褐煤水热脱水提质制备高浓度水煤浆的基础研究
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摘要
水煤浆是一种清洁的代油燃料,也是水煤浆气化技术的原料。褐煤等低阶煤储量丰富,价格低廉,且反应活性较高,是一种理想的气化原料。利用褐煤制备水煤浆,可以降低原料成本,拓宽褐煤的应用范围,推动煤炭资源的清洁高效利用。
褐煤含水量较高,热值较低,在应用之前需要进行干燥提质。水热脱水提质是一种“非蒸发”的干燥方式,能够对褐煤进行深度的脱水改性,使得褐煤在干燥之后的重吸水能力大幅度降低,热值大幅度的升高。
本文主要对褐煤进行水热脱水提质,围绕褐煤水煤浆的性质以及褐煤水分的脱除规律,进行了以下工作：
采用多种褐煤制备水煤浆,对褐煤水煤浆的成浆浓度、流变特性和稳定性进行深入研究分析,并与常规的烟煤水煤浆进行对比,得到褐煤水煤浆成浆浓度低的最主要原因是褐煤的煤阶较低,表面亲水性的含氧官能团含量较多,束缚水含量较大。
采用密闭的高压反应釜对褐煤进行水热脱水提质,对水热提质过程中的固、液、气三相产物特性进行分析研究,发现随着水热温度的升高,褐煤的平衡水含量显著降低,热值大幅度的提高,煤阶明显升高。在液体产物中,含有大量的有机物和无机矿物质,且随着水热提质温度的升高,总有机碳的含量大幅度升高。在气体产物中,主要的成分是C02,同时还有一定浓度的CO、CH4、02、H2S、H2、N2等产物,其中CO、CH4在反应温度超过240℃后才有生成。
对水热提质前后褐煤的理化性质进行分析,可以发现影响褐煤水煤浆性质的几大因素均得到了改善：经过水热提质之后,褐煤中羧基、羰基和酚羟基的含量明显降低,从而使褐煤的亲水性减弱,表现为煤-水接触角的增大,以及zeta电位的降低,等电点的升高。另一方面,褐煤的孔隙结构也得到了改善,与原煤相比,水热提质固体产物的比表面积、比孔容积以及平均孔径均有不同程度的降低。两方面综合作用,使得褐煤的固水能力大幅度弱化。
将水热提质之后的煤样制备水煤浆,其定粘浓度大幅度升高,其中经过320℃水热提质,褐煤水煤浆的定粘浓度提高约9-14%,同时流变特性和稳定性也得到了进一步的改善；将水热提质的液体产物与固体产物混合制浆,能够使褐煤水煤浆的定粘浓度再度提高约1%,同时回收液体中可燃性物质的能量。
采用热重-差示扫描量热分析研究了水热提质对褐煤水分的赋存形式的影响,发现根据煤水结合能(Eb)的大小可以将褐煤的平衡水分为四个部分：自由水(Eb=0)、物理束缚水(09000kJ/kg)。经过水热提质之后,褐煤与水分之间的结合能降低,自由水与物理吸附水所占的比例增大,化学吸附水的比例降低。根据薄层干燥理论对褐煤脱水活化能进行分析,发现普通褐煤在等温干燥过程中的干燥活化能范围约为21-27kJ/mol。经过水热提质后的褐煤,其平衡水的干燥活化能显著降低,褐煤的固水能力明显减弱。
采用量子化学密度泛函数理论对褐煤水热提质的过程进行优化计算,发现褐煤较长的侧链具有较强的反应活性,在水热提质过程中首先发生化学反应并断裂,使得褐煤的侧链缩短,缩合程度增加。通过计算羧基、羟基、甲基等基团对水分子吸附能的影响,发现褐煤含氧基团对水分子的吸附能约在10kJ/mol左右,且对褐煤亲水性的影响大小：羧基>羟基>甲基；对褐煤水热脱水提质过程中的脱羧和脱羰反应进行热力学和动力学分析,发现在水热提质条件下,脱羧反应的活化能小于脱羰的,羧基在较低的温度下即可脱除,而脱羰反应在较低温度下的热力学可行性较低。
Coal water slurry (CWS), as an oil substitute, is a clean liquid fuel. Preparing for CWS is necessary process to gasify by texaco technology. Low rank coals, such as brown coal, are very abundant and low price in China. Brown coal with high reaction activity is a good source for gasification. Preparing brown coal for slurry, which can reduce the cost of CWS and increase the field of application, has an important function on high efficient and clean utilization of coal resource.
Drying is the first essential step in brown coal utilization process because of its high moisture content and low heat value. Hydrothermal dewatering (HTD) is a non-evaporative method by which water is removed as a liquid. The coal rank can be upgraded and heat value of brown coal increased effectively after HTD process. And the HTD products reabsorb water no more.
A series of work are performed under the subjects of CWS preparation from brown coal, the effect of HTD process and the moisture distribution in brown coal.
Many types of brown coals are made into CWS. And the slurryability, rheological characteristics and stability of those brown coal water slurries (BCWS) are investigated. Results show that the solid ratio of BCWS is lower than bitumite water slurry, and the most important reason is the high inherent moisture content resulted from the high oxygen functional groups content.
Brown coals were hydrothermally treated for dewatering and upgrading in an autoclave. The chemical composition of solid liquid and gas products during HTD process are studied. It can be concluded that the equilibrium moisture and volatile decrease, while the fixed carbon and heating value increase. And the coal rank is upgraded with the mole ratio of oxygen or hydrogen and carbon element goes down. Many organic matters and inorganic salts dissolve into the liquid product. The total organic carbon and total inorganic carbon concentrations in the wastewater increase as the increase of HTD temperature. CO2content Make up a large proportion of gas product, which consist of CO、CH4、O2、H2S、H2. Especially, CO and CH4appear when the temperature is above240℃
Some physical and chemical properties of brown coal have improved after HTD. It can be concluded as follows:phenolic hydroxyl, carbonyl and carboxyl content decrease, leading a decrease of hydrophilicity of coal surface, which is expressed as the increase of contact angle between coal and water, and the point of zero charge. Moreover, the pore volume, surface and diameter of HTD products are smaller than raw coals. As a result, water holding capacity of brown coals weakened.
The fixed-viscosity concentration of BCWS is significant increased. When HTD temperature is up to320℃, the increment of fixed-viscosity concentration is about9-13%. At the same time, the fluidity and stability of BCWS are also improved. Preparing the liquid products for BCWS can recover the energy of combustible organic matter from the wastewater. Furthermore, the fixed-viscosity concentration can raise1%more using liquid products.
The method of thermogravimetric analysis-differential scanning calorimetry is employed to analyze the moisture distribution in brown coal. According to coal-water binding energy (Eb), the moisture in brown coal can be divided into four parts:free water (Eb=0), physical absorption water (Eb<2000kJ/kg), interim water (20009000kJ/kg). The ratios of free water and physical water increase during HTD. The dewatering activation energy of brown, which is about21～27kJ/mol during isothermal drying process, decreased by HTD.
The density functional theory of quantum chemistry is used to optimize the structure and energy of brown coal. Result show that the long side chain with high active reaction in brown coal has weaken chemical bonds, which will rupture firstly during HTD process. As a result, the side chains are shortened and concentration increase in brown coal. The adsorption energy of H2O on coal surface is about10kJ/mol. And the effects on hydrophilicity of brown coal:carboxyl> hydroxyl> methyl. Thermodynamic and kinetic analyses of deoxidization reaction of brown coal show that the activation energy of decarboxylation is lower thande-carbonyl reaction. It is more difficulty to remove carbonyl.
褐煤含水量较高,热值较低,在应用之前需要进行干燥提质。水热脱水提质是一种“非蒸发”的干燥方式,能够对褐煤进行深度的脱水改性,使得褐煤在干燥之后的重吸水能力大幅度降低,热值大幅度的升高。
本文主要对褐煤进行水热脱水提质,围绕褐煤水煤浆的性质以及褐煤水分的脱除规律,进行了以下工作：
采用多种褐煤制备水煤浆,对褐煤水煤浆的成浆浓度、流变特性和稳定性进行深入研究分析,并与常规的烟煤水煤浆进行对比,得到褐煤水煤浆成浆浓度低的最主要原因是褐煤的煤阶较低,表面亲水性的含氧官能团含量较多,束缚水含量较大。
采用密闭的高压反应釜对褐煤进行水热脱水提质,对水热提质过程中的固、液、气三相产物特性进行分析研究,发现随着水热温度的升高,褐煤的平衡水含量显著降低,热值大幅度的提高,煤阶明显升高。在液体产物中,含有大量的有机物和无机矿物质,且随着水热提质温度的升高,总有机碳的含量大幅度升高。在气体产物中,主要的成分是C02,同时还有一定浓度的CO、CH4、02、H2S、H2、N2等产物,其中CO、CH4在反应温度超过240℃后才有生成。
对水热提质前后褐煤的理化性质进行分析,可以发现影响褐煤水煤浆性质的几大因素均得到了改善：经过水热提质之后,褐煤中羧基、羰基和酚羟基的含量明显降低,从而使褐煤的亲水性减弱,表现为煤-水接触角的增大,以及zeta电位的降低,等电点的升高。另一方面,褐煤的孔隙结构也得到了改善,与原煤相比,水热提质固体产物的比表面积、比孔容积以及平均孔径均有不同程度的降低。两方面综合作用,使得褐煤的固水能力大幅度弱化。
将水热提质之后的煤样制备水煤浆,其定粘浓度大幅度升高,其中经过320℃水热提质,褐煤水煤浆的定粘浓度提高约9-14%,同时流变特性和稳定性也得到了进一步的改善；将水热提质的液体产物与固体产物混合制浆,能够使褐煤水煤浆的定粘浓度再度提高约1%,同时回收液体中可燃性物质的能量。
采用热重-差示扫描量热分析研究了水热提质对褐煤水分的赋存形式的影响,发现根据煤水结合能(Eb)的大小可以将褐煤的平衡水分为四个部分：自由水(Eb=0)、物理束缚水(0
采用量子化学密度泛函数理论对褐煤水热提质的过程进行优化计算,发现褐煤较长的侧链具有较强的反应活性,在水热提质过程中首先发生化学反应并断裂,使得褐煤的侧链缩短,缩合程度增加。通过计算羧基、羟基、甲基等基团对水分子吸附能的影响,发现褐煤含氧基团对水分子的吸附能约在10kJ/mol左右,且对褐煤亲水性的影响大小：羧基>羟基>甲基；对褐煤水热脱水提质过程中的脱羧和脱羰反应进行热力学和动力学分析,发现在水热提质条件下,脱羧反应的活化能小于脱羰的,羧基在较低的温度下即可脱除,而脱羰反应在较低温度下的热力学可行性较低。
Coal water slurry (CWS), as an oil substitute, is a clean liquid fuel. Preparing for CWS is necessary process to gasify by texaco technology. Low rank coals, such as brown coal, are very abundant and low price in China. Brown coal with high reaction activity is a good source for gasification. Preparing brown coal for slurry, which can reduce the cost of CWS and increase the field of application, has an important function on high efficient and clean utilization of coal resource.
Drying is the first essential step in brown coal utilization process because of its high moisture content and low heat value. Hydrothermal dewatering (HTD) is a non-evaporative method by which water is removed as a liquid. The coal rank can be upgraded and heat value of brown coal increased effectively after HTD process. And the HTD products reabsorb water no more.
A series of work are performed under the subjects of CWS preparation from brown coal, the effect of HTD process and the moisture distribution in brown coal.
Many types of brown coals are made into CWS. And the slurryability, rheological characteristics and stability of those brown coal water slurries (BCWS) are investigated. Results show that the solid ratio of BCWS is lower than bitumite water slurry, and the most important reason is the high inherent moisture content resulted from the high oxygen functional groups content.
Brown coals were hydrothermally treated for dewatering and upgrading in an autoclave. The chemical composition of solid liquid and gas products during HTD process are studied. It can be concluded that the equilibrium moisture and volatile decrease, while the fixed carbon and heating value increase. And the coal rank is upgraded with the mole ratio of oxygen or hydrogen and carbon element goes down. Many organic matters and inorganic salts dissolve into the liquid product. The total organic carbon and total inorganic carbon concentrations in the wastewater increase as the increase of HTD temperature. CO2content Make up a large proportion of gas product, which consist of CO、CH4、O2、H2S、H2. Especially, CO and CH4appear when the temperature is above240℃
Some physical and chemical properties of brown coal have improved after HTD. It can be concluded as follows:phenolic hydroxyl, carbonyl and carboxyl content decrease, leading a decrease of hydrophilicity of coal surface, which is expressed as the increase of contact angle between coal and water, and the point of zero charge. Moreover, the pore volume, surface and diameter of HTD products are smaller than raw coals. As a result, water holding capacity of brown coals weakened.
The fixed-viscosity concentration of BCWS is significant increased. When HTD temperature is up to320℃, the increment of fixed-viscosity concentration is about9-13%. At the same time, the fluidity and stability of BCWS are also improved. Preparing the liquid products for BCWS can recover the energy of combustible organic matter from the wastewater. Furthermore, the fixed-viscosity concentration can raise1%more using liquid products.
The method of thermogravimetric analysis-differential scanning calorimetry is employed to analyze the moisture distribution in brown coal. According to coal-water binding energy (Eb), the moisture in brown coal can be divided into four parts:free water (Eb=0), physical absorption water (Eb<2000kJ/kg), interim water (2000
The density functional theory of quantum chemistry is used to optimize the structure and energy of brown coal. Result show that the long side chain with high active reaction in brown coal has weaken chemical bonds, which will rupture firstly during HTD process. As a result, the side chains are shortened and concentration increase in brown coal. The adsorption energy of H2O on coal surface is about10kJ/mol. And the effects on hydrophilicity of brown coal:carboxyl> hydroxyl> methyl. Thermodynamic and kinetic analyses of deoxidization reaction of brown coal show that the activation energy of decarboxylation is lower thande-carbonyl reaction. It is more difficulty to remove carbonyl.
引文
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