi first order reaction kinetics, and the apparent rate constant on the two-dimensional and porous BDD electrode has a larger comparison table for the 0.208,0.344h-1. porous BDD electrode, respectively. The area provides more reactive sites for the direct electron transfer of paracetamol on the BDD electrode, promoting the electroformation of the strongly oxidized active hydroxyl radical in the process of indirect electrocatalytic oxidation acetaminophen, and eventually showing a faster electrochemical reaction kinetic rate. The mechanism and degradation pathway on the BDD electrode are proposed. (3) the electrocatalytic mineralization of hydroquinone on different electrode materials shows that the electrocatalytic oxidation activity of the electrode has an important relation with the electrode oxygen evolution potential and the surface generation of hydroxyl radical. The substituent phenols of different substituent groups are in the BD The electrochemical degradation experiments on the D electrode show that the activity of the electrocatalytic reaction is restricted by the electronic effect of the substituent functional group itself. The substituent is separated from the benzene ring in the mineralization process and becomes the quick step of the whole electrocatalytic reaction process, and the electrocatalytic reaction rate is approximately linear with the Hammett constant of the substituent group, which has an approximate linear relationship with the electrocatalytic oxygen (.Bdd). The mechanism mainly produces the strong oxidation active hydroxyl radical as the medium, and the existence of porous structure of porous BDD electrode makes the amount of hydroxyl radical produced on the surface of the porous BDD electrode is about 2.7 times that of the two-dimensional electrode, and the step current of the porous BDD electrode is 2 times that of the two dimensional electrode for different kinds of organic matter, showing a higher indirect electrical stimulation. The degradation of different kinds of organic compounds by electrocatalytic oxidation shows that the porous BDD electrode can achieve faster removal rate and current efficiency. However, the irregular pore structure inside the porous electrode leads to the difficulty in the mass transfer process of organic matter in the porous electrode, which is a limiting step for the whole degradation process and causes much more. The utilization rate of hydroxyl radical of hole electrode is only 50~60%, which weakens the advantage of high catalytic oxidation ability of porous BDD electrode. (4) to further design the three dimension network BDD electrode for enhancing the mass transfer process of electrode / solution interface for the problem of the internal mass transfer in the porous electrode hole. A three-dimensional network BDD electrode with surface microstructures is prepared. The electrode microstructural surface provides more active sites for the electrocatalytic oxidation reaction, and the effective electrochemical surface area is 1.6 times as high as that of the two-dimensional BDD electrode. Due to the enhancement of surface area and the natural network structure, the three-dimensional network BDD electrode redox to the solution of the solution of the potassium ferricyanide Higher electrocatalytic activity and lower mass transfer resistance were shown in the related electrochemical tests, and the enhancement of surface hydrophobicity made the hydroxyl radicals produced on the surface of the electrode more easily detached from the surface of the electrode to enter the bulk solution and the organic matter to be electrochemical oxidation, and increased the efficiency of the hydroxyl radical. The mass transfer process of organics on the electrode surface makes the organic matter have a faster mass transfer coefficient on the surface of the electrode and weakens the restriction of the mass transfer process control. The above factors make the three-dimensional network BDD electrode show a faster removal rate and dynamic process in the mineralizing experiment of different kinds of organic matter. In addition, the three-dimensional network is used. The complex titanium matrix can also be extended to other network titanium and active coatings for water treatment. The obtained network PbO2 electrode shows excellent electrocatalytic oxidation performance compared to the BDD electrode, and the applicability and efficiency of this kind of network electrode have been verified.
【學(xué)位授予單位】：吉林大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2017
【分類號】：O646.5;O643.3
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