神华煤直接液化动力学及机理研究
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摘要
本论文以提高神华煤直接液化转化率和油产率为目标,以实际应用的液化体系为研究对象,考察了神华煤液化的主要影响因素,建立了适合神华煤液化的动力学模型,综合分析了煤直接液化机理,提出了提高神华煤液化转化率和油收率的关键因素。论文的主要研究内容和结果如下:
在热重分析仪上考察了神华煤非等温热解和催化热解规律,并对其热解动力学进行了研究。研究结果表明:铁基催化剂明显促进了神华煤的热解,使热解总失重率由原煤的约35%提高到约60%;在300℃～600℃范围内原煤热解活化能在135 kJ·mol~(-1)～460kJ·mol~(-1)之间,催化热解活化能在150 kJ·mol~(-1)～310 kJ·mol~(-1)之间,催化剂的加入明显降低了神华煤热解活化能。另外,建立了一种新的计算煤热解赝反应级数的方法。此方法以至少三条相同升温速率但不同初始质量的煤热解失重数据为基础,可以计算出煤热解赝反应级数随温度或转化率的变化规律。计算结果得到,在300℃～700℃范围内神华煤热解和催化热解赝反应级数分别在(0.2～1.6)和(0.6～1.2)之间,因此可将神华煤热解和催化热解近似视为一级反应。
在高压反应釜中考察了搅拌速率、温度、氢初压、催化剂负载量、溶煤比、液化气氛等液化工艺参数对神华煤液化的影响。实验结果表明:在400℃～460℃范围内煤液化转化率和油产率随温度的升高有明显增加趋势,增加速率先快后慢;氢气是煤直接液化的重要条件之一,但过高的氢初压对油收率不利,在考察范围内(5MPa～10MPa),初压为8MPa时油产率最高;催化剂负载量超过2.00%时油产率有下降趋势;高溶煤比对提高转化率和油产率、降低沥青烯产率有明显作用。
对神华煤液化动力学进行研究,分别建立了能较准确地反映神华煤升温阶段和恒温阶段液化反应途径且比较简洁的动力学模型,计算了相应的动力学参数。研究结果表明,在液化动力学模型中将神华煤分为易反应部分、难反应部分和不反应部分是合适的:液化升温阶段和恒温阶段的转化途径不同,升温阶段主要存在煤转变成沥青烯与前沥青烯和煤转变成油和气体两条反应途径,恒温阶段的主要反应途径是煤转变成沥青烯和前沥青烯,后者再进一步转变成油和气体。由动力学计算得到,神华煤液化的最大转化率为92.9%,此计算结果与实验结果较为接近(92.6%,430℃,150min)。
通过在不同供氢能力的溶剂和不同气氛下的液化实验考察了铁基催化剂在煤液化中的主要作用及液化过程中的氢传递途径。研究结果表明:煤液化过程可以分为热液化和催化液化两种途径。铁基催化剂在煤液化过程中促进了氢在整个反应体系(固、液和气三相)中的平衡分布,当以氢气为液化反应气氛时,催化剂的作用是促进气相氢到溶剂的转移和溶剂氢到煤上的转移;活性氢主要由供氢溶剂和H_2经过热作用和催化作用得到,H_2通过溶剂参与液化反应。溶剂的主要作用除溶解分散煤及产物外还有提供和传递活性氢。H_2、溶剂、催化剂三者的作用是相互促进、相辅相成的。
考察了神华煤多段液化和其液化残渣再液化规律,探讨了促进神华煤直接液化的关键因素。实验结果表明:在本论文所采用的液化条件下,高温对神华煤液化有一定的促进作用,但不是提高神华煤液化转化率和油产率的关键因素;活性氢的过量消耗和聚合反应的大量发生是抑制神华煤液化的根本原因。所以促进神华煤液化的关键因素是提供足够的活性氢,可以通过采用强供氢溶剂、提高溶煤比或者采用高活性催化剂等途径来实现。
The aim of this paper is to promote the conversion and oil yield of Shenhua(SH) bituminous coal direct liquefaction.The effects of main factors on SH coal liquefaction were studied;Kinetic models fiting SH coal liquefaction were developed and the mechanism of direct coal liquefaction was investigated;And main approach of promoting SH coal liquefaction was analysed.Main research works and results in this paper are as follows:
Kinetic characteristics of SH coal pyrolysis and catalytic pyrolysis were investigated by thermogravimetric analyzer.The results showed that Fe catalyst increases the weight loss of SH coal pyrolysis from 35%to 60%;Activation energy of SH coal pyrolysis and catalytic pyrolysis at the temperature of 300℃—600℃are 135kJ·mol~(-1)—460kJ·mol~(-1) and 150kJ·mol~(-1)—310kJ·mol~(-1),repectively.Catalyst reduce the activation energy of SH coal pyrolysis clearly.An new calculation method of coal pyrolysis fake reaction order distribution curves with temperature or conversion was developed,and the calculation results showed that fake reaction order for pyrolysis and catalytic pyrolysis of SH coal from 200℃to 700℃is 0.2—1.6 and 0.6—1.2,respectively.And it is appropriate comparatively for the regarding SH coal pyrolysis(200℃—700℃) as a serious of first-order reaction.
The effect of stirring rate,temperature,H_2 pressure,amount of catalyst loading,ratio of solvent to coal on coal liquefaction were investigated.The results showed that the conversion and oil yield increase with the increasing of temperature in 400℃—460℃and ratio of solvent to coal.The highest oil yield can be obtained with the H_2 original pressure of 8 MPa within the research range(5MPa—10MPa).Oil yield decreases if the amounts of catalyst loading are higher than 2%.
Direct liquefaction kinetics of SH coal was studied and kinetic models for heating-up and isothermal stages were developed respectively.In the models,the coal was divided into three parts,easy reactive part,hard reactive part and unreactive part.There were two main reaction approachs of coal liquefaction in heating-up stage,which are coal to preasphaltene & asphaltene and coal to oil & gas.The main reaction approach for isothermal stage is from coal to preasphaltene & asphaltene and then from preasphaltene & asphaltene to oil & gas. Calculation results also showed that the maximal conversion of direct SH coal liquefaction is 7.10%,which is similar to the experimental result(92.61%,430℃,150min).
Role of iron-based catalyst and hydrogen transfer mechanism in direct SH coal liquefaction were investigated by using three solvents with different hydrogen donation capability at H_2 or N_2 atmosphere.The results showed that the major role of the catalyst is promoting the formation of activated hydrogen and accelerating the secondary distribution of hydrogen in the whole reaction system including gas,liquid and solid phases.The main sources of activated hydrogen include thermal and catalytic cracking of solvent and H_2,and the major transfer approach of activated hydrogen is from molecular hydrogen to solvent and then from solvent to coal.The solvent acts as a "bridge" role in the hydrogen transfer process.
Single and multi-stage liquefaction of SH coal and re-liquefaction of its liquefaction residue were investigated to understand the essential approach of promoting SH coal liquefaction.The experimental results showed that there is positive function of two-stage liquefaction on shortening reaction time at high temperature stage,but little effect on conversion and yield of SH coal liquefaction.The main factor of inhibiting the liquefaction is consumption of activated hydrogen and appearing of polymerization.So the essential approach of increasing oil yield and conversion of SH coal liquefaction is providing enough activated hydrogen to stabilize the free radicals and inhibiting polymerization.
在热重分析仪上考察了神华煤非等温热解和催化热解规律,并对其热解动力学进行了研究。研究结果表明:铁基催化剂明显促进了神华煤的热解,使热解总失重率由原煤的约35%提高到约60%;在300℃～600℃范围内原煤热解活化能在135 kJ·mol~(-1)～460kJ·mol~(-1)之间,催化热解活化能在150 kJ·mol~(-1)～310 kJ·mol~(-1)之间,催化剂的加入明显降低了神华煤热解活化能。另外,建立了一种新的计算煤热解赝反应级数的方法。此方法以至少三条相同升温速率但不同初始质量的煤热解失重数据为基础,可以计算出煤热解赝反应级数随温度或转化率的变化规律。计算结果得到,在300℃～700℃范围内神华煤热解和催化热解赝反应级数分别在(0.2～1.6)和(0.6～1.2)之间,因此可将神华煤热解和催化热解近似视为一级反应。
在高压反应釜中考察了搅拌速率、温度、氢初压、催化剂负载量、溶煤比、液化气氛等液化工艺参数对神华煤液化的影响。实验结果表明:在400℃～460℃范围内煤液化转化率和油产率随温度的升高有明显增加趋势,增加速率先快后慢;氢气是煤直接液化的重要条件之一,但过高的氢初压对油收率不利,在考察范围内(5MPa～10MPa),初压为8MPa时油产率最高;催化剂负载量超过2.00%时油产率有下降趋势;高溶煤比对提高转化率和油产率、降低沥青烯产率有明显作用。
对神华煤液化动力学进行研究,分别建立了能较准确地反映神华煤升温阶段和恒温阶段液化反应途径且比较简洁的动力学模型,计算了相应的动力学参数。研究结果表明,在液化动力学模型中将神华煤分为易反应部分、难反应部分和不反应部分是合适的:液化升温阶段和恒温阶段的转化途径不同,升温阶段主要存在煤转变成沥青烯与前沥青烯和煤转变成油和气体两条反应途径,恒温阶段的主要反应途径是煤转变成沥青烯和前沥青烯,后者再进一步转变成油和气体。由动力学计算得到,神华煤液化的最大转化率为92.9%,此计算结果与实验结果较为接近(92.6%,430℃,150min)。
通过在不同供氢能力的溶剂和不同气氛下的液化实验考察了铁基催化剂在煤液化中的主要作用及液化过程中的氢传递途径。研究结果表明:煤液化过程可以分为热液化和催化液化两种途径。铁基催化剂在煤液化过程中促进了氢在整个反应体系(固、液和气三相)中的平衡分布,当以氢气为液化反应气氛时,催化剂的作用是促进气相氢到溶剂的转移和溶剂氢到煤上的转移;活性氢主要由供氢溶剂和H_2经过热作用和催化作用得到,H_2通过溶剂参与液化反应。溶剂的主要作用除溶解分散煤及产物外还有提供和传递活性氢。H_2、溶剂、催化剂三者的作用是相互促进、相辅相成的。
考察了神华煤多段液化和其液化残渣再液化规律,探讨了促进神华煤直接液化的关键因素。实验结果表明:在本论文所采用的液化条件下,高温对神华煤液化有一定的促进作用,但不是提高神华煤液化转化率和油产率的关键因素;活性氢的过量消耗和聚合反应的大量发生是抑制神华煤液化的根本原因。所以促进神华煤液化的关键因素是提供足够的活性氢,可以通过采用强供氢溶剂、提高溶煤比或者采用高活性催化剂等途径来实现。
The aim of this paper is to promote the conversion and oil yield of Shenhua(SH) bituminous coal direct liquefaction.The effects of main factors on SH coal liquefaction were studied;Kinetic models fiting SH coal liquefaction were developed and the mechanism of direct coal liquefaction was investigated;And main approach of promoting SH coal liquefaction was analysed.Main research works and results in this paper are as follows:
Kinetic characteristics of SH coal pyrolysis and catalytic pyrolysis were investigated by thermogravimetric analyzer.The results showed that Fe catalyst increases the weight loss of SH coal pyrolysis from 35%to 60%;Activation energy of SH coal pyrolysis and catalytic pyrolysis at the temperature of 300℃—600℃are 135kJ·mol~(-1)—460kJ·mol~(-1) and 150kJ·mol~(-1)—310kJ·mol~(-1),repectively.Catalyst reduce the activation energy of SH coal pyrolysis clearly.An new calculation method of coal pyrolysis fake reaction order distribution curves with temperature or conversion was developed,and the calculation results showed that fake reaction order for pyrolysis and catalytic pyrolysis of SH coal from 200℃to 700℃is 0.2—1.6 and 0.6—1.2,respectively.And it is appropriate comparatively for the regarding SH coal pyrolysis(200℃—700℃) as a serious of first-order reaction.
The effect of stirring rate,temperature,H_2 pressure,amount of catalyst loading,ratio of solvent to coal on coal liquefaction were investigated.The results showed that the conversion and oil yield increase with the increasing of temperature in 400℃—460℃and ratio of solvent to coal.The highest oil yield can be obtained with the H_2 original pressure of 8 MPa within the research range(5MPa—10MPa).Oil yield decreases if the amounts of catalyst loading are higher than 2%.
Direct liquefaction kinetics of SH coal was studied and kinetic models for heating-up and isothermal stages were developed respectively.In the models,the coal was divided into three parts,easy reactive part,hard reactive part and unreactive part.There were two main reaction approachs of coal liquefaction in heating-up stage,which are coal to preasphaltene & asphaltene and coal to oil & gas.The main reaction approach for isothermal stage is from coal to preasphaltene & asphaltene and then from preasphaltene & asphaltene to oil & gas. Calculation results also showed that the maximal conversion of direct SH coal liquefaction is 7.10%,which is similar to the experimental result(92.61%,430℃,150min).
Role of iron-based catalyst and hydrogen transfer mechanism in direct SH coal liquefaction were investigated by using three solvents with different hydrogen donation capability at H_2 or N_2 atmosphere.The results showed that the major role of the catalyst is promoting the formation of activated hydrogen and accelerating the secondary distribution of hydrogen in the whole reaction system including gas,liquid and solid phases.The main sources of activated hydrogen include thermal and catalytic cracking of solvent and H_2,and the major transfer approach of activated hydrogen is from molecular hydrogen to solvent and then from solvent to coal.The solvent acts as a "bridge" role in the hydrogen transfer process.
Single and multi-stage liquefaction of SH coal and re-liquefaction of its liquefaction residue were investigated to understand the essential approach of promoting SH coal liquefaction.The experimental results showed that there is positive function of two-stage liquefaction on shortening reaction time at high temperature stage,but little effect on conversion and yield of SH coal liquefaction.The main factor of inhibiting the liquefaction is consumption of activated hydrogen and appearing of polymerization.So the essential approach of increasing oil yield and conversion of SH coal liquefaction is providing enough activated hydrogen to stabilize the free radicals and inhibiting polymerization.
引文
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