金属钒离子与栲胶配位作用的研究
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摘要
栲胶脱硫工艺是我国特有的的二元湿式催化氧化脱硫法之一,广泛用于化肥、焦化、石油炼制等行业H2S气体的脱除。在脱硫过程中,五价钒离子被HS-还原成四价钒离子,四价钒离子又在栲胶等载氧体存在下被空气氧化再生为五价钒离子,从而达到钒离子的循环使用。栲胶在其中不仅起到载氧体的作用,同时还可作为四价钒离子的络合剂,保护四价钒离子不易生成沉淀,且维持钒离子在脱硫过程中稳定在一定的浓度。因此,本论文分别采用pH电位法和紫外-可见分光光度法,以邻苯二酚、连苯三酚、没食子酸作为栲胶的模型化合物,以单宁酸作为栲胶的替代物,全面系统地研究了栲胶脱硫工艺中催化氧化剂钒离子与栲胶的配位作用。
通过研究pH值、温度、浓度等因素对五价钒V(V)与HS-之间的反应的影响,发现脱硫液的pH值是影响该反应的主要因素,说明脱硫过程的pH值应严格控制。
栲胶是一类以单宁成分为主的多酚混合物,结构中既含有酚羟基,还有一定量的羧基,采用紫外-可见分光光度法研究了四价钒V(Ⅳ)离子与苯酚、对苯二酚、间苯二酚、邻苯二酚、间羟基苯甲酸、酒石酸钾钠及没食子酸等七种有机化合物的配位反应。结果表明,四价钒只与这些有机化合物中含有邻位羟基和羧基官能团的化合物发生了配位反应,而与含有一个羟基、含有间位羟基和羧基官能团的化合物均未发生配位反应。
采用pH电位法测定了含有邻位酚羟基的邻苯二酚、连苯三酚及没食子酸模型化合物在25℃、30℃、35℃、40℃、45℃下的加质子常数,加质子常数随温度的升高而减小。由测定的一系列加质子常数绘制了这些模型化合物各型体随pH值变化的分布图。溶液pH值对模型化合物各型体在溶液中分布分数有很大的影响,模型化合物的存在型体极大地影响模型化合物与金属离子形成配合物的稳定性。测定了四价钒离子与这些模型化合物在上述温度下的的表观稳定常数,这些稳定常数数值均较大,从热力学的角度分析,生成的配合物较稳定。由稳定常数计算了各配合物的热力学函数,发现标准摩尔反应吉布斯函数均为负值,从热力学角度表明这些配位反应均能自发进行；各配位反应的标准摩尔反应焓均为负值,表明了这类反应均为放热反应,低温对反应有利,且反应的推动力主要来自于焓变。
通过对单宁酸、还原态橡椀栲胶、氧化单宁、氧化态橡椀栲胶的红外光谱图的分析可知,单宁酸的红外谱图出现的特征峰比橡椀栲胶的要多,但经分析知,它们含有的主要官能团相似。氧化态橡椀栲胶和氧化单宁的红外谱图很相近,氧化之后,部分酚羟基转化为醌基。因此,可用单宁酸作为橡椀栲胶的替代物,定量研究橡椀栲胶与金属钒离子的配位作用。
采用pH电位滴定法,测定了25℃、30℃、35℃、40℃、45℃时单宁酸的加质子常数,温度升高,加质子常数减小,但影响不是很大。绘制了单宁酸赋存型体随pH值变化的分布图。pH值对其不同型体的存在形式影响很大,在栲胶脱硫体系pH值在8.5-9.5之间时,单宁酸在溶液中主要以H2L-形式存在。测定了不同温度下单宁酸与V(Ⅳ)配合物的表观稳定常数,从表观稳定常数的数值来看,表明单宁酸与V(Ⅳ)易形成稳定的配合物。
采用紫外-可见分光光度法研究了在栲胶脱硫的Na2CO3/NaHCO3缓冲体系中单宁酸与四价钒的配位反应,表明在此缓冲体系中,四价钒和单宁形成配合物。测定了所形成配合物的配位比为1：1,配位稳定常数K=5.34×104。
The tannin extract desulfurization technology belongs to the binary wet catalytic oxidation desulfurization method. At present, it is widely applied to remove H2S in the field of fertilizer, coking and oil refining in our country. In the process of removing H2S, vanadium(Ⅴ) ion is reduced to vanadium(Ⅳ) ion by HS", and then the vanadium(Ⅳ) ion is oxidized to vanadium(Ⅴ) ion by air in the presence of oxygen-carrying tannin extract. So the vanadium ion can be circled. In this process, the tannin extract also acts as a ligand agent, which can avoid vanadium(Ⅳ) to form deposition and keep its concentration stable. In this paper, pyrocatechol, pyrogallol and gallic acid have been used as model compounds for tannin extract, tannic acid as a substitute for tannin extract. By using the pH potential method and UV-vis spectrophotometry, the complexation of the tannin extract with vanadium ion has been investigated comprehensively and systematicly.
The reaction between pentavalent vanadium V (Ⅴ) and disulfide HS-and its influencing factors were investigated. The results show that the pH value of de-sulfurization liquid is the main influencing factor for the pH value of desulfuri-zation liquid, temperature, concentration of reactants.
The tannin extract is a tannic acid-containing polyphone mixture which contains phonehydroxyl and carboxyl groups. In order to define which groups form complexation, the coordination reaction of tetravalent vanadium (Ⅳ) ion with such organic compounds as phenol, hydroquinone, resorcinol, pyrocatechol, m-hydroxybenzoic acid, potassium sodium tartrate and gallic acid were investigated by using UV-visible spectrophotometry. The results show that tetravalent vanadium ion only reacts with these organic compounds containing ortho hydroxyl and carboxyl functional groups, and not with those containing a hydroxyl, or meta-hydroxyl and carboxyl functions.
The protonation constants of such model compounds as pyrocatechol, pyrogallol and gallic acid were determined at25℃,30℃,35℃,40℃,45℃by using pH potential method. The protonation constants decrease with the increase of temperatures. The distribution of various species of these model compounds with the pH value change can be mapped by using these protonation constants. The figure shows that the pH value of the solution markedly impacts the distribution fraction of various species. The species greatly affects the stability of the metal ions complexes with the model compounds. The apparent stability constants of tetravalent vanadium ion with these model compounds were determined. All the values are larger. These complexes are stable from the point of view of thermodynamics. The thermodynamic functions of the complexes were calculated by the stability constants. The standard molar Gibbs functions of these reactions are negative, which figure that these coordination reactions are spontaneous. The standard molar reaction enthalpies of these coordination reactions are negative, which figure these reactions are exothermic reactions and low temperature is favorable to the reactions. Moreover the enthalpy changes are the main driving force of the reactions.
Through the analysis of the infrared spectra of tannic acid, valonia tannin extract, oxidant of tannic acid and the one of valonia tannin extract, tannic acid appears more characteristic peaks than valonia tannin extract. But they contain the similar main functional groups. The infrared spectra of the oxidant of valonia tannin extract and the oxidant of tannic acid are very similar. After oxicidization, partial phenolic hydroxyl group turned into the quinone. Therefore, the tannic acid can be used as a substitute of valonia tannin extract. Then we can quantitatively research the complexation between valonia tannin extract and vanadium ions.
The protonation constants of tannic acid at defferent temperatures were determined by using the pH potential method. The protonation constants decrease with the temperature increasing, which is not markedly. The distribution of of various species of tannic acid with the pH value change can be mapped by using these protonation constants. The pH values have a great influence on the existence form of different body. At the pH value8.5～9.5of the tannin extract desulfurization system, the main form of tannic acid in solution is H2L". The apparent stability constants of V (Ⅳ) complex with tannic acid at different temperatures were determined. These values show that the tannic acid and V (Ⅳ) can form stable complex.
Using UV-vis spectrophotometry, the coordination reaction of tannic acid with vanadium ions was studied in Na2CO3/NaHCO3buffer solution. The results show that the tetravalent vanadium ion and tannin can form complex in this buffer system. The ligand ratio of the complex is1:1, the stability constant is K=5.34×104.
通过研究pH值、温度、浓度等因素对五价钒V(V)与HS-之间的反应的影响,发现脱硫液的pH值是影响该反应的主要因素,说明脱硫过程的pH值应严格控制。
栲胶是一类以单宁成分为主的多酚混合物,结构中既含有酚羟基,还有一定量的羧基,采用紫外-可见分光光度法研究了四价钒V(Ⅳ)离子与苯酚、对苯二酚、间苯二酚、邻苯二酚、间羟基苯甲酸、酒石酸钾钠及没食子酸等七种有机化合物的配位反应。结果表明,四价钒只与这些有机化合物中含有邻位羟基和羧基官能团的化合物发生了配位反应,而与含有一个羟基、含有间位羟基和羧基官能团的化合物均未发生配位反应。
采用pH电位法测定了含有邻位酚羟基的邻苯二酚、连苯三酚及没食子酸模型化合物在25℃、30℃、35℃、40℃、45℃下的加质子常数,加质子常数随温度的升高而减小。由测定的一系列加质子常数绘制了这些模型化合物各型体随pH值变化的分布图。溶液pH值对模型化合物各型体在溶液中分布分数有很大的影响,模型化合物的存在型体极大地影响模型化合物与金属离子形成配合物的稳定性。测定了四价钒离子与这些模型化合物在上述温度下的的表观稳定常数,这些稳定常数数值均较大,从热力学的角度分析,生成的配合物较稳定。由稳定常数计算了各配合物的热力学函数,发现标准摩尔反应吉布斯函数均为负值,从热力学角度表明这些配位反应均能自发进行；各配位反应的标准摩尔反应焓均为负值,表明了这类反应均为放热反应,低温对反应有利,且反应的推动力主要来自于焓变。
通过对单宁酸、还原态橡椀栲胶、氧化单宁、氧化态橡椀栲胶的红外光谱图的分析可知,单宁酸的红外谱图出现的特征峰比橡椀栲胶的要多,但经分析知,它们含有的主要官能团相似。氧化态橡椀栲胶和氧化单宁的红外谱图很相近,氧化之后,部分酚羟基转化为醌基。因此,可用单宁酸作为橡椀栲胶的替代物,定量研究橡椀栲胶与金属钒离子的配位作用。
采用pH电位滴定法,测定了25℃、30℃、35℃、40℃、45℃时单宁酸的加质子常数,温度升高,加质子常数减小,但影响不是很大。绘制了单宁酸赋存型体随pH值变化的分布图。pH值对其不同型体的存在形式影响很大,在栲胶脱硫体系pH值在8.5-9.5之间时,单宁酸在溶液中主要以H2L-形式存在。测定了不同温度下单宁酸与V(Ⅳ)配合物的表观稳定常数,从表观稳定常数的数值来看,表明单宁酸与V(Ⅳ)易形成稳定的配合物。
采用紫外-可见分光光度法研究了在栲胶脱硫的Na2CO3/NaHCO3缓冲体系中单宁酸与四价钒的配位反应,表明在此缓冲体系中,四价钒和单宁形成配合物。测定了所形成配合物的配位比为1：1,配位稳定常数K=5.34×104。
The tannin extract desulfurization technology belongs to the binary wet catalytic oxidation desulfurization method. At present, it is widely applied to remove H2S in the field of fertilizer, coking and oil refining in our country. In the process of removing H2S, vanadium(Ⅴ) ion is reduced to vanadium(Ⅳ) ion by HS", and then the vanadium(Ⅳ) ion is oxidized to vanadium(Ⅴ) ion by air in the presence of oxygen-carrying tannin extract. So the vanadium ion can be circled. In this process, the tannin extract also acts as a ligand agent, which can avoid vanadium(Ⅳ) to form deposition and keep its concentration stable. In this paper, pyrocatechol, pyrogallol and gallic acid have been used as model compounds for tannin extract, tannic acid as a substitute for tannin extract. By using the pH potential method and UV-vis spectrophotometry, the complexation of the tannin extract with vanadium ion has been investigated comprehensively and systematicly.
The reaction between pentavalent vanadium V (Ⅴ) and disulfide HS-and its influencing factors were investigated. The results show that the pH value of de-sulfurization liquid is the main influencing factor for the pH value of desulfuri-zation liquid, temperature, concentration of reactants.
The tannin extract is a tannic acid-containing polyphone mixture which contains phonehydroxyl and carboxyl groups. In order to define which groups form complexation, the coordination reaction of tetravalent vanadium (Ⅳ) ion with such organic compounds as phenol, hydroquinone, resorcinol, pyrocatechol, m-hydroxybenzoic acid, potassium sodium tartrate and gallic acid were investigated by using UV-visible spectrophotometry. The results show that tetravalent vanadium ion only reacts with these organic compounds containing ortho hydroxyl and carboxyl functional groups, and not with those containing a hydroxyl, or meta-hydroxyl and carboxyl functions.
The protonation constants of such model compounds as pyrocatechol, pyrogallol and gallic acid were determined at25℃,30℃,35℃,40℃,45℃by using pH potential method. The protonation constants decrease with the increase of temperatures. The distribution of various species of these model compounds with the pH value change can be mapped by using these protonation constants. The figure shows that the pH value of the solution markedly impacts the distribution fraction of various species. The species greatly affects the stability of the metal ions complexes with the model compounds. The apparent stability constants of tetravalent vanadium ion with these model compounds were determined. All the values are larger. These complexes are stable from the point of view of thermodynamics. The thermodynamic functions of the complexes were calculated by the stability constants. The standard molar Gibbs functions of these reactions are negative, which figure that these coordination reactions are spontaneous. The standard molar reaction enthalpies of these coordination reactions are negative, which figure these reactions are exothermic reactions and low temperature is favorable to the reactions. Moreover the enthalpy changes are the main driving force of the reactions.
Through the analysis of the infrared spectra of tannic acid, valonia tannin extract, oxidant of tannic acid and the one of valonia tannin extract, tannic acid appears more characteristic peaks than valonia tannin extract. But they contain the similar main functional groups. The infrared spectra of the oxidant of valonia tannin extract and the oxidant of tannic acid are very similar. After oxicidization, partial phenolic hydroxyl group turned into the quinone. Therefore, the tannic acid can be used as a substitute of valonia tannin extract. Then we can quantitatively research the complexation between valonia tannin extract and vanadium ions.
The protonation constants of tannic acid at defferent temperatures were determined by using the pH potential method. The protonation constants decrease with the temperature increasing, which is not markedly. The distribution of of various species of tannic acid with the pH value change can be mapped by using these protonation constants. The pH values have a great influence on the existence form of different body. At the pH value8.5～9.5of the tannin extract desulfurization system, the main form of tannic acid in solution is H2L". The apparent stability constants of V (Ⅳ) complex with tannic acid at different temperatures were determined. These values show that the tannic acid and V (Ⅳ) can form stable complex.
Using UV-vis spectrophotometry, the coordination reaction of tannic acid with vanadium ions was studied in Na2CO3/NaHCO3buffer solution. The results show that the tetravalent vanadium ion and tannin can form complex in this buffer system. The ligand ratio of the complex is1:1, the stability constant is K=5.34×104.
引文
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