本文關(guān)鍵詞： 甲基磺酸亞錫 電解 均勻設(shè)計 穩(wěn)定性 陽極溶解　出處：《沈陽理工大學》2010年碩士論文　論文類型：學位論文

【摘要】：隨著工業(yè)的迅速發(fā)展,人們越來越關(guān)注電鍍液的安全性、穩(wěn)定性及環(huán)保性。甲基磺酸亞錫鍍液體系不但穩(wěn)定、低毒性、低腐蝕、鍍層質(zhì)量高、可在高電流密度下操作,而且可生物降解為硫酸鹽和二氧化碳,更具環(huán)保性,故其工業(yè)化發(fā)展?jié)摿κ置黠@。然而,目前甲基磺酸亞錫的制備方法存在污染環(huán)境、產(chǎn)品質(zhì)量差、收率低等問題。因此,研發(fā)新的甲基磺酸亞錫合成方法對其生產(chǎn)及實際應(yīng)用具有重要意義。 基于甲基磺酸亞錫的現(xiàn)狀及電解法高效環(huán)保、投資省、效益高、應(yīng)用廣的優(yōu)勢,本文提出一種將電解法應(yīng)用于制備甲基磺酸亞錫的設(shè)計思想。以金屬錫板為陽極、石墨為陰極,甲基磺酸為陰極室和陽極室電解液,通過電解使陽極錫融入陽極電解液與甲基磺酸根結(jié)合,從而實現(xiàn)了電解法制備甲基磺酸亞錫。結(jié)合均勻設(shè)計及單因素實驗設(shè)計方法,探討了電解法制備甲基磺酸亞錫的最佳制備條件;對比研究了電解法和傳統(tǒng)化學法所制備甲基磺酸亞錫的穩(wěn)定性;考察了抗氧化劑提高甲基磺酸亞錫穩(wěn)定性的可行性;并通過電化學法對陽極錫的溶解行為進行了初步研究。 結(jié)果表明,電解法制備甲基磺酸亞錫的較優(yōu)制備條件為MSA為1.5mol·L~(-1)、電流密度為5.0A·dm~(-2)、體系溫度為25℃、攪拌速率為400r·min~(-1)、抗氧化劑投加量為2.5g·L~(-1),相應(yīng)的收率為99.4%。IR分析表明該條件下所得產(chǎn)品為甲基磺酸亞錫。通過均勻?qū)嶒灁?shù)據(jù)的回歸分析,建立了轉(zhuǎn)化率Y和與主要制備影響因素MSA濃度X_1、電流密度X_2、體系溫度X_3和攪拌速率X_4間的回歸方程:Y=55.2955+16.8906X_2+0.0389X_3-0.0069X_4-1.8886X_1X_2-1.6687X_2X_2+0.0167X_1X_4 -0.00025884X_3X_4,得到了各影響因素的主次順序為“電流密度電解質(zhì)濃度攪拌速率體系溫度”,且MSA濃度與電流密度之間、MSA濃度與攪拌速率之間、體系溫度與攪拌速率之間均存在相互作用。穩(wěn)定性對比實驗表明,電解法制備甲基磺酸亞錫的熱穩(wěn)定性及抗氧化性均明顯優(yōu)于傳統(tǒng)化學法所制備的甲基磺酸亞錫,但二者均會產(chǎn)生溶液變色現(xiàn)象。通過Sn2+水解及氧化實驗,揭示了溫度和酸度是影響甲基磺酸亞錫溶液變色現(xiàn)象的主要因素,而通過加入對苯二酚作為抗氧化劑可明顯減緩甲基磺酸亞錫溶液變色現(xiàn)象的產(chǎn)生。經(jīng)電化學測試的Tafel曲線及電解實驗結(jié)果,揭示了電解法制備甲基磺酸亞錫的陽極錫的溶解速率隨著電解液酸度、溫度、攪拌速率的增加而增加,這主要歸因于提高酸度會促進溶液中自由離子移動及電荷傳遞,升高溫度引起活化分子比例增加且分子運動速度加快,增加攪拌速率可消除由濃度梯度而導(dǎo)致的濃差極化并加快液相傳質(zhì)速率。由阿累尼烏斯公式計算出反應(yīng)表觀活化能Ea為1.44kJ·mol~(-1)(293.15K~323.15K),由塔菲爾公式得出表觀傳質(zhì)系數(shù)β為0.22、交換電流密度i0為1.012×10~(-3)A·cm~(-2)。
[Abstract]:With the rapid development of industry, people pay more and more attention to the safety of plating solution, stability and environmental protection. Methyl sulfonic acid tin plating solution is not only stable, low toxicity, low corrosion, high coating quality, can operate under high current density, and the biodegradability of sulfate and carbon dioxide, more environmentally friendly, so the industrial development potential is obvious. However, the preparation process of stannous methanesulfonate in environmental pollution, poor product quality, low yield. Therefore, the development of a new synthesis method of stannous methanesulfonate on its production and application has important significance.
The status quo of stannous methanesulfonate and electrolytic method based on efficient environmental protection, saving investment, high efficiency, wide application, the paper proposes a design idea of electrolysis was applied to the preparation of stannous methanesulfonate. Using metal tin plate as anode and graphite as cathode, methyl sulfonic acid as the cathode chamber and the anode chamber through the electrolyte. The anode electrolytic tin into the anode electrolyte with methyl sulfonic acid radical, so as to realize the electrolytic preparation of stannous methanesulfonate. Combined with uniform design and single factor experimental design method, discusses the conditions for preparation of electrolytic preparation of stannous methanesulfonate was optimized; a comparative study of the electrolytic method and traditional chemical method for preparing methyl sulfonic acid stability stannous; investigated the feasibility of improving the antioxidant stability of stannous methanesulfonate; and studied the electrochemical dissolution behavior of tin anode.
The results show that the electrolytic preparation of stannous methanesulfonate is the optimum preparation conditions of MSA 1.5mol L~ (-1), current density of 5.0A - dm~ (-2) system, the temperature is 25 DEG C, stirring rate of 400R - min~ (-1), antioxidant dosage was 2.5G - L~ (-1). The analysis showed that the product yield of 99.4%.IR under the condition of the stannous methanesulfonate. Even through the regression analysis of experimental data, set up the conversion rate of Y and the main influencing factors of preparation of MSA concentration X_1, current density X_2, temperature X_3 and stirring rate X_4 regression equation between Y=55.2955+ 16.8906X_2+0.0389X_3-0.0069X_4-1.8886X_1X_2-1.6687X_2X_2+0.0167X_1X_4 -0.00025884X_3X_4, has been the order of the influencing factors for the current density, electrolyte concentration, stirring rate and temperature system "between MSA concentration and current density, MSA concentration and stirring rate, temperature and stirring speed system There are interactions between rate. Experiments show that the stability and preparation of stannous methanesulfonate prepared by thermal stability and oxidation resistance of electrolytic preparation of stannous methanesulfonate was significantly better than the traditional chemical method, but the two will produce solution discoloration by Sn2+ hydrolysis and oxidation experiments revealed that the temperature and acidity is the main factors affecting the stannous methanesulfonate solution discoloration, and by adding hydroquinone as antioxidants could alleviate stannous methanesulfonate solution discoloration phenomenon. The Tafel curve and electrochemical electrolysis experimental results reveal the dissolution rate of tin anode electrolytic preparation of stannous methanesulfonate as the electrolyte acidity, temperature increase the stirring rate increased, this is mainly attributed to the increased acidity will promote the transfer of free ions in the solution and mobile charge, high temperature resulted in activation of molecular ratio Increased and molecular motion speed, increasing the stirring rate can eliminate the concentration polarization caused by concentration gradient and speed up the liquid mass transfer rate. By Arrhenius formula to calculate the activation energy for Ea 1.44kJ mol~ (-1) (293.15K~323.15K), by the Tafel formula to the apparent mass transfer coefficient is 0.22, exchange the current density of I0 is 1.012 * 10~ (-3) A - cm~ (-2).

【學位授予單位】：沈陽理工大學
【學位級別】：碩士
【學位授予年份】：2010
【分類號】：TQ134.32

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